data_MR289_sq _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H21 Cl0.50 Cu0.50 P' _chemical_formula_weight 449.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6222(3) _cell_length_b 13.4612(3) _cell_length_c 18.3551(5) _cell_angle_alpha 82.3313(9) _cell_angle_beta 84.5796(9) _cell_angle_gamma 74.1664(9) _cell_volume 2497.75(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9991 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.37 _exptl_crystal_description 'cube' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_F_000 932 _exptl_transmission_factor_min 0.8456 _exptl_transmission_factor_max 0.9143 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 0.590 _shelx_estimated_absorpt_T_min 0.901 _shelx_estimated_absorpt_T_max 0.965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'D8 Venture, Bruker Photon CMOS Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45604 _diffrn_reflns_av_unetI/netI 0.0473 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.243 _diffrn_reflns_theta_max 26.419 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 10236 _reflns_number_gt 8007 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'Microsoft Word' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+3.7413P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 10236 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6836(2) 0.58818(19) 0.76307(14) 0.0121(5) Uani 1 1 d . . . . . C2 C 0.7464(2) 0.52277(19) 0.81693(13) 0.0124(5) Uani 1 1 d . . . . . H2 H 0.8357 0.4864 0.8084 0.015 Uiso 1 1 calc R U . . . C3 C 0.6760(2) 0.50544(19) 0.89272(13) 0.0123(5) Uani 1 1 d . . . . . C4 C 0.5529(2) 0.4741(2) 0.87869(13) 0.0123(5) Uani 1 1 d . . . . . H4 H 0.5370 0.4118 0.9037 0.015 Uiso 1 1 calc R U . . . C5 C 0.4677(2) 0.53422(19) 0.83120(13) 0.0109(5) Uani 1 1 d . . . . . C6 C 0.3508(2) 0.5080(2) 0.80968(13) 0.0132(5) Uani 1 1 d . . . . . C7 C 0.3552(2) 0.4049(2) 0.80437(14) 0.0162(5) Uani 1 1 d . . . . . H7 H 0.4337 0.3520 0.8138 0.019 Uiso 1 1 calc R U . . . C8 C 0.2463(3) 0.3785(2) 0.78554(16) 0.0223(6) Uani 1 1 d . . . . . H8 H 0.2499 0.3078 0.7830 0.027 Uiso 1 1 calc R U . . . C9 C 0.1320(3) 0.4553(2) 0.77031(16) 0.0242(6) Uani 1 1 d . . . . . H9 H 0.0575 0.4371 0.7571 0.029 Uiso 1 1 calc R U . . . C10 C 0.1261(3) 0.5584(2) 0.77431(15) 0.0207(6) Uani 1 1 d . . . . . H10 H 0.0478 0.6110 0.7638 0.025 Uiso 1 1 calc R U . . . C11 C 0.2349(2) 0.5845(2) 0.79372(14) 0.0162(5) Uani 1 1 d . . . . . H11 H 0.2307 0.6553 0.7962 0.019 Uiso 1 1 calc R U . . . C12 C 0.7397(2) 0.60741(19) 0.68756(13) 0.0115(5) Uani 1 1 d . . . . . C13 C 0.7017(2) 0.7043(2) 0.64613(14) 0.0139(5) Uani 1 1 d . . . . . H13 H 0.6396 0.7599 0.6671 0.017 Uiso 1 1 calc R U . . . C14 C 0.7538(2) 0.7202(2) 0.57458(15) 0.0171(6) Uani 1 1 d . . . . . H14 H 0.7259 0.7862 0.5467 0.020 Uiso 1 1 calc R U . . . C15 C 0.8463(2) 0.6405(2) 0.54366(15) 0.0174(6) Uani 1 1 d . . . . . H15 H 0.8818 0.6515 0.4947 0.021 Uiso 1 1 calc R U . . . C16 C 0.8865(2) 0.5443(2) 0.58514(15) 0.0171(6) Uani 1 1 d . . . . . H16 H 0.9511 0.4897 0.5646 0.021 Uiso 1 1 calc R U . . . C17 C 0.8332(2) 0.5273(2) 0.65582(14) 0.0139(5) Uani 1 1 d . . . . . H17 H 0.8602 0.4608 0.6831 0.017 Uiso 1 1 calc R U . . . C18 C 0.7669(2) 0.4276(2) 0.94588(14) 0.0140(5) Uani 1 1 d . . . . . C19 C 0.7231(2) 0.3574(2) 0.99799(14) 0.0154(5) Uani 1 1 d . . . . . H19 H 0.6342 0.3552 0.9998 0.019 Uiso 1 1 calc R U . . . C20 C 0.8073(3) 0.2907(2) 1.04717(15) 0.0212(6) Uani 1 1 d . . . . . H20 H 0.7761 0.2424 1.0817 0.025 Uiso 1 1 calc R U . . . C21 C 0.9366(3) 0.2940(2) 1.04638(16) 0.0243(6) Uani 1 1 d . . . . . H21 H 0.9940 0.2487 1.0804 0.029 Uiso 1 1 calc R U . . . C22 C 0.9811(3) 0.3639(2) 0.99560(17) 0.0282(7) Uani 1 1 d . . . . . H22 H 1.0696 0.3669 0.9948 0.034 Uiso 1 1 calc R U . . . C23 C 0.8973(3) 0.4299(2) 0.94572(16) 0.0224(6) Uani 1 1 d . . . . . H23 H 0.9293 0.4774 0.9109 0.027 Uiso 1 1 calc R U . . . C24 C 0.5479(2) 0.6930(2) 0.87596(13) 0.0123(5) Uani 1 1 d . . . . . C25 C 0.6277(2) 0.6135(2) 0.92183(14) 0.0126(5) Uani 1 1 d . . . . . C26 C 0.6567(2) 0.6352(2) 0.98884(14) 0.0161(5) Uani 1 1 d . . . . . H26 H 0.7094 0.5821 1.0209 0.019 Uiso 1 1 calc R U . . . C27 C 0.6082(3) 0.7354(2) 1.00925(15) 0.0197(6) Uani 1 1 d . . . . . H27 H 0.6283 0.7501 1.0554 0.024 Uiso 1 1 calc R U . . . C28 C 0.5311(3) 0.8139(2) 0.96338(15) 0.0210(6) Uani 1 1 d . . . . . H28 H 0.4993 0.8819 0.9779 0.025 Uiso 1 1 calc R U . . . C29 C 0.5003(2) 0.7930(2) 0.89592(14) 0.0160(5) Uani 1 1 d . . . . . H29 H 0.4475 0.8463 0.8641 0.019 Uiso 1 1 calc R U . . . C30 C 0.0960(2) 0.82365(18) 0.63295(14) 0.0120(5) Uani 1 1 d . . . . . C31 C 0.0292(2) 0.83207(18) 0.57366(13) 0.0108(5) Uani 1 1 d . . . . . H31 H -0.0628 0.8625 0.5760 0.013 Uiso 1 1 calc R U . . . C32 C 0.0978(2) 0.79369(18) 0.50221(13) 0.0103(5) Uani 1 1 d . . . . . C33 C 0.1756(2) 0.67997(19) 0.52201(14) 0.0113(5) Uani 1 1 d . . . . . H33 H 0.1625 0.6273 0.4962 0.014 Uiso 1 1 calc R U . . . C34 C 0.2603(2) 0.65408(19) 0.57437(13) 0.0114(5) Uani 1 1 d . . . . . C35 C 0.3458(2) 0.54734(19) 0.59183(13) 0.0118(5) Uani 1 1 d . . . . . C36 C 0.2972(2) 0.4614(2) 0.59051(15) 0.0167(6) Uani 1 1 d . . . . . H36 H 0.2069 0.4715 0.5836 0.020 Uiso 1 1 calc R U . . . C37 C 0.3786(3) 0.3616(2) 0.59911(15) 0.0207(6) Uani 1 1 d . . . . . H37 H 0.3440 0.3037 0.5980 0.025 Uiso 1 1 calc R U . . . C38 C 0.5110(3) 0.3458(2) 0.60944(15) 0.0193(6) Uani 1 1 d . . . . . H38 H 0.5678 0.2775 0.6141 0.023 Uiso 1 1 calc R U . . . C39 C 0.5587(3) 0.4306(2) 0.61286(15) 0.0197(6) Uani 1 1 d . . . . . H39 H 0.6486 0.4201 0.6212 0.024 Uiso 1 1 calc R U . . . C40 C 0.4778(2) 0.5307(2) 0.60429(14) 0.0154(5) Uani 1 1 d . . . . . H40 H 0.5122 0.5882 0.6069 0.018 Uiso 1 1 calc R U . . . C41 C 0.0321(2) 0.85539(19) 0.70414(14) 0.0122(5) Uani 1 1 d . . . . . C42 C 0.0865(3) 0.9064(2) 0.74900(14) 0.0179(6) Uani 1 1 d . . . . . H42 H 0.1714 0.9162 0.7362 0.021 Uiso 1 1 calc R U . . . C43 C 0.0176(3) 0.9429(2) 0.81228(16) 0.0273(7) Uani 1 1 d . . . . . H43 H 0.0554 0.9775 0.8426 0.033 Uiso 1 1 calc R U . . . C44 C -0.1058(3) 0.9293(2) 0.83134(16) 0.0297(7) Uani 1 1 d . . . . . H44 H -0.1536 0.9562 0.8740 0.036 Uiso 1 1 calc R U . . . C45 C -0.1603(3) 0.8765(2) 0.78865(16) 0.0262(7) Uani 1 1 d . . . . . H45 H -0.2446 0.8661 0.8024 0.031 Uiso 1 1 calc R U . . . C46 C -0.0918(2) 0.8391(2) 0.72600(15) 0.0183(6) Uani 1 1 d . . . . . H46 H -0.1289 0.8019 0.6972 0.022 Uiso 1 1 calc R U . . . C47 C 0.0062(2) 0.80833(18) 0.44059(14) 0.0113(5) Uani 1 1 d . . . . . C48 C 0.0420(3) 0.7488(2) 0.38182(14) 