# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Manfred Scheer' 'Shining Deng.' 'Christiane Eichhorn' 'Otto Scherer' 'Christoph Schwarzmaier' 'Gotthelf Wolmershauser' 'Manfred Zabel' _publ_contact_author_name 'Manfred Scheer' _publ_contact_author_email MANFRED.SCHEER@CHEMIE.UNI-REGENSBURG.DE _publ_section_title ; Synthesis and unprecedented coordination behaviour of a novel 1,2,3-triphosphaferrocene ; # Attachment '3.cif' data_2028 _database_code_depnum_ccdc_archive 'CCDC 687163' _audit_update_record ; 2008-04-21 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C33 H41 Fe P' _chemical_formula_sum 'C33 H41 Fe P' _chemical_formula_weight 524.48 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.5821(7) _cell_length_b 16.6027(8) _cell_length_c 33.0952(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5814.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.6 _exptl_crystal_description 'transparent plate' _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.592 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.80057 _exptl_absorpt_correction_T_max 0.92982 _exptl_absorpt_process_details 'ABST/PLATON 98' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method Phi-Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64880 _diffrn_reflns_av_R_equivalents 0.1183 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.02 _reflns_number_total 5529 _reflns_number_gt 2960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS V2.63' _computing_cell_refinement 'Stoe IPDS V2.63' _computing_data_reduction 'Stoe IPDS V2.63' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5529 _refine_ls_number_parameters 370 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.844 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.21947(3) 0.11265(2) 0.370973(11) 0.04296(11) Uani 1 d . . . P1 P 0.2420(4) -0.0210(3) 0.35172(15) 0.0577(8) Uani 0.57 d PD A 1 C1 C 0.3584(16) 0.0518(11) 0.3423(7) 0.078(7) Uani 0.57 d PD A 1 H1 H 0.4400 0.0449 0.3521 0.094 Uiso 0.57 calc PR A 1 C2 C 0.3269(17) 0.1215(12) 0.3195(6) 0.047(5) Uani 0.57 d PD A 1 C3 C 0.194(2) 0.1153(14) 0.3112(8) 0.040(5) Uani 0.57 d PD A 1 H3 H 0.1508 0.1522 0.2952 0.048 Uiso 0.57 calc PR A 1 C4 C 0.134(2) 0.0495(13) 0.3291(8) 0.042(4) Uani 0.57 d PD A 1 P2 P 0.3765(6) 0.0343(5) 0.3431(2) 0.0608(12) Uani 0.43 d PD A 2 C10 C 0.2216(16) -0.0009(11) 0.3485(7) 0.069(6) Uani 0.43 d PD A 2 H10 H 0.2034 -0.0417 0.3668 0.082 Uiso 0.43 calc PR A 2 C40 C 0.123(3) 0.0338(16) 0.3245(10) 0.035(4) Uani 0.43 d PD A 2 C30 C 0.176(3) 0.1065(19) 0.3080(10) 0.043(6) Uani 0.43 d PD A 2 H30 H 0.1280 0.1455 0.2951 0.051 Uiso 0.43 calc PR A 2 C20 C 0.308(2) 0.1133(16) 0.3132(6) 0.034(4) Uani 0.43 d PD A 2 C5 C 0.2218(2) 0.11200(19) 0.43386(8) 0.0501(6) Uani 1 d . . . C6 C 0.3052(2) 0.17545(18) 0.41877(8) 0.0486(7) Uani 1 d . . . C7 C 0.2269(2) 0.22693(17) 0.39473(8) 0.0488(6) Uani 1 d . . . H7 H 0.2556 0.2719 0.3807 0.059 Uiso 1 calc R . . C8 C 0.0998(2) 0.20030(18) 0.39513(8) 0.0490(7) Uani 1 d . . . C9 C 0.0984(2) 0.13016(18) 0.41839(8) 0.0510(8) Uani 1 d . . . H9 H 0.0267 0.0992 0.4232 0.061 Uiso 1 calc R . . C21 C 0.3991(3) 0.1845(2) 0.30215(8) 0.0527(8) Uani 1 d . . . C22 C 0.3492(3) 0.2579(2) 0.29075(9) 0.0618(8) Uani 1 d . . . H22 H 0.2623 0.2659 0.2922 0.074 Uiso 1 calc R . . C23 C 0.4254(3) 0.3198(2) 0.27725(10) 0.0753(10) Uani 1 d . . . H23 H 0.3897 0.3687 0.2696 0.090 Uiso 1 calc R . . C24 C 0.5545(4) 0.3091(3) 0.27511(11) 0.0831(11) Uani 1 d . . . H24 H 0.6061 0.3508 0.2663 0.100 Uiso 1 calc R . . C25 C 0.6059(3) 0.2369(3) 0.28608(10) 0.0792(12) Uani 1 d . . . H25 H 0.6929 0.2297 0.2846 0.095 Uiso 1 calc R . . C26 C 0.5297(3) 0.1742(2) 0.29948(9) 0.0673(9) Uani 1 d . . . H26 H 0.5658 0.1251 0.3067 0.081 Uiso 1 calc R . . C41 C -0.0058(2) 0.02000(18) 0.32332(9) 0.0505(7) Uani 1 d . . . C42 C -0.0668(3) -0.0234(2) 0.35324(10) 0.0663(9) Uani 1 d . . . H42 H -0.0224 -0.0390 0.3762 0.080 Uiso 1 calc R . . C43 C -0.1932(3) -0.0438(2) 0.34939(12) 0.0804(11) Uani 1 d . . . H43 H -0.2331 -0.0724 0.3699 0.096 Uiso 1 calc R . . C44 C -0.2602(3) -0.0221(2) 0.31546(12) 0.0782(10) Uani 1 d . . . H44 H -0.3451 -0.0357 0.3130 0.094 Uiso 1 calc R . . C45 C -0.2005(3) 0.0196(2) 0.28543(11) 0.0764(10) Uani 1 d . . . H45 H -0.2449 0.0338 0.2623 0.092 Uiso 1 calc R . . C46 C -0.0742(3) 0.0410(2) 0.28913(10) 0.0634(9) Uani 1 d . . . H46 H -0.0351 0.0696 0.2685 0.076 Uiso 1 calc R . . C51 C 0.2380(3) 0.0449(2) 0.46506(9) 0.0641(8) Uani 1 d . . . C52 C 0.2183(5) 0.0815(3) 0.50718(11) 0.1163(16) Uani 1 d . . . H52A H 0.2824 0.1211 0.5122 0.174 Uiso 1 calc R . . H52B H 0.2236 0.0397 0.5272 0.174 Uiso 1 calc R . . H52C H 0.1366 0.1064 0.5085 0.174 Uiso 1 calc R . . C53 C 0.3636(4) 0.0010(3) 0.46394(15) 0.1298(19) Uani 1 d . . . H53A H 0.3801 -0.0171 0.4369 0.195 Uiso 1 calc R . . H53B H 0.3604 -0.0446 0.4818 0.195 Uiso 1 calc R . . H53C H 0.4297 0.0368 0.4724 0.195 Uiso 1 calc R . . C54 C 0.1358(4) -0.0191(2) 0.46027(12) 0.0973(13) Uani 1 d . . . H54A H 0.0541 0.0053 0.4634 0.146 Uiso 1 calc R . . H54B H 0.1469 -0.0599 0.4805 0.146 Uiso 1 calc R . . H54C H 0.1421 -0.0429 0.4339 0.146 Uiso 1 calc R . . C61 C 0.4423(3) 0.2000(2) 0.42861(10) 0.0646(9) Uani 1 d . . . C62 C 0.4490(4) 0.2228(3) 0.47263(12) 0.131(2) Uani 1 d . . . H62A H 0.3829 0.2605 0.4787 0.196 Uiso 1 calc R . . H62B H 0.5295 0.2470 0.4782 0.196 Uiso 1 calc R . . H62C H 0.4389 0.1755 0.4890 0.196 Uiso 1 calc R . . C63 C 0.4817(3) 0.2733(2) 0.40425(11) 0.0829(11) Uani 1 d . . . H63A H 0.4784 0.2608 0.3760 0.124 Uiso 1 calc R . . H63B H 0.5664 0.2884 0.4115 0.124 Uiso 1 calc R . . H63C H 0.4253 0.3172 0.4100 0.124 Uiso 1 calc R . . C64 C 0.5437(3) 0.1356(3) 0.41788(17) 0.1200(18) Uani 1 d . . . H64A H 0.5158 0.0836 0.4270 0.180 Uiso 1 calc R . . H64B H 0.6220 0.1490 0.4309 0.180 Uiso 1 calc R . . H64C H 0.5559 0.1344 0.3891 0.180 Uiso 1 calc R . . C81 C -0.0146(2) 0.2484(2) 0.38016(9) 0.0602(8) Uani 1 d . . . C82 C -0.0399(5) 0.3108(3) 0.41227(14) 0.147(2) Uani 1 d . . . H82A H 0.0310 0.3467 0.4141 0.220 Uiso 1 calc R . . H82B H -0.0526 0.2846 0.4378 0.220 Uiso 1 calc R . . H82C H -0.1143 0.3409 0.4053 0.220 Uiso 1 calc R . . C83 C -0.1299(3) 0.1947(3) 0.37609(18) 0.1289(19) Uani 1 d . . . H83A H -0.2003 0.2262 0.3669 0.193 Uiso 1 calc R . . H83B H -0.1496 0.1713 0.4019 0.193 Uiso 1 calc R . . H83C H -0.1127 0.1527 0.3569 0.193 Uiso 1 calc R . . C84 C 0.0072(4) 0.2893(3) 0.34033(12) 0.1112(17) Uani 1 d . . . H84A H -0.0617 0.3252 0.3347 0.167 Uiso 1 calc R . . H84B H 0.0126 0.2495 0.3193 0.167 Uiso 1 calc R . . H84C H 0.0847 0.3193 0.3414 0.167 Uiso 1 calc R . . 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 Fe 0.04176(17) 0.0408(2) 0.04630(19) 0.0003(2) -0.00117(17) 0.00336(18) P1 0.0607(11) 0.042(2) 0.0708(13) -0.0048(13) -0.0069(9) 0.0085(13) C1 0.046(6) 0.082(14) 0.107(10) -0.048(9) 0.013(6) 0.009(7) C2 0.040(6) 0.042(7) 0.058(8) -0.018(5) -0.015(4) 0.006(5) C3 0.055(12) 0.029(5) 0.037(5) 0.003(6) -0.001(6) -0.009(6) C4 0.043(5) 0.036(10) 0.048(7) -0.017(6) -0.003(4) -0.006(5) P2 0.0516(19) 0.054(2) 0.077(3) -0.005(2) 0.0059(14) 0.0130(17) C10 0.097(13) 0.025(9) 0.084(10) -0.003(6) 0.022(9) 0.006(7) C40 0.055(8) 0.015(7) 0.035(7) -0.015(6) -0.009(4) -0.009(5) C30 0.023(5) 0.067(14) 0.039(7) -0.021(7) -0.002(5) -0.009(7) C20 0.027(7) 0.051(7) 0.025(5) -0.013(6) 0.003(6) -0.014(5) C5 0.0548(14) 0.0520(18) 0.0433(14) 0.0020(14) -0.0049(12) 0.0011(15) C6 0.0539(16) 0.0445(19) 0.0472(16) -0.0039(14) -0.0080(12) -0.0006(13) C7 0.0580(15) 0.0388(17) 0.0496(15) 0.0007(12) -0.0024(13) 0.0016(13) C8 0.0512(16) 0.048(2) 0.0474(17) -0.0007(14) 0.0010(12) 0.0124(13) C9 0.0489(15) 0.057(2) 0.0470(16) 0.0001(14) 0.0037(12) 0.0017(13) C21 0.0523(16) 0.060(2) 0.0460(17) -0.0107(15) 0.0068(13) -0.0069(15) C22 0.0609(18) 0.065(3) 0.0595(19) 0.0000(18) 0.0043(14) -0.0090(16) C23 0.082(2) 0.070(3) 0.074(2) 0.001(2) 0.0046(17) -0.0171(19) C24 0.085(3) 0.088(3) 0.076(3) -0.004(2) 0.0124(19) -0.036(2) C25 0.0583(19) 0.114(4) 0.066(2) -0.015(2) 0.0151(16) -0.028(2) C26 0.0488(16) 0.090(3) 0.063(2) -0.0068(19) 0.0123(14) -0.0048(17) C41 0.0509(16) 0.044(2) 0.0561(17) -0.0004(14) 0.0001(13) -0.0010(13) C42 0.0708(19) 0.061(3) 0.067(2) 0.0119(17) -0.0043(16) -0.0135(16) C43 0.074(2) 0.076(3) 0.091(3) 0.022(2) 0.0041(19) -0.0221(18) C44 0.0542(18) 0.071(3) 0.110(3) 0.013(2) -0.0035(18) -0.0088(16) C45 0.059(2) 0.081(3) 0.090(3) 0.019(2) -0.0205(16) -0.0062(17) C46 0.0601(17) 0.067(2) 0.063(2) 0.0150(17) -0.0058(14) -0.0066(15) C51 0.077(2) 0.059(2) 0.0567(18) 0.0161(15) -0.0123(15) -0.0018(16) C52 0.188(4) 0.106(4) 0.055(2) 0.021(2) -0.013(3) -0.041(3) C53 0.114(3) 0.112(4) 0.164(5) 0.080(4) -0.003(3) 0.032(3) C54 0.129(3) 0.068(3) 0.095(3) 0.035(2) -0.025(2) -0.030(2) C61 0.0652(19) 0.063(2) 0.066(2) 0.0044(17) -0.0149(15) -0.0104(16) C62 0.135(4) 0.188(6) 0.070(3) -0.005(3) -0.023(2) -0.087(4) C63 0.072(2) 0.085(3) 0.091(3) 0.009(2) -0.0108(18) -0.0245(19) C64 0.056(2) 0.100(4) 0.204(6) -0.003(3) -0.035(3) 0.005(2) C81 0.0552(15) 0.065(2) 0.0600(18) 