data_MR290_2 _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 'C31 H24 Cl Cu N P' _chemical_formula_weight 540.47 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' _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+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.0577(8) _cell_length_b 8.4718(4) _cell_length_c 16.9486(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2449.23(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5908 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 24.93 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_F_000 1112 _exptl_transmission_factor_min 0.8861 _exptl_transmission_factor_max 0.9371 _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 1.088 _shelx_estimated_absorpt_T_min 0.837 _shelx_estimated_absorpt_T_max 0.928 _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 16075 _diffrn_reflns_av_unetI/netI 0.0603 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.388 _diffrn_reflns_theta_max 25.052 _diffrn_reflns_theta_full 25.052 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_full 0.988 _reflns_number_total 4286 _reflns_number_gt 3789 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.906 _reflns_Friedel_fraction_max 0.975 _reflns_Friedel_fraction_full 0.975 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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 APEX3' _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^)+(0.0223P)^2^] 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_abs_structure_details ; Flack x determined using 1578 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.023(9) _chemical_absolute_configuration ? _refine_ls_number_reflns 4286 _refine_ls_number_parameters 293 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Cu1 Cu 0.56421(3) 0.44169(6) 0.66935(3) 0.01162(14) Uani 1 1 d . . . . . P1 P 0.53576(7) 0.35670(15) 0.55191(7) 0.0085(3) Uani 1 1 d . . . . . N1 N 0.5861(2) 0.6535(5) 0.7130(2) 0.0138(9) Uani 1 1 d . . . . . Cl1 Cl 0.55988(8) 0.28311(15) 0.77431(7) 0.0225(3) Uani 1 1 d . . . . . C1 C 0.5856(3) 0.3969(5) 0.4565(3) 0.0074(10) Uani 1 1 d . . . . . C2 C 0.5209(3) 0.4084(5) 0.3964(3) 0.0096(10) Uani 1 1 d . . . . . H2 H 0.5310 0.4763 0.3492 0.011 Uiso 1 1 calc R U . . . C3 C 0.4429(3) 0.4213(5) 0.4335(3) 0.0099(5) Uani 1 1 d . . . . . H3 H 0.3973 0.4394 0.4026 0.012 Uiso 1 1 calc R U . . . C4 C 0.4384(3) 0.4068(5) 0.5119(3) 0.0099(5) Uani 1 1 d . . . . . C5 C 0.5694(3) 0.2522(5) 0.4029(2) 0.0076(10) Uani 1 1 d . . . . . C6 C 0.5420(2) 0.1158(5) 0.4511(3) 0.0083(10) Uani 1 1 d . . . . . C7 C 0.5292(3) 0.1459(6) 0.5316(2) 0.0085(10) Uani 1 1 d . . . . . C8 C 0.5099(3) 0.0257(6) 0.5834(3) 0.0122(11) Uani 1 1 d . . . . . H8 H 0.5010 0.0478 0.6376 0.015 Uiso 1 1 calc R U . . . C9 C 0.5038(3) -0.1272(5) 0.5551(3) 0.0115(10) Uani 1 1 d . . . . . H9 H 0.4922 -0.2111 0.5904 0.014 Uiso 1 1 calc R U . . . C10 C 0.5143(3) -0.1583(6) 0.4760(3) 0.0120(11) Uani 1 1 d . . . . . H10 H 0.5091 -0.2633 0.4571 0.014 Uiso 1 1 calc R U . . . C11 C 0.5324(3) -0.0368(6) 0.4233(3) 0.0112(11) Uani 1 1 d . . . . . H11 H 0.5382 -0.0588 0.3687 0.013 Uiso 1 1 calc R U . . . C12 C 0.6235(3) 0.2143(5) 0.3352(3) 0.0099(5) Uani 1 1 d . . . . . C13 C 0.6870(3) 0.1153(6) 0.3485(3) 0.0116(11) Uani 1 1 d . . . . . H13 H 0.6974 0.0790 0.4004 0.014 Uiso 1 1 calc R U . . . C14 C 0.7354(3) 0.0687(6) 0.2871(3) 0.0156(11) Uani 1 1 d . . . . . H14 H 0.7784 0.0004 0.2971 0.019 Uiso 1 1 calc R U . . . C15 C 0.7209(3) 0.1218(6) 0.2109(3) 0.0148(12) Uani 1 1 d . . . . . H15 H 0.7528 0.0877 0.1683 