0.0159(5) Uani 1 1 d . . . . . H48 H 0.1230 0.6967 0.3814 0.019 Uiso 1 1 calc R U . . . C49 C -0.0389(3) 0.7644(2) 0.32373(16) 0.0219(6) Uani 1 1 d . . . . . H49 H -0.0127 0.7231 0.2840 0.026 Uiso 1 1 calc R U . . . C50 C -0.1575(3) 0.8396(2) 0.32343(15) 0.0205(6) Uani 1 1 d . . . . . H50 H -0.2139 0.8491 0.2845 0.025 Uiso 1 1 calc R U . . . C51 C -0.1926(3) 0.9009(2) 0.38056(15) 0.0181(6) Uani 1 1 d . . . . . H51 H -0.2729 0.9538 0.3803 0.022 Uiso 1 1 calc R U . . . C52 C -0.1116(2) 0.88562(19) 0.43828(14) 0.0140(5) Uani 1 1 d . . . . . H52 H -0.1369 0.9287 0.4770 0.017 Uiso 1 1 calc R U . . . C53 C 0.2973(2) 0.84384(18) 0.53022(14) 0.0115(5) Uani 1 1 d . . . . . C54 C 0.2040(2) 0.85394(18) 0.47884(14) 0.0108(5) Uani 1 1 d . . . . . C55 C 0.2123(2) 0.91243(19) 0.41146(14) 0.0128(5) Uani 1 1 d . . . . . H55 H 0.1465 0.9230 0.3775 0.015 Uiso 1 1 calc R U . . . C56 C 0.3184(2) 0.95588(19) 0.39379(14) 0.0151(5) Uani 1 1 d . . . . . H56 H 0.3251 0.9954 0.3474 0.018 Uiso 1 1 calc R U . . . C57 C 0.4135(2) 0.9416(2) 0.44354(15) 0.0158(5) Uani 1 1 d . . . . . H57 H 0.4867 0.9694 0.4305 0.019 Uiso 1 1 calc R U . . . C58 C 0.4026(2) 0.88662(19) 0.51251(14) 0.0141(5) Uani 1 1 d . . . . . H58 H 0.4666 0.8785 0.5472 0.017 Uiso 1 1 calc R U . . . P1 P 0.51217(6) 0.65326(5) 0.79041(3) 0.01021(13) Uani 1 1 d . . . . . P2 P 0.27403(6) 0.76688(5) 0.61764(4) 0.01034(13) Uani 1 1 d . . . . . Cl1 Cl 0.44496(6) 0.92398(5) 0.71411(3) 0.01598(13) Uani 1 1 d . . . . . Cu1 Cu 0.40112(3) 0.77176(2) 0.70609(2) 0.01186(8) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0097(12) 0.0170(13) 0.0124(13) -0.0055(10) -0.0021(10) -0.0059(10) C2 0.0080(11) 0.0172(13) 0.0142(13) -0.0037(10) -0.0016(10) -0.0055(10) C3 0.0101(12) 0.0171(13) 0.0113(12) 0.0016(10) -0.0040(10) -0.0067(10) C4 0.0114(12) 0.0144(13) 0.0115(12) 0.0003(10) 0.0003(10) -0.0054(10) C5 0.0094(11) 0.0143(12) 0.0092(12) -0.0008(10) 0.0005(9) -0.0042(10) C6 0.0129(12) 0.0205(14) 0.0074(12) -0.0001(10) -0.0005(10) -0.0073(11) C7 0.0131(12) 0.0208(14) 0.0158(14) -0.0030(11) -0.0031(10) -0.0051(11) C8 0.0217(14) 0.0214(15) 0.0277(16) -0.0059(12) -0.0028(12) -0.0102(12) C9 0.0144(13) 0.0361(17) 0.0278(16) -0.0088(13) -0.0029(12) -0.0131(13) C10 0.0106(12) 0.0282(16) 0.0225(15) -0.0031(12) -0.0041(11) -0.0025(11) C11 0.0114(12) 0.0194(14) 0.0176(14) -0.0009(11) -0.0011(10) -0.0044(11) C12 0.0077(11) 0.0180(13) 0.0115(12) -0.0025(10) -0.0013(9) -0.0074(10) C13 0.0098(12) 0.0176(13) 0.0156(13) -0.0025(11) 0.0009(10) -0.0059(10) C14 0.0155(13) 0.0203(14) 0.0170(14) 0.0011(11) -0.0014(11) -0.0089(11) C15 0.0144(13) 0.0279(15) 0.0140(13) -0.0051(11) 0.0035(10) -0.0126(12) C16 0.0117(12) 0.0223(14) 0.0203(14) -0.0082(11) 0.0032(11) -0.0081(11) C17 0.0102(12) 0.0165(13) 0.0170(13) -0.0031(11) -0.0040(10) -0.0054(10) C18 0.0118(12) 0.0159(13) 0.0138(13) -0.0011(10) -0.0053(10) -0.0015(10) C19 0.0127(12) 0.0201(14) 0.0141(13) -0.0019(11) -0.0039(10) -0.0043(11) C20 0.0226(14) 0.0227(15) 0.0170(14) 0.0037(12) -0.0044(11) -0.0054(12) C21 0.0200(14) 0.0285(16) 0.0218(15) 0.0056(13) -0.0129(12) -0.0018(12) C22 0.0112(13) 0.0432(19) 0.0287(17) 0.0074(14) -0.0103(12) -0.0070(13) C23 0.0159(13) 0.0282(16) 0.0234(15) 0.0074(12) -0.0076(12) -0.0089(12) C24 0.0086(11) 0.0204(13) 0.0100(12) -0.0007(10) -0.0006(9) -0.0080(10) C25 0.0096(11) 0.0182(13) 0.0123(13) 0.0002(10) 0.0006(10) -0.0087(10) C26 0.0135(12) 0.0238(14) 0.0127(13) 0.0020(11) -0.0031(10) -0.0087(11) C27 0.0210(14) 0.0292(16) 0.0143(14) -0.0062(12) -0.0036(11) -0.0132(12) C28 0.0262(15) 0.0193(14) 0.0196(15) -0.0066(12) -0.0016(12) -0.0074(12) C29 0.0164(13) 0.0184(14) 0.0139(13) -0.0013(11) -0.0008(10) -0.0063(11) C30 0.0099(12) 0.0092(12) 0.0169(13) 0.0003(10) -0.0020(10) -0.0028(10) C31 0.0084(11) 0.0099(12) 0.0142(13) 0.0007(10) -0.0027(10) -0.0026(9) C32 0.0084(11) 0.0095(12) 0.0137(13) -0.0009(10) -0.0033(10) -0.0030(9) C33 0.0101(12) 0.0097(12) 0.0148(13) -0.0028(10) 0.0002(10) -0.0034(10) C34 0.0111(12) 0.0106(12) 0.0127(13) -0.0019(10) -0.0003(10) -0.0031(10) C35 0.0137(12) 0.0117(12) 0.0081(12) 0.0008(10) -0.0020(10) -0.0007(10) C36 0.0127(12) 0.0182(14) 0.0204(14) 0.0012(11) -0.0062(11) -0.0061(11) C37 0.0225(14) 0.0141(13) 0.0266(16) -0.0020(12) -0.0066(12) -0.0051(11) C38 0.0210(14) 0.0143(13) 0.0191(14) -0.0034(11) -0.0053(11) 0.0032(11) C39 0.0112(12) 0.0222(15) 0.0236(15) -0.0044(12) -0.0043(11) 0.0011(11) C40 0.0128(12) 0.0138(13) 0.0201(14) -0.0034(11) -0.0034(10) -0.0030(10) C41 0.0125(12) 0.0094(12) 0.0121(13) 0.0011(10) -0.0026(10) 0.0012(10) C42 0.0205(14) 0.0164(13) 0.0161(14) -0.0001(11) -0.0048(11) -0.0033(11) C43 0.0343(17) 0.0268(16) 0.0202(15) -0.0077(13) -0.0050(13) -0.0035(13) C44 0.0317(17) 0.0338(18) 0.0154(15) -0.0058(13) 0.0026(13) 0.0053(14) C45 0.0176(14) 0.0330(17) 0.0218(16) 0.0032(13) 0.0021(12) -0.0006(13) C46 0.0143(13) 0.0213(14) 0.0173(14) 0.0013(11) -0.0045(11) -0.0019(11) C47 0.0110(12) 0.0099(12) 0.0143(13) 0.0021(10) -0.0041(10) -0.0053(10) C48 0.0159(13) 0.0131(13) 0.0181(14) -0.0012(11) -0.0060(11) -0.0016(10) C49 0.0296(16) 0.0177(14) 0.0200(15) -0.0058(12) -0.0091(12) -0.0047(12) C50 0.0222(14) 0.0204(14) 0.0214(15) 0.0026(12) -0.0141(12) -0.0078(12) C51 0.0145(13) 0.0180(14) 0.0199(14) 0.0033(11) -0.0056(11) -0.0021(11) C52 0.0149(12) 0.0138(13) 0.0133(13) 0.0014(10) -0.0040(10) -0.0038(10) C53 0.0125(12) 0.0075(12) 0.0133(13) -0.0010(10) -0.0017(10) -0.0006(10) C54 0.0085(11) 0.0089(12) 0.0152(13) -0.0035(10) -0.0022(10) -0.0014(9) C55 0.0120(12) 0.0121(12) 0.0147(13) -0.0030(10) -0.0053(10) -0.0015(10) C56 0.0165(13) 0.0110(12) 0.0162(13) 0.0010(10) 0.0001(10) -0.0025(10) C57 0.0137(12) 0.0147(13) 0.0211(14) -0.0033(11) 0.0001(11) -0.0071(10) C58 0.0109(12) 0.0139(13) 0.0193(14) -0.0022(11) -0.0041(10) -0.0052(10) P1 0.0079(3) 0.0138(3) 0.0096(3) -0.0003(3) -0.0023(2) -0.0038(2) P2 0.0091(3) 0.0104(3) 0.0121(3) -0.0009(2) -0.0038(2) -0.0027(2) Cl1 0.0177(3) 0.0133(3) 0.0179(3) 0.0010(2) -0.0064(2) -0.0054(2) Cu1 0.01020(15) 0.01394(16) 0.01221(16) -0.00055(12) -0.00448(12) -0.00362(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.330(3) . ? C1 C12 1.475(3) . ? C1 P1 1.846(2) . ? C2 C3 1.536(3) . ? C2 H2 0.9500 . ? C3 C18 1.528(3) . ? C3 C4 1.532(3) . ? C3 C25 1.553(4) . ? C4 C5 1.340(3) . ? C4 H4 0.9500 . ? C5 C6 1.481(3) . ? C5 P1 1.838(2) . ? C6 C7 1.392(4) . ? C6 C11 1.399(4) . ? C7 C8 1.383(4) . ? C7 H7 0.9500 . ? C8 C9 1.387(4) . ? C8 H8 0.9500 . ? C9 C10 1.383(4) . ? C9 H9 0.9500 . ? C10 C11 1.385(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.396(4) . ? C12 C17 1.401(4) . ? C13 