data_FN02B _audit_creation_date 2014-09-09 _audit_creation_method ; Olex2 1.2 (compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862) ; _shelxl_version_number 2014/6 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C50 H34 O4 P2 W, 2(C2 H3 N)' _chemical_formula_sum 'C54 H40 N2 O4 P2 W' _chemical_formula_weight 1026.67 _chemical_absolute_configuration ? _chemical_melting_point ? 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 9 _space_group_name_H-M_alt 'C 1 c 1' _space_group_name_Hall 'C -2yc' 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 29.1358(14) _cell_length_b 11.5350(6) _cell_length_c 15.4712(7) _cell_angle_alpha 90 _cell_angle_beta 119.7420(10) _cell_angle_gamma 90 _cell_volume 4514.6(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9977 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.312 _cell_measurement_theta_min 2.697 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.679 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/2 (Bruker,2014) was used for absorption correction. wR2(int) was 0.1068 before and 0.0675 after correction. The Ratio of minimum to maximum transmission is 0.8456. The \l/2 correction factor is 0.00150. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 2056 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.03 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_unetI/netI 0.0512 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 32070 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 28.360 _diffrn_reflns_theta_min 2.635 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.999 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.994 _reflns_number_gt 9315 _reflns_number_total 9939 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 3.971 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.111 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.011(7) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 571 _refine_ls_number_reflns 9939 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0293 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+1.1400P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.0679 _refine_special_details ; Refined as a 2-component inversion twin. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46) 2.b Idealised Me refined as rotating group: C53(H53A,H53B,H53C), C51(H51A,H51B,H51C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 W1 W 0.40742(2) 0.78092(2) 0.04613(2) 0.01006(6) Uani 1 1 d . . . . . P1 P 0.48205(6) 0.72685(13) 0.01852(11) 0.0143(3) Uani 1 1 d . . . . . P2 P 0.48076(6) 0.83942(13) 0.21376(10) 0.0134(3) Uani 1 1 d . . . . . O1 O 0.38535(19) 1.0342(4) -0.0457(3) 0.0295(11) Uani 1 1 d . . . . . O2 O 0.3181(2) 0.7246(4) -0.1710(3) 0.0267(11) Uani 1 1 d . . . . . O3 O 0.39130(19) 0.5217(4) 0.0924(3) 0.0266(10) Uani 1 1 d . . . . . O4 O 0.31913(19) 0.8203(5) 0.1033(4) 0.0319(11) Uani 1 1 d . . . . . C1 C 0.5431(2) 0.7949(5) 0.0626(4) 0.0137(11) Uani 1 1 d . . . . . C2 C 0.5878(2) 0.7331(5) 0.0793(4) 0.0157(12) Uani 1 1 d . . . . . H2 H 0.6199 0.7754 0.1039 0.019 Uiso 1 1 calc R . . . . C3 C 0.5897(2) 0.6145(5) 0.0629(4) 0.0167(12) Uani 1 1 d . . . . . C4 C 0.5435(2) 0.5479(5) 0.0177(4) 0.0168(12) Uani 1 1 d . . . . . H4 H 0.5471 0.4688 0.0049 0.020 Uiso 1 1 calc R . . . . C5 C 0.4931(2) 0.5870(5) -0.0100(4) 0.0152(11) Uani 1 1 d . . . . . C6 C 0.4481(2) 0.5064(5) -0.0641(4) 0.0162(12) Uani 1 1 d . . . . . C7 C 0.4472(3) 0.3968(6) -0.0286(5) 0.0256(14) Uani 1 1 d . . . . . H7 H 0.4754 0.3730 0.0342 0.031 Uiso 1 1 calc R . . . . C8 C 0.4055(3) 0.3209(6) -0.0837(5) 0.0309(16) Uani 1 1 d . . . . . H8 H 0.4054 0.2460 -0.0581 0.037 Uiso 1 1 calc R . . . . C9 C 0.3640(3) 0.3542(6) -0.1759(5) 0.0317(16) Uani 1 1 d . . . . . H9 H 0.3355 0.3025 -0.2137 0.038 Uiso 1 1 calc R . . . . C10 C 0.3647(3) 0.4639(6) -0.2120(5) 0.0269(15) Uani 1 1 d . . . . . H10 H 0.3366 0.4870 -0.2752 0.032 Uiso 1 1 calc R . . . . C11 C 0.4059(2) 0.5407(6) -0.1570(4) 0.0185(12) Uani 1 1 d . . . . . H11 H 0.4055 0.6161 -0.1822 0.022 Uiso 1 1 calc R . . . . C12 C 0.5487(2) 0.9221(5) 0.0826(4) 0.0152(11) Uani 1 1 d . . . . . C13 C 0.5120(2) 0.9980(5) 0.0121(4) 0.0159(12) Uani 1 1 d . . . . . H13 H 0.4817 0.9685 -0.0450 0.019 Uiso 1 1 calc R . . . . C14 C 0.5200(3) 1.1178(5) 0.0254(5) 0.0225(13) Uani 1 1 d . . . . . H14 H 0.4951 1.1694 -0.0231 0.027 Uiso 1 1 calc R . . . . C15 C 0.5636(3) 1.1616(6) 0.1085(5) 0.0269(14) Uani 1 1 d . . . . . H15 H 0.5690 1.2430 0.1170 0.032 Uiso 1 1 calc R . . . . C16 C 0.5998(3) 1.0859(6) 0.1798(5) 0.0238(14) Uani 1 1 d . . . . . H16 H 0.6297 1.1158 0.2375 0.029 Uiso 1 1 calc R . . . . C17 C 0.5923(2) 0.9656(6) 0.1670(4) 0.0192(12) Uani 1 1 d . . . . . H17 H 0.6169 0.9142 0.2160 0.023 Uiso 1 1 calc R . . . . C18 C 0.6413(2) 0.5575(5) 0.0940(4) 0.0191(13) Uani 1 1 d . . . . . C19 C 0.6873(2) 0.5947(6) 0.1819(4) 0.0205(13) Uani 1 1 d . . . . . H19 H 0.6853 0.6580 0.2191 0.025 Uiso 1 1 calc R . . . . C20 C 0.7352(4) 0.5386(8) 0.2134(6) 0.024(2) Uani 1 1 d . . . . . H20 H 0.7659 0.5643 0.2719 0.029 Uiso 1 1 calc R . . . . C21 C 0.7388(3) 0.4459(6) 0.1606(5) 0.0266(14) Uani 1 1 d . . . . . H21 H 0.7715 0.4067 0.1837 0.032 Uiso 1 1 calc R . . . . C22 C 0.6944(3) 0.4103(6) 0.0738(5) 0.0280(15) Uani 1 1 d . . . . . H22 H 0.6971 0.3480 0.0365 0.034 Uiso 1 1 calc R . . . . C23 C 0.6460(3) 0.4644(6) 0.0408(5) 0.0221(14) Uani 1 1 d . . . . . H23 H 0.6158 0.4382 -0.0183 0.026 Uiso 1 1 calc R . . . . C24 C 0.4910(2) 0.9792(5) 0.2606(4) 0.0141(11) Uani 1 1 d . . . . . C25 C 0.5401(2) 1.0173(5) 0.3359(4) 0.0172(12) Uani 1 1 d . . . . . H25 H 0.5432 1.0963 0.3553 0.021 Uiso 1 1 calc R . . . . C26 C 0.5854(3) 0.9467(8) 0.3852(5) 0.0154(16) Uani 1 1 d . . . . . C27 C 0.5837(2) 0.8289(6) 0.3638(4) 0.0163(12) Uani 1 1 d . . . . . H27 H 0.6150 0.7855 0.4028 0.020 Uiso 1 1 calc R . . . . C28 C 0.5404(2) 0.7688(5) 0.2908(4) 0.0129(11) Uani 1 1 d . . . . . C29 C 0.5451(2) 0.6414(5) 0.2807(4) 0.0142(11) Uani 1 1 d . . . . . C30 C 0.5083(2) 0.5657(5) 0.2809(4) 0.0169(12) Uani 1 1 d . . . . . H30 H 0.4786 0.5952 0.2836 0.020 Uiso 1 1 calc R . . . . C31 C 0.5146(3) 0.4463(5) 0.2770(4) 0.0206(13) Uani 1 1 d . . . . . H31 H 0.4895 0.3946 0.2779 0.025 Uiso 1 1 calc R . . . . C32 