0.018 Uiso 1 1 calc R U . . . C16 C 0.6597(3) 0.2246(6) 0.1979(3) 0.0173(13) Uani 1 1 d . . . . . H16 H 0.6507 0.2646 0.1463 0.021 Uiso 1 1 calc R U . . . C17 C 0.6109(3) 0.2706(6) 0.2595(3) 0.0123(11) Uani 1 1 d . . . . . H17 H 0.5687 0.3410 0.2497 0.015 Uiso 1 1 calc R U . . . C18 C 0.6613(3) 0.4840(6) 0.4528(2) 0.0100(11) Uani 1 1 d . . . . . C19 C 0.7228(3) 0.4379(6) 0.5021(3) 0.0144(11) Uani 1 1 d . . . . . H19 H 0.7149 0.3554 0.5392 0.017 Uiso 1 1 calc R U . . . C20 C 0.7952(3) 0.5112(6) 0.4974(3) 0.0152(12) Uani 1 1 d . . . . . H20 H 0.8362 0.4798 0.5320 0.018 Uiso 1 1 calc R U . . . C21 C 0.8082(3) 0.6291(6) 0.4433(3) 0.0138(11) Uani 1 1 d . . . . . H21 H 0.8580 0.6786 0.4398 0.017 Uiso 1 1 calc R U . . . C22 C 0.7476(3) 0.6751(6) 0.3937(3) 0.0150(12) Uani 1 1 d . . . . . H22 H 0.7561 0.7566 0.3562 0.018 Uiso 1 1 calc R U . . . C23 C 0.6751(3) 0.6033(5) 0.3985(3) 0.0116(11) Uani 1 1 d . . . . . H23 H 0.6342 0.6360 0.3641 0.014 Uiso 1 1 calc R U . . . C24 C 0.3664(3) 0.4116(5) 0.5594(3) 0.0099(5) Uani 1 1 d . . . . . C25 C 0.2995(3) 0.4921(6) 0.5311(3) 0.0139(11) Uani 1 1 d . . . . . H25 H 0.3024 0.5485 0.4828 0.017 Uiso 1 1 calc R U . . . C26 C 0.2300(3) 0.4898(6) 0.5730(3) 0.0182(12) Uani 1 1 d . . . . . H26 H 0.1858 0.5455 0.5534 0.022 Uiso 1 1 calc R U . . . C27 C 0.2244(3) 0.4066(6) 0.6434(3) 0.0196(13) Uani 1 1 d . . . . . H27 H 0.1762 0.4021 0.6713 0.024 Uiso 1 1 calc R U . . . C28 C 0.2897(3) 0.3310(6) 0.6720(4) 0.0199(11) Uani 1 1 d . . . . . H28 H 0.2862 0.2757 0.7206 0.024 Uiso 1 1 calc R U . . . C29 C 0.3605(3) 0.3332(6) 0.6320(3) 0.0168(12) Uani 1 1 d . . . . . H29 H 0.4050 0.2817 0.6537 0.020 Uiso 1 1 calc R U . . . C30 C 0.6058(3) 0.7563(6) 0.7510(3) 0.0099(5) Uani 1 1 d . . . . . C31 C 0.6313(3) 0.8838(6) 0.8027(3) 0.0206(12) Uani 1 1 d . . . . . H00A H 0.6878 0.8999 0.7965 0.031 Uiso 1 1 calc R U . . . H00B H 0.6197 0.8561 0.8576 0.031 Uiso 1 1 calc R U . . . H00D H 0.6035 0.9811 0.7887 0.031 Uiso 1 1 calc R U . . . 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 Cu1 0.0136(3) 0.0136(3) 0.0077(3) -0.0015(3) -0.0014(3) -0.0010(3) P1 0.0105(6) 0.0082(6) 0.0067(6) 0.0002(6) -0.0006(5) -0.0012(5) N1 0.013(2) 0.016(2) 0.013(2) 0.0032(19) 0.0001(17) -0.001(2) Cl1 0.0426(9) 0.0139(7) 0.0109(6) 0.0019(6) 0.0044(6) 0.0069(6) C1 0.011(3) 0.007(3) 0.004(2) -0.0001(19) -0.0011(18) -0.0003(19) C2 0.012(3) 0.009(3) 0.008(2) 0.003(2) -0.0009(19) -0.003(2) C3 0.0100(12) 0.0064(11) 0.0134(10) -0.0003(9) 0.0009(9) -0.0019(9) C4 0.0100(12) 0.0064(11) 0.0134(10) -0.0003(9) 0.0009(9) -0.0019(9) C5 0.009(2) 0.008(2) 0.006(2) -0.0001(19) -0.0032(19) -0.001(2) C6 0.005(2) 0.008(2) 0.012(2) 0.003(2) -0.0019(19) 0.0024(19) C7 0.006(2) 0.011(3) 0.008(2) -0.002(2) -0.0033(18) 0.003(2) C8 0.010(3) 0.015(3) 0.012(2) 0.002(2) -0.001(2) -0.001(2) C9 0.006(2) 0.010(3) 0.018(3) 0.006(2) 0.003(2) 0.001(2) C10 0.009(3) 0.005(3) 0.022(3) -0.001(2) 0.003(2) -0.002(2) C11 0.007(2) 0.013(3) 0.014(2) -0.003(2) -0.001(2) -0.002(2) C12 0.0100(12) 0.0064(11) 0.0134(10) -0.0003(9) 0.0009(9) -0.0019(9) C13 0.014(3) 0.012(3) 0.009(2) 0.004(2) -0.002(2) -0.005(2) C14 0.013(3) 0.015(3) 0.019(3) 0.000(2) 0.003(2) -0.001(2) C15 0.011(3) 0.021(3) 0.012(3) -0.006(2) 0.004(2) -0.005(2) C16 0.016(3) 0.027(3) 0.009(2) 0.001(2) -0.002(2) -0.009(2) C17 0.010(3) 0.019(3) 0.008(2) -0.001(2) -0.0019(19) -0.004(2) C18 0.012(3) 0.009(3) 0.009(2) -0.004(2) 0.0010(19) 0.000(2) C19 0.019(3) 0.011(3) 0.014(3) 0.000(2) -0.002(2) -0.001(2) C20 0.014(3) 0.017(3) 0.015(3) -0.002(2) -0.006(2) 0.002(2) C21 0.010(3) 