C14 1.389(4) . ? C13 H13 0.9500 . ? C14 C15 1.385(4) . ? C14 H14 0.9500 . ? C15 C16 1.392(4) . ? C15 H15 0.9500 . ? C16 C17 1.381(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.393(4) . ? C18 C23 1.393(3) . ? C19 C20 1.385(4) . ? C19 H19 0.9500 . ? C20 C21 1.385(4) . ? C20 H20 0.9500 . ? C21 C22 1.380(4) . ? C21 H21 0.9500 . ? C22 C23 1.387(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.388(4) . ? C24 C25 1.404(3) . ? C24 P1 1.829(3) . ? C25 C26 1.382(4) . ? C26 C27 1.394(4) . ? C26 H26 0.9500 . ? C27 C28 1.384(4) . ? C27 H27 0.9500 . ? C28 C29 1.393(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.330(3) . ? C30 C41 1.474(3) . ? C30 P2 1.846(2) . ? C31 C32 1.521(3) . ? C31 H31 0.9500 . ? C32 C47 1.520(3) . ? C32 C33 1.541(3) . ? C32 C54 1.558(3) . ? C33 C34 1.326(3) . ? C33 H33 0.9500 . ? C34 C35 1.487(3) . ? C34 P2 1.850(2) . ? C35 C36 1.393(4) . ? C35 C40 1.394(3) . ? C36 C37 1.383(4) . ? C36 H36 0.9500 . ? C37 C38 1.392(4) . ? C37 H37 0.9500 . ? C38 C39 1.380(4) . ? C38 H38 0.9500 . ? C39 C40 1.384(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.393(4) . ? C41 C46 1.406(4) . ? C42 C43 1.387(4) . ? C42 H42 0.9500 . ? C43 C44 1.379(4) . ? C43 H43 0.9500 . ? C44 C45 1.382(4) . ? C44 H44 0.9500 . ? C45 C46 1.379(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.392(3) . ? C47 C48 1.392(4) . ? C48 C49 1.391(4) . ? C48 H48 0.9500 . ? C49 C50 1.384(4) . ? C49 H49 0.9500 . ? C50 C51 1.381(4) . ? C50 H50 0.9500 . ? C51 C52 1.387(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C58 1.386(3) . ? C53 C54 1.400(3) . ? C53 P2 1.825(3) . ? C54 C55 1.384(3) . ? C55 C56 1.399(3) . ? C55 H55 0.9500 . ? C56 C57 1.383(4) . ? C56 H56 0.9500 . ? C57 C58 1.390(4) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? P1 Cu1 2.2339(7) . ? P2 Cu1 2.2256(7) . ? Cl1 Cu1 2.2475(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C12 125.2(2) . . ? C2 C1 P1 113.40(19) . . ? C12 C1 P1 121.39(18) . . ? C1 C2 C3 120.7(2) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C18 C3 C4 114.5(2) . . ? C18 C3 C2 111.6(2) . . ? C4 C3 C2 106.36(19) . . ? C18 C3 C25 111.0(2) . . ? C4 C3 C25 106.48(19) . . ? C2 C3 C25 106.34(19) . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 124.7(2) . . ? C4 C5 P1 113.70(18) . . ? C6 C5 P1 121.55(18) . . ? C7 C6 C11 118.4(2) . . ? C7 C6 C5 119.8(2) . . ? C11 C6 C5 121.8(2) . . ? C8 C7 C6 120.7(2) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.1(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.6(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C6 121.0(2) . . ? C10 C11 H11 119.5 . . ? C6 C11 H11 119.5 . . ? C13 C12 C17 118.5(2) . . ? C13 C12 C1 121.5(2) . . ? C17 C12 C1 120.0(2) . . ? C14 C13 C12 120.6(2) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.2(2) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 120.6(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C12 120.5(2) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C19 C18 C23 117.9(2) . . ? C19 C18 C3 122.6(2) . . ? C23 C18 C3 119.4(2) . . ? C20 C19 C18 120.9(2) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 119.3(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 121.1(3) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? C29 C24 C25 121.3(2) . . ? C29 C24 P1 123.9(2) . . ? C25 C24 P1 114.79(19) . . ? C26 C25 C24 119.0(2) . . ? C26 C25 C3 124.7(2) . . ? C24 C25 C3 116.3(2) . . ? C25 C26 C27 119.8(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 121.0(2) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 119.9(3) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C24 C29 C28 119.0(2) . . ? C24 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C31 C30 C41 122.6(2) . . ? C31 C30 P2 113.65(19) . . ? C41 C30 P2 123.79(18) . . ? C30 C31 C32 121.0(2) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C47 C32 C31 113.85(19) . . ? C47 C32 C33 113.8(2) . . ? C31 C32 C33 106.38(19) . . ? C47 C32 C54 110.31(19) . . ? C31 C32 C54 106.84(19) . . ? C33 C32 C54 105.02(18) . . ? C34 C33 C32 121.4(2) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C33 C34 C35 123.8(2) . . ? C33 C34 P2 113.11(18) . . ? C35 C34 P2 122.80(18) . . ? C36 C35 C40 118.6(2) . . ? C36 C35 C34 120.1(2) . . ? C40 C35 C34 121.1(2) . . ? C37 C36 C35 121.0(2) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C38 120.0(2) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 119.2(2) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 121.1(2) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C35 120.1(2) . . ? C39 C40 H40 119.9 . . ? C35 C40 H40 119.9 . . ? C42 C41 C46 118.4(2) . . ? C42 C41 C30 122.4(2) . . ? C46 C41 C30 119.1(2) . . ? C43 C42 C41 120.4(3) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 120.3(3) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.3(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 119.8(3) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C41 120.9(3) . . ? C45 C46 H46 119.6 . . ? C41 C46 H46 119.6 . . ? C52 C47 C48 117.7(2) . . ? C52 C47 C32 121.5(2) . . ? C48 C47 C32 120.6(2) . . ? C49 C48 C47 121.0(2) . . ? C49 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C50 C49 C48 120.4(3) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C51 C50 C49 119.1(2) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C50 C51 C52 120.5(2) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 C47 121.3(2) . . ? C51 C52 H52 119.4 . . ? C47 C52 H52 119.4 . . ? C58 C53 C54 120.5(2) . . ? C58 C53 P2 123.72(19) . . ? C54 C53 P2 115.68(18) . . ? C55 C54 C53 119.8(2) . . ? C55 C54 C32 124.3(2) . . ? C53 C54 C32 115.8(2) . . ? C54 C55 C56 119.5(2) . . ? C54 C55 H55 120.3 . . ? C56 C55 H55 120.3 . . ? C57 C56 C55 120.4(2) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C56 C57 C58 120.3(2) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C53 C58 C57 119.4(2) . . ? C53 C58 H58 120.3 . . ? C57 C58 H58 120.3 . . ? C24 P1 C5 97.20(11) . . ? C24 P1 C1 96.08(11) . . ? C5 P1 C1 95.81(11) . . ? C24 P1 Cu1 119.95(9) . . ? C5 P1 Cu1 125.29(8) . . ? C1 P1 Cu1 116.34(8) . . ? C53 P2 C30 97.52(11) . . ? C53 P2 C34 94.41(11) . . ? C30 P2 C34 95.97(11) . . ? C53 P2 Cu1 115.90(8) . . ? C30 P2 Cu1 117.31(8) . . ? C34 P2 Cu1 129.29(8) . . ? P2 Cu1 P1 134.43(3) . . ? P2 Cu1 Cl1 117.38(3) . . ? P1 Cu1 Cl1 108.08(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 C1 C2 C3 -177.3(2) . . . . ? P1 C1 C2 C3 1.1(3) . . . . ? C1 C2 C3 C18 -179.8(2) . . . . ? C1 C2 C3 C4 54.6(3) . . . . ? C1 C2 C3 C25 -58.6(3) . . . . ? C18 C3 C4 C5 -177.8(2) . . . . ? C2 C3 C4 C5 -54.0(3) . . . . ? C25 