0.0001(16) -0.0012(14) 0.0194(15) C82 0.176(4) 0.165(5) 0.100(4) -0.056(3) -0.042(3) 0.126(4) C83 0.056(2) 0.107(4) 0.224(6) 0.021(4) -0.022(3) 0.022(2) C84 0.095(3) 0.140(4) 0.099(3) 0.044(3) 0.004(2) 0.062(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 Fe C2 2.054(18) . ? Fe C9 2.047(3) . ? Fe C7 2.055(3) . ? Fe C8 2.088(3) . ? Fe C5 2.081(3) . ? Fe C40 2.26(3) . ? Fe C4 1.96(2) . ? Fe C6 2.101(3) . ? Fe C20 2.128(18) . ? Fe P2 2.304(8) . ? Fe P1 2.322(5) . ? P1 C4 1.80(2) . ? P1 C1 1.755(15) . ? C1 C2 1.42(3) . ? C1 H1 0.9300 . ? C2 C21 1.416(19) . ? C2 C3 1.44(3) . ? C3 C4 1.39(3) . ? C3 H3 0.9300 . ? C4 C41 1.571(19) . ? P2 C20 1.79(3) . ? P2 C10 1.750(16) . ? C10 C40 1.43(3) . ? C10 H10 0.9300 . ? C40 C41 1.39(3) . ? C40 C30 1.44(3) . ? C30 C20 1.41(3) . ? C30 H30 0.9300 . ? C20 C21 1.57(2) . ? C5 C9 1.435(4) . ? C5 C6 1.462(4) . ? C5 C51 1.528(4) . ? C6 C7 1.432(4) . ? C6 C61 1.542(4) . ? C7 C8 1.415(3) . ? C7 H7 0.9300 . ? C8 C9 1.396(4) . ? C8 C81 1.532(4) . ? C9 H9 0.9300 . ? C21 C22 1.380(4) . ? C21 C26 1.396(4) . ? C22 C23 1.380(4) . ? C22 H22 0.9300 . ? C23 C24 1.379(5) . ? C23 H23 0.9300 . ? C24 C25 1.366(5) . ? C24 H24 0.9300 . ? C25 C26 1.391(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C41 C46 1.388(4) . ? C41 C42 1.384(4) . ? C42 C43 1.386(4) . ? C42 H42 0.9300 . ? C43 C44 1.376(5) . ? C43 H43 0.9300 . ? C44 C45 1.366(5) . ? C44 H44 0.9300 . ? C45 C46 1.388(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C52 1.535(5) . ? C51 C54 1.524(5) . ? C51 C53 1.517(5) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C61 C62 1.507(5) . ? C61 C63 1.519(5) . ? C61 C64 1.556(5) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C81 C84 1.501(5) . ? C81 C82 1.509(5) . ? C81 C83 1.516(5) . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? 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 Fe C9 166.5(6) . . ? C2 Fe C7 103.3(6) . . ? C9 Fe C7 66.38(11) . . ? C2 Fe C8 127.1(6) . . ? C9 Fe C8 39.44(11) . . ? C7 Fe C8 39.94(10) . . ? C2 Fe C5 145.4(5) . . ? C9 Fe C5 40.67(10) . . ? C7 Fe C5 67.78(12) . . ? C8 Fe C5 68.16(11) . . ? C2 Fe C40 74.1(11) . . ? C9 Fe C40 108.8(8) . . ? C7 Fe C40 144.3(8) . . ? C8 Fe C40 113.0(8) . . ? C5 Fe C40 133.0(7) . . ? C2 Fe C4 73.0(6) . . ? C9 Fe C4 109.2(7) . . ? C7 Fe C4 141.5(7) . . ? C8 Fe C4 111.4(7) . . ? C5 Fe C4 135.2(7) . . ? C40 Fe C4 3.0(14) . . ? C2 Fe C6 110.5(6) . . ? C9 Fe C6 67.83(11) . . ? C7 Fe C6 40.30(10) . . ? C8 Fe C6 68.14(10) . . ? C5 Fe C6 40.93(11) . . ? C40 Fe C6 173.6(7) . . ? C4 Fe C6 176.2(7) . . ? C2 Fe C20 8.5(12) . . ? C9 Fe C20 164.4(7) . . ? C7 Fe C20 108.8(7) . . ? C8 Fe C20 127.4(7) . . ? C5 Fe C20 153.2(6) . . ? C40 Fe C20 65.8(8) . . ? C4 Fe C20 64.6(12) . . ? C6 Fe C20 118.9(7) . . ? C2 Fe P2 46.3(6) . . ? C9 Fe P2 147.07(18) . . ? C7 Fe P2 130.3(2) . . ? C8 Fe P2 169.9(2) . . ? C5 Fe P2 112.9(2) . . ? C40 Fe P2 74.0(8) . . ? C4 Fe P2 75.3(7) . . ? C6 Fe P2 105.7(2) . . ? C20 Fe P2 47.6(7) . . ? C2 Fe P1 77.5(6) . . ? C9 Fe P1 114.24(15) . . ? C7 Fe P1 169.65(12) . . ? C8 Fe P1 146.47(13) . . ? C5 Fe P1 105.56(15) . . ? C40 Fe P1 46.0(8) . . ? C4 Fe P1 48.8(7) . . ? C6 Fe P1 129.56(13) . . ? C20 Fe P1 73.3(7) . . ? P2 Fe P1 43.6(3) . . ? C4 P1 C1 85.6(9) . . ? C4 P1 Fe 55.0(7) . . ? C1 P1 Fe 57.4(6) . . ? C2 C1 P1 119.4(13) . . ? C2 C1 H1 120.3 . . ? P1 C1 H1 120.3 . . ? C1 C2 C21 133.6(15) . . ? C1 C2 C3 105.8(15) . . ? C21 C2 C3 120.3(16) . . ? C1 C2 Fe 68.3(10) . . ? C21 C2 Fe 133.4(13) . . ? C3 C2 Fe 67.1(12) . . ? C4 C3 C2 114.8(8) . . ? C4 C3 H3 122.6 . . ? C2 C3 H3 122.6 . . ? C3 C4 C41 128.2(19) . . ? C3 C4 P1 113.6(14) . . ? C41 C4 P1 116.5(12) . . ? C3 C4 Fe 70.9(14) . . ? C41 C4 Fe 133.5(15) . . ? P1 C4 Fe 76.2(9) . . ? C20 P2 C10 85.5(10) . . ? C20 P2 Fe 61.1(7) . . ? C10 P2 Fe 58.1(7) . . ? C40 C10 P2 119.3(16) . . ? C40 C10 H10 120.3 . . ? P2 C10 H10 120.3 . . ? C10 C40 C41 132(2) . . ? C10 C40 C30 105(2) . . ? C41 C40 C30 121(2) . . ? C10 C40 Fe 61.9(13) . . ? C41 C40 Fe 124(2) . . ? C30 C40 Fe 66.2(17) . . ? C20 C30 C40 113.9(12) . . ? C20 C30 H30 123.0 . . ? C40 C30 H30 123.0 . . ? C30 C20 C21 130(2) . . ? C30 C20 P2 114.2(16) . . ? C21 C20 P2 115.5(14) . . ? C30 C20 Fe 71.0(16) . . ? C21 C20 Fe 118.9(15) . . ? P2 C20 Fe 71.4(7) . . ? C9 C5 C6 106.0(2) . . ? C9 C5 C51 119.7(3) . . ? C6 C5 C51 133.5(2) . . ? C9 C5 Fe 68.37(15) . . ? C6 C5 Fe 70.25(15) . . ? C51 C5 Fe 132.9(2) . . ? C7 C6 C5 105.7(2) . . ? C7 C6 C61 120.3(3) . . ? C5 C6 C61 133.3(2) . . ? C7 C6 Fe 68.14(15) . . ? C5 C6 Fe 68.83(14) . . ? C61 C6 Fe 134.1(2) . . ? C8 C7 C6 111.0(3) . . ? C8 C7 Fe 71.29(16) . . ? C6 C7 Fe 71.56(16) . . ? C8 C7 H7 124.5 . . ? C6 C7 H7 124.5 . . ? Fe C7 H7 124.2 . . ? C9 C8 C7 106.0(2) . . ? C9 C8 C81 127.2(3) . . ? C7 C8 C81 125.8(3) . . ? C9 C8 Fe 68.68(15) . . ? C7 C8 Fe 68.77(15) . . ? C81 C8 Fe 135.9(2) . . ? C8 C9 C5 111.2(2) . . ? C8 C9 Fe 71.88(16) . . ? C5 C9 Fe 70.96(15) . . ? C8 C9 H9 124.4 . . ? C5 C9 H9 124.4 . . ? Fe C9 H9 124.3 . . ? C22 C21 C26 118.0(3) . . ? C22 C21 C2 123.8(8) . . ? C26 C21 C2 117.9(8) . . ? C22 C21 C20 119.7(9) . . ? C26 C21 C20 122.0(9) . . ? C23 C22 C21 121.5(3) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.7(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 120.1(4) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C46 C41 C42 118.1(3) . . ? C46 C41 C40 119.8(13) . . ? C42 C41 C40 121.6(13) . . ? C46 C41 C4 120.9(9) . . ? C42 C41 C4 120.9(10) . . ? C41 C42 C43 120.8(3) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 120.6(3) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 119.2(3) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 120.7(3) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C41 C46 C45 120.7(3) . . ? C41 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C5 C51 C52 108.1(3) . . ? C5 C51 C54 111.0(3) . . ? C52 C51 C54 105.9(3) . . ? C5 C51 C53 115.6(3) . . ? C52 C51 C53 109.3(3) . . ? C54 C51 C53 106.5(4) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C6 C61 C62 108.4(3) . . ? C6 C61 C63 111.0(2) . . ? C62 C61 C63 107.3(3) . . ? C6 C61 C64 114.8(3) . . ? C62 C61 C64 111.2(3) . . ? C63 C61 C64 103.9(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C84 C81 C82 109.6(4) . . ? C84 C81 C83 108.1(3) . . ? C82 C81 C83 108.9(4) . . ? C84 C81 C8 113.5(2) . . ? C82 C81 C8 105.7(3) . . ? C83 C81 C8 111.0(3) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.870 _refine_diff_density_max 0.254 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.041 # start Validation Reply Form _vrf_PLAT029_2028 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.87 RESPONSE:A missing cusp of data due to datacollection by rotation around the spindle axis only ; # end Validation Reply Form # Attachment '5sq.cif' # CIF-file generated for DS 210 Deng/Scheer #============================================================================== data_ds210 _database_code_depnum_ccdc_archive 'CCDC 687164' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H76 Br4 Cu4 Fe2 N2 P6, 1.5(C H2 Cl2)' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural 'C54 H76 Br4 Cu4 Fe2 N2 P6, 1.5(C H2 Cl2)' _chemical_formula_sum 'C55.50 H79 Br4 Cl3 Cu4 Fe2 N2 P6' _chemical_formula_iupac ? _chemical_formula_weight 1751.88 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 15.1002(10) _cell_length_b 15.5709(11) _cell_length_c 16.3950(12) _cell_angle_alpha 110.545(7) _cell_angle_beta 94.432(6) _cell_angle_gamma 104.171(6) _cell_volume 3442.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 11859 _cell_measurement_theta_min 3.0603 _cell_measurement_theta_max 62.7798 _cell_special_details ; ; _exptl_crystal_description platelike _exptl_crystal_colour orange _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1750 _exptl_absorpt_coefficient_mu 10.019 _exptl_crystal_density_meas_temp ? # Permitted for # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.89630 _exptl_absorpt_correction_T_max 1.07613 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra' _diffrn_measurement_method omega-scan _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 phi -180.00 -120.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames -40.0000 -1.3492 0.0000 - 0.0000 0.0000 60 #__ type_ start__ end____ width___ exp.time_ 2 omega -79.00 -24.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -1.3492 -75.0000 240.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 3 omega -29.00 22.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -1.3492 45.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 4 omega 27.00 78.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 3.0060 45.0000 0.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 5 omega -22.00 26.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 3.0060 45.0000 120.0000 0.0000 0.0000 48 #__ type_ start__ end____ width___ exp.time_ 6 omega -24.00 26.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 3.0060 45.0000 0.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 7 omega -60.00 -9.