C 0.5575(3) 0.4032(6) 0.2719(4) 0.0225(13) Uani 1 1 d . . . . . H32 H 0.5618 0.3219 0.2690 0.027 Uiso 1 1 calc R . . . . C33 C 0.5941(3) 0.4789(5) 0.2710(4) 0.0198(13) Uani 1 1 d . . . . . H33 H 0.6232 0.4493 0.2663 0.024 Uiso 1 1 calc R . . . . C34 C 0.5885(2) 0.5977(6) 0.2770(4) 0.0175(12) Uani 1 1 d . . . . . H34 H 0.6144 0.6491 0.2786 0.021 Uiso 1 1 calc R . . . . C35 C 0.4462(2) 1.0615(5) 0.2215(4) 0.0153(11) Uani 1 1 d . . . . . C36 C 0.4021(2) 1.0369(6) 0.2321(4) 0.0194(12) Uani 1 1 d . . . . . H36 H 0.4006 0.9662 0.2621 0.023 Uiso 1 1 calc R . . . . C37 C 0.3608(3) 1.1150(6) 0.1993(5) 0.0272(15) Uani 1 1 d . . . . . H37 H 0.3316 1.0988 0.2087 0.033 Uiso 1 1 calc R . . . . C38 C 0.3618(3) 1.2171(6) 0.1527(6) 0.0294(16) Uani 1 1 d . . . . . H38 H 0.3330 1.2699 0.1291 0.035 Uiso 1 1 calc R . . . . C39 C 0.4050(3) 1.2416(6) 0.1409(6) 0.0294(16) Uani 1 1 d . . . . . H39 H 0.4058 1.3113 0.1090 0.035 Uiso 1 1 calc R . . . . C40 C 0.4468(3) 1.1648(6) 0.1755(5) 0.0226(13) Uani 1 1 d . . . . . H40 H 0.4764 1.1827 0.1677 0.027 Uiso 1 1 calc R . . . . C41 C 0.6350(2) 0.9978(6) 0.4672(5) 0.0221(13) Uani 1 1 d . . . . . C42 C 0.6486(3) 1.1133(6) 0.4609(5) 0.0264(15) Uani 1 1 d . . . . . H42 H 0.6267 1.1586 0.4038 0.032 Uiso 1 1 calc R . . . . C43 C 0.6948(3) 1.1610(7) 0.5398(6) 0.0350(18) Uani 1 1 d . . . . . H43 H 0.7042 1.2387 0.5352 0.042 Uiso 1 1 calc R . . . . C44 C 0.7261(3) 1.0976(9) 0.6226(6) 0.043(2) Uani 1 1 d . . . . . H44 H 0.7567 1.1316 0.6762 0.052 Uiso 1 1 calc R . . . . C45 C 0.7133(3) 0.9826(8) 0.6290(5) 0.0372(19) Uani 1 1 d . . . . . H45 H 0.7356 0.9375 0.6860 0.045 Uiso 1 1 calc R . . . . C46 C 0.6675(3) 0.9339(7) 0.5511(5) 0.0292(16) Uani 1 1 d . . . . . H46 H 0.6587 0.8558 0.5558 0.035 Uiso 1 1 calc R . . . . C47 C 0.3975(2) 0.9460(5) -0.0073(4) 0.0166(12) Uani 1 1 d . . . . . C48 C 0.3504(3) 0.7431(5) -0.0935(5) 0.0157(12) Uani 1 1 d . . . . . C49 C 0.4014(2) 0.6124(5) 0.0787(4) 0.0152(11) Uani 1 1 d . . . . . C50 C 0.3511(3) 0.8098(5) 0.0826(4) 0.0190(13) Uani 1 1 d . . . . . N2 N 0.7187(5) 1.2569(8) 0.3375(7) 0.073(3) Uani 1 1 d . . . . . C53 C 0.7520(4) 1.4447(8) 0.4423(6) 0.045(2) Uani 1 1 d . . . . . H53A H 0.7280 1.5090 0.4065 0.068 Uiso 1 1 calc GR . . . . H53B H 0.7875 1.4632 0.4545 0.068 Uiso 1 1 calc GR . . . . H53C H 0.7531 1.4328 0.5060 0.068 Uiso 1 1 calc GR . . . . C54 C 0.7333(4) 1.3405(9) 0.3833(6) 0.046(2) Uani 1 1 d . . . . . N1 N 0.7080(3) 0.7729(7) 0.3793(6) 0.0435(18) Uani 1 1 d . . . . . C51 C 0.7548(3) 0.9722(7) 0.4200(6) 0.043(2) Uani 1 1 d . . . . . H51A H 0.7755 0.9789 0.3860 0.065 Uiso 1 1 calc GR . . . . H51B H 0.7784 0.9790 0.4920 0.065 Uiso 1 1 calc GR . . . . H51C H 0.7283 1.0341 0.3972 0.065 Uiso 1 1 calc GR . . . . C52 C 0.7284(3) 0.8600(7) 0.3974(5) 0.0303(16) 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 W1 0.00952(9) 0.00891(8) 0.01026(8) -0.00110(15) 0.00377(6) -0.00031(16) P1 0.0147(7) 0.0126(7) 0.0151(7) -0.0026(6) 0.0069(6) -0.0016(6) P2 0.0122(7) 0.0131(7) 0.0136(6) -0.0019(6) 0.0055(5) -0.0008(6) O1 0.028(3) 0.016(2) 0.037(3) 0.006(2) 0.010(2) 0.003(2) O2 0.022(3) 0.026(3) 0.021(2) -0.0057(19) 0.002(2) 0.000(2) O3 0.030(3) 0.019(2) 0.031(2) 0.0060(19) 0.015(2) 0.000(2) O4 0.024(3) 0.041(3) 0.041(3) -0.004(2) 0.024(2) 0.003(2) C1 0.016(3) 0.012(3) 0.014(2) -0.001(2) 0.008(2) -0.001(2) C2 0.014(3) 0.018(3) 0.018(3) -0.002(2) 0.009(2) -0.003(2) C3 0.017(3) 0.017(3) 0.017(3) 0.001(2) 0.009(2) 0.002(2) C4 0.019(3) 0.015(3) 0.018(3) -0.001(2) 0.010(2) 0.003(2) C5 0.018(3) 0.013(3) 0.014(2) -0.002(2) 0.008(2) -0.003(2) C6 0.014(3) 0.016(3) 0.019(3) -0.004(2) 0.008(2) -0.002(2) C7 0.027(4) 0.021(3) 0.026(3) 0.000(3) 0.012(3) -0.001(3) C8 0.031(4) 0.017(3) 0.042(4) -0.003(3) 0.015(3) -0.003(3) C9 0.024(4) 0.028(4) 0.038(4) -0.014(3) 0.012(3) -0.011(3) C10 0.017(3) 0.028(4) 0.025(3) -0.007(3) 0.003(3) 0.001(3) C11 0.017(3) 0.021(3) 0.017(3) -0.002(2) 0.008(2) 0.001(2) C12 0.019(3) 0.013(3) 0.020(3) -0.001(2) 0.015(2) 0.001(2) C13 0.018(3) 0.014(3) 0.020(3) -0.002(2) 0.013(2) -0.002(2) C14 0.029(4) 0.016(3) 0.030(3) 0.002(3) 0.020(3) 0.003(3) C15 0.037(4) 0.016(3) 0.040(4) -0.006(3) 0.028(3) -0.003(3) C16 0.026(4) 0.023(3) 0.028(3) -0.011(3) 0.017(3) -0.010(3) C17 0.020(3) 0.022(3) 0.020(3) -0.003(2) 0.013(2) -0.006(3) C18 0.015(3) 0.020(3) 0.021(3) 0.001(2) 0.008(2) -0.001(2) C19 0.020(3) 0.019(3) 0.023(3) -0.002(2) 0.011(3) 0.000(3) C20 0.019(4) 0.023(4) 0.030(4) -0.002(3) 0.012(3) -0.001(3) C21 0.017(3) 0.025(3) 0.038(4) -0.003(3) 0.014(3) 0.002(3) C22 0.023(3) 0.029(4) 0.036(4) -0.009(3) 0.018(3) -0.001(3) C23 0.020(3) 0.021(3) 0.028(3) -0.006(3) 0.014(3) -0.003(3) C24 0.014(3) 0.013(3) 0.016(3) -0.002(2) 0.009(2) 0.000(2) C25 0.016(3) 0.019(3) 0.016(3) -0.005(2) 0.008(2) -0.005(2) C26 0.012(4) 0.025(4) 0.011(3) -0.004(3) 0.007(3) -0.003(3) C27 0.014(3) 0.024(3) 0.010(2) 0.000(2) 0.005(2) -0.001(3) C28 0.012(3) 0.014(3) 0.012(2) 0.001(2) 0.006(2) -0.002(2) C29 0.016(3) 0.014(3) 0.010(2) 0.002(2) 0.004(2) 0.000(2) C30 0.017(3) 0.018(3) 0.016(3) 0.000(2) 0.008(2) 0.001(2) C31 0.023(3) 0.018(3) 0.018(3) 0.003(2) 0.008(2) 0.000(3) C32 0.030(4) 0.016(3) 0.020(3) 0.003(2) 0.011(3) 0.007(3) C33 0.022(3) 0.019(3) 0.018(3) 0.003(2) 0.010(2) 0.007(3) C34 0.019(3) 0.020(3) 0.012(2) 0.002(2) 0.006(2) 0.002(2) C35 0.016(3) 0.015(3) 0.014(2) -0.007(2) 0.006(2) -0.004(2) C36 0.020(3) 0.018(3) 0.020(3) -0.005(2) 0.011(2) -0.003(2) C37 0.016(3) 0.032(4) 0.036(3) -0.011(3) 0.014(3) -0.004(3) C38 0.021(3) 0.024(4) 0.037(4) -0.004(3) 0.010(3) 0.007(3) C39 0.032(4) 0.015(3) 0.037(4) 0.000(3) 0.013(3) 0.003(3) C40 0.022(3) 0.015(3) 0.034(3) -0.004(3) 0.016(3) -0.004(3) C41 0.013(3) 0.031(4) 0.023(3) -0.012(3) 0.010(2) -0.006(3) C42 0.021(3) 0.028(3) 0.034(3) -0.019(3) 0.016(3) -0.007(3) C43 0.023(4) 0.040(4) 0.045(4) -0.026(4) 0.019(3) -0.013(3) C44 0.018(4) 0.068(6) 0.036(4) -0.036(4) 0.007(3) -0.011(4) C45 0.017(4) 0.063(6) 0.022(3) -0.015(3) 0.002(3) 0.001(4) C46 0.016(3) 0.050(5) 0.018(3) -0.011(3) 0.005(3) -0.006(3) C47 0.014(3) 0.011(3) 0.020(3) -0.003(2) 0.005(2) -0.001(2) C48 0.018(3) 0.014(3) 0.020(3) 0.009(2) 0.014(3) 0.009(2) C49 0.022(3) 0.008(3) 0.012(2) -0.003(2) 0.005(2) 0.000(2) C50 0.025(3) 0.019(3) 0.010(2) -0.004(2) 