C3 C4 C5 59.1(3) . . . . ? C3 C4 C5 C6 175.6(2) . . . . ? C3 C4 C5 P1 -1.9(3) . . . . ? C4 C5 C6 C7 -34.2(4) . . . . ? P1 C5 C6 C7 143.1(2) . . . . ? C4 C5 C6 C11 146.3(3) . . . . ? P1 C5 C6 C11 -36.4(3) . . . . ? C11 C6 C7 C8 -1.6(4) . . . . ? C5 C6 C7 C8 178.9(2) . . . . ? C6 C7 C8 C9 1.2(4) . . . . ? C7 C8 C9 C10 -0.4(4) . . . . ? C8 C9 C10 C11 -0.1(4) . . . . ? C9 C10 C11 C6 -0.3(4) . . . . ? C7 C6 C11 C10 1.1(4) . . . . ? C5 C6 C11 C10 -179.4(2) . . . . ? C2 C1 C12 C13 -148.2(3) . . . . ? P1 C1 C12 C13 33.5(3) . . . . ? C2 C1 C12 C17 31.9(4) . . . . ? P1 C1 C12 C17 -146.4(2) . . . . ? C17 C12 C13 C14 1.1(4) . . . . ? C1 C12 C13 C14 -178.7(2) . . . . ? C12 C13 C14 C15 -1.2(4) . . . . ? C13 C14 C15 C16 -0.1(4) . . . . ? C14 C15 C16 C17 1.3(4) . . . . ? C15 C16 C17 C12 -1.3(4) . . . . ? C13 C12 C17 C16 0.1(4) . . . . ? C1 C12 C17 C16 179.9(2) . . . . ? C4 C3 C18 C19 -23.5(3) . . . . ? C2 C3 C18 C19 -144.4(2) . . . . ? C25 C3 C18 C19 97.2(3) . . . . ? C4 C3 C18 C23 160.3(2) . . . . ? C2 C3 C18 C23 39.3(3) . . . . ? C25 C3 C18 C23 -79.1(3) . . . . ? C23 C18 C19 C20 -1.1(4) . . . . ? C3 C18 C19 C20 -177.5(2) . . . . ? C18 C19 C20 C21 1.2(4) . . . . ? C19 C20 C21 C22 -0.5(4) . . . . ? C20 C21 C22 C23 -0.2(5) . . . . ? C21 C22 C23 C18 0.3(5) . . . . ? C19 C18 C23 C22 0.4(4) . . . . ? C3 C18 C23 C22 176.8(3) . . . . ? C29 C24 C25 C26 1.4(4) . . . . ? P1 C24 C25 C26 -177.93(18) . . . . ? C29 C24 C25 C3 -179.3(2) . . . . ? P1 C24 C25 C3 1.4(3) . . . . ? C18 C3 C25 C26 -3.5(3) . . . . ? C4 C3 C25 C26 121.8(3) . . . . ? C2 C3 C25 C26 -125.1(2) . . . . ? C18 C3 C25 C24 177.3(2) . . . . ? C4 C3 C25 C24 -57.5(3) . . . . ? C2 C3 C25 C24 55.6(3) . . . . ? C24 C25 C26 C27 -0.9(4) . . . . ? C3 C25 C26 C27 179.8(2) . . . . ? C25 C26 C27 C28 0.0(4) . . . . ? C26 C27 C28 C29 0.5(4) . . . . ? C25 C24 C29 C28 -1.0(4) . . . . ? P1 C24 C29 C28 178.4(2) . . . . ? C27 C28 C29 C24 0.0(4) . . . . ? C41 C30 C31 C32 -177.0(2) . . . . ? P2 C30 C31 C32 2.0(3) . . . . ? C30 C31 C32 C47 179.3(2) . . . . ? C30 C31 C32 C33 53.1(3) . . . . ? C30 C31 C32 C54 -58.7(3) . . . . ? C47 C32 C33 C34 179.6(2) . . . . ? C31 C32 C33 C34 -54.2(3) . . . . ? C54 C32 C33 C34 58.9(3) . . . . ? C32 C33 C34 C35 -174.9(2) . . . . ? C32 C33 C34 P2 -0.7(3) . . . . ? C33 C34 C35 C36 -39.1(4) . . . . ? P2 C34 C35 C36 147.3(2) . . . . ? C33 C34 C35 C40 136.1(3) . . . . ? P2 C34 C35 C40 -37.5(3) . . . . ? C40 C35 C36 C37 -2.0(4) . . . . ? C34 C35 C36 C37 173.3(2) . . . . ? C35 C36 C37 C38 0.2(4) . . . . ? C36 C37 C38 C39 1.7(4) . . . . ? C37 C38 C39 C40 -1.7(4) . . . . ? C38 C39 C40 C35 -0.1(4) . . . . ? C36 C35 C40 C39 1.9(4) . . . . ? C34 C35 C40 C39 -173.3(2) . . . . ? C31 C30 C41 C42 -140.0(3) . . . . ? P2 C30 C41 C42 41.0(3) . . . . ? C31 C30 C41 C46 36.3(4) . . . . ? P2 C30 C41 C46 -142.6(2) . . . . ? C46 C41 C42 C43 -2.1(4) . . . . ? C30 C41 C42 C43 174.3(2) . . . . ? C41 C42 C43 C44 -0.1(4) . . . . ? C42 C43 C44 C45 1.8(5) . . . . ? C43 C44 C45 C46 -1.2(4) . . . . ? C44 C45 C46 C41 -1.1(4) . . . . ? C42 C41 C46 C45 2.7(4) . . . . ? C30 C41 C46 C45 -173.8(2) . . . . ? C31 C32 C47 C52 25.8(3) . . . . ? C33 C32 C47 C52 148.0(2) . . . . ? C54 C32 C47 C52 -94.3(3) . . . . ? C31 C32 C47 C48 -158.5(2) . . . . ? C33 C32 C47 C48 -36.3(3) . . . . ? C54 C32 C47 C48 81.4(3) . . . . ? C52 C47 C48 C49 -1.6(4) . . . . ? C32 C47 C48 C49 -177.5(2) . . . . ? C47 C48 C49 C50 -0.2(4) . . . . ? C48 C49 C50 C51 1.7(4) . . . . ? C49 C50 C51 C52 -1.4(4) . . . . ? C50 C51 C52 C47 -0.4(4) . . . . ? C48 C47 C52 C51 1.9(4) . . . . ? C32 C47 C52 C51 177.8(2) . . . . ? C58 C53 C54 C55 -4.0(4) . . . . ? P2 C53 C54 C55 178.87(18) . . . . ? C58 C53 C54 C32 174.3(2) . . . . ? P2 C53 C54 C32 -2.8(3) . . . . ? C47 C32 C54 C55 0.2(3) . . . . ? C31 C32 C54 C55 -124.0(2) . . . . ? C33 C32 C54 C55 123.2(2) . . . . ? C47 C32 C54 C53 -178.0(2) . . . . ? C31 C32 C54 C53 57.8(3) . . . . ? C33 C32 C54 C53 -55.0(3) . . . . ? C53 C54 C55 C56 3.7(4) . . . . ? C32 C54 C55 C56 -174.4(2) . . . . ? C54 C55 C56 C57 -0.7(4) . . . . ? C55 C56 C57 C58 -2.0(4) . . . . ? C54 C53 C58 C57 1.2(4) . . . . ? P2 C53 C58 C57 178.13(19) . . . . ? C56 C57 C58 C53 1.8(4) . . . . ? C29 C24 P1 C5 -132.3(2) . . . . ? C25 C24 P1 C5 47.1(2) . . . . ? C29 C24 P1 C1 131.1(2) . . . . ? C25 C24 P1 C1 -49.6(2) . . . . ? C29 C24 P1 Cu1 5.9(2) . . . . ? C25 C24 P1 Cu1 -174.79(14) . . . . ? C4 C5 P1 C24 -47.3(2) . . . . ? C6 C5 P1 C24 135.1(2) . . . . ? C4 C5 P1 C1 49.6(2) . . . . ? C6 C5 P1 C1 -128.0(2) . . . . ? C4 C5 P1 Cu1 177.79(15) . . . . ? C6 C5 P1 Cu1 0.2(2) . . . . ? C2 C1 P1 C24 48.7(2) . . . . ? C12 C1 P1 C24 -132.8(2) . . . . ? C2 C1 P1 C5 -49.2(2) . . . . ? C12 C1 P1 C5 129.3(2) . . . . ? C2 C1 P1 Cu1 176.54(16) . . . . ? C12 C1 P1 Cu1 -5.0(2) . . . . ? C58 C53 P2 C30 138.0(2) . . . . ? C54 C53 P2 C30 -44.9(2) . . . . ? C58 C53 P2 C34 -125.4(2) . . . . ? C54 C53 P2 C34 51.7(2) . . . . ? C58 C53 P2 Cu1 12.7(2) . . . . ? C54 C53 P2 Cu1 -170.29(15) . . . . ? C31 C30 P2 C53 46.0(2) . . . . ? C41 C30 P2 C53 -135.0(2) . . . . ? C31 C30 P2 C34 -49.2(2) . . . . ? C41 C30 P2 C34 129.8(2) . . . . ? C31 C30 P2 Cu1 170.38(16) . . . . ? C41 C30 P2 Cu1 -10.6(2) . . . . ? C33 C34 P2 C53 -49.9(2) . . . . ? C35 C34 P2 C53 124.4(2) . . . . ? C33 C34 P2 C30 48.2(2) . . . . ? C35 C34 P2 C30 -137.6(2) . . . . ? C33 C34 P2 Cu1 -178.88(14) . . . . ? C35 C34 P2 Cu1 -4.6(2) . . . . ? _refine_diff_density_max 0.544 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.071 _shelx_res_file ; MR289_sq.res created by SHELXL-2014/7 TITL MR289.res in P-1 REM Old TITL unvoll in P-1 REM SHELXT solution in P-1 REM R1 0.131, Rweak 0.011, Alpha 0.052, Orientation as input REM Formula found by SHELXT: C61 Cl6 Cu CELL 0.71073 10.6222 13.4612 18.3551 82.3313 84.5796 74.1664 ZERR 4.000 0.0003 0.0003 0.0005 0.0009 0.0009 0.0009 LATT 1 SFAC C H P CL CU UNIT 116 84 4 2 2 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.120 SIZE 0.06 0.09 0.18 L.S. 30 0 99 BOND $H acta conf FMAP 2 PLAN 20 ABIN WGHT 0.029600 3.741300 FVAR 0.46912 C1 1 0.683551 0.588180 0.763069 11.00000 0.00968 0.01703 = 0.01239 -0.00546 -0.00206 -0.00593 C2 1 0.746378 0.522770 0.816927 11.00000 0.00798 0.01723 = 0.01417 -0.00369 -0.00156 -0.00554 AFIX 43 H2 2 0.835665 0.486404 0.808439 11.00000 -1.20000 AFIX 0 C3 1 0.676008 0.505444 0.892715 11.00000 0.01005 0.01708 = 0.01127 0.00163 -0.00402 -0.00666 C4 1 0.552921 0.474057 0.878693 11.00000 0.01140 0.01439 = 0.01152 0.00030 0.00031 -0.00543 AFIX 43 H4 2 0.536974 0.411788 0.903734 11.00000 -1.20000 AFIX 0 C5 1 0.467728 0.534224 0.831199 11.00000 0.00940 