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 45.0000 120.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 8 omega -106.00 -51.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 -75.0000 0.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 9 omega -159.00 -108.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 -47.0000 322.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 10 omega -106.00 -54.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 -62.0000 51.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 11 omega -118.00 -65.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 117.0000 233.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 12 omega -162.00 -107.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 -75.0000 240.0000 0.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 13 omega -158.00 -106.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 -59.0000 77.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 14 omega -118.00 -65.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 117.0000 50.0000 0.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 15 omega -112.00 -61.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 45.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 16 omega -158.00 -108.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 -45.0000 0.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 17 omega -60.00 -15.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 45.0000 0.0000 0.0000 0.0000 45 #__ type_ start__ end____ width___ exp.time_ 18 omega -112.00 -61.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 45.0000 0.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 19 omega -105.00 -55.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -84.2355 -57.0000 182.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 20 omega 12.00 63.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 85.8923 -75.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 21 omega 55.00 84.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 85.8923 63.0000 171.0000 0.0000 0.0000 29 #__ type_ start__ end____ width___ exp.time_ 22 omega 24.00 63.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 85.8923 -75.0000 120.0000 0.0000 0.0000 39 #__ type_ start__ end____ width___ exp.time_ 23 omega 108.00 160.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 85.8923 62.0000 78.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 24 omega 72.00 119.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 85.8923 -75.0000 240.0000 0.0000 0.0000 47 #__ type_ start__ end____ width___ exp.time_ 25 omega 11.00 39.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 85.8923 -116.0000 93.0000 0.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 26 omega 52.00 92.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 85.8923 -116.0000 93.0000 0.0000 0.0000 40 #__ type_ start__ end____ width___ exp.time_ 27 omega 64.00 98.00 1.0000 85.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 85.8923 -75.0000 120.0000 0.0000 0.0000 34 ; _diffrn_detector_area_resol_mean 10.5431 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 25040 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 62.95 _diffrn_reflns_theta_full 62.95 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.972 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 10799 # number of observed reflections (> n sig(I)) _reflns_number_gt 8052 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.2447P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 10799 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0779 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.776 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.089 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Br1 Br Uani -0.10371(3) -0.24363(3) 0.07541(3) 1.000 0.0250(2) . . Br2 Br Uani -0.32933(3) -0.19062(3) 0.00035(3) 1.000 0.0223(1) . . Br3 Br Uani -0.24059(3) -0.09451(3) 0.26046(3) 1.000 0.0318(2) . . Br4 Br Uani -0.51561(3) -0.19609(3) 0.14694(3) 1.000 0.0285(2) . . Cu1 Cu Uani -0.17341(4) -0.11058(5) 0.12878(4) 1.000 0.0293(2) . . Cu2 Cu Uani -0.20510(4) -0.26434(4) -0.06060(4) 1.000 0.0254(2) . . Cu3 Cu Uani -0.36047(4) -0.22238(4) 0.14376(4) 1.000 0.0257(2) . . Cu4 Cu Uani -0.51033(5) -0.24617(4) -0.01274(4) 1.000 0.0270(2) . . Fe1 Fe Uani 0.05144(4) 0.13919(5) 0.22810(4) 1.000 0.0172(2) . . Fe2 Fe Uani -0.33842(4) -0.46182(4) 0.20090(4) 1.000 0.0173(2) . . P1 P Uani -0.06265(8) 0.01025(8) 0.12101(7) 1.000 0.0212(3) . . P2 P Uani -0.03157(8) 0.13992(8) 0.09834(7) 1.000 0.0218(3) . . P3 P Uani -0.11480(8) -0.16726(8) -0.11205(7) 1.000 0.0197(3) . . P4 P Uani -0.36923(8) -0.37256(8) 0.12028(7) 1.000 0.0208(3) . . P5 P Uani -0.48552(8) -0.48225(8) 0.11916(8) 1.000 0.0228(3) . . P6 P Uani -0.57475(8) -0.40365(8) -0.07879(7) 1.000 0.0211(3) . . N1 N Uani -0.5508(3) -0.1532(3) -0.0529(3) 1.000 0.0288(12) . . N2 N Uani -0.2631(2) -0.4075(3) -0.1201(3) 1.000 0.0249(12) . . C1 C Uani -0.0052(3) 0.2277(3) 0.3268(3) 1.000 0.0225(14) . . C2 C Uani 0.0915(3) 0.2753(3) 0.3319(3) 1.000 0.0198(12) . . C3 C Uani 0.1434(3) 0.2142(3) 0.3462(3) 1.000 0.0191(12) . . C4 C Uani 0.0823(3) 0.1314(3) 0.3523(3) 1.000 0.0193(12) . . C5 C Uani -0.0074(3) 0.1394(3) 0.3383(3) 1.000 0.0206(12) . . C6 C Uani -0.0967(3) 0.2558(3) 0.3260(3) 1.000 0.0254(16) . . C7 C Uani -0.1805(3) 0.1694(4) 0.2709(4) 1.000 0.0413(17) . . C8 C Uani -0.1113(4) 0.2888(4) 0.4229(3) 1.000 0.0437(17) . . C9 C Uani -0.1001(4) 0.3342(4) 0.2928(4) 1.000 0.0453(19) . . C10 C Uani 0.1425(3) 0.3773(3) 0.3381(3) 1.000 0.0230(14) . . C11 C Uani 0.1082(3) 0.4069(3) 0.2646(3) 1.000 0.0336(17) . . C12 C Uani 0.1356(4) 0.4485(3) 0.4293(3) 1.000 0.0367(16) . . C13 C Uani 0.2467(3) 0.3873(3) 0.3369(3) 1.000 0.0312(16) . . C14 C Uani 0.1106(3) 0.0599(3) 0.3841(3) 1.000 0.0223(14) . . C15 C Uani 0.0357(3) -0.0365(3) 0.3496(3) 1.000 0.0284(16) . . C16 C Uani 0.1200(3) 0.1037(3) 0.4856(3) 1.000 0.0288(16) . . C17 C Uani 0.2038(3) 0.0458(3) 0.3606(3) 1.000 0.0283(16) . . C18 C Uani 0.0497(3) 0.0023(3) 0.1406(3) 1.000 0.0193(12) . . C19 C Uani -0.3625(3) -0.4054(3) 0.3312(3) 1.000 0.0196(12) . . C20 C Uani -0.3547(3) -0.5020(3) 0.3095(3) 1.000 0.0178(12) . . C21 C Uani -0.2642(3) -0.4997(3) 0.2866(3) 1.000 0.0189(12) . . C22 C Uani -0.2150(3) -0.4057(3) 0.2959(3) 1.000 0.0205(12) . . C23 C Uani -0.2765(3) -0.3497(3) 0.3203(3) 1.000 0.0201(12) . . C24 C Uani -0.4293(3) -0.3514(3) 0.3766(3) 1.000 0.0251(14) . . C25 C Uani -0.4323(3) -0.2693(3) 0.3460(3) 1.000 0.0337(17) . . C26 C Uani -0.5304(3) -0.4113(3) 0.3634(3) 1.000 0.0267(17) . . C27 C Uani -0.3885(3) -0.3064(3) 0.4768(3) 1.000 0.0313(17) . . C28 C Uani -0.4156(3) -0.5911(3) 0.3201(3) 1.000 0.0237(14) . . C29 C Uani -0.4171(3) -0.5661(3) 0.4194(3) 1.000 0.0308(17) . . C30 C Uani -0.5152(3) -0.6301(3) 0.2664(3) 1.000 0.0267(16) . . C31 C Uani -0.3708(3) -0.6734(3) 0.2905(3) 1.000 0.0287(16) . . C32 C Uani -0.1113(3) -0.3680(3) 0.2972(3) 1.000 0.0230(12) . . C33 C Uani -0.0886(3) -0.2703(3) 0.2895(3) 1.000 0.0292(16) . . C34 C Uani -0.0632(3) -0.3574(3) 0.3867(3) 1.000 0.0311(17) . . C35 C Uani -0.0760(3) -0.4370(3) 0.2245(3) 1.000 0.0297(16) . . C36 C Uani -0.2892(3) -0.4377(3) 0.0920(3) 1.000 0.0210(12) . . C37 C Uani -0.1290(3) -0.0685(3) -0.1364(3) 1.000 0.0192(12) . . C38 C Uani -0.2213(3) -0.0532(3) -0.1491(3) 1.000 0.0206(12) . . C39 C Uani -0.3023(3) -0.1280(3) -0.1939(3) 1.000 0.0277(16) . . C40 C Uani -0.3857(3) -0.1091(3) -0.2062(4) 1.000 0.0377(19) . . C41 C Uani -0.3913(3) -0.0155(3) -0.1741(4) 1.000 0.0393(19) . . C42 C Uani -0.3122(3) 0.0580(3) -0.1278(3) 1.000 0.0329(17) . . C43 C Uani -0.2291(3) 0.0397(3) -0.1149(3) 1.000 0.0264(16) . . C44 C Uani -0.6892(3) -0.4641(3) -0.0727(3) 1.000 0.0201(12) . . C45 C Uani -0.7583(3) -0.4107(3) -0.0494(3) 1.000 0.0240(14) . . C46 C Uani -0.8288(3) -0.4397(3) -0.0061(3) 1.000 0.0288(17) . . C47 C Uani -0.8943(3) -0.3905(3) 0.0152(3) 1.000 0.0353(17) . . C48 C Uani -0.8908(3) -0.3124(3) -0.0071(3) 1.000 0.0361(17) . . C49 C Uani -0.8208(3) -0.2823(3) -0.0493(3) 1.000 0.0312(17) . . C50 C Uani -0.7562(3) -0.3307(3) -0.0698(3) 1.000 0.0232(14) . . C51 C Uani -0.5840(3) -0.1028(3) -0.0700(3) 1.000 0.0357(17) . . C52 C Uani -0.6266(4) -0.0358(4) -0.0917(4) 1.000 0.055(2) . . C53 C Uani -0.2832(3) -0.4846(4) -0.1438(3) 1.000 0.0352(17) . . C54 C Uani -0.3093(4) -0.5918(3) -0.1792(4) 1.000 0.046(2) . . H3A H Uiso 0.20890 0.22700 0.35100 1.000 0.0230 calc R H5A H Uiso -0.06240 0.09300 0.33670 1.000 0.0250 calc R H7A H Uiso -0.23760 0.18850 0.27670 1.000 0.0500 calc R H7B H Uiso -0.18350 0.11760 0.29240 1.000 0.0500 calc R H7C H Uiso -0.17370 0.14700 0.20860 1.000 0.0500 calc R H8A H Uiso -0.06060 0.34610 0.45940 1.000 0.0520 calc R H8B H Uiso -0.11190 0.23750 0.44460 1.000 0.0520 calc R H8C H Uiso -0.17060 0.30370 0.42640 1.000 0.0520 calc R H9A H Uiso -0.05260 0.39370 0.33080 1.000 0.0550 calc R H9B H Uiso -0.16160 0.34450 0.29410 1.000 0.0550 calc R H9C H Uiso -0.08840 0.31540 0.23190 1.000 0.0550 calc R