0.007(2) -0.011(3) N2 0.103(9) 0.037(4) 0.064(6) -0.005(4) 0.030(6) -0.021(5) C53 0.046(5) 0.044(5) 0.038(4) -0.005(4) 0.015(4) -0.001(4) C54 0.047(5) 0.043(5) 0.045(4) 0.008(4) 0.020(4) -0.003(4) N1 0.039(4) 0.051(5) 0.045(4) -0.017(3) 0.025(4) -0.015(4) C51 0.040(5) 0.032(4) 0.053(5) -0.011(4) 0.020(4) 0.001(4) C52 0.019(3) 0.040(4) 0.028(3) -0.004(3) 0.009(3) 0.005(3) _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 W1 P1 2.4940(16) . ? W1 P2 2.4998(14) . ? W1 C47 2.038(6) . ? W1 C48 2.014(6) . ? W1 C49 2.037(6) . ? W1 C50 2.010(7) . ? P1 C1 1.743(6) . ? P1 C5 1.744(6) . ? P2 C24 1.732(6) . ? P2 C28 1.745(6) . ? O1 C47 1.142(7) . ? O2 C48 1.118(8) . ? O3 C49 1.136(7) . ? O4 C50 1.132(8) . ? C1 C2 1.393(9) . ? C1 C12 1.492(8) . ? C2 C3 1.398(8) . ? C3 C4 1.398(8) . ? C3 C18 1.485(8) . ? C4 C5 1.387(8) . ? C5 C6 1.481(8) . ? C6 C7 1.384(9) . ? C6 C11 1.408(8) . ? C7 C8 1.394(10) . ? C8 C9 1.391(10) . ? C9 C10 1.388(10) . ? C10 C11 1.392(9) . ? C12 C13 1.394(8) . ? C12 C17 1.387(8) . ? C13 C14 1.399(8) . ? C14 C15 1.380(9) . ? C15 C16 1.391(10) . ? C16 C17 1.403(9) . ? C18 C19 1.421(8) . ? C18 C23 1.401(9) . ? C19 C20 1.389(11) . ? C20 C21 1.379(11) . ? C21 C22 1.386(9) . ? C22 C23 1.387(9) . ? C24 C25 1.392(8) . ? C24 C35 1.480(8) . ? C25 C26 1.412(10) . ? C26 C27 1.393(11) . ? C26 C41 1.492(9) . ? C27 C28 1.391(8) . ? C28 C29 1.493(8) . ? C29 C30 1.385(8) . ? C29 C34 1.388(8) . ? C30 C31 1.394(8) . ? C31 C32 1.384(9) . ? C32 C33 1.382(9) . ? C33 C34 1.389(8) . ? C35 C36 1.402(8) . ? C35 C40 1.392(9) . ? C36 C37 1.383(9) . ? C37 C38 1.387(10) . ? C38 C39 1.388(11) . ? C39 C40 1.382(10) . ? C41 C42 1.407(10) . ? C41 C46 1.380(10) . ? C42 C43 1.405(9) . ? C43 C44 1.361(12) . ? C44 C45 1.394(13) . ? C45 C46 1.397(9) . ? N2 C54 1.146(12) . ? C53 C54 1.444(13) . ? N1 C52 1.128(10) . ? C51 C52 1.457(11) . ? 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 P1 W1 P2 82.88(5) . . ? C47 W1 P1 97.15(18) . . ? C47 W1 P2 92.58(16) . . ? C48 W1 P1 94.99(18) . . ? C48 W1 P2 175.54(18) . . ? C48 W1 C47 83.8(2) . . ? C48 W1 C49 86.1(2) . . ? C49 W1 P1 89.59(18) . . ? C49 W1 P2 97.77(15) . . ? C49 W1 C47 168.3(2) . . ? C50 W1 P1 172.72(17) . . ? C50 W1 P2 93.51(16) . . ? C50 W1 C47 89.3(2) . . ? C50 W1 C48 89.0(2) . . ? C50 W1 C49 84.6(2) . . ? C1 P1 W1 128.8(2) . . ? C1 P1 C5 103.6(3) . . ? C5 P1 W1 124.1(2) . . ? C24 P2 W1 124.5(2) . . ? C24 P2 C28 104.0(3) . . ? C28 P2 W1 129.2(2) . . ? C2 C1 P1 121.4(4) . . ? C2 C1 C12 117.9(5) . . ? C12 C1 P1 120.7(4) . . ? C1 C2 C3 125.8(6) . . ? C2 C3 C4 120.9(5) . . ? C2 C3 C18 120.0(5) . . ? C4 C3 C18 119.1(5) . . ? C5 C4 C3 125.8(6) . . ? C4 C5 P1 121.5(4) . . ? C4 C5 C6 118.4(5) . . ? C6 C5 P1 120.1(4) . . ? C7 C6 C5 122.3(5) . . ? C7 C6 C11 118.9(6) . . ? C11 C6 C5 118.7(5) . . ? C6 C7 C8 120.9(6) . . ? C9 C8 C7 120.3(7) . . ? C10 C9 C8 119.1(6) . . ? C9 C10 C11 121.0(6) . . ? C10 C11 C6 119.8(6) . . ? C13 C12 C1 119.5(5) . . ? C17 C12 C1 120.4(5) . . ? C17 C12 C13 119.9(6) . . ? C12 C13 C14 119.9(6) . . ? C15 C14 C13 120.5(6) . . ? C14 C15 C16 119.6(6) . . ? C15 C16 C17 120.3(6) . . ? C12 C17 C16 119.7(6) . . ? C19 C18 C3 120.0(6) . . ? C23 C18 C3 121.8(5) . . ? C23 C18 C19 118.2(6) . . ? C20 C19 C18 120.1(6) . . ? C21 C20 C19 120.7(8) . . ? C20 C21 C22 119.7(7) . . ? C21 C22 C23 120.8(6) . . ? C22 C23 C18 120.4(6) . . ? C25 C24 P2 122.4(5) . . ? C25 C24 C35 118.1(5) . . ? C35 C24 P2 119.4(4) . . ? C24 C25 C26 124.5(6) . . ? C25 C26 C41 118.9(7) . . ? C27 C26 C25 121.4(6) . . ? C27 C26 C41 119.6(7) . . ? C28 C27 C26 126.2(6) . . ? C27 C28 P2 121.1(5) . . ? C27 C28 C29 118.8(5) . . ? C29 C28 P2 120.1(4) . . ? C30 C29 C28 120.5(5) . . ? C30 C29 C34 119.6(6) . . ? C34 C29 C28 119.7(5) . . ? C29 C30 C31 120.3(6) . . ? C32 C31 C30 120.0(6) . . ? C33 C32 C31 119.7(6) . . ? C32 C33 C34 120.5(6) . . ? C29 C34 C33 119.9(6) . . ? C36 C35 C24 119.8(5) . . ? C40 C35 C24 121.7(5) . . ? C40 C35 C36 118.5(6) . . ? C37 C36 C35 120.4(6) . . ? C36 C37 C38 120.3(6) . . ? C37 C38 C39 119.7(6) . . ? C40 C39 C38 120.1(7) . . ? C39 C40 C35 120.9(6) . . ? C42 C41 C26 120.2(6) . . ? C46 C41 C26 120.8(7) . . ? C46 C41 C42 119.0(6) . . ? C43 C42 C41 119.5(7) . . ? C44 C43 C42 120.9(8) . . ? C43 C44 C45 120.0(7) . . ? C44 C45 C46 119.7(8) . . ? C41 C46 C45 120.9(8) . . ? O1 C47 W1 171.1(5) . . ? O2 C48 W1 178.2(6) . . ? O3 C49 W1 171.0(5) . . ? O4 C50 W1 176.6(6) . . ? N2 C54 C53 179.2(10) . . ? N1 C52 C51 179.4(9) . . ? 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 W1 P1 C1 C2 151.6(4) . . . . ? W1 P1 C1 C12 -29.1(6) . . . . ? W1 P1 C5 C4 -150.7(4) . . . . ? W1 P1 C5 C6 28.6(5) . . . . ? W1 P2 C24 C25 -157.6(4) . . . . ? W1 P2 C24 C35 23.7(5) . . . . ? W1 P2 C28 C27 157.9(4) . . . . ? W1 P2 C28 C29 -23.6(6) . . . . ? P1 C1 C2 C3 0.6(9) . . . . ? P1 C1 C12 C13 -46.8(7) . . . . ? P1 C1 C12 C17 138.0(5) . . . . ? P1 C5 C6 C7 -126.4(6) . . . . ? P1 C5 C6 C11 56.5(7) . . . . ? P2 C24 C25 C26 -3.4(9) . . . . ? P2 C24 C35 C36 61.5(6) . . . . ? P2 C24 C35 C40 -119.7(5) . . . . ? P2 C28 C29 C30 -51.1(7) . . . . ? P2 C28 C29 C34 132.8(5) . . . . ? C1 P1 C5 C4 9.8(5) . . . . ? C1 P1 C5 C6 -170.9(4) . . . . ? C1 C2 C3 C4 6.3(9) . . . . ? C1 C2 C3 C18 -173.5(6) . . . . ? C1 C12 C13 C14 -173.5(5) . . . . ? C1 C12 C17 C16 173.6(5) . . . . ? C2 C1 C12 C13 132.5(6) . . . . ? C2 C1 C12 C17 -42.6(8) . . . . ? C2 C3 C4 C5 -3.7(9) . . . . ? C2 C3 C18 C19 35.1(8) . . . . ? C2 C3 C18 C23 -147.1(6) . . . . ? C3 C4 C5 P1 -5.3(8) . . . . ? C3 C4 C5 C6 175.4(5) . . . . ? C3 C18 C19 C20 177.4(7) . . . . ? C3 C18 C23 C22 -177.6(6) . . . . ? C4 C3 C18 C19 -144.7(6) . . . . ? C4 C3 C18 C23 33.1(8) . . . . ? C4 C5 C6 C7 52.9(8) . . . . ? C4 C5 C6 C11 -124.2(6) . . . . ? C5 P1 C1 C2 -7.7(6) . . . . ? C5 P1 C1 C12 171.6(4) . . . . ? C5 C6 C7 C8 -176.7(6) . . . . ? C5 C6 C11 C10 176.2(6) . . . . ? C6 C7 C8 C9 0.2(11) . . . . ? C7 C6 C11 C10 -1.0(9) . . . . ? C7 C8 C9 C10 -0.1(11) . . . . ? C8 C9 C10 C11 -0.5(11) . . . . ? C9 C10 C11 C6 1.1(10) . . . . ? C11 C6 C7 C8 0.4(10) . . . . ? C12 C1 C2 C3 -178.7(5) . . . . ? C12 C13 C14 C15 -0.7(9) . . . . ? C13 C12 C17 C16 -1.5(9) . . . . ? C13 C14 C15 C16 -0.5(10) . . . . ? C14 C15 C16 C17 0.7(10) . . . . ? C15 C16 C17 C12 0.3(9) . . . . ? C17 C12 