0.01430 = 0.00919 -0.00080 0.00052 -0.00424 C6 1 0.350814 0.508005 0.809680 11.00000 0.01289 0.02052 = 0.00740 -0.00014 -0.00046 -0.00732 C7 1 0.355154 0.404883 0.804375 11.00000 0.01310 0.02082 = 0.01581 -0.00298 -0.00313 -0.00507 AFIX 43 H7 2 0.433703 0.352049 0.813796 11.00000 -1.20000 AFIX 0 C8 1 0.246337 0.378536 0.785536 11.00000 0.02174 0.02138 = 0.02775 -0.00593 -0.00280 -0.01023 AFIX 43 H8 2 0.249922 0.307775 0.783020 11.00000 -1.20000 AFIX 0 C9 1 0.131993 0.455333 0.770314 11.00000 0.01443 0.03609 = 0.02782 -0.00881 -0.00293 -0.01314 AFIX 43 H9 2 0.057542 0.437094 0.757108 11.00000 -1.20000 AFIX 0 C10 1 0.126085 0.558422 0.774312 11.00000 0.01058 0.02821 = 0.02246 -0.00308 -0.00407 -0.00249 AFIX 43 H10 2 0.047830 0.611048 0.763802 11.00000 -1.20000 AFIX 0 C11 1 0.234876 0.584474 0.793721 11.00000 0.01138 0.01943 = 0.01763 -0.00085 -0.00112 -0.00444 AFIX 43 H11 2 0.230735 0.655337 0.796239 11.00000 -1.20000 AFIX 0 C12 1 0.739693 0.607413 0.687560 11.00000 0.00773 0.01804 = 0.01151 -0.00249 -0.00126 -0.00743 C13 1 0.701702 0.704308 0.646133 11.00000 0.00983 0.01760 = 0.01561 -0.00253 0.00091 -0.00592 AFIX 43 H13 2 0.639600 0.759906 0.667075 11.00000 -1.20000 AFIX 0 C14 1 0.753828 0.720228 0.574576 11.00000 0.01553 0.02035 = 0.01699 0.00108 -0.00145 -0.00891 AFIX 43 H14 2 0.725907 0.786189 0.546660 11.00000 -1.20000 AFIX 0 C15 1 0.846271 0.640530 0.543659 11.00000 0.01437 0.02792 = 0.01405 -0.00508 0.00351 -0.01264 AFIX 43 H15 2 0.881817 0.651456 0.494707 11.00000 -1.20000 AFIX 0 C16 1 0.886453 0.544294 0.585136 11.00000 0.01170 0.02226 = 0.02027 -0.00816 0.00316 -0.00811 AFIX 43 H16 2 0.951137 0.489737 0.564641 11.00000 -1.20000 AFIX 0 C17 1 0.833202 0.527320 0.655820 11.00000 0.01022 0.01654 = 0.01698 -0.00311 -0.00401 -0.00541 AFIX 43 H17 2 0.860211 0.460800 0.683123 11.00000 -1.20000 AFIX 0 C18 1 0.766932 0.427613 0.945882 11.00000 0.01185 0.01592 = 0.01377 -0.00110 -0.00526 -0.00151 C19 1 0.723087 0.357374 0.997985 11.00000 0.01270 0.02006 = 0.01413 -0.00192 -0.00389 -0.00434 AFIX 43 H19 2 0.634204 0.355160 0.999814 11.00000 -1.20000 AFIX 0 C20 1 0.807299 0.290712 1.047168 11.00000 0.02260 0.02269 = 0.01698 0.00370 -0.00436 -0.00544 AFIX 43 H20 2 0.776139 0.242365 1.081690 11.00000 -1.20000 AFIX 0 C21 1 0.936558 0.294033 1.046376 11.00000 0.01995 0.02846 = 0.02177 0.00556 -0.01286 -0.00177 AFIX 43 H21 2 0.993967 0.248661 1.080431 11.00000 -1.20000 AFIX 0 C22 1 0.981104 0.363943 0.995599 11.00000 0.01117 0.04323 = 0.02869 0.00738 -0.01032 -0.00701 AFIX 43 H22 2 1.069564 0.366920 0.994787 11.00000 -1.20000 AFIX 0 C23 1 0.897302 0.429906 0.945725 11.00000 0.01587 0.02818 = 0.02336 0.00743 -0.00761 -0.00887 AFIX 43 H23 2 0.929340 0.477430 0.910885 11.00000 -1.20000 AFIX 0 C24 1 0.547946 0.692977 0.875957 11.00000 0.00863 0.02041 = 0.01000 -0.00068 -0.00057 -0.00800 C25 1 0.627744 0.613491 0.921825 11.00000 0.00955 0.01817 = 0.01226 0.00016 0.00057 -0.00874 C26 1 0.656693 0.635227 0.988838 11.00000 0.01349 0.02382 = 0.01267 0.00197 -0.00309 -0.00868 AFIX 43 H26 2 0.709445 0.582105 1.020875 11.00000 -1.20000 AFIX 0 C27 1 0.608187 0.735419 1.009253 11.00000 0.02105 0.02923 = 0.01430 -0.00624 -0.00359 -0.01319 AFIX 43 H27 2 0.628339 0.750057 1.055356 11.00000 -1.20000 AFIX 0 C28 1 0.531131 0.813868 0.963379 11.00000 0.02616 0.01933 = 0.01958 -0.00662 -0.00164 -0.00738 AFIX 43 H28 2 0.499309 0.881880 0.977884 11.00000 -1.20000 AFIX 0 C29 1 0.500311 0.792953 0.895917 11.00000 0.01642 0.01843 = 0.01392 -0.00130 -0.00081 -0.00634 AFIX 43 H29 2 0.447496 0.846296 0.864052 11.00000 -1.20000 AFIX 0 C30 1 0.096009 0.823653 0.632948 11.00000 0.00989 0.00925 = 0.01689 0.00029 -0.00197 -0.00280 C31 1 0.029198 0.832075 0.573660 11.00000 0.00836 0.00989 = 0.01422 0.00066 -0.00269 -0.00261 AFIX 43 H31 2 -0.062773 0.862525 0.575987 11.00000 -1.20000 AFIX 0 C32 1 0.097835 0.793691 0.502212 11.00000 0.00838 0.00951 = 0.01368 -0.00085 -0.00334 -0.00301 C33 1 0.175578 0.679967 0.522007 11.00000 0.01007 0.00974 = 0.01482 -0.00283 0.00019 -0.00343 AFIX 43 H33 2 0.162507 0.627324 0.496154 11.00000 -1.20000 AFIX 0 C34 1 0.260322 0.654078 0.574369 11.00000 0.01113 0.01057 = 0.01270 -0.00189 -0.00033 -0.00312 C35 1 0.345840 0.547338 0.591825 11.00000 0.01368 0.01168 = 0.00809 0.00085 -0.00203 -0.00066 C36 1 0.297208 0.461397 0.590512 11.00000 0.01269 0.01820 = 0.02039 0.00123 -0.00622 -0.00612 AFIX 43 H36 2 0.206866 0.471521 0.583612 11.00000 -1.20000 AFIX 0 C37 1 0.378567 0.361559 0.599108 11.00000 0.02251 0.01412 = 0.02656 -0.00198 -0.00658 -0.00515 AFIX 43 H37 2 0.344021 0.303743 0.597959 11.00000 -1.20000 AFIX 0 C38 1 0.510994 0.345772 0.609440 11.00000 0.02096 0.01433 = 0.01911 -0.00342 -0.00530 0.00315 AFIX 43 H38 2 0.567831 0.277496 0.614080 11.00000 -1.20000 AFIX 0 C39 1 0.558719 0.430588 0.612860 11.00000 0.01121 0.02219 = 0.02361 -0.00439 -0.00426 0.00108 AFIX 43 H39 2 0.648554 0.420099 0.621230 11.00000 -1.20000 AFIX 0 C40 1 0.477768 0.530692 0.604287 11.00000 0.01285 0.01381 = 0.02015 -0.00335 -0.00343 -0.00302 AFIX 43 H40 2 0.512232 0.588158 0.606906 11.00000 -1.20000 AFIX 0 C41 1 0.032095 0.855389 0.704135 11.00000 0.01253 0.00940 = 0.01205 0.00108 -0.00261 0.00122 C42 1 0.086546 0.906371 0.749005 11.00000 0.02051 0.01639 = 0.01605 -0.00008 -0.00484 -0.00333 AFIX 43 H42 2 0.171446 0.916153 0.736173 11.00000 -1.20000 AFIX 0 C43 1 0.017558 0.942917 0.812279 11.00000 0.03430 0.02681 = 0.02016 -0.00768 -0.00496 -0.00350 AFIX 43 H43 2 0.055448 0.977495 0.842618 11.00000 -1.20000 AFIX 0 C44 1 -0.105848 0.929263 0.831339 11.00000 0.03172 0.03382 = 0.01545 -0.00577 0.00259 0.00526 AFIX 43 H44 2 -0.153638 0.956219 0.873992 11.00000 -1.20000 AFIX 0 C45 1 -0.160293 0.876526 0.788647 11.00000 0.01763 0.03299 = 0.02184 0.00315 0.00206 -0.00059 AFIX 43 H45 2 -0.244622 0.866083 0.802422 11.00000 -1.20000 AFIX 0 C46 1 -0.091814 0.839117 0.725997 11.00000 0.01434 0.02128 = 0.01727 0.00129 -0.00449 -0.00186 AFIX 43 H46 2 -0.128870 0.801866 0.697244 11.00000 -1.20000 AFIX 0 C47 1 0.006198 0.808327 0.440591 11.00000 0.01101 0.00987 = 0.01427 0.00210 -0.00411 -0.00531 C48 1 0.042024 0.748775 0.381822 11.00000 0.01589 0.01308 = 0.01813 -0.00125 -0.00603 -0.00160 AFIX 43 H48 2 0.122997 0.696696 0.381375 11.00000 -1.20000 AFIX 0 C49 1 -0.038933 0.764355 0.323732 11.00000 0.02956 0.01773 = 0.01999 -0.00583 -0.00910 -0.00466 AFIX 43 H49 2 -0.012694 0.723083 0.284033 11.00000 -1.20000 AFIX 0 C50 1 -0.157504 0.839642 0.323431 11.00000 0.02220 0.02043 = 0.02135 0.00262 -0.01410 -0.00781 AFIX 43 H50 2 -0.213927 0.849056 0.284453 11.00000 -1.20000 