H11A H Uiso 0.10860 0.35900 0.20680 1.000 0.0400 calc R H11B H Uiso 0.14910 0.46940 0.27150 1.000 0.0400 calc R H11C H Uiso 0.04480 0.41110 0.26830 1.000 0.0400 calc R H12A H Uiso 0.16900 0.51390 0.43660 1.000 0.0440 calc R H12B H Uiso 0.16330 0.43280 0.47640 1.000 0.0440 calc R H12C H Uiso 0.07020 0.44390 0.43290 1.000 0.0440 calc R H13A H Uiso 0.25390 0.34240 0.28030 1.000 0.0370 calc R H13B H Uiso 0.27300 0.37290 0.38540 1.000 0.0370 calc R H13C H Uiso 0.27930 0.45300 0.34430 1.000 0.0370 calc R H15A H Uiso -0.02320 -0.02680 0.36610 1.000 0.0340 calc R H15B H Uiso 0.05390 -0.07890 0.37550 1.000 0.0340 calc R H15C H Uiso 0.02810 -0.06580 0.28490 1.000 0.0340 calc R H16A H Uiso 0.16760 0.16610 0.50940 1.000 0.0350 calc R H16B H Uiso 0.13800 0.06080 0.51100 1.000 0.0350 calc R H16C H Uiso 0.06040 0.11220 0.50100 1.000 0.0350 calc R H17A H Uiso 0.19730 0.01460 0.29630 1.000 0.0340 calc R H17B H Uiso 0.22270 0.00560 0.38890 1.000 0.0340 calc R H17C H Uiso 0.25100 0.10830 0.38170 1.000 0.0340 calc R H18A H Uiso 0.05750 -0.04970 0.15490 1.000 0.0230 calc R H21A H Uiso -0.24080 -0.55350 0.26800 1.000 0.0230 calc R H23A H Uiso -0.26290 -0.28400 0.32840 1.000 0.0240 calc R H25A H Uiso -0.36960 -0.22520 0.35900 1.000 0.0400 calc R H25B H Uiso -0.47340 -0.23460 0.37730 1.000 0.0400 calc R H25C H Uiso -0.45570 -0.29570 0.28210 1.000 0.0400 calc R H26A H Uiso -0.55580 -0.44410 0.29990 1.000 0.0320 calc R H26B H Uiso -0.56730 -0.36910 0.39160 1.000 0.0320 calc R H26C H Uiso -0.53270 -0.45880 0.39010 1.000 0.0320 calc R H27A H Uiso -0.38600 -0.35730 0.49820 1.000 0.0370 calc R H27B H Uiso -0.42790 -0.26980 0.50890 1.000 0.0370 calc R H27C H Uiso -0.32560 -0.26360 0.48680 1.000 0.0370 calc R H29A H Uiso -0.44790 -0.62410 0.42880 1.000 0.0370 calc R H29B H Uiso -0.45100 -0.51860 0.44020 1.000 0.0370 calc R H29C H Uiso -0.35330 -0.53960 0.45250 1.000 0.0370 calc R H30A H Uiso -0.51500 -0.67060 0.20520 1.000 0.0320 calc R H30B H Uiso -0.53820 -0.57640 0.26670 1.000 0.0320 calc R H30C H Uiso -0.55570 -0.66810 0.29300 1.000 0.0320 calc R H31A H Uiso -0.41070 -0.73030 0.29600 1.000 0.0350 calc R H31B H Uiso -0.30990 -0.65390 0.32800 1.000 0.0350 calc R H31C H Uiso -0.36320 -0.68830 0.22870 1.000 0.0350 calc R H33A H Uiso -0.10350 -0.22390 0.34060 1.000 0.0350 calc R H33B H Uiso -0.12540 -0.27580 0.23500 1.000 0.0350 calc R H33C H Uiso -0.02240 -0.24860 0.28780 1.000 0.0350 calc R H34A H Uiso 0.00390 -0.32960 0.39320 1.000 0.0370 calc R H34B H Uiso -0.07560 -0.42050 0.39050 1.000 0.0370 calc R H34C H Uiso -0.08680 -0.31520 0.43390 1.000 0.0370 calc R H35A H Uiso -0.00800 -0.41570 0.23530 1.000 0.0360 calc R H35B H Uiso -0.10000 -0.43780 0.16680 1.000 0.0360 calc R H35C H Uiso -0.09750 -0.50160 0.22470 1.000 0.0360 calc R H36A H Uiso -0.22810 -0.40460 0.08970 1.000 0.0250 calc R H39 H Uiso -0.29980 -0.19240 -0.21600 1.000 0.0330 calc R H40 H Uiso -0.44010 -0.16060 -0.23710 1.000 0.0450 calc R H41 H Uiso -0.44860 -0.00260 -0.18400 1.000 0.0470 calc R H42 H Uiso -0.31530 0.12210 -0.10450 1.000 0.0400 calc R H43 H Uiso -0.17560 0.09150 -0.08200 1.000 0.0320 calc R H46 H Uiso -0.83190 -0.49380 0.00900 1.000 0.0340 calc R H47 H Uiso -0.94160 -0.41070 0.04510 1.000 0.0430 calc R H48 H Uiso -0.93630 -0.27930 0.00650 1.000 0.0430 calc R H49 H Uiso -0.81760 -0.22800 -0.06410 1.000 0.0370 calc R H50 H Uiso -0.70860 -0.30930 -0.09880 1.000 0.0280 calc R H52A H Uiso -0.66270 -0.01130 -0.04640 1.000 0.0660 calc R H52B H Uiso -0.66760 -0.06950 -0.14960 1.000 0.0660 calc R H52C H Uiso -0.57770 0.01770 -0.09340 1.000 0.0660 calc R H54A H Uiso -0.33330 -0.61740 -0.24300 1.000 0.0550 calc R H54B H Uiso -0.35720 -0.61590 -0.14920 1.000 0.0550 calc R H54C H Uiso -0.25450 -0.61220 -0.16890 1.000 0.0550 calc R 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 Br1 0.0227(3) 0.0265(2) 0.0295(3) 0.0153(2) 0.0063(2) 0.0064(2) Br2 0.0181(2) 0.0259(2) 0.0258(2) 0.0128(2) 0.0057(2) 0.0066(2) Br3 0.0277(3) 0.0301(3) 0.0287(3) 0.0070(2) 0.0076(2) -0.0013(2) Br4 0.0265(3) 0.0314(3) 0.0308(3) 0.0119(2) 0.0081(2) 0.0132(2) Cu1 0.0252(4) 0.0258(4) 0.0347(4) 0.0112(3) 0.0097(3) 0.0031(3) Cu2 0.0262(4) 0.0226(3) 0.0290(4) 0.0126(3) 0.0074(3) 0.0052(3) Cu3 0.0263(4) 0.0196(3) 0.0335(4) 0.0116(3) 0.0059(3) 0.0083(3) Cu4 0.0272(4) 0.0197(3) 0.0317(4) 0.0089(3) 0.0027(3) 0.0048(3) Fe1 0.0172(4) 0.0157(3) 0.0175(3) 0.0057(3) 0.0027(3) 0.0040(3) Fe2 0.0177(4) 0.0145(3) 0.0192(4) 0.0072(3) 0.0025(3) 0.0031(3) P1 0.0179(6) 0.0198(6) 0.0227(6) 0.0068(5) 0.0023(5) 0.0023(5) P2 0.0181(6) 0.0244(6) 0.0243(6) 0.0111(5) 0.0017(5) 0.0065(5) P3 0.0191(6) 0.0205(6) 0.0224(6) 0.0109(5) 0.0049(5) 0.0066(5) P4 0.0226(6) 0.0185(6) 0.0231(6) 0.0104(5) 0.0029(5) 0.0061(5) P5 0.0177(6) 0.0221(6) 0.0274(6) 0.0092(5) 0.0013(5) 0.0051(5) P6 0.0190(6) 0.0181(6) 0.0246(6) 0.0078(5) 0.0015(5) 0.0037(5) N1 0.035(2) 0.022(2) 0.033(2) 0.0111(19) 0.0058(19) 0.0136(19) N2 0.024(2) 0.022(2) 0.035(2) 0.0186(19) 0.0104(18) 0.0045(17) C1 0.024(3) 0.021(2) 0.019(2) 0.0035(19) 0.006(2) 0.006(2) C2 0.023(2) 0.019(2) 0.016(2) 0.0055(19) 0.0018(19) 0.0060(19) C3 0.021(2) 0.018(2) 0.015(2) 0.0034(18) 0.0028(19) 0.0044(19) C4 0.022(2) 0.022(2) 0.013(2) 0.0051(19) 0.0043(18) 0.0071(19) C5 0.017(2) 0.024(2) 0.019(2) 0.0074(19) 0.0066(19) 0.0030(19) C6 0.019(2) 0.028(3) 0.031(3) 0.010(2) 0.004(2) 0.012(2) C7 0.019(3) 0.042(3) 0.055(3) 0.008(3) 0.002(2) 0.012(2) C8 0.044(3) 0.051(3) 0.036(3) 0.010(3) 0.009(3) 0.023(3) C9 0.039(3) 0.049(3) 0.062(4) 0.030(3) 0.013(3) 0.023(3) C10 0.029(3) 0.015(2) 0.022(2) 0.0049(19) 0.002(2) 0.005(2) C11 0.039(3) 0.024(3) 0.042(3) 0.016(2) 0.009(2) 0.011(2) C12 0.049(3) 0.020(2) 0.032(3) 0.003(2) 0.012(3) 0.003(2) C13 0.026(3) 0.023(2) 0.039(3) 0.014(2) 0.000(2) -0.004(2) C14 0.026(3) 0.020(2) 0.023(2) 0.011(2) 0.006(2) 0.006(2) C15 0.034(3) 0.022(2) 0.029(3) 0.013(2) 0.003(2) 0.004(2) C16 0.031(3) 0.034(3) 0.024(2) 0.015(2) -0.001(2) 0.010(2) C17 0.034(3) 0.022(2) 0.030(3) 0.010(2) 0.003(2) 0.011(2) C18 0.023(2) 0.018(2) 0.017(2) 0.0066(19) 0.0055(19) 0.0057(19) C19 0.016(2) 0.020(2) 0.022(2) 0.0081(19) 0.0039(19) 0.0035(18) C20 0.016(2) 0.020(2) 0.018(2) 0.0092(19) -0.0018(18) 0.0049(19) C21 0.019(2) 0.021(2) 0.020(2) 0.0100(19) 0.0015(19) 0.0092(19) C22 0.021(2) 0.021(2) 0.016(2) 0.0070(19) 0.0011(19) 0.0007(19) C23 0.023(2) 0.018(2) 0.018(2) 0.0075(19) -0.0019(19) 0.0046(19) C24 0.027(3) 0.025(2) 0.023(2) 0.010(2) 0.004(2) 0.006(2) C25 0.037(3) 0.028(3) 0.044(3) 0.016(2) 0.021(2) 0.016(2) C26 0.023(3) 0.028(3) 0.028(3) 0.010(2) 0.006(2) 0.006(2) C27 0.028(3) 0.032(3) 0.029(3) 0.008(2) 0.010(2) 0.004(2) C28 0.026(3) 0.020(2) 0.027(2) 0.014(2) 0.007(2) 0.002(2) C29 0.029(3) 0.031(3) 0.036(3) 0.021(2) 0.008(2) 0.002(2) C30 0.018(2) 0.027(3) 0.033(3) 0.014(2) 0.002(2) 0.000(2) C31 0.029(3) 0.019(2) 0.037(3) 0.013(2) 0.008(2) 0.001(2) C32 0.019(2) 0.024(2) 0.024(2) 0.009(2) 0.000(2) 0.004(2) C33 0.027(3) 0.023(2) 0.031(3) 0.009(2) 0.008(2) -0.003(2) C34 0.023(3) 0.033(3) 0.033(3) 0.013(2) -0.001(2) 0.002(2) C35 0.016(2) 0.032(3) 0.037(3) 0.010(2) 0.004(2) 0.005(2) C36 0.023(2) 0.025(2) 0.021(2) 0.015(2) 0.0073(19) 0.007(2) C37 0.023(2) 0.022(2) 0.014(2) 0.0060(19) 0.0053(19) 0.0099(19) C38 0.022(2) 0.026(2) 0.020(2) 0.013(2) 0.0061(19) 0.011(2) C39 0.025(3) 0.016(2) 0.039(3) 0.009(2) 0.009(2) 0.002(2) C40 0.021(3) 0.029(3) 0.063(4) 0.018(3) 0.003(3) 0.008(2) C41 0.022(3) 0.038(3) 0.064(4) 0.023(3) 0.005(3) 0.015(2) C42 0.031(3) 0.027(3) 0.041(3) 0.009(2) 0.006(2) 0.015(2) C43 0.027(3) 0.021(2) 0.028(3) 0.007(2) 0.004(2) 0.005(2) C44 0.021(2) 0.021(2) 0.017(2) 0.0060(19) 0.0055(19) 0.0049(19) C45 0.023(3) 0.024(2) 0.017(2) 0.001(2) 0.000(2) 0.004(2) C46 0.029(3) 0.026(3) 0.030(3) 0.009(2) 0.003(2) 0.009(2) C47 0.026(3) 0.037(3) 0.036(3) 0.007(2) 0.010(2) 0.006(2) C48 0.027(3) 0.037(3) 0.043(3) 0.007(3) 0.005(2) 0.020(2) C49 0.029(3) 0.027(3) 0.038(3) 0.010(2) 0.001(2) 0.014(2) C50 0.016(2) 0.024(2) 0.029(3) 0.009(2) 0.003(2) 0.007(2) C51 0.031(3) 0.020(3) 0.039(3) 0.001(2) -0.001(2) -0.005(2) C52 0.047(4) 0.028(3) 0.083(5) 0.019(3) -0.018(3) 0.009(3) C53 0.035(3) 0.042(3) 0.031(3) 0.015(3) 0.006(2) 0.014(3) C54 0.052(4) 0.026(3) 0.057(4) 0.014(3) -0.001(3) 0.014(3) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu1 2.4704(9) . . yes Br1 Cu2 2.4792(8) . . yes Br2 Cu1 2.7359(8) . . yes Br2 Cu2 2.5247(8) . . yes Br2 Cu3 2.6205(8) . . yes Br2 Cu4 2.6241(9) . . yes Br3 Cu1 2.4158(8) . . yes Br3 Cu3 2.4348(8) . . yes Br4 Cu3 2.4762(8) . . yes Br4 Cu4 2.4694(8) . . yes Cu1 P1 2.2391(15) . . yes Cu2 P3 2.2180(14) . . yes Cu2 N2 2.018(5) . . yes Cu3 P4 2.2006(14) . . yes Cu4 P6 2.2220(14) . . yes Cu4 N1 1.986(5) . . yes Fe1 P1 2.3337(14) . . yes Fe1 P2 2.3894(13) . . yes Fe1 C1 2.116(5) . . yes Fe1 C2 2.106(5) . . yes Fe1 C3 2.060(5) . . yes Fe1 C4 2.105(5) . . yes Fe1 C5 2.073(5) . . yes Fe1 C18 2.103(5) . . yes Fe1 P3 2.3209(13) . 2_555 yes Fe1 C37 2.141(5) . 2_555 yes Fe2 P4 2.3251(14) . . yes Fe2 P5 2.3929(14) . . yes Fe2 C19 2.104(5) . . yes Fe2 C20 2.097(5) . . yes Fe2 C21 2.059(5) . . yes Fe2 C22 2.112(5) . . yes Fe2 C23 2.067(5) . . yes Fe2 C36 2.102(5) . . yes Fe2 P6 2.3283(13) . 