C13 C14 1.7(9) . . . . ? C18 C3 C4 C5 176.1(6) . . . . ? C18 C19 C20 C21 -0.5(11) . . . . ? C19 C18 C23 C22 0.3(10) . . . . ? C19 C20 C21 C22 1.7(12) . . . . ? C20 C21 C22 C23 -1.9(11) . . . . ? C21 C22 C23 C18 0.9(11) . . . . ? C23 C18 C19 C20 -0.5(10) . . . . ? C24 P2 C28 C27 -5.1(6) . . . . ? C24 P2 C28 C29 173.4(4) . . . . ? C24 C25 C26 C27 -2.4(11) . . . . ? C24 C25 C26 C41 -177.8(6) . . . . ? C24 C35 C36 C37 177.5(5) . . . . ? C24 C35 C40 C39 -178.8(6) . . . . ? C25 C24 C35 C36 -117.3(6) . . . . ? C25 C24 C35 C40 61.5(7) . . . . ? C25 C26 C27 C28 3.9(11) . . . . ? C25 C26 C41 C42 -36.7(9) . . . . ? C25 C26 C41 C46 141.9(7) . . . . ? C26 C27 C28 P2 0.6(9) . . . . ? C26 C27 C28 C29 -177.9(6) . . . . ? C26 C41 C42 C43 178.5(6) . . . . ? C26 C41 C46 C45 -178.4(6) . . . . ? C27 C26 C41 C42 147.9(7) . . . . ? C27 C26 C41 C46 -33.5(10) . . . . ? C27 C28 C29 C30 127.5(6) . . . . ? C27 C28 C29 C34 -48.6(7) . . . . ? C28 P2 C24 C25 6.4(6) . . . . ? C28 P2 C24 C35 -172.3(4) . . . . ? C28 C29 C30 C31 -176.4(5) . . . . ? C28 C29 C34 C33 177.8(5) . . . . ? C29 C30 C31 C32 -0.7(8) . . . . ? C30 C29 C34 C33 1.6(8) . . . . ? C30 C31 C32 C33 0.3(9) . . . . ? C31 C32 C33 C34 1.1(9) . . . . ? C32 C33 C34 C29 -2.1(8) . . . . ? C34 C29 C30 C31 -0.2(8) . . . . ? C35 C24 C25 C26 175.4(6) . . . . ? C35 C36 C37 C38 1.9(9) . . . . ? C36 C35 C40 C39 0.0(9) . . . . ? C36 C37 C38 C39 -1.3(10) . . . . ? C37 C38 C39 C40 -0.1(11) . . . . ? C38 C39 C40 C35 0.7(10) . . . . ? C40 C35 C36 C37 -1.3(8) . . . . ? C41 C26 C27 C28 179.2(6) . . . . ? C41 C42 C43 C44 -0.9(10) . . . . ? C42 C41 C46 C45 0.2(10) . . . . ? C42 C43 C44 C45 1.7(11) . . . . ? C43 C44 C45 C46 -1.6(11) . . . . ? C44 C45 C46 C41 0.7(11) . . . . ? C46 C41 C42 C43 -0.1(10) . . . . ? _shelx_res_file ; TITL cc in Cc #9 CELL 0.71073 29.1358 11.535 15.4712 90 119.742 90 ZERR 4 0.0014 0.0006 0.0007 0 0.001 0 LATT -7 SYMM +X,-Y,0.5+Z SFAC C H N O P W UNIT 216 160 8 16 8 4 L.S. 100 PLAN 20 TEMP -173.15 REM reset to Cc #9 BOND MORE -1 CONF fmap 2 53 acta 52 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM C:/Users/Wiecko/Desktop/Strukturen/Massimo/FN02B-non%20centro/cc.hkl< REM /HKL> WGHT 0.036000 1.140000 BASF 0.01082 FVAR 0.05561 W1 6 0.407421 0.780923 0.046130 11.00000 0.00952 0.00891 = 0.01026 -0.00110 0.00377 -0.00031 P1 5 0.482046 0.726854 0.018524 11.00000 0.01470 0.01259 = 0.01507 -0.00258 0.00688 -0.00163 P2 5 0.480764 0.839421 0.213756 11.00000 0.01225 0.01312 = 0.01358 -0.00186 0.00548 -0.00082 O1 4 0.385351 1.034162 -0.045740 11.00000 0.02765 0.01620 = 0.03718 0.00566 0.01033 0.00340 O2 4 0.318082 0.724553 -0.171009 11.00000 0.02178 0.02637 = 0.02098 -0.00566 0.00233 -0.00037 O3 4 0.391301 0.521689 0.092442 11.00000 0.02999 0.01880 = 0.03064 0.00598 0.01486 0.00037 O4 4 0.319126 0.820293 0.103339 11.00000 0.02391 0.04109 = 0.04097 -0.00388 0.02385 0.00299 C1 1 0.543058 0.794931 0.062588 11.00000 0.01606 0.01232 = 0.01383 -0.00102 0.00823 -0.00142 C2 1 0.587784 0.733148 0.079250 11.00000 0.01356 0.01814 = 0.01762 -0.00173 0.00948 -0.00275 AFIX 43 H2 2 0.619851 0.775411 0.103902 11.00000 -1.20000 AFIX 0 C3 1 0.589711 0.614497 0.062943 11.00000 0.01654 0.01682 = 0.01718 0.00085 0.00880 0.00241 C4 1 0.543536 0.547898 0.017743 11.00000 0.01887 0.01455 = 0.01798 -0.00130 0.00979 0.00346 AFIX 43 H4 2 0.547060 0.468804 0.004920 11.00000 -1.20000 AFIX 0 C5 1 0.493053 0.586975 -0.010045 11.00000 0.01836 0.01335 = 0.01417 -0.00191 0.00836 -0.00341 C6 1 0.448089 0.506418 -0.064093 11.00000 0.01351 0.01632 = 0.01928 -0.00411 0.00845 -0.00189 C7 1 0.447181 0.396823 -0.028587 11.00000 0.02716 0.02129 = 0.02628 0.00032 0.01173 -0.00107 AFIX 43 H7 2 0.475376 0.373020 0.034224 11.00000 -1.20000 AFIX 0 C8 1 0.405478 0.320862 -0.083686 11.00000 0.03069 0.01664 = 0.04165 -0.00316 0.01507 -0.00288 AFIX 43 H8 2 0.405413 0.246021 -0.058118 11.00000 -1.20000 AFIX 0 C9 1 0.363953 0.354159 -0.175948 11.00000 0.02423 0.02807 = 0.03821 -0.01442 0.01195 -0.01065 AFIX 43 H9 2 0.335521 0.302501 -0.213722 11.00000 -1.20000 AFIX 0 C10 1 0.364653 0.463907 -0.212020 11.00000 0.01740 0.02841 = 0.02497 -0.00720 0.00301 0.00084 AFIX 43 H10 2 0.336561 0.486973 -0.275208 11.00000 -1.20000 AFIX 0 C11 1 0.405881 0.540717 -0.157044 11.00000 0.01654 0.02088 = 0.01736 -0.00234 0.00783 0.00056 AFIX 43 H11 2 0.405540 0.616053 -0.182168 11.00000 -1.20000 AFIX 0 C12 1 0.548726 0.922144 0.082554 11.00000 0.01937 0.01305 = 0.02015 -0.00083 0.01505 0.00133 C13 1 0.512029 0.998039 0.012057 11.00000 0.01825 0.01426 = 0.02033 -0.00195 0.01346 -0.00168 AFIX 43 H13 2 0.481670 0.968506 -0.044967 11.00000 -1.20000 AFIX 0 C14 1 0.519979 1.117823 0.025420 11.00000 0.02860 0.01575 = 0.02974 0.00183 0.01951 0.00261 AFIX 43 H14 2 0.495125 1.169401 -0.023101 11.00000 -1.20000 AFIX 0 C15 1 0.563640 1.161586 0.108528 11.00000 0.03689 0.01552 = 0.03972 -0.00624 0.02759 -0.00252 AFIX 43 H15 2 0.569004 1.242967 0.117013 11.00000 -1.20000 AFIX 0 C16 1 0.599760 1.085900 0.179821 11.00000 0.02562 0.02312 = 0.02791 -0.01137 0.01726 -0.01048 AFIX 43 H16 2 0.629664 1.115791 0.237472 11.00000 -1.20000 AFIX 0 C17 1 0.592255 0.965607 0.167024 11.00000 0.02032 0.02189 = 0.01963 -0.00344 0.01308 -0.00592 AFIX 43 H17 2 0.616895 0.914153 0.216033 11.00000 -1.20000 AFIX 0 C18 1 0.641295 0.557540 0.094038 11.00000 0.01508 0.01986 = 0.02136 0.00118 0.00819 -0.00108 C19 1 0.687280 0.594664 0.181857 11.00000 0.01980 0.01901 = 0.02312 -0.00248 0.01088 -0.00005 AFIX 43 H19 2 0.685258 0.657963 0.219111 11.00000 -1.20000 AFIX 0 C20 1 0.735209 0.538583 0.213372 11.00000 0.01918 0.02280 = 0.02957 -0.00220 0.01200 -0.00142 AFIX 43 H20 2 0.765853 0.564315 0.271861 11.00000 -1.20000 AFIX 0 C21 1 0.738755 0.445937 0.160617 11.00000 0.01726 0.02462 = 0.03797 -0.00277 0.01374 0.00160 AFIX 43 H21 2 0.771461 0.406739 0.183663 11.00000 -1.20000 AFIX 0 C22 1 0.694371 0.410288 0.073809 11.00000 0.02264 0.02925 = 0.03618 -0.00914 0.01760 -0.00056 AFIX 43 H22 2 0.697134 0.347993 0.036479 11.00000 -1.20000 AFIX 0 C23 1 0.645994 0.464404 0.040776 11.00000 0.02009 0.02079 = 0.02789 -0.00589 0.01389 -0.00313 AFIX 43 H23 2 0.615844 0.438174 -0.018338 11.00000 -1.20000 AFIX 0 C24 1 0.491035 0.979213 0.260635 11.00000 0.01433 0.01345 = 0.01613 -0.00155 0.00870 -0.00023 C25 1 0.540053 1.017312 0.335857 11.00000 0.01613 0.01940 = 0.01641 -0.00490 0.00826 -0.00503 AFIX 43 H25 2 0.543195 1.096338 0.355299 11.00000 -1.20000 AFIX 0 C26 1 0.585410 0.946662 0.385239 11.00000 0.01179 0.02457 = 0.01148 -0.00400 0.00693 -0.00282 C27 1 0.583668 0.828906 0.363843 11.00000 0.01398 0.02372 = 0.01038 -0.00027 0.00539 -0.00101 AFIX 43 H27 2 0.615033 0.785520 0.402834 11.00000 -1.20000 AFIX 0 C28 1 0.540364 0.768837 0.290811 11.00000 0.01163 0.01443 = 0.01245 0.00067 0.00576 -0.00166 C29 1 0.545141 0.641361 0.280671 11.00000 0.01583 0.01358 = 0.00967 0.00152 0.00365 0.00043 C30 1 0.508297 0.565669 0.280854 11.00000 0.01676 0.01820 = 0.01601 0.00049 0.00841 0.00095 AFIX 43 H30 2 0.478614 0.595189 0.283622 11.00000 -1.20000 AFIX 0 C31 1 0.514598 0.446296 0.276991 11.00000 0.02294 0.01833 = 0.01807 0.00264 0.00831 0.00030 AFIX 43 H31 2 0.489450 0.394602 0.277872 11.00000 -1.20000 AFIX 0 C32 1 0.557504 0.403184 0.271873 11.00000 0.03009 0.01594 = 0.01973 0.00266 0.01098 0.00658 AFIX 43 H32 2 0.561820 0.321905 0.268955 11.00000 -1.20000 AFIX 0 C33 1 0.594055 0.478853 0.271024 11.00000 0.02188 0.01936 = 0.01830 0.00275 0.01002 0.00713 AFIX 43 H33 2 0.623179 0.449343 0.266320 11.00000 -1.20000 AFIX 0 C34 1 0.588529 0.597732 0.276997 11.00000 0.01900 0.02027 = 0.01173 0.00188 0.00646 0.00156 AFIX 43 H34 2 0.614419 0.649099 0.278566 11.00000 -1.20000 AFIX 0 C35 1 0.446181 1.061501 0.221462 11.00000 0.01605 0.01491 = 0.01370 -0.00747 0.00646 -0.00354 C36 1 0.402107 1.036922 0.232115 11.00000 0.02033 0.01820 = 0.02031 -0.00516 0.01059 -0.00294 AFIX 43 H36 2 0.400620 0.966175 0.262066 11.00000 -1.20000 AFIX 0 C37 1 0.360803 1.115042 0.199289 11.00000 0.01588 0.03185 = 0.03601 -0.01103 0.01443 -0.00396 AFIX 43 H37 2 0.331602 1.098772 0.208662 11.00000 -1.20000 AFIX 0 C38 1 0.361779 1.217069 0.152731 11.00000 0.02095 0.02421 = 0.03676 -0.00445 0.00954 0.00655 AFIX 43 H38 2 0.333025 1.269869 0.129064 11.00000 -1.20000 AFIX 0 C39 1 0.404981 1.241587 0.140917 11.00000 0.03174 0.01469 = 0.03705 -0.00016 0.01350 0.00316 AFIX 43 H39 2 0.405800 1.311302 0.109018 11.00000 -1.20000 AFIX 0 C40 1 0.446805 1.164777 0.175468 11.00000 0.02239 0.01460 = 0.03401 -0.00398 0.01638 -0.00365 AFIX 43 H40 2 0.476393 1.182682 0.167734 11.00000 -1.20000 AFIX 0 C41 1 0.635003 0.997847 0.467239 11.00000 0.01329 0.03111 = 0.02312 -0.01250 0.01001 -0.00556 C42 1 0.648593 1.113296 0.460913 11.00000 0.02111 0.02775 = 0.03401 -0.01863 0.01645 -0.00698 AFIX 43 H42 2 0.626717 1.158630 0.403753 11.00000 -1.20000 AFIX 0 C43 1 0.694764 1.161036 0.539773 11.00000 0.02318 0.04044 = 0.04478 -0.02603 0.01947 -0.01320 AFIX 43 H43 2 0.704240 1.238665 0.535190 11.00000 -1.20000 AFIX 0 C44 1 0.726102 1.097587 0.622648 11.00000 0.01771 0.06837 = 0.03619 -0.03582 0.00729 -0.01111 AFIX 43 H44 2 0.756698 1.131639 0.676194 11.00000 -1.20000 AFIX 0 C45 1 0.713306 0.982585 0.628978 11.00000 0.01704 0.06270 = 0.02177 -0.01463 0.00185 0.00114 AFIX 43 H45 2 0.735619 0.937525 0.686027 11.00000 -1.20000 AFIX 0 C46 1 0.667535 0.933922 0.551064 11.00000 0.01563 0.05007 = 0.01810 -0.01127 0.00537 -0.00556 AFIX 43 H46 2 0.658691 0.855817 0.555849 11.00000 -1.20000 AFIX 0 C47 1 0.397484 0.945956 -0.007327 11.00000 0.01396 0.01136 = 0.01991 -0.00323 0.00493 -0.00060 C48 1 0.350427 0.743088 -0.093517 11.00000 0.01846 0.01423 = 0.01995 0.00867 0.01374 0.00853 C49 1 0.401412 0.612415 0.078667 11.00000 0.02182 0.00833 = 0.01183 -0.00316 0.00550 -0.00042 C50 1 0.351078 0.809758 0.082554 11.00000 0.02535 0.01923 = 0.01038 -0.00361 0.00740 -0.01068 N2 3 0.718693 1.256917 0.337460 11.00000 0.10269 0.03705 = 0.06387 -0.00503 0.02964 -0.02096 C53 1 0.751983 1.444730 0.442304 11.00000 0.04576 0.04440 = 0.03756 -0.00526 0.01466 -0.00140 AFIX 137 H53A 2 0.728003 1.508993 0.406511 11.00000 -1.50000 H53B 2 0.787533 1.463199 0.454450 11.00000 -1.50000 H53C 2 0.753096 1.432783 0.506031 11.00000 -1.50000 AFIX 0 C54 1 0.733301 1.340463 0.383263 11.00000 0.04696 0.04290 = 0.04522 0.00783 0.02049 -0.00306 N1 3 0.708050 0.772889 0.379296 11.00000 0.03947 0.05083 = 0.04530 -0.01731 0.02502 -0.01492 C51 1 0.754802 0.972169 0.420008 11.00000 0.04017 0.03168 = 0.05317 -0.01059 0.01971 0.00112 AFIX 137 H51A 2 0.775483 0.978870 0.386002 11.00000 -1.50000 H51B 2 0.778378 0.979000 0.492037 11.00000 -1.50000 H51C 2 0.728314 1.034109 0.397201 11.00000 -1.50000 AFIX 0 C52 1 0.728383 0.859957 0.397382 11.00000 0.01949 0.04003 = 0.02812 -0.00384 0.00932 0.00522 HKLF 4 REM cc in Cc #9 REM R1 = 0.0293 for 9315 Fo > 4sig(Fo) and 0.0332 for all 9939 data REM 571 parameters refined using 2 restraints END WGHT 0.0361 1.1398 REM Highest difference peak 3.971, deepest hole -0.765, 1-sigma level 0.111 Q1 1 0.4017 0.7797 0.1034 11.00000 0.05 3.97 Q2 1 0.4039 0.7797 -0.0240 11.00000 0.05 3.74 Q3 1 0.4034 0.7809 0.1747 11.00000 0.05 1.65 Q4 1 0.4016 0.7818 -0.0960 11.00000 0.05 1.59 Q5 1 0.4807 0.8405 0.0787 11.00000 0.05 0.64 Q6 1 0.4400 0.8331 0.0466 11.00000 0.05 0.49 Q7 1 0.4808 0.7274 0.1534 11.00000 0.05 0.47 Q8 1 0.3401 0.7318 -0.1860 11.00000 0.05 0.44 Q9 1 0.4002 0.9147 0.0421 11.00000 0.05 0.43 Q10 1 0.4805 0.8325 0.1480 11.00000 0.05 0.40 Q11 1 0.3995 0.5383 -0.0197 11.00000 0.05 0.38 Q12 1 0.4202 0.5393 0.1154 11.00000 0.05 0.38 Q13 1 0.5398 0.7759 0.1217 11.00000 0.05 0.38 Q14 1 0.4011 0.7784 -0.1608 11.00000 0.05 0.38 Q15 1 0.4786 0.7149 0.2809 11.00000 0.05 0.37 Q16 1 0.3412 0.8412 0.1558 11.00000 0.05 0.37 Q17 1 0.4048 0.6763 0.0844 11.00000 0.05 0.35 Q18 1 0.4363 0.7289 0.0452 11.00000 0.05 0.35 Q19 1 0.7998 0.4816 0.3060 11.00000 0.05 0.35 Q20 1 0.4839 0.7232 0.0805 11.00000 0.05 0.33 ; _shelx_res_checksum 20645 _shelx_hkl_file ; -4 0 0 285.32 15.69 -4 0 0 283.28 15.69 4 0 0 281.88 15.69 4 0 0 282.93 15.68 -6 0 0 757.53 39.40 6 0 0 670.23 39.38 6 0 0 672.68 39.38 -6 0 0 752.42 39.40 8 0 0 60.15 3.52 8 0 0 59.47 3.52 -10 0 0 282.81 15.04 10 0 0 256.84 15.00 10 0 0 259.88 15.01 -10 0 0 273.08 15.02 -12 0 0 428.02 23.04 12 0 0 397.22 23.00 -12 0 0 435.63 23.04 12 0 0 390.40 23.00 -14 0 0 192.95 10.65 -14 0 0 191.05 10.86 14 0 0 176.36 10.59 -14 0 0 189.86 10.64 14 0 0 180.49 10.61 16 0 0 225.39 12.90 16 0 0 228.80 12.93 18 0 0 111.07 6.24 -18 0 0 91.97 6.05 18 0 0 109.28 6.26 20 0 0 100.69 6.12 20 0 0 100.88 6.15 22 0 0 230.70 13.35 22 0 0 233.15 13.40 24 0 0 102.61 6.84 24 0 0 108.42 6.56 26 0 0 120.75 7.32 26 0 0 114.82 7.34 28 0 0 133.70 8.38 28 0 0 136.72 8.43 30 0 0 65.29 4.77 30 0 0 62.42 4.85 32 0 0 29.91 3.51 32 0 0 32.06 3.67 -3 -1 0 0.60 0.14 3 -1 0 0.21 0.12 3 -1 0 0.31 0.13 3 -1 0 0.12 0.05 3 -1 0 0.27 0.12 3 1 0 0.36 0.12 3 1 0 0.18 0.11 -3 1 0 0.62 0.15 5 -1 0 2.79 0.37 -5 -1 0 1.88 0.29 5 -1 0 2.64 0.32 5 -1 0 2.60 0.32 5 1 0 2.55 0.33 -5 1 0 2.21 0.22 5 1 0 2.56 0.32 -5 1 0 2.06 0.33 7 -1 0 3.64 0.45 7 -1 0 3.60 0.46 -7 -1 0 4.24 0.46 -7 -1 0 4.06 0.47 -7 1 0 3.64 0.48 -7 1 0 3.91 0.55 -7 1 0 4.04 0.36 -7 1 0 4.59 0.49 7 1 0 3.53 0.47 7 1 0 2.95 0.44 -9 -1 0 4.79 0.58 -9 -1 0 4.66 0.55 9 -1 0 2.46 0.47 -9 1 0 4.45 0.67 -9 1 0 4.45 0.57 9 1 0 3.28 0.51 9 1 0 2.99 0.47 -9 1 0 5.07 0.60 -11 -1 0 4.03 0.62 -11 -1 0 4.87 0.68 11 -1 0 4.88 0.70 11 -1 0 4.84 0.67 11 1 0 4.95 0.67 -11 1 0 4.14 0.52 -11 1 0 5.34 0.74 11 1 0 5.05 0.72 -11 1 0 5.01 0.73 -11 1 0 4.69 0.77 -13 -1 0 16.21 1.39 13 -1 0 14.61 1.33 -13 -1 0 17.25 1.43 13 -1 0 17.58 1.35 -13 1 0 17.52 1.43 -13 1 0 18.62 1.20 13 1 0 14.43 1.33 -13 1 0 18.55 1.63 13 1 0 15.61 1.35 -13 1 0 17.39 1.40 -15 -1 0 6.83 0.96 -15 -1 0 5.36 1.28 15 -1 0 4.96 0.79 15 -1 0 6.44 0.98 -15 1 0 8.27 0.81 -15 1 0 7.15 1.12 15 1 0 4.52 0.79 15 1 0 4.30 0.81 -15 1 0 6.26 0.90 17 -1 0 12.38 1.30 17 -1 0 12.99 1.27 17 1 0 12.36 1.35 -17 1 0 10.36 1.09 17 1 0 10.36 1.24 19 -1 0 3.64 0.87 19 -1 0 4.88 0.91 19 1 0 4.50 0.96 -19 1 0 5.78 0.80 19 1 0 4.48 0.93 21 -1 0 4.09 0.94 21 -1 0 4.23 0.99 -21 1 0 3.71 0.88 21 1 0 3.51 1.00 21 1 0 3.69 0.98 23 -1 0 6.76 1.23 23 -1 0 7.93 1.30 -23 1 0 9.77 1.22 23 1 0 7.18 1.36 23 1 0 7.75 1.29 25 -1 0 2.18 1.16 25 -1 0 1.66 1.39 25 1 0 0.91 1.20 27 -1 0 2.22 1.28 27 -1 0 2.99 1.34 27 1 0 0.60 1.36 27 1 0 2.09 1.36 29 -1 0 2.96 1.56 29 -1 0 1.94 1.40 29 1 0 2.04 1.52 29 1 0 2.58 1.67 31 -1 0 2.28 1.69 31 -1 0 -1.04 1.70 31 1 0 6.72 2.03 31 1 0 2.57 1.75 33 -1 0 -1.65 1.99 33 -1 0 -0.32 1.83 -33 -1 0 -1.19 2.04 33 1 0 1.42 1.98 33 1 0 -0.03 2.12 0 -2 0 11.33 0.78 0 -2 0 11.52 0.81 0 -2 0 11.34 0.78 0 2 0 11.94 0.79 2 -2 0 400.88 21.82 -2 -2 0 402.92 21.83 2 -2 0 387.77 21.82 -2 2 0 386.91 21.87 -2 2 0 382.36 21.91 -2 2 0 424.40 21.83 2 2 0 390.75 21.84 2 2 0 379.58 21.82 -4 -2 0 123.29 6.52 -4 -2 0 120.40 6.55 4 -2 0 106.38 6.50 4 -2 0 110.96 6.50 4 -2 0 109.19 6.52 -4 -2 0 118.69 6.54 -4 2 0 121.71 6.53 4 2 0 111.54 6.52 -4 2 0 122.58 6.55 4 2 0 110.09 6.52 -6 -2 0 47.79 2.54 6 -2 0 36.23 2.49 -6 -2 0 49.50 2.54 6 -2 0 35.89 2.52 6 -2 0 36.67 2.51 -6 2 0 49.09 2.58 -6 2 0 47.59 2.58 -6 2 0 47.93 2.55 6 2 0 36.45 2.51 6 2 0 36.93 2.52 -8 -2 0 73.89 4.28 -8 -2 0 75.12 4.28 -8 2 0 73.07 4.30 -8 2 0 72.12 4.13 -8 2 0 73.88 4.36 -8 2 0 74.32 4.32 -10 -2 0 154.58 9.05 -10 -2 0 160.75 9.08 10 -2 0 159.98 9.08 10 -2 0 159.34 9.08 -10 2 0 162.70 9.20 10 2 0 159.04 9.11 -10 2 0 162.86 9.13 -10 2 0 168.51 8.93 10 2 0 154.25 9.12 -10 2 0 159.98 9.10 -12 -2 0 152.37 8.55 12 -2 0 143.81 8.53 12 -2 0 143.31 8.53 -12 -2 0 151.57 8.54 -12 2 0 157.16 8.73 -12 2 0 151.10 8.58 12 2 0 141.66 8.58 12 2 0 142.73 8.57 -12 2 0 153.64 8.62 -12 2 0 157.55 8.37 -14 -2 0 269.19 15.55 14 -2 0 289.10 15.57 14 -2 0 285.57 15.57 -14 -2 0 274.75 15.56 -14 2 0 268.09 15.58 -14 2 0 253.96 15.58 -14 2 0 281.63 15.35 -14 2 0 275.08 15.75 14 2 0 281.93 15.60 14 2 0 280.74 15.61 16 -2 0 183.54 10.06 16 -2 0 180.51 10.05 16 2 0 172.89 10.08 16 2 0 175.24 10.07 -16 2 0 159.75 9.77 18 -2 0 106.45 6.08 18 -2 0 105.16 6.06 18 2 0 102.71 6.10 18 2 0 98.18 6.10 -18 2 0 89.84 5.75 20 -2 0 94.70 5.61 20 -2 0 94.09 5.59 20 2 0 92.09 5.65 -20 2 0 79.27 5.26 20 2 0 92.40 5.67 22 -2 0 49.73 3.54 22 -2 0 51.18 3.61 22 2 0 51.62 3.68 22 2 0 55.67 3.77 24 -2 0 95.67 5.93 24 -2 0 90.40 5.99 24 2 0 98.20 6.06 24 2 0 89.84 7.11 26 -2 0 50.00 3.87 26 -2 0 53.14 3.83 26 2 0 55.16 4.04 26 2 0 53.13 4.11 28 -2 0 58.86 4.26 28 -2 0 55.45 4.16 28 2 0 56.92 4.47 28 2 0 52.91 4.28 30 -2 0 42.96 3.68 -30 -2 0 34.08 4.10 30 -2 0 49.84 3.84 30 2 0 44.31 4.04 30 2 0 43.33 3.91 32 -2 0 36.47 3.89 -32 -2 0 38.12 4.48 32 -2 0 38.24 3.82 32 2 0 44.70 4.41 32 2 0 47.78 4.21 -1 -3 0 118.53 6.88 1 -3 0 124.38 6.88 -1 -3 0 125.78 6.91 1 -3 0 120.29 6.86 1 3 0 126.20 6.92 -1 3 0 118.12 6.86 -1 3 0 115.61 6.86 1 3 0 124.50 6.88 -3 -3 0 80.19 4.65 3 -3 0 75.44 4.61 -3 -3 0 87.87 4.67 3 -3 0 77.20 4.62 -3 -3 0 86.10 4.67 3 -3 0 78.29 4.66 -3 3 0 83.17 4.68 3 3 0 76.70 4.65 -3 3 0 83.39 4.63 3 3 0 77.91 4.62 5 -3 0 24.71 1.55 5 -3 0 23.94 1.39 5 -3 0 23.96 1.54 -5 -3 0 23.61 1.56 5 -3 0 23.18 1.56 -5 -3 0 23.83 1.55 -5 -3 0 21.56 1.56 -5 3 0 24.75 1.56 -5 3 0 25.00 1.56 -5 3 0 24.09 1.60 5 3 0 24.42 1.58 5 3 0 23.82 1.58 7 -3 0 22.53 1.43 7 -3 0 22.31 1.43 -7 -3 0 18.21 1.44 -7 -3 0 20.14 1.40 -7 -3 0 19.47 1.39 7 -3 0 23.24 1.43 7 3 0 21.59 1.45 -7 3 0 19.27 1.40 -7 3 0 20.07 1.45 7 3 0 20.91 1.45 -7 3 0 20.93 1.44 9 -3 0 32.86 1.89 -9 -3 0 24.87 1.82 -9 -3 0 26.13 1.95 9 -3 0 32.13 1.92 -9 -3 0 25.97 1.84 9 -3 0 31.11 1.91 9 3 0 34.48 1.98 -9 3 0 24.61 1.85 -9 3 0 26.51 1.91 -9 3 0 26.62 1.92 11 -3 0 9.90 0.98 11 -3 0 9.84 1.00 -11 -3 0 12.81 1.03 -11 -3 0 9.52 0.99 11 3 0 10.28 1.07 -11 3 0 10.88 1.04 -11 3 0 12.19 1.11 11 3 0 9.74 1.07 -11 3 0 10.18 1.14 -13 -3 0 36.48 2.57 13 -3 0 45.01 2.67 -13 -3 0 36.83 2.59 13 -3 0 42.85 2.65 -13 3 0 39.65 2.79 -13 3 0 39.92 2.35 13 3 0 42.43 2.74 -13 3 0 36.76 2.70 13 3 0 43.53 2.73 -13 3 0 40.48 2.68 15 -3 0 33.69 2.36 15 -3 0 32.57 2.33 -15 3 0 32.06 2.59 15 3 0 34.91 2.43 15 3 0 34.73 2.50 -15 3 0 34.36 2.65 -15 3 0 34.44 2.05 17 -3 0 35.51 2.55 17 -3 0 37.87 2.52 17 3 0 32.58 2.61 -17 3 0 36.66 2.19 17 3 0 33.47 2.60 19 -3 0 32.81 2.47 19 -3 0 34.02 2.47 -19 3 0 28.80 2.05 19 3 0 32.41 2.56 19 3 0 31.50 2.53 21 -3 0 31.23 2.48 21 -3 0 32.58 2.57 -21 3 0 30.94 2.14 21 3 0 29.11 2.66 21 3 0 31.72 2.65 23 -3 0 8.77 1.87 23 -3 0 11.34 1.55 23 3 0 10.09 1.61 23 3 0 11.68 1.70 -25 -3 0 39.69 3.47 25 -3 0 37.63 3.06 25 -3 0 34.17 2.93 25 3 0 36.44 3.27 25 3 0 34.47 3.20 -27 -3 0 17.96 2.85 27 -3 0 17.18 2.38 27 -3 0 15.04 2.29 27 3 0 17.47 2.33 27 3 0 14.64 2.21 29 -3 0 14.72 