AFIX 0 C51 1 -0.192639 0.900866 0.380555 11.00000 0.01451 0.01799 = 0.01986 0.00333 -0.00561 -0.00206 AFIX 43 H51 2 -0.272876 0.953790 0.380318 11.00000 -1.20000 AFIX 0 C52 1 -0.111586 0.885620 0.438279 11.00000 0.01486 0.01375 = 0.01328 0.00138 -0.00399 -0.00380 AFIX 43 H52 2 -0.136938 0.928748 0.476970 11.00000 -1.20000 AFIX 0 C53 1 0.297291 0.843838 0.530215 11.00000 0.01247 0.00749 = 0.01335 -0.00102 -0.00169 -0.00062 C54 1 0.203986 0.853936 0.478842 11.00000 0.00853 0.00891 = 0.01522 -0.00346 -0.00220 -0.00139 C55 1 0.212275 0.912430 0.411461 11.00000 0.01197 0.01212 = 0.01469 -0.00297 -0.00527 -0.00154 AFIX 43 H55 2 0.146460 0.923003 0.377477 11.00000 -1.20000 AFIX 0 C56 1 0.318383 0.955877 0.393793 11.00000 0.01654 0.01096 = 0.01620 0.00097 0.00012 -0.00251 AFIX 43 H56 2 0.325123 0.995422 0.347380 11.00000 -1.20000 AFIX 0 C57 1 0.413529 0.941559 0.443543 11.00000 0.01365 0.01471 = 0.02113 -0.00327 0.00006 -0.00707 AFIX 43 H57 2 0.486733 0.969414 0.430506 11.00000 -1.20000 AFIX 0 C58 1 0.402578 0.886623 0.512514 11.00000 0.01086 0.01387 = 0.01932 -0.00216 -0.00407 -0.00523 AFIX 43 H58 2 0.466642 0.878483 0.547180 11.00000 -1.20000 AFIX 0 P1 3 0.512170 0.653264 0.790410 11.00000 0.00789 0.01384 = 0.00955 -0.00035 -0.00227 -0.00382 P2 3 0.274034 0.766879 0.617636 11.00000 0.00909 0.01039 = 0.01215 -0.00091 -0.00382 -0.00270 CL1 4 0.444962 0.923978 0.714108 11.00000 0.01773 0.01332 = 0.01795 0.00104 -0.00640 -0.00545 CU1 5 0.401116 0.771759 0.706091 11.00000 0.01020 0.01394 = 0.01221 -0.00055 -0.00448 -0.00362 HKLF 4 REM MR289.res in P-1 REM R1 = 0.0426 for 8007 Fo > 4sig(Fo) and 0.0628 for all 10236 data REM 559 parameters refined using 0 restraints END WGHT 0.0296 3.7413 REM Highest difference peak 0.544, deepest hole -0.461, 1-sigma level 0.071 Q1 1 0.4120 0.7014 0.7381 11.00000 0.05 0.54 Q2 1 0.2772 0.8147 0.5741 11.00000 0.05 0.48 Q3 1 0.3992 0.8360 0.6730 11.00000 0.05 0.47 Q4 1 0.6531 0.5569 0.9069 11.00000 0.05 0.39 Q5 1 0.5028 0.5825 0.8080 11.00000 0.05 0.38 Q6 1 0.4851 0.7186 0.7592 11.00000 0.05 0.37 Q7 1 0.3927 0.8294 0.7398 11.00000 0.05 0.35 Q8 1 0.2658 0.6979 0.5997 11.00000 0.05 0.35 Q9 1 0.5452 0.7603 0.9888 11.00000 0.05 0.35 Q10 1 0.1648 0.7981 0.6308 11.00000 0.05 0.33 Q11 1 0.1438 0.7339 0.5120 11.00000 0.05 0.31 Q12 1 0.7024 0.6431 0.6587 11.00000 0.05 0.31 Q13 1 0.6209 0.6806 1.0151 11.00000 0.05 0.31 Q14 1 0.4713 0.8598 0.7438 11.00000 0.05 0.30 Q15 1 0.7174 0.5240 0.8607 11.00000 0.05 0.30 Q16 1 0.3240 0.5082 0.6090 11.00000 0.05 0.29 Q17 1 0.1535 0.8189 0.4893 11.00000 0.05 0.29 Q18 1 0.3596 0.4565 0.7850 11.00000 0.05 0.29 Q19 1 0.5649 0.6603 0.8396 11.00000 0.05 0.29 Q20 1 0.0816 0.8551 0.5980 11.00000 0.05 0.29 ; _shelx_res_checksum 26784 _shelx_hkl_file ; -2 0 0 151.68 5.90 -2 0 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10 10 -3 376.76 36.00 -10 -10 3 366.66 33.60 -10 -10 3 402.66 38.80 -10 -10 3 313.17 40.90 9 10 -3 62.79 18.10 9 10 -3 67.89 19.00 9 10 -3 74.69 17.70 -9 -10 3 76.29 20.10 -9 -10 3 46.00 16.50 -9 -10 3 38.70 18.20 8 10 -3 107.29 17.70 8 10 -3 90.49 15.50 -8 -10 3 97.99 20.50 -8 -10 3 60.19 15.40 -8 -10 3 84.89 18.00 7 10 -3 23.00 11.20 7 10 -3 12.10 11.90 -7 -10 3 28.20 12.90 -7 -10 3 47.00 25.10 -7 -10 3 34.30 14.80 6 10 -3 10.30 10.00 6 10 -3 -1.60 8.80 -6 -10 3 -2.40 13.00 -6 -10 3 5.70 11.70 -6 -10 3 -12.30 9.90 5 10 -3 140.29 16.00 5 10 -3 135.69 14.00 5 10 -3 143.59 19.70 -5 -10 3 151.68 19.90 -5 -10 3 200.88 19.00 -5 -10 3 182.18 21.30 4 10 -3 410.76 15.40 -4 -10 3 397.26 23.20 -4 -10 3 413.06 21.40 -4 -10 3 398.06 23.50 3 10 -3 130.49 15.90 -3 -10 3 127.09 16.80 -3 -10 3 99.39 14.20 -3 -10 3 108.99 13.50 2 10 -3 473.85 24.40 -2 -10 3 453.25 18.40 -2 -10 3 445.26 20.30 -2 -10 3 447.96 23.00 -1 -10 3 0.90 6.20 -1 -10 3 9.10 8.60 -1 -10 3 -6.30 6.70 0 -10 3 157.38 16.40 0 -10 3 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23.40 7 -9 3 489.55 25.70 7 -9 3 495.75 23.90 8 -9 3 108.49 14.80 8 -9 3 124.89 17.20 8 -9 3 103.09 17.10 12 8 -3 9.80 22.80 12 8 -3 18.40 20.30 12 8 -3 23.40 20.80 -12 -8 3 32.80 20.10 -12 -8 3 -14.40 26.90 -12 -8 3 -23.20 23.70 11 8 -3 54.39 18.30 11 8 -3 36.90 17.60 11 8 -3 63.69 22.20 -11 -8 3 57.39 17.80 -11 -8 3 76.59 23.60 -11 -8 3 78.49 22.60 10 8 -3 168.38 20.70 10 8 -3 180.98 23.90 -10 -8 3 240.28 27.60 -10 -8 3 209.08 24.70 9 8 -3 312.97 26.70 9 8 -3 338.17 26.50 -9 -8 3 294.87 33.70 -9 -8 3 316.67 31.00 8 8 -3 13.30 11.20 8 8 -3 5.30 11.90 8 8 -3 35.40 11.10 -8 -8 3 16.40 13.90 -8 -8 3 21.30 12.60 -8 -8 3 23.20 12.80 7 8 -3 417.26 23.60 7 8 -3 438.36 26.20 7 8 -3 441.96 25.10 -7 -8 3 420.26 28.10 -7 -8 3 417.26 26.10 -7 -8 3 432.66 25.30 6 8 -3 452.15 25.10 6 8 -3 480.85 22.20 6 8 -3 459.55 22.50 -6 -8 3 455.75 24.10 -6 -8 3 435.86 25.90 -6 -8 3 449.36 24.20 5 8 -3 82.19 12.50 5 8 -3 78.89 11.00 5 8 -3 68.59 10.50 -5 -8 3 69.79 12.70 -5 -8 3 57.89 10.40 -5 -8 3 50.99 9.70 4 8 -3 316.27 15.40 4 8 -3 309.17 19.40 4 8 -3 297.57 14.10 -4 -8 3 312.97 19.30 -4 -8 3 290.47 18.30 -4 -8 3 313.77 17.50 3 8 -3 31.40 8.90 3 8 -3 31.40 5.10 -3 -8 3 13.40 6.50 -3 -8 3 22.90 8.30 -3 -8 3 20.40 7.50 2 8 -3 1024.20 30.00 -2 -8 3 1002.30 26.00 -2 -8 3 1009.90 29.10 -2 -8 3 1026.00 24.90 -1 -8 3 284.37 16.00 -1 -8 3 255.97 12.50 -1 -8 3 259.47 11.50 0 -8 3 526.45 12.60 0 -8 3 540.25 20.50 0 -8 3 538.05 22.90 0 -8 3 520.85 13.70 1 -8 3 61.19 10.80 1 -8 3 59.49 8.80 2 -8 3 -1.90 5.60 2 -8 3 9.80 7.90 3 -8 3 228.38 15.30 3 -8 3 245.88 19.20 4 -8 3 139.09 18.10 4 -8 3 144.99 14.60 5 -8 3 567.04 23.10 5 -8 3 561.84 17.10 5 -8 3 601.44 28.60 5 -8 3 554.94 17.00 6 -8 3 546.45 20.40 6 -8 3 524.35 29.50 6 -8 3 544.95 20.20 7 -8 3 98.29 13.40 7 -8 3 115.29 13.20 8 -8 3 193.88 24.20 8 -8 3 228.08 24.60 9 -8 3 137.79 20.00 9 -8 3 99.59 14.80 12 7 -3 45.00 20.90 12 7 -3 14.10 21.90 12 7 -3 9.30 23.50 -12 -7 3 53.99 25.70 -12 -7 3 9.00 17.80 -12 -7 3 19.40 24.70 11 7 -3 10.10 17.00 11 7 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2165.98 42.70 -3 -7 3 2183.48 45.80 2 7 -3 374.96 17.90 2 7 -3 376.16 9.80 2 7 -3 370.56 9.90 -2 -7 3 372.26 15.70 -2 -7 3 363.46 14.20 -2 -7 3 353.56 17.00 1 7 -3 379.26 17.60 -1 -7 3 397.36 17.00 -1 -7 3 364.66 12.10 -1 -7 3 345.57 13.20 0 -7 3 92.79 7.00 0 -7 3 109.19 6.20 0 -7 3 131.69 11.70 1 -7 3 917.51 28.10 1 -7 3 935.21 25.60 2 -7 3 382.16 17.10 2 -7 3 408.06 19.80 3 -7 3 215.88 13.50 3 -7 3 194.68 16.70 4 -7 3 50.69 11.40 5 -7 3 270.47 13.20 5 -7 3 292.37 13.30 5 -7 3 272.47 21.20 6 -7 3 46.30 9.40 6 -7 3 51.59 9.20 6 -7 3 30.40 12.60 -7 7 -3 63.39 13.90 7 -7 3 60.49 11.90 7 -7 3 58.19 11.40 -8 