2_445 yes Fe2 C44 2.143(5) . 2_445 yes P1 P2 2.1272(18) . . yes P1 C18 1.745(5) . . yes P2 P3 2.1242(18) . 2_555 yes P3 C37 1.775(5) . . yes P4 P5 2.1226(18) . . yes P4 C36 1.750(5) . . yes P5 P6 2.1171(18) . 2_445 yes P6 C44 1.783(5) . . yes N1 C51 1.127(7) . . yes N2 C53 1.077(8) . . yes C1 C2 1.448(7) . . no C1 C5 1.445(7) . . no C1 C6 1.549(7) . . no C2 C3 1.438(7) . . no C2 C10 1.550(7) . . no C3 C4 1.430(7) . . no C4 C5 1.399(7) . . no C4 C14 1.517(7) . . no C6 C7 1.538(8) . . no C6 C8 1.541(7) . . no C6 C9 1.511(8) . . no C10 C11 1.531(7) . . no C10 C12 1.547(7) . . no C10 C13 1.545(7) . . no C14 C15 1.525(7) . . no C14 C16 1.541(6) . . no C14 C17 1.534(7) . . no C18 C37 1.400(7) . 2_555 no C19 C20 1.456(7) . . no C19 C23 1.437(7) . . no C19 C24 1.540(7) . . no C20 C21 1.440(7) . . no C20 C28 1.539(7) . . no C21 C22 1.418(7) . . no C22 C23 1.411(7) . . no C22 C32 1.527(7) . . no C24 C25 1.537(7) . . no C24 C26 1.535(7) . . no C24 C27 1.547(6) . . no C28 C29 1.539(6) . . no C28 C30 1.542(7) . . no C28 C31 1.541(7) . . no C32 C33 1.528(7) . . no C32 C34 1.521(6) . . no C32 C35 1.529(7) . . no C36 C44 1.395(7) . 2_445 no C37 C38 1.482(7) . . no C38 C39 1.398(7) . . no C38 C43 1.395(7) . . no C39 C40 1.377(7) . . no C40 C41 1.392(7) . . no C41 C42 1.376(7) . . no C42 C43 1.370(7) . . no C44 C45 1.480(7) . . no C45 C46 1.396(7) . . no C45 C50 1.393(7) . . no C46 C47 1.387(7) . . no C47 C48 1.378(7) . . no C48 C49 1.383(7) . . no C49 C50 1.366(7) . . no C51 C52 1.477(8) . . no C53 C54 1.497(8) . . no C3 H3A 0.9500 . . no C5 H5A 0.9500 . . no C7 H7A 0.9800 . . no C7 H7B 0.9800 . . no C7 H7C 0.9800 . . no C8 H8A 0.9800 . . no C8 H8B 0.9800 . . no C8 H8C 0.9800 . . no C9 H9A 0.9800 . . no C9 H9B 0.9800 . . no C9 H9C 0.9800 . . no C11 H11A 0.9800 . . no C11 H11B 0.9800 . . no C11 H11C 0.9800 . . no C12 H12A 0.9800 . . no C12 H12B 0.9800 . . no C12 H12C 0.9800 . . no C13 H13A 0.9800 . . no C13 H13B 0.9800 . . no C13 H13C 0.9800 . . no C15 H15A 0.9800 . . no C15 H15B 0.9800 . . no C15 H15C 0.9800 . . no C16 H16A 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C17 H17A 0.9800 . . no C17 H17B 0.9800 . . no C17 H17C 0.9800 . . no C18 H18A 0.9500 . . no C21 H21A 0.9500 . . no C23 H23A 0.9500 . . no C25 H25A 0.9800 . . no C25 H25B 0.9800 . . no C25 H25C 0.9800 . . no C26 H26A 0.9800 . . no C26 H26B 0.9800 . . no C26 H26C 0.9800 . . no C27 H27A 0.9800 . . no C27 H27B 0.9800 . . no C27 H27C 0.9800 . . no C29 H29A 0.9800 . . no C29 H29B 0.9800 . . no C29 H29C 0.9800 . . no C30 H30A 0.9800 . . no C30 H30B 0.9800 . . no C30 H30C 0.9800 . . no C31 H31A 0.9800 . . no C31 H31B 0.9800 . . no C31 H31C 0.9800 . . no C33 H33A 0.9800 . . no C33 H33B 0.9800 . . no C33 H33C 0.9800 . . no C34 H34A 0.9800 . . no C34 H34B 0.9800 . . no C34 H34C 0.9800 . . no C35 H35A 0.9800 . . no C35 H35B 0.9800 . . no C35 H35C 0.9800 . . no C36 H36A 0.9500 . . no C39 H39 0.9500 . . no C40 H40 0.9500 . . no C41 H41 0.9500 . . no C42 H42 0.9500 . . no C43 H43 0.9500 . . no C46 H46 0.9500 . . no C47 H47 0.9500 . . no C48 H48 0.9500 . . no C49 H49 0.9500 . . no C50 H50 0.9500 . . no C52 H52A 0.9800 . . no C52 H52B 0.9800 . . no C52 H52C 0.9800 . . no C54 H54A 0.9800 . . no C54 H54B 0.9800 . . no C54 H54C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 Br1 Cu2 77.48(3) . . . yes Cu1 Br2 Cu2 72.01(2) . . . yes Cu1 Br2 Cu3 68.38(2) . . . yes Cu1 Br2 Cu4 138.97(3) . . . yes Cu2 Br2 Cu3 109.17(3) . . . yes Cu2 Br2 Cu4 137.19(3) . . . yes Cu3 Br2 Cu4 73.59(2) . . . yes Cu1 Br3 Cu3 76.76(3) . . . yes Cu3 Br4 Cu4 78.86(3) . . . yes Br1 Cu1 Br2 97.04(3) . . . yes Br1 Cu1 Br3 116.38(3) . . . yes Br1 Cu1 P1 100.98(4) . . . yes Br2 Cu1 Br3 101.15(3) . . . yes Br2 Cu1 P1 117.58(4) . . . yes Br3 Cu1 P1 121.66(4) . . . yes Br1 Cu2 Br2 102.57(3) . . . yes Br1 Cu2 P3 102.64(4) . . . yes Br1 Cu2 N2 103.98(13) . . . yes Br2 Cu2 P3 108.45(4) . . . yes Br2 Cu2 N2 107.91(10) . . . yes P3 Cu2 N2 128.22(13) . . . yes Br2 Cu3 Br3 103.98(3) . . . yes Br2 Cu3 Br4 97.83(3) . . . yes Br2 Cu3 P4 109.25(4) . . . yes Br3 Cu3 Br4 112.81(3) . . . yes Br3 Cu3 P4 119.26(4) . . . yes Br4 Cu3 P4 111.15(4) . . . yes Br2 Cu4 Br4 97.91(3) . . . yes Br2 Cu4 P6 114.38(5) . . . yes Br2 Cu4 N1 102.85(14) . . . yes Br4 Cu4 P6 109.07(4) . . . yes Br4 Cu4 N1 106.98(14) . . . yes P6 Cu4 N1 122.67(14) . . . yes P1 Fe1 P2 53.52(5) . . . yes P1 Fe1 C1 112.45(13) . . . yes P1 Fe1 C2 150.56(14) . . . yes P1 Fe1 C3 157.18(14) . . . yes P1 Fe1 C4 117.41(14) . . . yes P1 Fe1 C5 98.18(14) . . . yes P1 Fe1 C18 45.94(13) . . . yes P1 Fe1 P3 87.09(5) . . 2_555 yes P1 Fe1 C37 76.53(13) . . 2_555 yes P2 Fe1 C1 100.15(13) . . . yes P2 Fe1 C2 111.77(14) . . . yes P2 Fe1 C3 148.83(14) . . . yes P2 Fe1 C4 161.87(14) . . . yes P2 Fe1 C5 123.06(14) . . . yes P2 Fe1 C18 82.25(13) . . . yes P2 Fe1 P3 53.59(4) . . 2_555 yes P2 Fe1 C37 83.18(13) . . 2_555 yes C1 Fe1 C2 40.12(18) . . . yes C1 Fe1 C3 67.24(18) . . . yes C1 Fe1 C4 67.46(18) . . . yes C1 Fe1 C5 40.34(19) . . . yes C1 Fe1 C18 150.22(19) . . . yes P3 Fe1 C1 129.14(14) 2_555 . . yes C1 Fe1 C37 170.73(19) . . 2_555 yes C2 Fe1 C3 40.36(19) . . . yes C2 Fe1 C4 67.91(19) . . . yes C2 Fe1 C5 67.21(19) . . . yes C2 Fe1 C18 162.98(18) . . . yes P3 Fe1 C2 103.93(14) 2_555 . . yes C2 Fe1 C37 130.61(18) . . 2_555 yes C3 Fe1 C4 40.15(19) . . . yes C3 Fe1 C5 66.29(18) . . . yes C3 Fe1 C18 123.28(19) . . . yes P3 Fe1 C3 111.12(14) 2_555 . . yes C3 Fe1 C37 105.52(18) . . 2_555 yes C4 Fe1 C5 39.11(18) . . . yes C4 Fe1 C18 101.92(19) . . . yes P3 Fe1 C4 144.50(14) 2_555 . . yes C4 Fe1 C37 111.19(18) . . 2_555 yes C5 Fe1 C18 114.11(19) . . . yes P3 Fe1 C5 169.46(14) 2_555 . . yes C5 Fe1 C37 143.48(19) . . 2_555 yes P3 Fe1 C18 76.09(13) 2_555 . . yes C18 Fe1 C37 38.50(18) . . 2_555 yes P3 Fe1 C37 46.65(13) 2_555 . 2_555 yes P4 Fe2 P5 53.45(5) . . . yes P4 Fe2 C19 111.65(14) . . . yes P4 Fe2 C20 149.86(14) . . . yes P4 Fe2 C21 158.05(14) . . . yes P4 Fe2 C22 118.64(14) . . . yes P4 Fe2 C23 98.31(14) . . . yes P4 Fe2 C36 46.21(13) . . . yes P4 Fe2 P6 86.28(5) . . 2_445 yes P4 Fe2 C44 76.48(13) . . 2_445 yes P5 Fe2 C19 100.35(13) . . . yes P5 Fe2 C20 111.22(13) . . . yes P5 Fe2 C21 148.07(14) . . . yes P5 Fe2 C22 163.23(14) . . . yes P5 Fe2 C23 123.93(14) . . . yes P5 Fe2 C36 82.78(13) . . . yes P5 Fe2 P6 53.27(5) . . 2_445 yes P5 Fe2 C44 83.64(13) . . 2_445 yes C19 Fe2 C20 40.57(19) . . . yes C19 Fe2 C21 67.67(18) . . . yes C19 Fe2 C22 67.58(18) . . . yes C19 Fe2 C23 40.28(18) . . . yes C19 Fe2 C36 148.83(19) . . . yes P6 Fe2 C19 130.74(14) 2_445 . . yes C19 Fe2 C44 171.82(19) . . 2_445 yes C20 Fe2 C21 40.54(18) . . . yes C20 Fe2 C22 67.77(18) . . . yes C20 Fe2 C23 67.49(19) . . . yes C20 Fe2 C36 163.33(19) . . . yes P6 Fe2 C20 104.80(14) 2_445 . . yes C20 Fe2 C44 131.33(19) . . 2_445 yes C21 Fe2 C22 39.72(19) . . . yes C21 Fe2 C23 66.49(19) . . . yes C21 Fe2 C36 123.25(18) . . . yes P6 Fe2 C21 111.12(14) 2_445 . . yes C21 Fe2 C44 105.22(18) . . 2_445 yes C22 Fe2 C23 39.45(18) . . . yes C22 Fe2 C36 101.53(18) . . . yes P6 Fe2 C22 143.45(14) 2_445 . . yes C22 Fe2 C44 109.89(18) . . 2_445 yes C23 Fe2 C36 112.96(19) . . . yes P6 Fe2 C23 170.97(14) 2_445 . . yes C23 Fe2 C44 141.85(18) . . 2_445 yes P6 Fe2 C36 75.81(13) 2_445 . . yes C36 Fe2 C44 38.34(19) . . 2_445 yes P6 Fe2 C44 46.77(13) 2_445 . 2_445 yes Cu1 P1 Fe1 132.64(6) . . . yes Cu1 P1 P2 146.60(7) . . . yes Cu1 P1 C18 114.03(17) . . . yes Fe1 P1 P2 64.58(5) . . . yes Fe1 P1 C18 60.03(16) . . . yes P2 P1 C18 99.37(17) . . . yes Fe1 P2 P1 61.90(5) . . . yes Fe1 P2 P3 61.56(5) . . 2_555 yes P1 P2 P3 97.93(7) . . 2_555 yes Cu2 P3 C37 131.93(17) . . . yes Cu2 P3 Fe1 150.31(6) . . 2_555 yes Cu2 P3 P2 124.00(7) . . 2_555 yes Fe1 P3 C37 61.34(15) 2_555 . . yes P2 P3 C37 100.83(17) 2_555 . . yes Fe1 P3 P2 64.85(5) 2_555 . 2_555 yes Cu3 P4 Fe2 138.38(6) . . . yes Cu3 P4 P5 127.98(7) . . . yes Cu3 P4 C36 131.74(17) . . . yes Fe2 P4 P5 64.91(5) . . . yes Fe2 P4 C36 60.17(16) . . . yes P5 P4 C36 100.20(17) . . . yes Fe2 P5 P4 61.64(5) . . . yes Fe2 P5 P6 61.81(5) . . 2_445 yes P4 P5 P6 97.27(7) . . 2_445 yes Cu4 P6 C44 123.92(17) . . . yes Cu4 P6 Fe2 150.77(6) . . 2_445 yes Cu4 P6 P5 131.11(7) . . 2_445 yes Fe2 P6 C44 61.13(15) 2_445 . . yes P5 P6 C44 101.62(17) 2_445 . . yes Fe2 P6 P5 64.93(5) 2_445 . 