0.015(3) 0.017(3) -0.008(2) 0.001(2) -0.004(2) C22 0.022(3) 0.011(3) 0.012(3) 0.004(2) 0.003(2) -0.006(2) C23 0.011(3) 0.013(3) 0.011(2) 0.001(2) -0.001(2) 0.002(2) C24 0.0100(12) 0.0064(11) 0.0134(10) -0.0003(9) 0.0009(9) -0.0019(9) C25 0.016(3) 0.015(3) 0.011(2) -0.002(2) 0.001(2) 0.000(2) C26 0.008(3) 0.023(3) 0.023(3) -0.007(2) -0.002(2) 0.002(2) C27 0.017(3) 0.024(3) 0.018(3) -0.012(2) 0.011(2) -0.008(2) C28 0.026(3) 0.019(3) 0.015(2) -0.001(3) 0.000(3) -0.005(2) C29 0.017(3) 0.018(3) 0.015(3) -0.003(2) -0.002(2) 0.000(2) C30 0.0100(12) 0.0064(11) 0.0134(10) -0.0003(9) 0.0009(9) -0.0019(9) C31 0.029(3) 0.011(3) 0.022(3) -0.004(2) 0.004(2) -0.002(2) _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 Cu1 N1 1.976(4) . ? Cu1 P1 2.1716(13) . ? Cu1 Cl1 2.2303(13) . ? P1 C7 1.822(5) . ? P1 C4 1.844(5) . ? P1 C1 1.859(4) . ? N1 C30 1.134(6) . ? C1 C18 1.489(6) . ? C1 C2 1.505(6) . ? C1 C5 1.550(6) . ? C2 C3 1.476(6) . ? C2 C5 1.565(6) . ? C2 H2 1.0000 . ? C3 C4 1.338(6) . ? C3 H3 0.9500 . ? C4 C24 1.469(6) . ? C5 C6 1.490(6) . ? C5 C12 1.507(6) . ? C6 C11 1.385(6) . ? C6 C7 1.406(6) . ? C7 C8 1.384(6) . ? C8 C9 1.386(6) . ? C8 H8 0.9500 . ? C9 C10 1.378(7) . ? C9 H9 0.9500 . ? C10 C11 1.396(7) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.384(6) . ? C12 C13 1.389(7) . ? C13 C14 1.385(6) . ? C13 H13 0.9500 . ? C14 C15 1.390(6) . ? C14 H14 0.9500 . ? C15 C16 1.376(7) . ? C15 H15 0.9500 . ? C16 C17 1.391(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.388(6) . ? C18 C19 1.396(6) . ? C19 C20 1.384(7) . ? C19 H19 0.9500 . ? C20 C21 1.375(7) . ? C20 H20 0.9500 . ? C21 C22 1.388(7) . ? C21 H21 0.9500 . ? C22 C23 1.380(6) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.401(7) . ? C24 C25 1.413(7) . ? C25 C26 1.381(7) . ? C25 H25 0.9500 . ? C26 C27 1.389(7) . ? C26 H26 0.9500 . ? C27 C28 1.374(7) . ? C27 H27 0.9500 . ? C28 C29 1.385(7) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.458(7) . ? C31 H00A 0.9800 . ? C31 H00B 0.9800 . ? C31 H00D 0.9800 . ? 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 N1 Cu1 P1 133.34(12) . . ? N1 Cu1 Cl1 104.75(12) . . ? P1 Cu1 Cl1 121.60(6) . . ? C7 P1 C4 95.8(2) . . ? C7 P1 C1 92.5(2) . . ? C4 P1 C1 92.9(2) . . ? C7 P1 Cu1 120.79(15) . . ? C4 P1 Cu1 117.50(15) . . ? C1 P1 Cu1 129.39(15) . . ? C30 N1 Cu1 165.0(4) . . ? C18 C1 C2 125.2(4) . . ? C18 C1 C5 121.5(4) . . ? C2 C1 C5 61.6(3) . . ? C18 C1 P1 121.6(3) . . ? C2 C1 P1 105.4(3) . . ? C5 C1 P1 106.4(3) . . ? C3 C2 C1 112.2(4) . . ? C3 C2 C5 120.6(4) . . ? C1 C2 C5 60.6(3) . . ? C3 C2 H2 116.9 . . ? C1 C2 H2 116.9 . . ? C5 C2 H2 116.9 . . ? C4 C3 C2 117.9(4) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C24 126.2(4) . . ? C3 C4 P1 109.5(4) . . ? C24 C4 P1 124.0(3) . . ? C6 C5 C12 116.4(4) . . ? C6 C5 C1 110.4(4) . . ? C12 C5 C1 120.4(4) . . ? C6 C5 C2 121.9(4) . . ? C12 C5 C2 116.7(4) . . ? C1 C5 C2 57.8(3) . . ? C11 C6 C7 118.7(4) . . ? C11 C6 C5 125.1(4) . . ? C7 C6 C5 116.1(4) . . ? C8 C7 C6 121.3(4) . . ? C8 C7 P1 128.0(3) . . ? C6 C7 P1 110.6(3) . . ? C7 C8 C9 119.1(4) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.6(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 119.8(4) . . ? C6 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C17 C12 C13 118.6(4) . . ? C17 C12 C5 122.5(4) . . ? C13 C12 C5 118.8(4) . . ? C14 C13 C12 121.1(4) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.9(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 119.2(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 120.7(5) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C12 