7 -3 162.78 20.90 8 -7 3 179.78 20.70 8 -7 3 158.18 20.80 -9 7 -3 39.60 21.30 9 -7 3 46.00 22.90 9 -7 3 45.10 16.20 9 -7 3 12.20 12.60 12 6 -3 23.50 21.60 12 6 -3 72.59 22.70 12 6 -3 7.90 18.50 -12 -6 3 14.10 21.70 -12 -6 3 50.59 19.60 -12 -6 3 53.89 23.80 11 6 -3 235.68 29.50 11 6 -3 195.58 24.40 11 6 -3 214.38 27.50 -11 -6 3 148.79 26.20 -11 -6 3 151.68 24.10 -11 -6 3 170.48 21.50 10 6 -3 397.46 28.00 10 6 -3 390.16 33.50 -10 -6 3 381.56 32.70 -10 -6 3 360.26 30.10 9 6 -3 12.70 11.40 9 6 -3 15.80 10.50 9 6 -3 4.60 12.80 -9 -6 3 -6.50 16.00 -9 -6 3 -8.50 12.20 -9 -6 3 28.80 12.10 8 6 -3 632.54 31.60 8 6 -3 578.34 41.70 8 6 -3 663.33 29.50 -8 -6 3 668.73 33.10 -8 -6 3 659.23 28.90 -8 -6 3 605.94 30.80 7 6 -3 2.90 7.90 7 6 -3 8.20 8.50 7 6 -3 1.40 9.30 -7 -6 3 5.90 9.80 -7 -6 3 -1.40 10.60 -7 -6 3 6.60 7.80 6 6 -3 17.80 9.00 6 6 -3 25.60 9.20 6 6 -3 37.40 8.90 -6 -6 3 43.30 10.10 -6 -6 3 29.30 10.60 -6 -6 3 27.30 8.30 5 6 -3 1665.33 38.50 5 6 -3 1673.53 39.90 5 6 -3 1600.14 37.50 -5 -6 3 1666.23 39.40 -5 -6 3 1700.23 41.70 -5 -6 3 1658.23 39.80 4 6 -3 0.10 5.70 4 6 -3 3.00 5.20 4 6 -3 -0.20 5.80 -4 -6 3 2.00 6.50 -4 -6 3 7.80 5.40 -4 -6 3 2.30 5.40 3 6 -3 501.35 19.70 3 6 -3 462.65 15.30 3 6 -3 486.45 15.80 -3 -6 3 488.15 18.80 -3 -6 3 482.75 17.50 -3 -6 3 458.55 18.60 2 6 -3 2051.89 33.10 2 6 -3 2175.58 42.70 2 6 -3 2009.30 33.70 -2 -6 3 2021.70 38.70 -2 -6 3 2006.20 37.10 -2 -6 3 2094.89 41.40 1 6 -3 2334.37 44.80 -1 -6 3 2331.17 44.30 -1 -6 3 2326.57 37.60 -1 -6 3 2253.77 38.60 0 -6 3 1522.15 32.20 0 -6 3 1377.16 23.60 1 -6 3 974.70 27.70 1 -6 3 1014.90 25.60 2 -6 3 70.49 10.10 2 -6 3 89.39 11.80 3 -6 3 114.69 13.10 -4 6 -3 55.69 9.10 4 -6 3 45.20 5.50 4 -6 3 50.89 7.10 4 -6 3 42.80 9.70 -5 6 -3 25.60 9.10 5 -6 3 21.30 6.30 5 -6 3 20.10 8.80 5 -6 3 13.30 5.90 -6 6 -3 167.98 17.20 6 -6 3 183.78 14.80 6 -6 3 172.78 19.00 6 -6 3 161.38 14.00 -7 6 -3 142.89 18.30 7 -6 3 138.49 16.50 7 -6 3 127.69 16.70 -8 6 -3 155.08 22.40 8 -6 3 147.89 16.90 8 -6 3 152.88 18.80 -9 6 -3 291.07 28.20 9 -6 3 303.07 28.40 9 -6 3 286.57 25.20 9 -6 3 244.38 22.10 -10 6 -3 9.70 17.50 10 -6 3 20.40 17.70 10 -6 3 -16.10 15.50 10 -6 3 1.60 13.40 12 5 -3 -5.10 17.40 12 5 -3 28.80 19.40 12 5 -3 -37.00 19.70 -12 -5 3 -3.20 21.80 -12 -5 3 32.30 23.20 11 5 -3 35.50 22.30 11 5 -3 32.50 14.90 11 5 -3 -7.70 16.60 -11 -5 3 13.70 15.80 -11 -5 3 25.30 18.20 -11 -5 3 3.00 19.70 10 5 -3 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446.56 32.20 -11 -5 4 441.66 40.50 -11 -5 4 434.06 36.80 10 5 -4 87.59 19.70 10 5 -4 75.49 15.90 -10 -5 4 67.09 18.00 -10 -5 4 68.89 15.70 9 5 -4 54.69 16.00 9 5 -4 31.00 20.10 9 5 -4 52.49 13.90 -9 -5 4 38.50 11.70 -9 -5 4 49.99 15.20 -9 -5 4 32.60 14.50 8 5 -4 517.85 29.10 8 5 -4 498.15 25.70 8 5 -4 550.54 27.10 -8 -5 4 528.25 29.30 -8 -5 4 539.75 29.90 -8 -5 4 531.85 25.40 7 5 -4 27.00 9.70 7 5 -4 24.90 9.40 7 5 -4 17.50 10.40 -7 -5 4 26.70 9.00 -7 -5 4 13.10 11.00 -7 -5 4 15.20 9.30 6 5 -4 -4.50 7.60 6 5 -4 8.50 7.10 6 5 -4 1.80 7.00 -6 -5 4 11.20 8.20 -6 -5 4 -1.80 6.20 -6 -5 4 5.40 8.80 5 5 -4 199.18 14.40 5 5 -4 188.38 15.10 5 5 -4 201.58 14.90 -5 -5 4 200.48 14.10 -5 -5 4 198.78 15.60 -5 -5 4 209.08 17.40 4 5 -4 175.98 12.50 4 5 -4 187.38 12.80 4 5 -4 200.88 14.40 -4 -5 4 177.28 13.10 -4 -5 4 197.58 13.80 -4 -5 4 190.48 15.10 3 5 -4 3.60 5.80 3 5 -4 0.70 4.90 3 5 -4 0.90 3.90 -3 -5 4 6.30 6.00 -3 -5 4 5.50 4.70 -3 -5 4 -0.90 4.80 2 5 -4 23.50 4.60 2 5 -4 18.70 6.10 2 5 -4 15.50 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0.00 -5 7 18 0.94 0.00 9 7 18 -1.94 0.00 -5 8 18 0.46 0.00 9 8 18 3.64 0.00 -4 9 18 1.58 0.00 9 9 18 4.62 0.00 -3 10 18 2.96 0.00 8 10 18 -1.64 0.00 -2 11 18 4.76 0.00 -1 11 18 -0.86 0.00 7 11 18 1.74 0.00 8 11 18 0.77 0.00 0 12 18 2.75 0.00 1 12 18 -3.19 0.00 5 12 18 0.43 0.00 6 12 18 -5.20 0.00 7 12 18 -1.68 0.00 2 13 18 -4.18 0.00 3 13 18 -0.45 0.00 4 13 18 3.62 0.00 5 13 18 2.03 0.00 -4 -8 19 0.78 0.00 -3 -8 19 -0.10 0.00 -2 -8 19 -0.69 0.00 -1 -8 19 -0.32 0.00 0 -8 19 2.40 0.00 1 -8 19 1.35 0.00 2 -8 19 -1.53 0.00 -5 -7 19 -1.77 0.00 -4 -7 19 0.67 0.00 2 -7 19 0.10 0.00 3 -7 19 0.25 0.00 -6 -6 19 -0.04 0.00 -5 -6 19 -1.12 0.00 4 -6 19 -0.24 0.00 -6 -5 19 0.57 0.00 5 -5 19 -2.59 0.00 -6 -4 19 0.23 0.00 6 -4 19 3.15 0.00 -7 -3 19 -1.72 0.00 7 -3 19 0.89 0.00 -7 -2 19 -0.72 0.00 7 -2 19 1.86 0.00 -7 -1 19 -1.44 0.00 8 -1 19 2.25 0.00 -7 0 19 -1.91 0.00 8 0 19 2.22 0.00 -7 1 19 0.19 0.00 -7 2 19 1.34 0.00 9 2 19 -1.66 0.00 -6 3 19 1.11 0.00 9 3 19 -1.40 0.00 -6 4 19 -2.49 0.00 9 4 19 -0.87 0.00 -6 5 19 -3.97 0.00 9 5 19 -1.05 0.00 -5 6 19 0.98 0.00 9 6 19 -2.36 0.00 -5 7 19 0.51 0.00 -4 7 19 1.37 0.00 9 7 19 -3.06 0.00 -4 8 19 1.01 0.00 8 8 19 3.55 0.00 -3 9 19 -0.49 0.00 8 9 19 2.24 0.00 -2 10 19 -0.25 0.00 -1 10 19 -1.45 0.00 7 10 19 -1.30 0.00 -1 11 19 -0.73 0.00 0 11 19 -5.09 0.00 1 11 19 -1.59 0.00 5 11 19 -0.79 0.00 6 11 19 0.41 0.00 7 11 19 1.14 0.00 1 12 19 -3.26 0.00 2 12 19 1.56 0.00 3 12 19 3.21 0.00 4 12 19 1.82 0.00 5 12 19 -1.17 0.00 -3 -7 20 0.27 0.00 -2 -7 20 -1.79 0.00 -1 -7 20 -1.29 0.00 0 -7 20 3.47 0.00 1 -7 20 1.65 0.00 -4 -6 20 -0.47 0.00 -3 -6 20 -0.75 0.00 1 -6 20 2.24 0.00 2 -6 20 -0.80 0.00 3 -6 20 0.17 0.00 -5 -5 20 -0.41 0.00 -4 -5 20 -0.72 0.00 3 -5 20 2.20 0.00 4 -5 20 -0.24 0.00 -5 -4 20 3.31 0.00 5 -4 20 -1.13 0.00 -6 -3 20 -0.84 0.00 -5 -3 20 6.01 0.00 6 -3 20 3.54 0.00 -6 -2 20 -0.60 0.00 6 -2 20 5.15 0.00 -6 -1 20 2.53 0.00 7 -1 20 1.58 0.00 -6 0 20 3.85 0.00 7 0 20 -0.94 0.00 -6 1 20 1.96 0.00 8 1 20 1.11 0.00 -6 2 20 1.18 0.00 8 2 20 -0.21 0.00 -6 3 20 1.28 0.00 -5 3 20 -4.05 0.00 8 3 20 0.94 0.00 -5 4 20 -1.30 0.00 8 4 20 3.40 0.00 -5 5 20 1.73 0.00 8 5 20 2.91 0.00 -4 6 20 3.01 0.00 8 6 20 -0.45 0.00 -4 7 20 0.92 0.00 -3 7 20 2.46 0.00 8 7 20 -2.09 0.00 -3 8 20 0.60 0.00 -2 8 20 1.22 0.00 7 8 20 3.99 0.00 8 8 20 0.36 0.00 -2 9 20 0.09 0.00 -1 9 20 2.02 0.00 6 9 20 -4.74 0.00 7 9 20 0.14 0.00 -1 10 20 0.04 0.00 0 10 20 -0.48 0.00 1 10 20 0.49 0.00 5 10 20 0.46 0.00 6 10 20 -0.82 0.00 1 11 20 0.55 0.00 2 11 20 2.74 0.00 3 11 20 -1.48 0.00 4 11 20 -1.08 0.00 5 11 20 0.85 0.00 -2 -6 21 -2.12 0.00 -1 -6 21 -1.86 0.00 0 -6 21 3.36 0.00 1 -6 21 1.48 0.00 -3 -5 21 -0.33 0.00 -2 -5 21 -0.74 0.00 -1 -5 21 -2.22 0.00 0 -5 21 2.21 0.00 1 -5 21 1.85 0.00 2 -5 21 -1.48 0.00 3 -5 21 0.11 0.00 -4 -4 21 -0.11 0.00 -3 -4 21 -3.37 0.00 3 -4 21 1.15 0.00 4 -4 21 -0.04 0.00 -5 -3 21 2.86 0.00 -4 -3 21 2.09 0.00 4 -3 21 0.21 0.00 5 -3 21 0.30 0.00 -5 -2 21 3.97 0.00 -4 -2 21 4.83 0.00 5 -2 21 1.55 0.00 -5 -1 21 1.61 0.00 6 -1 21 3.26 0.00 -5 0 21 1.73 0.00 6 0 21 0.94 