2_445 yes Cu4 N1 C51 170.4(4) . . . yes Cu2 N2 C53 169.0(4) . . . yes Fe1 C1 C2 69.6(3) . . . yes Fe1 C1 C5 68.3(3) . . . yes Fe1 C1 C6 133.4(3) . . . yes C2 C1 C5 106.2(4) . . . no C2 C1 C6 135.5(4) . . . no C5 C1 C6 117.6(4) . . . no Fe1 C2 C1 70.3(3) . . . yes Fe1 C2 C3 68.1(3) . . . yes Fe1 C2 C10 133.3(3) . . . yes C1 C2 C3 106.5(4) . . . no C1 C2 C10 132.4(4) . . . no C3 C2 C10 120.4(4) . . . no Fe1 C3 C2 71.5(3) . . . yes Fe1 C3 C4 71.6(3) . . . yes C2 C3 C4 110.2(4) . . . no Fe1 C4 C3 68.2(3) . . . yes Fe1 C4 C5 69.2(3) . . . yes Fe1 C4 C14 135.2(3) . . . yes C3 C4 C5 106.0(4) . . . no C3 C4 C14 126.3(4) . . . no C5 C4 C14 126.8(4) . . . no Fe1 C5 C1 71.4(3) . . . yes Fe1 C5 C4 71.7(3) . . . yes C1 C5 C4 111.0(4) . . . no C1 C6 C7 111.9(4) . . . no C1 C6 C8 105.4(4) . . . no C1 C6 C9 117.0(4) . . . no C7 C6 C8 107.4(4) . . . no C7 C6 C9 106.3(4) . . . no C8 C6 C9 108.5(4) . . . no C2 C10 C11 116.4(4) . . . no C2 C10 C12 107.1(4) . . . no C2 C10 C13 109.8(4) . . . no C11 C10 C12 109.9(4) . . . no C11 C10 C13 106.3(4) . . . no C12 C10 C13 107.0(4) . . . no C4 C14 C15 111.8(4) . . . no C4 C14 C16 104.9(4) . . . no C4 C14 C17 112.7(4) . . . no C15 C14 C16 107.9(4) . . . no C15 C14 C17 110.2(4) . . . no C16 C14 C17 109.1(4) . . . no Fe1 C18 P1 74.03(18) . . . yes Fe1 C18 C37 72.2(3) . . 2_555 yes P1 C18 C37 123.6(4) . . 2_555 yes Fe2 C19 C20 69.5(3) . . . yes Fe2 C19 C23 68.5(3) . . . yes Fe2 C19 C24 135.6(3) . . . yes C20 C19 C23 106.2(4) . . . no C20 C19 C24 134.8(4) . . . no C23 C19 C24 117.7(4) . . . no Fe2 C20 C19 70.0(3) . . . yes Fe2 C20 C21 68.3(3) . . . yes Fe2 C20 C28 133.3(3) . . . yes C19 C20 C21 106.3(4) . . . no C19 C20 C28 132.3(4) . . . no C21 C20 C28 120.6(4) . . . no Fe2 C21 C20 71.1(3) . . . yes Fe2 C21 C22 72.2(3) . . . yes C20 C21 C22 110.4(4) . . . no Fe2 C22 C21 68.1(3) . . . yes Fe2 C22 C23 68.6(3) . . . yes Fe2 C22 C32 136.6(3) . . . yes C21 C22 C23 106.2(4) . . . no C21 C22 C32 126.8(4) . . . no C23 C22 C32 126.1(4) . . . no Fe2 C23 C19 71.2(3) . . . yes Fe2 C23 C22 72.0(3) . . . yes C19 C23 C22 110.8(4) . . . no C19 C24 C25 111.0(4) . . . no C19 C24 C26 116.6(4) . . . no C19 C24 C27 106.1(4) . . . no C25 C24 C26 106.6(4) . . . no C25 C24 C27 107.8(4) . . . no C26 C24 C27 108.5(4) . . . no C20 C28 C29 107.9(4) . . . no C20 C28 C30 114.7(4) . . . no C20 C28 C31 110.0(4) . . . no C29 C28 C30 110.8(4) . . . no C29 C28 C31 106.3(4) . . . no C30 C28 C31 107.0(4) . . . no C22 C32 C33 110.7(4) . . . no C22 C32 C34 105.4(4) . . . no C22 C32 C35 113.0(4) . . . no C33 C32 C34 109.5(4) . . . no C33 C32 C35 109.6(4) . . . no C34 C32 C35 108.6(4) . . . no Fe2 C36 P4 73.62(17) . . . yes Fe2 C36 C44 72.4(3) . . 2_445 yes P4 C36 C44 123.1(4) . . 2_445 yes P3 C37 C38 121.8(4) . . . yes Fe1 C37 P3 72.01(17) 2_555 . . yes P3 C37 C18 118.3(4) . . 2_555 yes Fe1 C37 C38 132.0(3) 2_555 . . yes C18 C37 C38 119.9(4) 2_555 . . no Fe1 C37 C18 69.3(3) 2_555 . 2_555 yes C37 C38 C39 123.1(4) . . . no C37 C38 C43 119.3(4) . . . no C39 C38 C43 117.6(4) . . . no C38 C39 C40 120.5(5) . . . no C39 C40 C41 120.9(5) . . . no C40 C41 C42 118.7(4) . . . no C41 C42 C43 120.7(5) . . . no C38 C43 C42 121.5(4) . . . no P6 C44 C45 120.2(4) . . . yes Fe2 C44 P6 72.09(17) 2_445 . . yes P6 C44 C36 117.8(4) . . 2_445 yes Fe2 C44 C45 128.9(3) 2_445 . . yes C36 C44 C45 122.0(4) 2_445 . . no Fe2 C44 C36 69.3(3) 2_445 . 2_445 yes C44 C45 C46 120.6(4) . . . no C44 C45 C50 121.9(4) . . . no C46 C45 C50 117.5(4) . . . no C45 C46 C47 120.9(4) . . . no C46 C47 C48 120.0(4) . . . no C47 C48 C49 119.8(4) . . . no C48 C49 C50 120.0(5) . . . no C45 C50 C49 121.8(4) . . . no N1 C51 C52 179.3(5) . . . yes N2 C53 C54 178.1(5) . . . yes Fe1 C3 H3A 124.00 . . . no C2 C3 H3A 125.00 . . . no C4 C3 H3A 125.00 . . . no Fe1 C5 H5A 124.00 . . . no C1 C5 H5A 125.00 . . . no C4 C5 H5A 124.00 . . . no C6 C7 H7A 109.00 . . . no C6 C7 H7B 109.00 . . . no C6 C7 H7C 109.00 . . . no H7A C7 H7B 109.00 . . . no H7A C7 H7C 110.00 . . . no H7B C7 H7C 109.00 . . . no C6 C8 H8A 109.00 . . . no C6 C8 H8B 109.00 . . . no C6 C8 H8C 110.00 . . . no H8A C8 H8B 109.00 . . . no H8A C8 H8C 110.00 . . . no H8B C8 H8C 109.00 . . . no C6 C9 H9A 110.00 . . . no C6 C9 H9B 109.00 . . . no C6 C9 H9C 110.00 . . . no H9A C9 H9B 109.00 . . . no H9A C9 H9C 109.00 . . . no H9B C9 H9C 109.00 . . . no C10 C11 H11A 109.00 . . . no C10 C11 H11B 110.00 . . . no C10 C11 H11C 109.00 . . . no H11A C11 H11B 109.00 . . . no H11A C11 H11C 109.00 . . . no H11B C11 H11C 109.00 . . . no C10 C12 H12A 110.00 . . . no C10 C12 H12B 109.00 . . . no C10 C12 H12C 110.00 . . . no H12A C12 H12B 109.00 . . . no H12A C12 H12C 109.00 . . . no H12B C12 H12C 109.00 . . . no C10 C13 H13A 109.00 . . . no C10 C13 H13B 109.00 . . . no C10 C13 H13C 109.00 . . . no H13A C13 H13B 109.00 . . . no H13A C13 H13C 109.00 . . . no H13B C13 H13C 109.00 . . . no C14 C15 H15A 109.00 . . . no C14 C15 H15B 110.00 . . . no C14 C15 H15C 109.00 . . . no H15A C15 H15B 109.00 . . . no H15A C15 H15C 109.00 . . . no H15B C15 H15C 109.00 . . . no C14 C16 H16A 109.00 . . . no C14 C16 H16B 110.00 . . . no C14 C16 H16C 109.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 109.00 . . . no H16B C16 H16C 109.00 . . . no C14 C17 H17A 110.00 . . . no C14 C17 H17B 109.00 . . . no C14 C17 H17C 109.00 . . . no H17A C17 H17B 109.00 . . . no H17A C17 H17C 109.00 . . . no H17B C17 H17C 109.00 . . . no Fe1 C18 H18A 128.00 . . . no P1 C18 H18A 118.00 . . . no C37 C18 H18A 118.00 2_555 . . no Fe2 C21 H21A 124.00 . . . no C20 C21 H21A 125.00 . . . no C22 C21 H21A 125.00 . . . no Fe2 C23 H23A 124.00 . . . no C19 C23 H23A 125.00 . . . no C22 C23 H23A 125.00 . . . no C24 C25 H25A 109.00 . . . no C24 C25 H25B 110.00 . . . no C24 C25 H25C 109.00 . . . no H25A C25 H25B 109.00 . . . no H25A C25 H25C 109.00 . . . no H25B C25 H25C 109.00 . . . no C24 C26 H26A 109.00 . . . no C24 C26 H26B 109.00 . . . no C24 C26 H26C 110.00 . . . no H26A C26 H26B 109.00 . . . no H26A C26 H26C 109.00 . . . no H26B C26 H26C 110.00 . . . no C24 C27 H27A 110.00 . . . no C24 C27 H27B 110.00 . . . no C24 C27 H27C 109.00 . . . no H27A C27 H27B 109.00 . . . no H27A C27 H27C 109.00 . . . no H27B C27 H27C 110.00 . . . no C28 C29 H29A 109.00 . . . no C28 C29 H29B 109.00 . . . no C28 C29 H29C 109.00 . . . no H29A C29 H29B 109.00 . . . no H29A C29 H29C 109.00 . . . no H29B C29 H29C 109.00 . . . no C28 C30 H30A 110.00 . . . no C28 C30 H30B 109.00 . . . no C28 C30 H30C 110.00 . . . no H30A C30 H30B 109.00 . . . no H30A C30 H30C 109.00 . . . no H30B C30 H30C 110.00 . . . no C28 C31 H31A 110.00 . . . no C28 C31 H31B 109.00 . . . no C28 C31 H31C 109.00 . . . no H31A C31 H31B 109.00 . . . no H31A C31 H31C 109.00 . . . no H31B C31 H31C 109.00 . . . no C32 C33 H33A 110.00 . . . no C32 C33 H33B 109.00 . . . no C32 C33 H33C 110.00 . . . no H33A C33 H33B 109.00 . . . no H33A C33 H33C 109.00 . . . no H33B C33 H33C 109.00 . . . no C32 C34 H34A 109.00 . . . no C32 C34 H34B 109.00 . . . no C32 C34 H34C 109.00 . . . no H34A C34 H34B 110.00 . . . no H34A C34 H34C 109.00 . . . no H34B C34 H34C 110.00 . . . no C32 C35 H35A 109.00 . . . no C32 C35 H35B 109.00 . . . no C32 C35 H35C 109.00 . . . no H35A C35 H35B 109.00 . . . no H35A C35 H35C 110.00 . . . no H35B C35 H35C 109.00 . . . no Fe2 C36 H36A 128.00 . . . no P4 C36 H36A 118.00 . . . no C44 C36 H36A 118.00 2_445 . . no C38 C39 H39 120.00 . . . no C40 C39 H39 120.00 . . . no C39 C40 H40 120.00 . . . no C41 C40 H40 120.00 . . . no C40 C41 H41 121.00 . . . no C42 C41 H41 121.00 . . . no C41 C42 H42 120.00 . . . no C43 C42 H42 120.00 . . . no C38 C43 H43 119.00 . . . no C42 C43 H43 119.00 . . . no C45 C46 H46 120.00 . . . no C47 C46 H46 120.00 . . . no C46 C47 H47 120.00 . . . no C48 C47 H47 120.00 . . . no C47 C48 H48 120.00 . . . no C49 C48 H48 120.00 . . . no C48 C49 H49 120.00 . . . no C50 C49 H49 120.00 . . . no C45 C50 H50 119.00 . . . no C49 C50 H50 119.00 . . . no C51 C52 H52A 109.00 . . . no C51 C52 H52B 109.00 . . . no C51 C52 H52C 109.00 . . . no H52A C52 H52B 110.00 . . . no H52A C52 H52C 110.00 . . . no H52B C52 H52C 110.00 . . . no C53 C54 H54A 109.00 . . . no C53 C54 H54B 109.00 . . . no C53 C54 H54C 110.00 . . . no H54A C54 H54B 109.00 . . . no H54A C54 H54C 109.00 . . . no H54B C54 H54C 110.00 . . . no 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 Cu2 Br1 Cu1 Br2 24.07(3) . . . . no Cu2 Br1 Cu1 Br3 130.25(4) . . . . no Cu2 Br1 Cu1 P1 -95.87(4) . . . . no Cu1 Br1 Cu2 N2 -139.06(11) . . . . no Cu1 Br1 Cu2 Br2 -26.71(3) . . . . no Cu1 Br1 Cu2 P3 85.77(4) . . . . no Cu3 Br2 Cu1 Br1 95.73(3) . . . . no Cu3 Br2 Cu1 Br3 -23.00(3) . . . . no Cu4 Br2 Cu1 Br1 119.04(4) . . . . no Cu2 Br2 Cu1 Br3 -143.00(3) . . . . no Cu2 Br2 Cu1 Br1 -24.27(3) . . . . no Cu4 Br2 Cu1 P1 -134.64(5) . . . . no Cu2 Br2 Cu4 Br4 126.05(4) . . . . no Cu3 Br2 Cu4 Br4 25.35(3) . . . . no Cu1 Br2 Cu4 P6 -112.35(5) . . . . no Cu4 Br2 Cu1 Br3 0.31(6) . . . . no Cu2 Br2 Cu1 P1 82.05(5) . . . . no Cu3 Br2 Cu1 P1 -157.95(5) . . . . no Cu1 Br2 Cu2 Br1 24.61(3) . . . . no Cu3 Br2 Cu2 Br1 -33.85(3) . . . . no Cu4 Br2 Cu2 Br1 -120.13(4) . . . . no Cu1 Br2 Cu2 P3 -83.49(4) . . . . no Cu3 Br2 Cu2 P3 -141.95(4) . . . . no Cu4 Br2 Cu2 P3 131.77(5) . . . . no Cu1 Br2 Cu2 N2 134.02(14) . . . . no Cu3 Br2 Cu2 N2 75.55(14) . . . . no Cu4 Br2 Cu2 N2 -10.72(15) . . . . no Cu1 Br2 Cu3 Br3 23.07(3) . . . . no Cu2 Br2 Cu3 Br3 83.77(3) . . . . no Cu4 Br2 Cu3 Br3 -141.22(3) . . . . no Cu1 Br2 Cu3 Br4 139.02(3) . . . . no Cu2 Br2 Cu3 Br4 -160.28(3) . . . . no Cu4 Br2 Cu3 Br4 -25.27(3) . . . . no Cu1 Br2 Cu3 P4 -105.27(5) . . . . no Cu2 Br2 Cu3 P4 -44.57(5) . . . . no Cu4 Br2 Cu3 P4 90.44(4) . . . . no Cu3 Br2 Cu4 N1 134.86(14) . . . . no Cu3 Br2 Cu4 P6 -89.80(4) . . . . no Cu1 Br2 Cu4 N1 112.32(14) . . . . no Cu2 Br2 Cu4 P6 10.90(6) . . . . no Cu2 Br2 Cu4 N1 -124.44(14) . . . . no Cu1 Br2 Cu4 Br4 2.80(5) . . . . no Cu1 Br3 Cu3 P4 96.84(5) . . . . no Cu1 Br3 Cu3 Br4 -129.97(3) . . . . no Cu3 Br3 Cu1 Br2 23.68(3) . . . . no Cu3 Br3 Cu1 P1 156.20(5) . . . . no Cu1 Br3 Cu3 Br2 -25.08(3) . . . . no Cu3 Br3 Cu1 Br1 -80.04(3) . . . . no Cu4 Br4 Cu3 P4 -87.88(4) . . . . no Cu4 Br4 Cu3 Br2 26.33(3) . . . . no Cu4 Br4 Cu3 Br3 135.13(3) . . . . no Cu3 Br4 Cu4 Br2 -26.29(3) . . . . no Cu3 Br4 Cu4 P6 92.98(5) . . . . no Cu3 Br4 Cu4 N1 -132.38(15) . . . . no Br1 Cu1 P1 Fe1 -102.70(8) . . . . no Br2 Cu1 P1 Fe1 153.29(6) . . . . no Br3 Cu1 P1 Fe1 27.95(10) . . . . no Br1 Cu1 P1 P2 147.63(11) . . . . no Br2 Cu1 P1 P2 43.61(13) . . . . no Br3 Cu1 P1 P2 -81.72(12) . . . . no Br1 Cu1 P1 C18 -32.14(17) . . . . no Br2 Cu1 P1 C18 -136.16(17) . . . . no Br3 Cu1 P1 C18 98.51(17) . . . . no Br2 Cu2 P3 Fe1 -120.27(12) . . . 