C17 C16 120.4(5) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C23 C18 C19 118.2(4) . . ? C23 C18 C1 122.4(4) . . ? C19 C18 C1 119.2(4) . . ? C20 C19 C18 120.7(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.2(5) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 120.6(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C18 120.8(4) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? C29 C24 C25 118.0(4) . . ? C29 C24 C4 121.8(4) . . ? C25 C24 C4 120.2(4) . . ? C26 C25 C24 120.8(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.5(5) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 118.9(5) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 121.9(5) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C24 119.9(5) . . ? C28 C29 H29 120.1 . . ? C24 C29 H29 120.1 . . ? N1 C30 C31 177.5(5) . . ? C30 C31 H00A 109.5 . . ? C30 C31 H00B 109.5 . . ? H00A C31 H00B 109.5 . . ? C30 C31 H00D 109.5 . . ? H00A C31 H00D 109.5 . . ? H00B C31 H00D 109.5 . . ? 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 C7 P1 C1 C18 -126.7(4) . . . . ? C4 P1 C1 C18 137.4(4) . . . . ? Cu1 P1 C1 C18 7.6(5) . . . . ? C7 P1 C1 C2 82.8(3) . . . . ? C4 P1 C1 C2 -13.1(3) . . . . ? Cu1 P1 C1 C2 -142.9(2) . . . . ? C7 P1 C1 C5 18.4(3) . . . . ? C4 P1 C1 C5 -77.5(3) . . . . ? Cu1 P1 C1 C5 152.8(2) . . . . ? C18 C1 C2 C3 -136.1(4) . . . . ? C5 C1 C2 C3 113.7(4) . . . . ? P1 C1 C2 C3 13.0(4) . . . . ? C18 C1 C2 C5 110.2(5) . . . . ? P1 C1 C2 C5 -100.7(3) . . . . ? C1 C2 C3 C4 -6.0(6) . . . . ? C5 C2 C3 C4 62.1(6) . . . . ? C2 C3 C4 C24 -178.2(4) . . . . ? C2 C3 C4 P1 -4.6(5) . . . . ? C7 P1 C4 C3 -82.2(4) . . . . ? C1 P1 C4 C3 10.6(4) . . . . ? Cu1 P1 C4 C3 148.6(3) . . . . ? C7 P1 C4 C24 91.6(4) . . . . ? C1 P1 C4 C24 -175.6(4) . . . . ? Cu1 P1 C4 C24 -37.7(4) . . . . ? C18 C1 C5 C6 128.5(4) . . . . ? C2 C1 C5 C6 -115.6(4) . . . . ? P1 C1 C5 C6 -16.7(4) . . . . ? C18 C1 C5 C12 -11.6(6) . . . . ? C2 C1 C5 C12 104.3(4) . . . . ? P1 C1 C5 C12 -156.8(3) . . . . ? C18 C1 C5 C2 -115.9(5) . . . . ? P1 C1 C5 C2 98.9(3) . . . . ? C3 C2 C5 C6 -4.5(6) . . . . ? C1 C2 C5 C6 95.4(4) . . . . ? C3 C2 C5 C12 149.6(4) . . . . ? C1 C2 C5 C12 -110.6(4) . . . . ? C3 C2 C5 C1 -99.8(5) . . . . ? C12 C5 C6 C11 -29.0(6) . . . . ? C1 C5 C6 C11 -170.9(4) . . . . ? C2 C5 C6 C11 125.1(5) . . . . ? C12 C5 C6 C7 147.5(4) . . . . ? C1 C5 C6 C7 5.6(5) . . . . ? C2 C5 C6 C7 -58.4(6) . . . . ? C11 C6 C7 C8 2.1(7) . . . . ? C5 C6 C7 C8 -174.6(4) . . . . ? C11 C6 C7 P1 -174.4(3) . . . . ? C5 C6 C7 P1 8.9(5) . . . . ? C4 P1 C7 C8 -99.3(4) . . . . ? C1 P1 C7 C8 167.6(4) . . . . ? Cu1 P1 C7 C8 27.6(5) . . . . ? C4 P1 C7 C6 77.0(3) . . . . ? C1 P1 C7 C6 -16.2(3) . . . . ? Cu1 P1 C7 C6 -156.1(3) . . . . ? C6 C7 C8 C9 0.5(7) . . . . ? P1 C7 C8 C9 176.4(3) . . . . ? C7 C8 C9 C10 -2.1(7) . . . . ? C8 C9 C10 C11 1.0(7) . . . . ? C7 C6 C11 C10 -3.2(6) . . . . ? C5 C6 C11 C10 173.2(4) . . . . ? C9 C10 C11 C6 1.7(7) . . . . ? C6 C5 C12 C17 130.1(5) . . . . ? C1 C5 C12 C17 -92.0(6) . . . . ? C2 C5 C12 C17 -25.4(6) . . . . ? C6 C5 C12 C13 -47.9(6) . . . . ? C1 C5 C12 C13 90.0(5) . . . . ? C2 C5 C12 C13 156.6(4) . . . . ? C17 C12 C13 C14 -2.3(7) . . . . ? C5 C12 C13 C14 175.7(4) . . . . ? C12 C13 C14 C15 0.3(7) . . . . ? C13 C14 C15 C16 2.0(7) . . . . ? C14 C15 C16 C17 -2.4(7) . . . . ? C13 C12 C17 C16 1.9(7) . . . . ? C5 C12 C17 C16 -176.1(4) . . . . ? C15 C16 C17 C12 0.4(7) . . . . ? C2 C1 C18 C23 9.6(7) . . . . ? C5 C1 C18 C23 85.1(6) . . . . ? P1 C1 C18 C23 -134.9(4) . . . . ? C2 C1 C18 C19 -166.1(4) . . . . ? C5 