2.25 29 -3 0 13.69 2.07 -29 -3 0 19.10 3.08 29 3 0 14.46 2.38 29 3 0 16.60 2.45 31 -3 0 19.43 2.98 31 -3 0 20.30 2.82 -31 -3 0 14.29 2.85 31 3 0 16.88 2.68 31 3 0 18.41 2.70 33 -3 0 7.99 2.60 33 -3 0 4.69 2.13 -33 -3 0 7.50 2.68 33 3 0 6.23 2.54 33 3 0 8.60 2.54 0 -4 0 280.08 15.85 0 -4 0 278.65 15.85 0 -4 0 293.38 15.91 0 4 0 283.63 15.83 2 -4 0 210.90 12.26 2 -4 0 207.13 12.27 2 -4 0 207.20 12.31 -2 -4 0 223.48 12.30 -2 -4 0 232.49 12.33 2 4 0 215.39 12.31 -2 4 0 224.51 12.26 -2 4 0 228.28 12.27 2 4 0 219.52 12.26 4 -4 0 113.50 6.66 4 -4 0 112.90 6.67 -4 -4 0 120.36 6.72 -4 -4 0 111.92 6.70 -4 -4 0 122.16 6.72 -4 4 0 121.39 6.68 -4 4 0 118.90 6.68 4 4 0 110.87 6.71 4 4 0 118.48 6.68 -6 -4 0 124.18 6.97 6 -4 0 119.95 6.95 -6 -4 0 126.84 6.97 6 -4 0 115.24 6.92 -6 -4 0 120.11 6.99 6 -4 0 119.38 6.74 6 -4 0 115.93 6.97 6 4 0 110.44 7.09 -6 4 0 127.78 6.96 -6 4 0 123.54 7.02 -6 4 0 128.19 6.97 8 -4 0 119.97 7.29 8 -4 0 118.32 7.26 -8 -4 0 135.50 7.30 8 -4 0 110.56 7.24 -8 -4 0 136.68 7.39 -8 -4 0 134.74 7.29 -8 4 0 136.70 7.33 8 4 0 118.48 7.32 -8 4 0 128.20 7.35 -8 4 0 133.13 7.30 8 4 0 121.49 7.33 10 -4 0 146.45 8.05 10 -4 0 143.79 8.01 10 -4 0 136.55 8.02 -10 -4 0 139.40 8.01 -10 -4 0 135.86 8.12 -10 -4 0 136.36 7.99 -10 4 0 136.44 8.02 10 4 0 147.43 8.11 10 4 0 142.24 8.10 -10 4 0 133.02 8.07 -10 4 0 135.88 8.06 -12 -4 0 90.81 5.50 12 -4 0 88.23 5.57 12 -4 0 88.38 5.53 12 -4 0 87.88 5.50 -12 -4 0 99.02 5.56 -12 -4 0 99.82 5.73 12 4 0 92.93 5.62 -12 4 0 95.49 5.65 -12 4 0 95.91 5.75 -12 4 0 97.66 5.59 12 4 0 92.31 5.62 -14 -4 0 83.82 5.20 14 -4 0 85.00 5.00 14 -4 0 80.85 5.00 14 4 0 83.05 5.09 14 4 0 82.43 5.12 -14 4 0 79.28 5.04 -14 4 0 84.69 5.17 -16 -4 0 79.49 4.96 16 -4 0 75.29 4.69 16 -4 0 73.60 4.68 16 4 0 76.30 4.87 16 4 0 75.84 4.82 -18 -4 0 32.17 2.86 18 -4 0 38.19 2.73 18 -4 0 39.36 2.73 18 4 0 37.03 2.90 18 4 0 40.14 2.90 20 -4 0 45.81 3.24 -20 -4 0 48.49 3.52 20 -4 0 42.37 3.15 20 4 0 42.85 3.42 20 4 0 44.81 3.34 22 -4 0 42.17 3.26 22 -4 0 44.16 3.22 -22 -4 0 51.96 3.71 22 4 0 38.25 3.42 22 4 0 39.26 3.42 24 -4 0 36.80 2.97 24 -4 0 36.82 2.94 -24 -4 0 28.05 3.25 24 4 0 30.82 3.15 24 4 0 36.23 3.22 26 -4 0 29.75 2.94 -26 -4 0 36.35 3.45 26 -4 0 29.01 3.05 26 4 0 29.96 3.22 26 4 0 30.00 3.31 28 -4 0 11.23 1.97 -28 -4 0 6.45 2.28 28 -4 0 14.00 1.95 28 4 0 13.29 2.28 28 4 0 11.14 2.23 30 -4 0 43.34 3.87 -30 -4 0 37.81 4.43 30 -4 0 41.25 3.76 30 4 0 38.18 4.12 30 4 0 39.39 4.35 32 -4 0 13.38 2.47 -32 -4 0 15.58 3.07 32 -4 0 14.07 2.60 32 4 0 22.46 3.12 32 4 0 17.19 2.94 -1 -5 0 210.68 12.63 -1 -5 0 220.03 12.69 1 -5 0 237.71 12.67 1 -5 0 225.65 12.63 1 -5 0 245.78 12.74 -1 -5 0 202.97 12.62 1 5 0 239.09 12.63 -1 5 0 212.57 12.60 3 -5 0 101.00 5.61 -3 -5 0 86.51 5.52 3 -5 0 102.57 5.56 -3 -5 0 87.81 5.53 3 -5 0 97.94 5.51 -3 5 0 91.69 5.49 3 5 0 88.73 5.69 3 5 0 101.96 5.52 -3 5 0 91.42 5.48 5 -5 0 71.70 4.42 -5 -5 0 78.35 4.48 -5 -5 0 79.75 4.48 5 -5 0 70.19 4.46 5 -5 0 68.69 4.37 -5 5 0 78.99 4.42 5 5 0 70.78 4.48 5 5 0 70.62 4.40 -5 5 0 78.85 4.43 7 -5 0 153.80 8.75 -7 -5 0 153.31 9.06 -7 -5 0 157.36 9.01 7 -5 0 158.98 9.05 7 -5 0 157.02 9.00 -7 -5 0 160.01 9.02 7 -5 0 148.44 8.95 -7 5 0 161.70 9.10 -7 5 0 164.33 9.02 -7 5 0 157.33 9.00 7 5 0 156.82 9.07 9 -5 0 66.43 4.30 -9 -5 0 74.55 4.37 -9 -5 0 73.21 4.46 9 -5 0 71.68 4.35 -9 -5 0 71.86 4.34 9 -5 0 69.47 4.36 -9 5 0 74.14 4.38 9 5 0 71.91 4.43 -9 5 0 72.90 4.38 -9 5 0 71.16 4.44 11 -5 0 132.96 7.37 11 -5 0 133.17 7.33 11 -5 0 126.86 7.32 -11 -5 0 120.87 7.43 -11 -5 0 117.83 7.29 11 5 0 128.69 7.43 11 5 0 123.63 7.40 -11 5 0 123.88 7.36 -11 5 0 119.14 7.30 -13 -5 0 95.00 5.66 13 -5 0 90.92 5.42 13 -5 0 87.76 5.44 13 -5 0 84.42 5.45 13 5 0 90.35 5.55 -13 5 0 90.00 5.49 13 5 0 86.67 5.54 -13 5 0 95.57 5.56 15 -5 0 68.86 4.49 15 -5 0 72.01 4.41 15 -5 0 70.37 4.41 15 5 0 71.00 4.59 15 5 0 68.77 4.52 -17 -5 0 90.20 5.82 17 -5 0 89.60 5.54 17 -5 0 89.49 5.53 17 5 0 91.30 5.71 17 5 0 90.28 5.73 19 -5 0 49.82 3.37 -19 -5 0 48.03 3.70 19 -5 0 46.57 3.34 19 5 0 46.71 3.60 19 5 0 47.40 3.53 -21 -5 0 67.25 4.91 21 -5 0 74.00 4.64 21 -5 0 67.89 4.59 21 5 0 70.60 4.84 21 5 0 65.40 4.88 23 -5 0 71.63 4.75 -23 -5 0 68.56 5.11 23 -5 0 76.71 4.79 23 5 0 66.74 6.33 23 5 0 60.44 4.84 -25 -5 0 23.56 3.10 25 -5 0 27.17 2.74 25 -5 0 26.95 2.70 25 5 0 22.56 3.13 25 5 0 21.29 2.96 27 -5 0 27.09 2.90 27 -5 0 25.58 3.01 -27 -5 0 29.91 3.61 27 5 0 27.82 3.45 27 5 0 28.47 3.61 29 -5 0 31.36 3.30 -29 -5 0 36.15 4.03 29 -5 0 36.27 3.56 29 5 0 33.85 3.92 29 5 0 27.88 4.04 31 -5 0 25.45 3.43 31 -5 0 21.96 3.04 -31 -5 0 31.64 4.40 31 5 0 27.63 3.56 31 5 0 27.45 4.02 0 -6 0 40.75 2.79 0 -6 0 43.78 2.84 0 -6 0 44.60 2.92 0 6 0 46.07 2.79 -2 -6 0 4.72 0.73 -2 -6 0 4.36 0.76 2 -6 0 3.39 0.78 2 -6 0 3.99 0.77 -2 -6 0 3.84 0.69 2 -6 0 4.46 0.69 2 -6 0 5.10 0.78 -2 6 0 4.37 0.69 2 6 0 4.87 0.70 -4 -6 0 24.02 1.78 4 -6 0 22.10 1.74 4 -6 0 21.33 1.63 -4 -6 0 22.69 1.74 4 -6 0 21.87 1.70 -4 6 0 22.20 1.65 -4 6 0 21.67 1.64 4 6 0 22.11 1.76 4 6 0 21.31 1.63 -6 -6 0 33.17 2.21 -6 -6 0 30.25 2.18 6 -6 0 29.21 2.17 -6 -6 0 33.20 2.24 6 -6 0 28.35 2.12 6 -6 0 26.30 2.04 -6 6 0 32.07 2.12 6 6 0 30.42 2.23 -6 6 0 32.05 2.12 6 6 0 28.63 2.09 8 -6 0 25.52 1.53 8 -6 0 24.03 1.89 -8 -6 0 22.54 1.93 -8 -6 0 21.48 1.87 8 -6 0 26.08 1.89 -8 6 0 26.38 1.92 8 6 0 27.00 2.01 -8 6 0 23.97 1.88 10 -6 0 29.09 2.13 -10 -6 0 27.99 2.19 10 -6 0 27.05 2.03 10 -6 0 29.03 2.08 10 6 0 28.87 2.20 -10 6 0 24.99 2.10 -10 6 0 26.08 2.13 12 -6 0 22.26 1.80 -12 -6 0 18.93 1.94 12 -6 0 23.19 1.83 12 -6 0 23.42 1.84 12 6 0 24.62 2.02 -12 6 0 19.15 1.95 -12 6 0 16.98 2.07 -14 -6 0 14.37 1.73 14 -6 0 12.90 1.52 14 -6 0 14.88 1.50 14 -6 0 12.58 1.44 14 6 0 14.29 1.70 14 6 0 14.98 1.77 -14 6 0 11.79 1.76 16 -6 0 22.20 1.99 -16 -6 0 23.86 2.30 16 -6 0 20.61 1.95 16 -6 0 21.61 2.13 16 6 0 22.68 2.30 16 6 0 25.30 2.28 18 -6 0 12.43 1.62 -18 -6 0 14.06 2.08 18 -6 0 13.59 1.73 18 6 0 14.44 2.02 18 6 0 13.96 1.99 -20 -6 0 22.51 2.68 20 -6 0 21.72 2.19 20 -6 0 21.69 2.22 20 6 0 20.38 2.62 20 6 0 25.00 2.61 -22 -6 0 18.45 2.67 22 -6 0 20.47 2.27 22 -6 0 16.73 2.23 22 6 0 18.39 2.61 24 -6 0 7.91 1.70 -24 -6 0 7.60 1.99 24 -6 0 10.37 1.73 24 6 0 6.06 2.06 24 6 0 8.79 1.94 -26 -6 0 3.37 1.99 26 -6 0 8.76 