2_555 no N2 Cu2 P3 Fe1 12.2(2) . . . 2_555 no Br1 Cu2 P3 P2 33.15(8) . . . 2_555 no Br1 Cu2 P3 C37 -122.4(2) . . . . no Br2 Cu2 P3 C37 -14.4(2) . . . . no N2 Cu2 P3 C37 118.1(3) . . . . no Br1 Cu2 P3 Fe1 131.68(12) . . . 2_555 no Br2 Cu2 P3 P2 141.21(6) . . . 2_555 no N2 Cu2 P3 P2 -86.30(16) . . . 2_555 no Br2 Cu3 P4 C36 60.0(2) . . . . no Br3 Cu3 P4 P5 124.75(7) . . . . no Br4 Cu3 P4 P5 -9.15(9) . . . . no Br3 Cu3 P4 Fe2 30.80(11) . . . . no Br4 Cu3 P4 Fe2 -103.09(9) . . . . no Br2 Cu3 P4 P5 -115.99(7) . . . . no Br3 Cu3 P4 C36 -59.2(2) . . . . no Br4 Cu3 P4 C36 166.9(2) . . . . no Br2 Cu3 P4 Fe2 150.07(8) . . . . no N1 Cu4 P6 P5 133.87(18) . . . 2_445 no N1 Cu4 P6 Fe2 19.8(2) . . . 2_445 no Br2 Cu4 P6 Fe2 -105.69(13) . . . 2_445 no Br4 Cu4 P6 C44 55.3(2) . . . . no N1 Cu4 P6 C44 -70.8(3) . . . . no Br4 Cu4 P6 Fe2 145.87(12) . . . 2_445 no Br2 Cu4 P6 P5 8.38(10) . . . 2_445 no Br4 Cu4 P6 P5 -100.07(8) . . . 2_445 no Br2 Cu4 P6 C44 163.73(19) . . . . no C2 Fe1 P1 Cu1 -76.8(3) . . . . no C1 Fe1 C2 C10 -130.3(6) . . . . no C3 Fe1 P1 Cu1 25.5(4) . . . . no P2 Fe1 P1 Cu1 -144.98(10) . . . . no C2 Fe1 P2 P1 -150.58(15) . . . . no C1 Fe1 P1 Cu1 -58.90(17) . . . . no C5 Fe1 P2 P1 -74.33(17) . . . . no C4 Fe1 P1 Cu1 16.46(18) . . . . no C3 Fe1 P2 P1 -172.9(3) . . . . no C37 Fe1 P2 P1 78.27(14) 2_555 . . . no P1 Fe1 P2 P3 -117.84(7) . . . 2_555 no C1 Fe1 P2 P3 131.67(14) . . . 2_555 no C2 Fe1 P2 P3 91.58(15) . . . 2_555 no C3 Fe1 P2 P3 69.3(3) . . . 2_555 no C5 Fe1 P2 P3 167.83(17) . . . 2_555 no C18 Fe1 P2 P3 -78.39(14) . . . 2_555 no C3 Fe1 C2 C10 111.7(5) . . . . no C4 Fe1 C2 C10 148.9(5) . . . . no C1 Fe1 P2 P1 -110.49(14) . . . . no P1 Fe1 C5 C4 124.1(3) . . . . no P2 Fe1 C5 C4 175.6(2) . . . . no C1 Fe1 C5 C4 -120.7(4) . . . . no C18 Fe1 P2 P1 39.45(14) . . . . no P3 Fe1 P2 P1 117.84(7) 2_555 . . . no C3 Fe1 P1 C18 -70.7(4) . . . . no C4 Fe1 P1 C18 -79.7(2) . . . . no C5 Fe1 P1 C18 -115.8(2) . . . . no P3 Fe1 P1 C18 73.38(18) 2_555 . . . no C37 Fe1 P1 C18 27.4(2) 2_555 . . . no P3 Fe1 C37 C18 131.0(3) . 2_555 . 2_555 no C18 Fe1 C37 C38 112.1(6) 2_555 2_555 . . no C37 Fe1 P3 Cu2 125.4(2) . 2_555 . . no P1 Fe1 P3 Cu2 -160.47(13) 2_555 2_555 . . no P2 Fe1 P3 Cu2 -115.09(14) 2_555 2_555 . . no C1 Fe1 P3 Cu2 -43.6(2) 2_555 2_555 . . no C2 Fe1 P3 Cu2 -8.12(19) 2_555 2_555 . . no C3 Fe1 P3 Cu2 33.7(2) 2_555 2_555 . . no C4 Fe1 P3 Cu2 63.2(3) 2_555 2_555 . . no C18 Fe1 P3 Cu2 154.34(19) 2_555 2_555 . . no P1 Fe1 P3 C37 74.16(18) 2_555 2_555 . . no P2 Fe1 P3 C37 119.55(18) 2_555 2_555 . . no C1 Fe1 P3 C37 -169.0(2) 2_555 2_555 . . no C2 Fe1 P3 C37 -133.5(2) 2_555 2_555 . . no C3 Fe1 P3 C37 -91.7(2) 2_555 2_555 . . no C4 Fe1 P3 C37 -62.1(3) 2_555 2_555 . . no C18 Fe1 P3 C37 29.0(2) 2_555 2_555 . . no C37 Fe1 P3 P2 -119.55(18) . 2_555 . 2_555 no C37 Fe1 P2 P3 -39.58(14) 2_555 . . 2_555 no C18 Fe1 C5 C1 -160.4(3) . . . . no C37 Fe1 C5 C1 166.4(3) 2_555 . . . no C18 Fe1 P1 P2 -118.82(19) . . . . no P3 Fe1 P1 P2 -45.44(5) 2_555 . . . no C37 Fe1 P1 P2 -91.45(14) 2_555 . . . no P2 Fe1 P1 C18 118.82(19) . . . . no C1 Fe1 P1 C18 -155.1(2) . . . . no C2 Fe1 P1 C18 -173.0(3) . . . . no C1 Fe1 C2 C3 118.0(4) . . . . no C4 Fe1 C2 C3 37.2(3) . . . . no C5 Fe1 C2 C3 79.7(3) . . . . no P3 Fe1 C2 C3 -106.4(3) 2_555 . . . no C37 Fe1 C2 C3 -62.3(3) 2_555 . . . no P1 Fe1 C2 C10 -104.1(5) . . . . no P2 Fe1 C2 C10 -50.7(5) . . . . no C5 Fe1 C37 C38 58.7(6) 2_555 2_555 . . no C5 Fe1 C3 C4 37.5(3) . . . . no C18 Fe1 C3 C4 -66.7(3) . . . . no C5 Fe1 C2 C10 -168.6(5) . . . . no P3 Fe1 C2 C10 5.3(5) 2_555 . . . no C37 Fe1 C2 C10 49.4(5) 2_555 . . . no C3 Fe1 C1 C2 38.3(3) . . . . no C4 Fe1 C1 C2 82.0(3) . . . . no C5 Fe1 C1 C2 118.0(4) . . . . no C18 Fe1 C1 C2 156.0(3) . . . . no P3 Fe1 C1 C2 -61.0(3) 2_555 . . . no P1 Fe1 C1 C5 75.6(3) . . . . no P2 Fe1 C1 C5 130.2(2) . . . . no C2 Fe1 C1 C5 -118.0(4) . . . . no C3 Fe1 C1 C5 -79.7(3) . . . . no C4 Fe1 C1 C5 -36.0(3) . . . . no C18 Fe1 C1 C5 38.1(5) . . . . no P3 Fe1 C1 C5 -179.0(2) 2_555 . . . no P1 Fe1 C1 C6 -32.4(5) . . . . no P2 Fe1 C1 C6 22.2(5) . . . . no P1 Fe1 C3 C2 -132.2(3) . . . . no P2 Fe1 C3 C2 33.0(4) . . . . no C1 Fe1 C3 C2 -38.1(3) . . . . no C4 Fe1 C3 C2 -119.6(4) . . . . no C5 Fe1 C3 C2 -82.2(3) . . . . no C18 Fe1 C3 C2 173.7(3) . . . . no P3 Fe1 C3 C2 86.8(3) 2_555 . . . no C37 Fe1 C3 C2 135.8(3) 2_555 . . . no P1 Fe1 C3 C4 -12.5(5) . . . . no P2 Fe1 C3 C4 152.6(2) . . . . no C1 Fe1 C3 C4 81.5(3) . . . . no C2 Fe1 C3 C4 119.6(4) . . . . no C4 Fe1 C37 C38 29.7(5) 2_555 2_555 . . no C5 Fe1 C18 P1 77.5(2) . . . . no P3 Fe1 C3 C4 -153.6(2) 2_555 . . . no C37 Fe1 C3 C4 -104.6(3) 2_555 . . . no P2 Fe1 C18 C37 88.8(3) . . . 2_555 no C1 Fe1 C18 C37 -174.3(3) . . . 2_555 no C3 Fe1 C18 C37 -71.9(3) . . . 2_555 no C4 Fe1 C18 C37 -109.1(3) . . . 2_555 no C5 Fe1 C18 C37 -148.4(3) . . . 2_555 no P1 Fe1 C4 C3 174.6(2) . . . . no C5 Fe1 P1 Cu1 -19.59(16) . . . . no C18 Fe1 P1 Cu1 96.2(2) . . . . no P3 Fe1 P1 Cu1 169.58(8) 2_555 . . . no C37 Fe1 P1 Cu1 123.58(16) 2_555 . . . no C1 Fe1 P1 P2 86.08(15) . . . . no C2 Fe1 P1 P2 68.2(3) . . . . no C3 Fe1 P1 P2 170.5(4) . . . . no C4 Fe1 P1 P2 161.44(15) . . . . no C5 Fe1 P1 P2 125.39(14) . . . . no C3 Fe1 C4 C5 118.0(4) . . . . no C18 Fe1 C4 C5 -113.7(3) . . . . no P3 Fe1 C4 C5 163.6(2) 2_555 . . . no C37 Fe1 C4 C5 -152.8(3) 2_555 . . . no P1 Fe1 C4 C14 54.3(5) . . . . no C1 Fe1 C4 C14 158.8(5) . . . . no C2 Fe1 C4 C14 -157.7(5) . . . . no C3 Fe1 C4 C14 -120.2(6) . . . . no C5 Fe1 C4 C14 121.8(6) . . . . no C18 Fe1 C4 C14 8.1(5) . . . . no P3 Fe1 C4 C14 -74.6(5) 2_555 . . . no C37 Fe1 C4 C14 -31.1(5) 2_555 . . . no C4 Fe1 C18 P1 116.78(18) . . . . no P2 Fe1 C5 C1 -63.8(3) . . . . no P3 Fe1 C18 P1 -99.62(14) 2_555 . . . no C37 Fe1 C18 P1 -134.1(3) 2_555 . . . no P1 Fe1 C1 C2 -166.4(2) . . . . no P2 Fe1 C1 C2 -111.9(2) . . . . no C3 Fe1 C1 C6 172.4(5) . . . . no C4 Fe1 C1 C6 -144.0(5) . . . . no C5 Fe1 C1 C6 -108.0(5) . . . . no C18 Fe1 C1 C6 -69.9(6) . . . . no P3 Fe1 C18 C37 34.5(2) 2_555 . . 2_555 no C18 Fe1 C5 C4 79.0(3) . . . . no C1 Fe1 C4 C3 -80.9(3) . . . . no C2 Fe1 C4 C3 -37.4(3) . . . . no C5 Fe1 C4 C3 -118.0(4) . . . . no P1 Fe1 C5 C1 -115.3(2) . . . . no C3 Fe1 C37 C38 -12.3(5) 2_555 2_555 . . no C2 Fe1 C5 C1 38.1(3) . . . . no C3 Fe1 C5 C1 82.2(3) . . . . no C4 Fe1 C5 C1 120.7(4) . . . . no C2 Fe1 C1 C6 134.1(6) . . . . no C4 Fe1 C2 C1 -80.8(3) . . . . no C5 Fe1 C2 C1 -38.3(3) . . . . no P3 Fe1 C2 C1 135.6(2) 2_555 . . . no C37 Fe1 C2 C1 179.7(3) 2_555 . . . no P3 Fe1 C1 C6 73.0(5) 2_555 . . . no P2 Fe1 C2 C3 -162.3(2) . . . . no C37 Fe1 C5 C4 45.7(4) 2_555 . . . no P2 Fe1 C18 P1 -45.31(12) . . . . no C1 Fe1 C18 P1 51.6(4) . . . . no C3 Fe1 C18 P1 154.03(18) . . . . no C18 Fe1 C4 C3 128.3(3) . . . . no P3 Fe1 C4 C3 45.6(4) 2_555 . . . no P1 Fe1 C2 C1 26.2(4) . . . . no P2 Fe1 C2 C1 79.7(3) . . . . no P1 Fe1 C18 C37 134.1(3) . . . 2_555 no P1 Fe1 C4 C5 -67.4(3) . . . . no C1 Fe1 C4 C5 37.1(3) . . . . no C2 Fe1 C4 C5 80.6(3) . . . . no P2 Fe1 C37 P3 -44.84(12) 2_555 2_555 . . no P1 Fe1 C2 C3 144.2(3) . . . . no C3 Fe1 C37 P3 104.60(19) 2_555 2_555 . . no C18 Fe1 C37 P3 -131.0(3) 2_555 2_555 . . no P3 Fe1 C37 C38 -116.9(5) . 2_555 . . no P1 Fe1 C37 C38 144.2(5) 2_555 2_555 . . no P2 Fe1 C37 C38 -161.8(5) 2_555 2_555 . . no C2 Fe1 C37 C38 -48.8(5) 2_555 2_555 . . no C3 Fe1 C2 C1 -118.0(4) . . . . no C2 Fe1 C37 P3 68.1(3) 2_555 2_555 . . no P1 Fe1 C37 P3 -98.89(14) 2_555 2_555 . . no C5 Fe1 C37 P3 175.6(2) 2_555 2_555 . . no C2 Fe1 C5 C4 -82.5(3) . . . . no C3 Fe1 C5 C4 -38.4(3) . . . . no C4 Fe1 C37 P3 146.60(17) 2_555 2_555 . . no C37 Fe1 C4 C3 89.2(3) 2_555 . . . no P6 Fe2 P4 Cu3 165.48(9) 2_445 . . . no C19 Fe2 P4 P5 -86.93(15) . . . . no C44 Fe2 P4 P5 92.09(14) 2_445 . . . no C44 Fe2 P4 Cu3 -148.17(16) 2_445 . . . no C36 Fe2 P4 P5 119.60(19) . . . . no P6 Fe2 P4 P5 45.74(5) 2_445 . . . no C44 Fe2 P6 P5 120.79(19) . 2_445 . 2_445 no C36 Fe2 P6 C44 -29.2(2) 2_445 2_445 . . no C22 Fe2 P6 C44 61.1(3) 2_445 2_445 . . no C21 Fe2 P6 C44 91.3(2) 2_445 2_445 . . no C23 Fe2 P4 P5 -126.44(14) . . . . no C44 Fe2 P5 P6 39.04(14) 2_445 . . 