C1 C18 C19 -90.6(5) . . . . ? P1 C1 C18 C19 49.4(6) . . . . ? C23 C18 C19 C20 0.9(7) . . . . ? C1 C18 C19 C20 176.8(4) . . . . ? C18 C19 C20 C21 -1.1(7) . . . . ? C19 C20 C21 C22 0.6(7) . . . . ? C20 C21 C22 C23 -0.1(7) . . . . ? C21 C22 C23 C18 0.0(7) . . . . ? C19 C18 C23 C22 -0.4(7) . . . . ? C1 C18 C23 C22 -176.1(4) . . . . ? C3 C4 C24 C29 152.6(5) . . . . ? P1 C4 C24 C29 -20.1(6) . . . . ? C3 C4 C24 C25 -25.2(7) . . . . ? P1 C4 C24 C25 162.2(4) . . . . ? C29 C24 C25 C26 -1.7(7) . . . . ? C4 C24 C25 C26 176.2(4) . . . . ? C24 C25 C26 C27 -0.7(8) . . . . ? C25 C26 C27 C28 2.1(8) . . . . ? C26 C27 C28 C29 -1.1(8) . . . . ? C27 C28 C29 C24 -1.3(8) . . . . ? C25 C24 C29 C28 2.6(7) . . . . ? C4 C24 C29 C28 -175.2(4) . . . . ? _refine_diff_density_max 0.269 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.064 _shelx_res_file ; MR290_2 - Kopie.res created by SHELXL-2014/7 TITL MR290_2_a.res in Pna2(1) REM Old TITL MR290_2 in Pna2(1) REM SHELXT solution in Pna2(1) REM R1 0.069, Rweak 0.014, Alpha 0.005, Orientation as input REM Flack x = 0.024 ( 0.009 ) from Parsons' quotients REM Formula found by SHELXT: C32 Cl2 Cu CELL 0.71073 17.0577 8.4718 16.9486 90.000 90.000 90.000 ZERR 4.000 0.0008 0.0004 0.0006 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, Z SYMM 1/2-X, 1/2+Y, 1/2+Z SFAC C H P CL CU N UNIT 124 96 4 4 4 4 TEMP -173.270 SIZE 0.07 0.12 0.17 L.S. 30 BOND $H LIST 6 FMAP 2 eadp C3 C4 C12 C24 C30 PLAN 20 ACTA CONF WGHT 0.022300 FVAR 0.12527 CU1 5 0.564211 0.441686 0.669354 11.00000 0.01362 0.01356 = 0.00769 -0.00153 -0.00143 -0.00102 P1 3 0.535759 0.356695 0.551912 11.00000 0.01051 0.00823 = 0.00672 0.00020 -0.00056 -0.00122 N1 6 0.586109 0.653454 0.712998 11.00000 0.01315 0.01582 = 0.01258 0.00320 0.00014 -0.00060 CL1 4 0.559883 0.283115 0.774305 11.00000 0.04258 0.01391 = 0.01089 0.00189 0.00437 0.00688 C1 1 0.585606 0.396902 0.456487 11.00000 0.01130 0.00722 = 0.00358 -0.00006 -0.00113 -0.00033 C2 1 0.520908 0.408396 0.396398 11.00000 0.01165 0.00928 = 0.00776 0.00342 -0.00090 -0.00275 AFIX 13 H2 2 0.530976 0.476306 0.349214 11.00000 -1.20000 AFIX 0 C3 1 0.442876 0.421332 0.433454 11.00000 0.01002 0.00644 = 0.01335 -0.00028 0.00087 -0.00187 AFIX 43 H3 2 0.397283 0.439393 0.402556 11.00000 -1.20000 AFIX 0 C4 1 0.438363 0.406821 0.511949 11.00000 0.01002 0.00644 = 0.01335 -0.00028 0.00087 -0.00187 C5 1 0.569424 0.252175 0.402947 11.00000 0.00885 0.00815 = 0.00584 -0.00010 -0.00320 -0.00113 C6 1 0.541973 0.115812 0.451068 11.00000 0.00455 0.00809 = 0.01226 0.00266 -0.00188 0.00241 C7 1 0.529158 0.145931 0.531614 11.00000 0.00564 0.01139 = 0.00841 -0.00240 -0.00328 0.00268 C8 1 0.509874 0.025737 0.583379 11.00000 0.00995 0.01512 = 0.01159 0.00225 -0.00102 -0.00094 AFIX 43 H8 2 0.500952 0.047785 0.637598 11.00000 -1.20000 AFIX 0 C9 1 0.503751 -0.127206 0.555073 11.00000 0.00626 0.01003 = 0.01832 0.00557 0.00261 0.00054 AFIX 43 H9 2 0.492231 -0.211123 0.590399 11.00000 -1.20000 AFIX 0 C10 1 0.514275 -0.158274 0.475975 11.00000 0.00904 0.00536 = 0.02166 -0.00132 0.00260 -0.00212 AFIX 43 H10 2 0.509139 -0.263327 0.457063 11.00000 -1.20000 AFIX 0 C11 1 0.532417 -0.036831 0.423350 11.00000 0.00679 0.01261 = 0.01427 -0.00283 -0.00093 -0.00223 AFIX 43 H11 2 0.538190 -0.058812 0.368693 11.00000 -1.20000 AFIX 0 C12 1 0.623457 0.214331 0.335199 11.00000 0.01002 0.00644 = 0.01335 -0.00028 0.00087 -0.00187 C13 1 0.686977 0.115319 0.348454 11.00000 0.01382 0.01229 = 0.00881 0.00426 -0.00218 -0.00521 AFIX 43 H13 2 0.697408 0.078980 0.400431 11.00000 -1.20000 AFIX 0 C14 