1.81 26 -6 0 6.80 1.75 26 6 0 4.28 2.11 26 6 0 2.17 1.91 28 -6 0 6.25 1.93 28 -6 0 6.65 1.98 -28 -6 0 6.68 2.44 28 6 0 6.74 2.42 28 6 0 7.62 2.27 -30 -6 0 5.28 2.57 30 -6 0 0.45 2.08 30 -6 0 2.80 2.00 30 6 0 8.91 2.71 30 6 0 5.87 2.40 1 -7 0 110.82 7.40 1 -7 0 118.27 7.43 1 -7 0 120.68 7.53 -1 -7 0 138.22 7.56 -1 -7 0 140.21 7.51 -1 -7 0 138.22 7.50 1 7 0 112.88 7.33 -1 7 0 135.75 7.40 3 -7 0 153.80 9.40 -3 -7 0 170.36 9.35 3 -7 0 154.38 9.29 -3 -7 0 171.91 9.36 3 -7 0 150.88 9.36 -3 -7 0 167.37 9.37 -3 7 0 168.97 9.25 3 7 0 145.68 9.20 5 -7 0 292.38 18.00 -5 -7 0 335.47 17.99 5 -7 0 311.45 17.97 5 -7 0 315.99 17.90 -5 -7 0 321.10 17.94 -5 7 0 321.64 17.85 -5 7 0 323.92 17.85 5 7 0 323.65 17.98 5 7 0 306.66 17.85 7 -7 0 264.98 15.25 7 -7 0 267.51 14.90 -7 -7 0 259.39 15.26 7 -7 0 278.12 15.17 7 -7 0 270.09 15.19 -7 7 0 263.83 15.16 7 7 0 278.81 15.31 -7 7 0 257.09 15.14 9 -7 0 111.54 6.11 9 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24.41 3.42 27 7 0 29.91 3.62 29 -7 0 31.74 3.70 -29 -7 0 37.35 4.68 29 -7 0 23.62 3.67 29 7 0 24.13 3.71 29 7 0 25.74 3.54 0 -8 0 0.80 0.68 0 -8 0 0.17 0.65 0 8 0 0.66 0.66 2 -8 0 0.62 0.64 2 -8 0 0.28 0.68 -2 -8 0 1.08 0.73 -2 -8 0 0.90 0.68 2 -8 0 0.95 0.65 2 8 0 0.66 0.66 -2 8 0 -0.35 0.65 4 -8 0 0.69 0.69 -4 -8 0 0.85 0.69 -4 -8 0 0.95 0.73 4 -8 0 0.44 0.71 4 -8 0 0.18 0.69 4 8 0 0.02 0.63 -4 8 0 0.93 0.70 6 -8 0 1.15 0.70 -6 -8 0 0.06 0.73 6 -8 0 0.29 0.71 6 -8 0 1.02 0.74 6 8 0 0.45 0.80 -6 8 0 2.24 0.82 -6 8 0 1.68 0.78 8 -8 0 2.92 0.79 8 -8 0 2.96 0.86 8 -8 0 1.65 0.81 -8 -8 0 2.04 0.91 8 -8 0 2.94 0.54 -8 8 0 0.99 0.86 8 8 0 2.25 0.94 10 -8 0 0.15 0.41 10 -8 0 0.60 0.75 10 -8 0 0.67 0.76 10 -8 0 0.67 0.72 -10 -8 0 0.83 0.88 10 8 0 -0.35 0.90 -10 8 0 0.85 0.95 -12 -8 0 2.77 1.08 12 -8 0 2.18 0.94 12 -8 0 1.11 0.81 12 -8 0 2.03 0.89 -12 8 0 0.27 1.09 12 8 0 3.70 1.10 14 -8 0 3.09 1.00 14 -8 0 0.44 0.93 14 -8 0 0.86 0.92 -14 -8 0 1.72 1.10 14 8 0 2.80 1.15 16 -8 0 3.07 1.08 16 -8 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144.87 9.38 -7 -9 0 170.25 9.47 -7 9 0 162.05 9.30 9 -9 0 268.20 14.77 9 -9 0 258.56 14.90 9 -9 0 269.69 14.87 -9 -9 0 248.02 14.97 9 -9 0 260.60 14.42 -9 9 0 233.32 14.72 9 9 0 265.71 14.97 11 -9 0 34.60 2.20 11 -9 0 38.23 2.88 11 -9 0 34.25 2.78 11 -9 0 34.73 2.82 11 9 0 35.87 3.05 13 -9 0 60.97 4.01 -13 -9 0 47.08 4.15 13 -9 0 61.13 4.09 13 -9 0 57.39 4.02 13 9 0 61.14 4.32 -15 -9 0 55.26 4.30 15 -9 0 56.43 4.01 15 9 0 60.62 4.36 17 -9 0 79.96 5.27 17 -9 0 78.16 5.19 17 -9 0 77.21 5.25 17 9 0 76.97 5.58 -19 -9 0 108.22 7.24 19 -9 0 99.95 6.66 19 -9 0 106.21 6.73 21 -9 0 104.15 6.66 -21 -9 0 85.24 7.10 21 -9 0 108.33 6.68 21 9 0 107.62 7.23 23 -9 0 56.80 4.27 -23 -9 0 40.47 4.90 23 -9 0 58.45 4.39 23 9 0 59.41 5.06 25 -9 0 36.05 3.83 25 -9 0 43.74 3.81 -25 -9 0 28.38 4.52 25 9 0 34.87 4.76 -27 -9 0 13.30 3.26 27 -9 0 12.42 2.62 27 -9 0 8.12 2.32 27 9 0 15.23 3.39 0 -10 0 1.19 0.95 0 -10 0 0.69 0.95 0 -10 0 0.35 0.95 -2 -10 0 6.46 1.32 2 -10 0 7.68 1.36 2 -10 0 7.00 1.33 -2 -10 0 6.55 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43.58 3.98 -19 -11 0 50.08 4.81 19 11 0 43.37 4.67 -21 -11 0 32.18 4.37 21 -11 0 29.63 3.65 21 -11 0 28.54 3.51 21 11 0 28.94 3.81 23 -11 0 29.35 3.79 -23 -11 0 36.92 4.97 23 -11 0 31.32 3.89 23 11 0 38.05 5.22 0 -12 0 25.83 2.87 0 -12 0 24.46 2.82 0 -12 0 24.28 2.85 2 -12 0 34.55 3.35 2 -12 0 30.53 3.44 -2 -12 0 42.10 3.55 -2 -12 0 39.33 3.43 2 -12 0 39.64 3.40 -4 -12 0 47.03 3.75 4 -12 0 41.74 3.62 4 -12 0 39.13 3.71 -4 -12 0 41.69 3.73 4 -12 0 40.32 3.54 -6 -12 0 52.57 4.17 -6 -12 0 50.90 4.28 6 -12 0 52.79 4.19 6 -12 0 54.12 3.99 6 -12 0 47.52 4.12 -8 -12 0 63.59 4.67 -8 -12 0 59.64 4.49 8 -12 0 55.61 3.78 8 -12 0 56.46 4.20 8 -12 0 55.29 4.34 8 -12 0 52.87 4.41 10 -12 0 25.28 2.88 -10 -12 0 22.42 3.20 -10 -12 0 24.38 3.09 10 -12 0 28.84 2.87 10 -12 0 26.80 3.08 12 -12 0 24.56 2.98 -12 -12 0 24.60 3.24 -12 -12 0 29.58 3.40 12 -12 0 23.50 2.89 12 -12 0 28.36 3.04 -14 -12 0 18.17 2.80 -14 -12 0 16.54 2.50 14 -12 0 17.06 2.61 14 -12 0 13.47 2.26 14 -12 0 10.30 2.13 16 -12 0 37.29 3.58 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1.57 19 3 -4 18.52 1.67 19 3 -4 17.26 1.65 -19 3 4 23.12 1.59 17 -3 -4 23.08 1.79 -17 -3 4 24.90 1.74 17 -3 -4 23.10 1.74 17 -3 -4 22.72 1.98 -17 -3 4 24.77 1.80 17 -3 -4 22.89 1.61 -17 3 4 24.37 1.89 17 3 -4 20.86 1.78 -17 3 4 27.02 1.73 17 3 -4 22.13 1.78 15 -3 -4 22.00 1.44 -15 -3 4 19.56 1.63 15 -3 -4 22.65 1.81 -15 -3 4 20.55 1.55 -15 -3 4 17.59 1.78 15 -3 -4 23.02 1.57 15 -3 -4 23.37 1.63 -15 -3 4 18.97 1.49 -15 3 4 22.27 1.53 -15 3 4 19.68 1.63 -15 3 4 19.17 1.85 15 3 -4 23.23 1.59 -15 3 4 17.72 1.66 15 3 -4 22.67 1.61 -13 -3 4 32.78 2.22 13 -3 -4 24.48 2.10 -13 -3 4 34.80 2.12 -13 -3 4 34.52 2.12 -13 -3 4 31.72 2.36 -13 3 4 35.41 2.23 -13 3 4 34.39 2.11 -13 3 4 36.56 2.47 -13 3 4 36.64 2.29 -11 -3 4 54.51 3.12 -11 -3 4 54.32 3.12 -11 -3 4 53.05 3.32 -11 -3 4 54.05 3.24 11 -3 -4 52.12 3.21 11 -3 -4 52.32 3.37 11 -3 -4 51.37 3.17 11 -3 -4 51.06 3.12 -11 3 4 52.05 3.25 -11 3 4 51.79 3.39 -11 3 4 53.02 3.14 -11 3 4 55.58 3.24 11 3 -4 51.08 3.17 11 3 -4 51.05 3.10 -9 -3 4 114.78 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2 20 21.16 3.00 12 -2 -20 12.25 2.83 12 -2 -20 11.82 2.47 -12 2 20 11.67 3.28 12 2 -20 10.73 2.34 23 -3 -20 11.19 2.25 23 -3 -20 5.22 2.78 23 3 -20 8.99 2.21 21 -3 -20 9.82 2.19 21 -3 -20 7.48 2.68 21 3 -20 10.37 2.19 19 -3 -20 19.06 2.62 19 -3 -20 10.90 3.02 19 3 -20 13.08 2.34 17 -3 -20 17.19 2.62 17 -3 -20 19.30 3.29 17 3 -20 18.63 2.63 15 -3 -20 6.49 2.73 15 -3 -20 5.46 2.09 15 3 -20 7.34 2.09 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 471 _olex2_submission_special_instructions 'No special instructions were received' #============================================================================== _publ_requested_journal 'Chemistry - A European 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 ; 'Wiecko, Jelena' ; 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 ; ; _publ_section_abstract ; ... and following paragraphs: see the published paper. ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _publ_section_figure_captions ; ; #END==================================================== ;