0.00 -5 1 21 4.75 0.00 7 1 21 -0.42 0.00 -5 2 21 4.05 0.00 7 2 21 -2.97 0.00 -5 3 21 -0.04 0.00 -4 3 21 1.54 0.00 7 3 21 -2.10 0.00 -4 4 21 0.17 0.00 7 4 21 1.60 0.00 -4 5 21 0.63 0.00 -3 5 21 2.08 0.00 7 5 21 2.57 0.00 -3 6 21 2.20 0.00 7 6 21 0.35 0.00 -3 7 21 2.18 0.00 -2 7 21 -1.69 0.00 6 7 21 -2.61 0.00 7 7 21 -0.55 0.00 -2 8 21 0.74 0.00 -1 8 21 -1.68 0.00 5 8 21 -3.39 0.00 6 8 21 -0.35 0.00 -1 9 21 1.43 0.00 0 9 21 0.40 0.00 1 9 21 -4.61 0.00 2 9 21 1.54 0.00 3 9 21 8.61 0.00 4 9 21 1.12 0.00 5 9 21 -5.73 0.00 6 9 21 -2.92 0.00 1 10 21 -2.37 0.00 2 10 21 -2.22 0.00 3 10 21 3.66 0.00 4 10 21 2.62 0.00 -2 -4 22 -0.66 0.00 -1 -4 22 -1.58 0.00 0 -4 22 1.87 0.00 1 -4 22 1.04 0.00 2 -4 22 -1.52 0.00 -3 -3 22 -1.68 0.00 -2 -3 22 -1.18 0.00 -1 -3 22 2.48 0.00 0 -3 22 2.54 0.00 1 -3 22 0.31 0.00 2 -3 22 -2.04 0.00 3 -3 22 0.13 0.00 -3 -2 22 -3.31 0.00 -2 -2 22 -3.82 0.00 3 -2 22 -0.44 0.00 4 -2 22 0.40 0.00 -4 -1 22 3.63 0.00 -3 -1 22 -2.73 0.00 4 -1 22 -1.32 0.00 5 -1 22 1.00 0.00 -4 0 22 1.81 0.00 -3 0 22 -1.81 0.00 5 0 22 -0.94 0.00 -4 1 22 -1.90 0.00 -3 1 22 -3.59 0.00 5 1 22 -2.34 0.00 6 1 22 0.51 0.00 -4 2 22 -1.79 0.00 -3 2 22 -4.47 0.00 5 2 22 0.71 0.00 6 2 22 -1.08 0.00 -3 3 22 -1.29 0.00 6 3 22 -0.29 0.00 -3 4 22 1.56 0.00 -2 4 22 1.83 0.00 6 4 22 1.28 0.00 -3 5 22 1.38 0.00 -2 5 22 0.55 0.00 5 5 22 -2.92 0.00 6 5 22 -0.03 0.00 -2 6 22 -1.97 0.00 -1 6 22 -1.93 0.00 5 6 22 -3.46 0.00 6 6 22 -3.03 0.00 -1 7 22 -3.83 0.00 0 7 22 -1.06 0.00 1 7 22 3.46 0.00 2 7 22 -1.13 0.00 3 7 22 -2.11 0.00 4 7 22 5.44 0.00 5 7 22 0.40 0.00 6 7 22 -3.62 0.00 0 8 22 -3.06 0.00 1 8 22 2.03 0.00 2 8 22 4.18 0.00 3 8 22 -0.10 0.00 4 8 22 0.37 0.00 5 8 22 0.85 0.00 2 9 22 3.86 0.00 3 9 22 4.23 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 50315) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.022 0.000 0.000 465 175 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 0 0 1.997 0 1 0 1.582 1 1 0 2.196 0 -1 1 2.040 0 0 1 1.121 1 0 1 2.230 0 1 1 1.834 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL MR289.res in P-1 CELL 10.6222 13.4612 18.3551 82.33 84.58 74.17 SPGR P-1 # Solvent Accessible Volume = 475.2 # Electrons Found in S.A.V. = 174.9 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.722 0.921 0.124 ! 25.71 eA-3 C102 0.229 0.772 0.158 ! 23.78 eA-3 C103 0.420 0.880 0.186 ! 23.28 eA-3 C104 0.821 0.053-0.002 ! 19.13 eA-3 C105 0.289 0.809 0.238 ! 7.36 eA-3 C106 0.841 0.907 0.048 ! 5.70 eA-3 C107 0.273 0.703 0.221 ! 5.08 eA-3 C108 0.994 0.796 0.129 ! 3.88 eA-3 C109 0.803 0.861 0.113 ! 1.64 eA-3 C110 0.501 0.822 0.235 ! 1.42 eA-3 C111 0.194 0.838 0.182 ! 1.41 eA-3 C112 0.316 0.907 0.219 ! 1.31 eA-3 C113 0.677 0.974 0.076 ! 1.29 eA-3 C114 0.416 0.924 0.128 ! 1.17 eA-3 C115 0.840 0.980 0.064 ! 1.09 eA-3 C116 0.375 0.953 0.203 ! 1.07 eA-3 C117 0.130 0.827 0.137 ! 1.03 eA-3 C118 0.156 0.046-0.008 ! 1.03 eA-3 C119 0.388 0.799 0.195 ! 1.03 eA-3 C120 0.845 0.058 0.060 ! 1.02 eA-3 C121 0.468 0.801 0.170 ! 1.01 eA-3 C122 0.471 0.781 0.213 ! 0.97 eA-3 Q123 0.384 0.953 0.426 ! 0.96 eA-3 Q124 0.312 0.705 0.153 ! 0.95 eA-3 C125 0.762 0.867 0.078 ! 0.95 eA-3 Q126 0.741 0.603 0.200 ! 0.94 eA-3 C127 0.125 0.920 0.046 ! 0.92 eA-3 C128 0.776 0.098 0.048 ! 0.91 eA-3 Q129 0.890 0.833 0.018 ! 0.88 eA-3 Q130 0.128 0.996 0.049 ! 0.88 eA-3 Q131 0.256 0.702 0.126 ! 0.88 eA-3 Q132 0.957 0.331 0.017 ! 0.88 eA-3 C133 0.777 0.062 0.063 ! 0.87 eA-3 C134 0.727 0.848 0.107 ! 0.87 eA-3 C135 0.719 0.935 0.187 ! 0.86 eA-3 C136 0.826 0.920 0.109 ! 0.86 eA-3 C137 0.652 0.872 0.157 ! 0.84 eA-3 C138 0.327 0.758 0.281 ! 0.84 eA-3 C139 0.680 0.969 0.172 ! 0.84 eA-3 C140 0.752 0.863 0.170 ! 0.83 eA-3 C141 0.955 0.859 0.062 ! 0.82 eA-3 C142 0.470 0.936 0.201 ! 0.81 eA-3 Q143 0.815 0.124 0.014 ! 0.80 eA-3 Q144 0.223 0.774 0.095 ! 0.79 eA-3 Q145 0.535 0.640 0.410 ! 0.79 eA-3 C146 0.072 0.944 0.013 ! 0.78 eA-3 C147 0.689 0.011 0.115 ! 0.77 eA-3 Q148 0.897 0.906 0.445 ! 0.77 eA-3 C149 0.222 0.904 0.045 ! 0.77 eA-3 Q150 0.130 0.460 0.376 ! 0.77 eA-3 Q151 0.418 0.359 0.090 ! 0.76 eA-3 Q152 0.089 0.591 0.046 ! 0.76 eA-3 Q153 0.557 0.049 0.314 ! 0.75 eA-3 C154 0.140 0.891 0.018 ! 0.75 eA-3 Q155 0.445 0.173 0.048 ! 0.74 eA-3 Q156 0.217 0.893 0.389 ! 0.74 eA-3 C157 0.743 0.978 0.153 ! 0.74 eA-3 Q158 0.311 0.396 0.268 ! 0.72 eA-3 Q159 0.649 0.606 0.019 ! 0.72 eA-3 Q160 0.209 0.296 0.424 ! 0.71 eA-3 Q161 0.814 0.936 0.372 ! 0.70 eA-3 Q162 0.150 0.498 0.328 ! 0.70 eA-3 Q163 0.725 0.182 0.424 ! 0.70 eA-3 Q164 0.088 0.028 0.190 ! 0.69 eA-3 C165 0.269 0.847 0.278 ! 0.69 eA-3 Q166 0.159 0.405 0.451 ! 0.69 eA-3 Q167 0.640 0.123 0.486 ! 0.68 eA-3 C168 0.258 0.968 0.014 ! 0.67 eA-3 Q169 0.499 0.518 0.372 ! 0.66 eA-3 Q170 0.180 0.328 0.436 ! 0.66 eA-3 Q171 0.590 0.298 0.265 ! 0.65 eA-3 Q172 0.681 0.514 0.410 ! 0.65 eA-3 Q173 0.944 0.067 0.233 ! 0.65 eA-3 C174 0.519 0.955 0.137 ! 0.64 eA-3 C175 0.595 0.857 0.160 ! 0.64 eA-3 C176 0.373 0.740 0.225 ! 0.64 eA-3 Q177 0.712 0.257 0.348 ! 0.63 eA-3 Q178 0.596 0.167 0.332 ! 0.63 eA-3 Q179 0.037 0.796 0.469 ! 0.62 eA-3 Q180 0.268 0.454 0.200 ! 0.61 eA-3 Q181 0.908 0.550 0.201 ! 0.61 eA-3 Q182 1.007 0.749 0.424 ! 0.61 eA-3 Q183 0.680 0.573 0.221 ! 0.60 eA-3 Q184 0.269 0.517 0.096 ! 0.59 eA-3 Q185 0.492 0.308 0.189 ! 0.59 eA-3 Q186 0.284 0.263 0.362 ! 0.58 eA-3 Q187 0.161 0.144 0.224 ! 0.57 eA-3 Q188 1.004 0.716 0.123 ! 0.57 eA-3 Q189 0.190 0.828 0.484 ! 0.56 eA-3 C190 0.601 0.955 0.125 ! 0.56 eA-3 Q191 0.495 0.417 0.188 ! 0.56 eA-3 Q192 0.497 0.302 0.233 ! 0.56 eA-3 Q193 0.683 0.344 0.001 ! 0.55 eA-3 Q194 0.589 0.480 0.166 ! 0.55 eA-3 Q195 0.499 0.484 0.125 ! 0.55 eA-3 Q196 0.803 0.256 0.059 ! 0.55 eA-3 Q197 0.960 0.110 0.281 ! 0.55 eA-3 Q198 0.925 0.185 0.435 ! 0.54 eA-3 Q199 0.619 0.694 0.015 ! 0.54 eA-3 ) ; _shelx_fab_checksum 18923 #=================================================================== _publ_requested_journal '??????' _publ_contact_author ; Prof. Dr.Christian M\"uller Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+49/(0)3083854004' _publ_contact_author_fax '+49/(0)3083852440' _publ_contact_author_email c.mueller@fu-berlin.de loop_ _publ_author_name _publ_author_address 'M\"uller, Christian' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Rigo, Massimo' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Weber, Manuela' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_section_title ; ... see the published paper. ; _publ_section_abstract ; ... and following paragraphs: see the published paper. ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END===============================================