1 0.735388 0.068670 0.287097 11.00000 0.01287 0.01538 = 0.01860 -0.00008 0.00349 -0.00121 AFIX 43 H14 2 0.778445 0.000416 0.297095 11.00000 -1.20000 AFIX 0 C15 1 0.720888 0.121845 0.210895 11.00000 0.01101 0.02097 = 0.01233 -0.00595 0.00387 -0.00508 AFIX 43 H15 2 0.752820 0.087669 0.168267 11.00000 -1.20000 AFIX 0 C16 1 0.659725 0.224596 0.197922 11.00000 0.01556 0.02727 = 0.00910 0.00100 -0.00233 -0.00891 AFIX 43 H16 2 0.650739 0.264551 0.146335 11.00000 -1.20000 AFIX 0 C17 1 0.610922 0.270564 0.259550 11.00000 0.01039 0.01898 = 0.00767 -0.00093 -0.00186 -0.00361 AFIX 43 H17 2 0.568719 0.341005 0.249654 11.00000 -1.20000 AFIX 0 C18 1 0.661323 0.483985 0.452815 11.00000 0.01209 0.00912 = 0.00889 -0.00405 0.00099 0.00005 C19 1 0.722835 0.437934 0.502076 11.00000 0.01887 0.01063 = 0.01355 0.00005 -0.00208 -0.00069 AFIX 43 H19 2 0.714919 0.355396 0.539172 11.00000 -1.20000 AFIX 0 C20 1 0.795186 0.511200 0.497448 11.00000 0.01365 0.01722 = 0.01478 -0.00182 -0.00575 0.00156 AFIX 43 H20 2 0.836199 0.479775 0.531963 11.00000 -1.20000 AFIX 0 C21 1 0.808171 0.629117 0.443284 11.00000 0.00965 0.01474 = 0.01714 -0.00828 0.00119 -0.00380 AFIX 43 H21 2 0.858040 0.678562 0.439827 11.00000 -1.20000 AFIX 0 C22 1 0.747578 0.675072 0.393718 11.00000 0.02211 0.01105 = 0.01179 0.00394 0.00288 -0.00616 AFIX 43 H22 2 0.756058 0.756614 0.356200 11.00000 -1.20000 AFIX 0 C23 1 0.675094 0.603306 0.398471 11.00000 0.01144 0.01274 = 0.01051 0.00129 -0.00115 0.00210 AFIX 43 H23 2 0.634164 0.635972 0.364145 11.00000 -1.20000 AFIX 0 C24 1 0.366375 0.411572 0.559414 11.00000 0.01002 0.00644 = 0.01335 -0.00028 0.00087 -0.00187 C25 1 0.299530 0.492092 0.531132 11.00000 0.01604 0.01464 = 0.01095 -0.00202 0.00084 0.00015 AFIX 43 H25 2 0.302395 0.548484 0.482770 11.00000 -1.20000 AFIX 0 C26 1 0.230047 0.489803 0.572967 11.00000 0.00774 0.02343 = 0.02332 -0.00694 -0.00235 0.00168 AFIX 43 H26 2 0.185782 0.545532 0.553444 11.00000 -1.20000 AFIX 0 C27 1 0.224405 0.406646 0.643356 11.00000 0.01697 0.02417 = 0.01769 -0.01244 0.01068 -0.00753 AFIX 43 H27 2 0.176153 0.402125 0.671256 11.00000 -1.20000 AFIX 0 C28 1 0.289720 0.331037 0.671988 11.00000 0.02596 0.01894 = 0.01475 -0.00147 0.00032 -0.00519 AFIX 43 H28 2 0.286227 0.275683 0.720607 11.00000 -1.20000 AFIX 0 C29 1 0.360526 0.333204 0.631991 11.00000 0.01685 0.01803 = 0.01538 -0.00260 -0.00186 0.00022 AFIX 43 H29 2 0.405031 0.281669 0.653716 11.00000 -1.20000 AFIX 0 C30 1 0.605751 0.756301 0.750952 11.00000 0.01002 0.00644 = 0.01335 -0.00028 0.00087 -0.00187 C31 1 0.631273 0.883813 0.802655 11.00000 0.02870 0.01131 = 0.02173 -0.00360 0.00373 -0.00186 AFIX 137 H00A 2 0.687833 0.899945 0.796493 11.00000 -1.50000 H00B 2 0.619674 0.856132 0.857570 11.00000 -1.50000 H00D 2 0.603471 0.981099 0.788665 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 REM MR290_2_a.res in Pna2(1) REM R1 = 0.0340 for 3789 Fo > 4sig(Fo) and 0.0447 for all 4286 data REM 293 parameters refined using 1 restraints END WGHT 0.0223 0.0000 REM Highest difference peak 0.269, deepest hole -0.311, 1-sigma level 0.064 Q1 1 0.6195 0.6859 0.7385 11.00000 0.05 0.27 Q2 1 0.5907 0.3364 0.6683 11.00000 0.05 0.27 Q3 1 0.5981 0.7751 0.6991 11.00000 0.05 0.27 Q4 1 0.6442 0.2826 0.2397 11.00000 0.05 0.26 Q5 1 0.6214 0.7903 0.7820 11.00000 0.05 0.25 Q6 1 0.6000 0.2547 0.3804 11.00000 0.05 0.25 Q7 1 0.5122 -0.1304 0.5181 11.00000 0.05 0.23 Q8 1 0.6295 0.1358 0.3372 11.00000 0.05 0.23 Q9 1 0.5530 0.1631 0.7843 11.00000 0.05 0.23 Q10 1 0.3427 0.4986 0.5590 11.00000 0.05 0.22 Q11 1 0.4644 0.0040 0.6636 11.00000 0.05 0.22 Q12 1 0.6149 0.6801 0.6656 11.00000 0.05 0.22 Q13 1 0.5587 0.4197 0.6009 11.00000 0.05 0.22 Q14 1 0.4807 -0.0596 0.5650 11.00000 0.05 0.21 Q15 1 0.4994 -0.2751 0.4398 11.00000 0.05 0.21 Q16 1 0.5367 0.2919 0.3814 11.00000 0.05 0.21 Q17 1 0.6847 0.4803 0.4820 11.00000 0.05 0.21 Q18 1 0.2608 0.1705 0.6806 11.00000 0.05 0.21 Q19 1 0.3640 0.3888 0.5973 11.00000 0.05 0.20 Q20 1 0.4851 -0.2204 0.5634 11.00000 0.05 0.20 ; _shelx_res_checksum 11613 _shelx_hkl_file ; 0 -1 0 0.26 0.20 0 -2 0 75.32 2.90 0 -3 0 0.65 0.54 0 -4 0 47.70 2.68 0 -5 0 0.91 1.07 0 -6 0 34.75 3.08 0 -6 0 38.67 2.07 0 -7 0 -0.35 0.82 0 -7 0 -0.04 1.69 0 -8 0 2.45 2.19 0 -8 0 4.00 1.22 0 -9 0 1.87 2.68 0 -9 0 3.26 1.57 0 -10 0 8.71 2.31 0 -10 0 6.94 4.02 0 -1 -1 249.13 7.66 0 -1 1 234.16 7.80 0 -2 1 -0.26 0.41 0 -2 -1 0.00 0.37 0 -3 -1 400.56 13.13 0 -3 1 399.15 13.27 0 -4 -1 -0.18 0.78 0 -4 1 1.50 0.94 0 -5 -1 64.38 3.39 0 -5 1 54.47 3.40 0 -6 1 -0.76 0.67 0 -6 1 1.10 1.41 0 -6 -1 0.21 1.24 0 -7 -1 68.76 3.19 0 -7 1 73.16 3.53 0 -7 -1 73.58 4.55 0 -8 1 -0.02 1.20 0 -8 -1 0.91 1.03 0 -8 -1 -3.98 1.80 0 -8 1 -1.58 2.17 0 -9 1 6.29 2.46 0 -9 -1 3.18 2.62 0 -9 1 9.97 3.02 0 -9 -1 4.25 1.56 0 -10 1 2.16 3.88 0 -10 -1 -1.72 2.04 0 -10 1 -1.65 2.19 0 -10 -1 -5.80 3.55 0 0 2 51.79 1.90 0 -1 -2 0.06 0.15 0 -1 2 -0.19 0.24 0 -1 2 -0.03 0.29 0 -2 2 441.98 14.54 0 -2 -2 478.64 14.50 0 -2 2 446.91 14.76 0 -3 -2 0.03 0.49 0 -3 2 0.51 0.66 0 -4 2 92.34 4.17 0 -4 2 86.26 3.52 0 -4 -2 88.83 3.83 0 -5 -2 1.28 0.95 0 -5 2 -0.59 0.56 0 -5 2 0.23 1.14 0 -6 -2 62.64 3.82 0 -6 2 73.53 3.34 0 -6 2 68.35 4.18 0 -7 2 -1.14 0.95 0 -7 -2 -1.39 0.66 0 -7 -2 1.39 1.49 0 -7 2 0.22 1.67 0 -8 -2 50.46 2.85 0 -8 2 52.08 3.44 0 -8 2 52.14 4.86 0 -8 -2 48.85 4.41 0 -9 -2 0.52 1.38 0 -9 2 -0.24 2.83 0 -9 -2 -0.05 2.60 0 -9 2 0.15 1.73 0 -10 -2 29.42 4.80 0 -10 2 31.81 3.51 0 -10 2 33.77 4.87 0 -10 -2 29.58 3.62 0 0 -3 0.11 0.31 0 0 3 0.10 0.27 0 1 -3 129.85 4.36 0 -1 3 118.50 4.34 0 -1 -3 125.89 4.06 0 -1 3 123.25 4.35 0 -2 3 0.09 0.35 0 -2 -3 -0.07 0.25 0 -2 3 -0.15 0.47 0 -3 3 122.39 4.59 0 -3 3 116.88 4.88 0 -3 -3 132.35 4.52 0 -4 3 0.52 0.96 0 -4 -3 -0.72 0.62 0 -4 3 0.49 0.58 0 -5 -3 104.20 4.67 0 -5 3 117.02 5.25 0 -5 3 110.97 4.50 0 -6 3 0.14 0.93 0 -6 3 -2.28 1.43 0 -6 -3 0.60 1.23 0 -7 -3 26.54 3.10 0 -7 3 30.70 3.48 0 -7 3 29.03 2.55 0 -8 3 2.25 2.40 0 -8 -3 0.41 3.63 0 -8 -3 -0.30 0.89 0 -8 3 0.28 2.22 0 -9 3 29.78 3.65 0 -9 3 28.76 4.25 0 -9 -3 25.86 3.66 0 -9 -3 22.55 2.41 0 0 -4 164.71 5.87 0 0 4 180.67 5.73 0 0 4 178.37 5.90 0 1 4 0.02 0.23 0 -1 4 0.22 0.40 0 1 -4 0.01 0.33 0 -1 4 0.26 0.37 0 -1 -4 0.24 0.28 0 -2 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6.21 0 -4 12 119.05 6.26 0 -5 12 0.06 2.12 0 -5 -12 0.68 0.83 0 -6 -12 45.09 2.46 0 -6 12 45.75 4.58 0 -7 12 3.50 2.87 0 -7 12 6.89 3.34 0 -8 12 50.54 8.82 0 0 -13 0.72 1.04 0 0 13 -0.58 1.04 0 0 13 0.44 0.93 0 -1 -13 3.37 1.18 0 1 13 2.14 0.75 0 -1 13 0.28 1.05 0 1 13 1.83 1.09 0 -1 13 4.01 1.44 0 2 13 -0.41 0.77 0 -2 13 -1.82 1.41 0 -2 13 -1.02 1.26 0 -2 -13 0.19 0.94 0 -3 13 136.05 6.53 0 -3 -13 142.17 5.69 0 -3 13 132.80 6.42 0 -4 13 -1.45 1.80 0 -4 13 1.72 2.41 0 -4 -13 -0.22 0.90 0 -5 -13 29.82 2.27 0 -5 13 21.02 3.23 0 -6 13 -2.85 2.50 0 -6 13 1.13 2.47 0 -7 13 26.42 4.54 0 -7 13 18.12 3.48 0 0 14 13.78 1.65 0 0 14 13.02 2.14 0 -1 -14 0.78 1.06 0 -1 14 0.54 1.21 0 -1 14 -0.56 1.60 0 1 14 0.52 0.74 0 1 14 0.35 1.18 0 -2 -14 135.08 5.80 0 -2 14 134.38 6.44 0 2 14 129.99 5.12 0 -2 14 123.87 5.99 0 -3 14 2.09 2.12 0 -3 -14 0.82 1.06 0 -3 14 0.64 1.79 0 -4 14 -2.60 1.90 0 -4 -14 -2.24 0.95 0 -5 -14 0.61 1.06 0 -6 14 7.59 2.92 0 -6 14 4.04 2.90 0 -7 14 2.58 4.08 0 0 15 -1.84 1.35 0 0 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-2 -4 7 17.49 1.91 2 -4 -7 17.02 1.15 2 -4 -7 15.96 1.33 -2 -4 7 16.06 2.13 -2 -5 -7 48.53 2.37 2 -5 7 41.91 3.14 2 -5 7 41.24 3.64 2 -5 -7 47.67 1.94 -2 -5 7 42.94 3.03 -2 -5 7 38.64 3.40 2 -5 -7 44.70 2.50 2 -6 7 34.77 3.23 2 -6 7 32.44 3.72 -2 -6 -7 35.17 2.50 2 -6 -7 33.93 1.65 -2 -6 7 36.12 3.65 -2 -6 7 31.24 2.92 2 -6 -7 34.78 2.66 2 -7 7 8.69 2.20 -2 -7 -7 12.64 1.85 2 -7 -7 11.68 1.97 -2 -7 7 9.94 2.02 2 -7 -7 9.43 1.25 2 -8 7 20.59 3.79 -2 -8 -7 15.47 2.36 2 -8 7 12.97 2.58 -2 -8 7 16.78 2.72 2 -8 -7 17.26 2.59 2 -8 -7 14.99 1.63 -2 -8 7 12.57 3.15 -2 -9 -7 3.23 2.40 2 -9 7 1.84 3.03 2 -9 7 4.01 3.93 -2 -9 7 2.74 4.01 -2 -9 7 0.21 2.53 2 -9 -7 2.33 1.23 2 0 8 160.65 5.95 -2 0 -8 157.28 6.00 -2 0 8 155.15 5.86 2 0 8 155.32 5.62 -2 1 8 27.50 1.71 -2 -1 -8 27.55 1.83 2 -1 8 27.77 1.98 2 -1 8 30.32 2.16 -2 1 -8 22.91 1.96 -2 -1 8 28.76 2.03 2 1 8 27.11 1.73 2 1 8 26.63 1.37 -2 2 8 43.38 1.81 -2 -2 -8 39.17 2.14 2 -2 8 42.74 2.68 -2 2 8 43.28 1.80 2 -2 8 41.10 2.65 -2 -2 8 43.38 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-1 14 14.42 3.67 2 1 14 14.77 1.89 -2 -2 -14 49.61 3.26 -2 2 14 47.36 2.55 2 -2 14 42.33 3.86 2 -2 14 41.45 3.58 -2 2 14 43.80 2.67 2 2 14 48.67 2.65 -2 -2 14 47.90 3.90 -2 -2 14 46.93 3.61 -2 2 -14 49.92 3.61 -2 -3 -14 66.96 3.68 2 -3 14 71.50 4.76 2 -3 14 55.10 6.86 -2 -3 14 56.60 5.22 -2 -3 14 64.38 4.43 -2 -4 -14 3.83 1.41 2 -4 14 5.04 2.39 -2 -4 14 8.76 2.45 -2 -5 -14 8.69 1.54 -2 -6 -14 21.53 2.34 2 -6 14 22.57 4.01 2 -6 14 26.01 3.94 -2 -6 14 25.26 3.86 -2 -6 14 21.50 3.81 2 -7 14 8.69 4.43 -2 -7 -14 8.86 1.60 -2 -7 14 4.78 4.09 -2 0 15 72.37 4.46 -2 0 -15 83.09 4.54 2 0 15 81.01 3.88 -2 0 15 75.36 3.89 2 0 15 74.64 4.51 -2 -1 -15 8.31 1.76 2 -1 15 4.10 1.83 -2 1 15 4.89 1.10 -2 1 15 4.86 1.61 2 -1 15 5.41 1.65 -2 -1 15 3.27 1.85 2 1 15 5.03 1.05 -2 1 -15 7.50 1.87 -2 -1 15 3.58 1.54 2 1 15 5.33 1.57 -2 2 15 9.41 1.35 -2 2 15 10.81 1.54 2 -2 15 9.18 2.15 -2 -2 -15 9.71 1.85 2 -2 15 10.78 2.39 2 2 15 11.23 1.50 -2 2 -15 6.61 1.88 -2 -2 15 12.74 2.23 -2 -2 15 5.83 1.91 -2 -3 -15 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8 -7 5 19.19 3.02 -8 -7 -5 17.66 2.28 8 -7 5 14.57 3.48 -8 7 5 20.75 2.86 -8 7 -5 10.32 3.64 8 -7 -5 22.74 2.54 8 -7 -5 17.92 2.79 8 -8 5 6.85 3.93 -8 -8 -5 3.78 1.44 8 -8 5 6.12 2.66 -8 8 5 6.77 2.38 8 -8 -5 1.30 2.47 -8 8 -5 -0.53 2.64 8 -8 -5 3.67 2.72 -8 0 6 83.46 4.02 8 0 6 82.74 4.13 -8 0 -6 84.38 4.18 -8 0 -6 84.97 4.15 8 0 6 89.28 4.17 -8 1 6 51.46 2.86 -8 -1 -6 53.42 3.07 8 -1 6 49.22 3.19 8 -1 6 53.27 3.22 -8 -1 -6 51.59 2.96 -8 1 6 47.25 2.95 -8 1 -6 49.03 3.14 -8 1 -6 51.15 3.18 8 1 6 50.14 2.84 -8 -1 6 47.88 2.94 -8 -2 -6 143.68 5.74 -8 2 6 141.72 5.83 -8 -2 -6 137.23 5.67 -8 2 6 137.97 5.52 8 -2 6 139.22 6.08 8 -2 6 133.59 6.07 -8 2 -6 139.66 6.10 -8 2 -6 133.22 5.91 8 -2 -6 134.36 5.68 8 2 6 134.23 5.31 8 -3 6 9.36 1.71 -8 -3 -6 10.14 1.40 -8 3 6 8.29 1.16 -8 3 6 9.90 1.59 8 -3 6 8.62 1.94 -8 -3 -6 9.41 1.42 -8 3 -6 9.19 1.75 8 -3 -6 6.55 1.36 -8 3 -6 8.34 1.54 -8 4 6 2.43 0.69 -8 4 6 0.03 1.19 -8 -4 -6 2.50 1.03 8 -4 6 3.69 1.51 8 -4 -6 2.29 1.16 -8 4 -6 1.45 1.13 8 -4 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; _shelx_hkl_checksum 55856 #=================================================================== _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===============================================