2_445 no C22 Fe2 P4 C36 78.0(2) . . . . no P4 Fe2 C20 C21 -145.9(3) . . . . no P5 Fe2 C20 C21 161.2(2) . . . . no C19 Fe2 C20 C21 -117.8(4) . . . . no C19 Fe2 P4 C36 153.5(2) . . . . no C21 Fe2 C22 C32 120.9(6) . . . . no C20 Fe2 P4 C36 172.7(3) . . . . no C44 Fe2 C20 C19 178.5(3) 2_445 . . . no P5 Fe2 C36 P4 44.76(12) . . . . no C19 Fe2 C36 P4 -53.3(4) . . . . no C21 Fe2 C36 P4 -155.22(18) . . . . no C23 Fe2 P4 C36 114.0(2) . . . . no P6 Fe2 P4 C36 -73.86(18) 2_445 . . . no C36 Fe2 C19 C23 -38.3(5) . . . . no P6 Fe2 C19 C23 178.7(2) 2_445 . . . no C20 Fe2 P4 P5 -67.7(3) . . . . no C21 Fe2 P4 P5 -170.7(4) . . . . no C22 Fe2 P4 P5 -162.40(15) . . . . no C19 Fe2 C23 C22 120.4(4) . . . . no P5 Fe2 P4 C36 -119.60(19) . . . . no C21 Fe2 C23 C22 37.7(3) . . . . no C36 Fe2 C23 C22 -80.0(3) . . . . no C21 Fe2 P4 C36 69.7(4) . . . . no C23 Fe2 P5 P4 73.63(17) . . . . no C36 Fe2 P5 P4 -39.25(14) . . . . no P6 Fe2 P5 P4 -116.90(6) 2_445 . . . no C44 Fe2 P5 P4 -77.86(14) 2_445 . . . no P4 Fe2 P5 P6 116.90(6) . . . 2_445 no C19 Fe2 P5 P6 -133.75(14) . . . 2_445 no C20 Fe2 P5 P6 -92.99(15) . . . 2_445 no C21 Fe2 P5 P6 -69.7(3) . . . 2_445 no C23 Fe2 P5 P6 -169.47(17) . . . 2_445 no C36 Fe2 P5 P6 77.65(14) . . . 2_445 no C23 Fe2 C20 C19 38.2(3) . . . . no C20 Fe2 C23 C22 81.9(3) . . . . no C44 Fe2 C22 C23 151.2(3) 2_445 . . . no P4 Fe2 C22 C32 -54.3(5) . . . . no C44 Fe2 C23 C22 -47.1(4) 2_445 . . . no C22 Fe2 C20 C21 -36.8(3) . . . . no C23 Fe2 C22 C32 -120.4(6) . . . . no C36 Fe2 C22 C32 -8.2(5) . . . . no P6 Fe2 C22 C32 73.5(6) 2_445 . . . no C44 Fe2 C22 C32 30.8(5) 2_445 . . . no C44 Fe2 C20 C21 60.7(4) 2_445 . . . no C44 Fe2 P4 C36 -27.5(2) 2_445 . . . no P4 Fe2 C36 C44 -133.6(3) . . . 2_445 no P5 Fe2 C36 C44 -88.9(3) . . . 2_445 no P6 Fe2 C21 C22 152.0(2) 2_445 . . . no C44 Fe2 C21 C22 103.0(3) 2_445 . . . no P6 Fe2 C20 C19 -136.8(2) 2_445 . . . no C21 Fe2 C36 C44 71.2(3) . . . 2_445 no C19 Fe2 P5 P4 109.35(14) . . . . no C19 Fe2 C22 C32 -157.5(5) . . . . no P5 Fe2 P4 Cu3 119.74(11) . . . . no C19 Fe2 P4 Cu3 32.81(17) . . . . no C20 Fe2 P4 Cu3 52.0(3) . . . . no C21 Fe2 P4 Cu3 -51.0(4) . . . . no C22 Fe2 P4 Cu3 -42.67(18) . . . . no C23 Fe2 P4 Cu3 -6.70(16) . . . . no C36 Fe2 P4 Cu3 -120.7(2) . . . . no C22 Fe2 C19 C23 36.4(3) . . . . no P5 Fe2 C23 C19 62.7(3) . . . . no C20 Fe2 C23 C19 -38.5(3) . . . . no P4 Fe2 C19 C24 31.4(5) . . . . no P5 Fe2 C19 C24 -23.3(5) . . . . no P4 Fe2 C21 C20 131.2(3) . . . . no P5 Fe2 C21 C20 -34.6(4) . . . . no C19 Fe2 C21 C20 38.4(3) . . . . no C22 Fe2 C21 C20 119.8(4) . . . . no C23 Fe2 C21 C20 82.3(3) . . . . no C36 Fe2 C21 C20 -174.8(3) . . . . no P6 Fe2 C21 C20 -88.3(3) 2_445 . . . no C44 Fe2 C21 C20 -137.3(3) 2_445 . . . no P4 Fe2 C21 C22 11.4(5) . . . . no C22 Fe2 C36 P4 -118.82(18) . . . . no C23 Fe2 C36 P4 -79.1(2) . . . . no P6 Fe2 C36 P4 98.61(14) 2_445 . . . no C44 Fe2 C36 P4 133.6(3) 2_445 . . . no C23 Fe2 C21 C22 -37.4(3) . . . . no C36 Fe2 C21 C22 65.5(3) . . . . no C19 Fe2 C36 C44 173.1(3) . . . 2_445 no P4 Fe2 C19 C20 165.3(2) . . . . no P5 Fe2 C19 C20 110.6(2) . . . . no P4 Fe2 C44 P6 97.73(14) 2_445 2_445 . . no C20 Fe2 P5 P4 150.11(15) . . . . no C21 Fe2 P5 P4 173.4(3) . . . . no C19 Fe2 C22 C21 81.6(3) . . . . no C20 Fe2 C22 C21 37.6(3) . . . . no C23 Fe2 C22 C21 118.7(4) . . . . no C36 Fe2 C22 C21 -129.1(3) . . . . no P6 Fe2 C22 C21 -47.4(4) 2_445 . . . no C44 Fe2 C22 C21 -90.1(3) 2_445 . . . no P4 Fe2 C22 C23 66.1(3) . . . . no C19 Fe2 C22 C23 -37.1(3) . . . . no C20 Fe2 C22 C23 -81.1(3) . . . . no C21 Fe2 C22 C23 -118.7(4) . . . . no C36 Fe2 C22 C23 112.3(3) . . . . no P6 Fe2 C22 C23 -166.1(2) 2_445 . . . no C22 Fe2 C44 C45 -31.6(5) 2_445 2_445 . . no C23 Fe2 C44 C45 -61.3(6) 2_445 2_445 . . no C36 Fe2 C44 C45 -115.1(5) 2_445 2_445 . . no C20 Fe2 C22 C32 158.5(5) . . . . no P6 Fe2 C19 C24 -73.1(5) 2_445 . . . no P6 Fe2 C19 C20 60.8(3) 2_445 . . . no C23 Fe2 C20 C21 -79.6(3) . . . . no P6 Fe2 C20 C21 105.3(3) 2_445 . . . no C20 Fe2 C19 C23 117.9(4) . . . . no P4 Fe2 C20 C28 101.8(5) . . . . no P5 Fe2 C20 C28 49.0(5) . . . . no C19 Fe2 C20 C28 129.9(6) . . . . no C21 Fe2 C20 C28 -112.3(5) . . . . no C21 Fe2 C23 C19 -82.7(3) . . . . no C22 Fe2 C23 C19 -120.4(4) . . . . no C44 Fe2 P6 Cu4 -108.6(2) . 2_445 . . no C21 Fe2 C19 C20 -38.4(3) . . . . no C22 Fe2 C19 C20 -81.5(3) . . . . no C23 Fe2 C19 C20 -117.9(4) . . . . no C36 Fe2 C19 C20 -156.2(3) . . . . no P6 Fe2 C44 C36 -130.2(3) . 2_445 . 2_445 no P4 Fe2 C19 C23 -76.8(3) . . . . no P5 Fe2 C19 C23 -131.5(3) . . . . no C20 Fe2 C44 P6 -68.9(3) 2_445 2_445 . . no C21 Fe2 C19 C23 79.5(3) . . . . no C20 Fe2 P6 C44 133.6(2) 2_445 2_445 . . no C36 Fe2 C44 P6 130.2(3) 2_445 2_445 . . no P4 Fe2 C20 C19 -28.1(4) . . . . no C23 Fe2 C36 C44 147.3(3) . . . 2_445 no P5 Fe2 C20 C19 -81.0(3) . . . . no C20 Fe2 C19 C24 -133.9(6) . . . . no C21 Fe2 C19 C24 -172.3(5) . . . . no C22 Fe2 C19 C24 144.6(5) . . . . no C23 Fe2 C19 C24 108.2(6) . . . . no C36 Fe2 C19 C24 69.9(6) . . . . no C20 Fe2 C21 C22 -119.8(4) . . . . no P6 Fe2 C36 C44 -35.0(2) 2_445 . . 2_445 no P4 Fe2 C22 C21 -175.2(2) . . . . no C22 Fe2 P6 Cu4 -47.6(3) 2_445 2_445 . . no C21 Fe2 C44 P6 -104.87(19) 2_445 2_445 . . no P5 Fe2 C21 C22 -154.4(2) . . . . no C19 Fe2 C21 C22 -81.3(3) . . . . no C22 Fe2 C36 C44 107.6(3) . . . 2_445 no P5 Fe2 C23 C22 -177.0(2) . . . . no C20 Fe2 P6 Cu4 24.91(19) 2_445 2_445 . . no C21 Fe2 C20 C19 117.8(4) . . . . no C22 Fe2 C20 C19 81.0(3) . . . . no P4 Fe2 P6 Cu4 176.46(13) 2_445 2_445 . . no P5 Fe2 P6 Cu4 130.57(15) 2_445 2_445 . . no C23 Fe2 C44 P6 -176.0(2) 2_445 2_445 . . no P4 Fe2 C23 C19 113.9(3) . . . . no C19 Fe2 P6 Cu4 60.9(2) 2_445 2_445 . . no C21 Fe2 P6 Cu4 -17.3(2) 2_445 2_445 . . no P6 Fe2 C44 C45 114.7(5) . 2_445 . . no C36 Fe2 P6 Cu4 -137.88(19) 2_445 2_445 . . no C22 Fe2 C44 P6 -146.35(17) 2_445 2_445 . . no C44 Fe2 C23 C19 -167.5(3) 2_445 . . . no P4 Fe2 C23 C22 -125.8(3) . . . . no C19 Fe2 P6 C44 169.5(3) 2_445 2_445 . . no P6 Fe2 C20 C28 -6.9(5) 2_445 . . . no C44 Fe2 C20 C28 -51.6(5) 2_445 . . . no P4 Fe2 C44 C45 -147.6(4) 2_445 2_445 . . no C21 Fe2 C44 C45 9.8(5) 2_445 2_445 . . no P4 Fe2 P6 C44 -74.91(18) 2_445 2_445 . . no P5 Fe2 P6 C44 -120.79(19) 2_445 2_445 . . no C23 Fe2 C20 C28 168.1(5) . . . . no C20 Fe2 C44 C45 45.8(5) 2_445 2_445 . . no P5 Fe2 C44 C45 158.6(4) 2_445 2_445 . . no C22 Fe2 C20 C28 -149.1(5) . . . . no P5 Fe2 C44 P6 43.85(12) 2_445 2_445 . . no C36 Fe2 C23 C19 159.6(3) . . . . no Cu1 P1 C18 C37 178.0(3) . . . 2_555 no Fe1 P1 C18 C37 -55.2(4) . . . 2_555 no P2 P1 C18 C37 -1.9(4) . . . 2_555 no Cu1 P1 C18 Fe1 -126.81(10) . . . . no Fe1 P1 P2 P3 51.72(5) . . . 2_555 no P2 P1 C18 Fe1 53.32(12) . . . . no C18 P1 P2 P3 1.44(16) . . . 2_555 no C18 P1 P2 Fe1 -50.29(16) . . . . no Cu1 P1 P2 P3 -178.36(10) . . . 2_555 no Cu1 P1 P2 Fe1 129.92(12) . . . . no P1 P2 P3 C37 -0.95(16) . . 2_555 2_555 no Fe1 P2 P3 C37 51.01(16) . . 2_555 2_555 no P1 P2 P3 Fe1 -51.96(5) . . 2_555 . no Fe1 P2 P3 Cu2 -147.24(8) . . 2_555 2_555 no P1 P2 P3 Cu2 160.81(6) . . 2_555 2_555 no Cu2 P3 C37 C38 -18.3(5) . . . . no P2 P3 C37 Fe1 53.30(11) 2_555 . . 2_555 no Fe1 P3 C37 C18 -53.3(3) 2_555 . . 2_555 no Cu2 P3 C37 C18 159.6(3) . . . 2_555 no P2 P3 C37 C18 0.0(4) 2_555 . . 2_555 no Cu2 P3 C37 Fe1 -147.12(12) . . . 2_555 no P2 P3 C37 C38 -177.9(3) 2_555 . . . no Fe1 P3 C37 C38 128.8(4) 2_555 . . . no Cu3 P4 C36 Fe2 130.04(13) . . . . no Cu3 P4 P5 Fe2 -132.98(8) . . . . no Cu3 P4 P5 P6 174.62(7) . . . 2_445 no Fe2 P4 P5 P6 -52.41(5) . . . 2_445 no Cu3 P4 C36 C44 -174.5(3) . . . 2_445 no Fe2 P4 C36 C44 55.4(4) . . . 2_445 no P5 P4 C36 C44 2.3(4) . . . 2_445 no C36 P4 P5 P6 -2.37(17) . . . 2_445 no C36 P4 P5 Fe2 50.04(16) . . . . no P5 P4 C36 Fe2 -53.14(12) . . . . no P4 P5 P6 C44 2.11(16) . . 2_445 2_445 no Fe2 P5 P6 C44 -50.18(16) . . 2_445 2_445 no P4 P5 P6 Fe2 52.29(5) . . 2_445 . no P4 P5 P6 Cu4 -157.20(7) . . 2_445 2_445 no Fe2 P5 P6 Cu4 150.51(9) . . 2_445 2_445 no P5 P6 C44 C45 -177.7(3) 2_445 . . . no Cu4 P6 C44 Fe2 146.11(9) . . . 2_445 no Fe2 P6 C44 C36 53.8(3) 2_445 . . 2_445 no Fe2 P6 C44 C45 -125.1(4) 2_445 . . . no Cu4 P6 C44 C36 -160.1(3) . . . 2_445 no P5 P6 C44 C36 1.2(4) 2_445 . . 2_445 no P5 P6 C44 Fe2 -52.60(12) 2_445 . . 2_445 no Cu4 P6 C44 C45 21.0(4) . . . . no C5 C1 C2 C10 -170.0(5) . . . . no Fe1 C1 C6 C9 -80.6(6) . . . . no C5 C1 C6 C8 73.4(5) . . . . no Fe1 C1 C6 C8 158.7(4) . . . . no C5 C1 C2 C3 0.0(5) . . . . no C5 C1 C2 Fe1 58.7(3) . . . . no C6 C1 C2 Fe1 -131.9(5) . . . . no C5 C1 C6 C9 -165.9(4) . . . . no C5 C1 C6 C7 -43.0(6) . . . . no C2 C1 C6 C8 -95.2(6) . . . . no Fe1 C1 C2 C10 131.3(5) . . . . no C2 C1 C5 C4 1.5(5) . . . . no C6 C1 C5 Fe1 128.8(4) . . . . no C6 C1 C5 C4 -170.2(4) . . . . no Fe1 C1 C6 C7 42.3(6) . . . . no Fe1 C1 C5 C4 61.0(3) . . . . no C2 C1 C6 C9 25.5(8) . . . . no Fe1 C1 C2 C3 -58.7(3) . . . . no C6 C1 C2 C10 -0.6(9) . . . . no C2 C1 C6 C7 148.4(5) . . . . no C2 C1 C5 Fe1 -59.6(3) . . . . no C6 C1 C2 C3 169.4(5) . . . . no Fe1 C2 C10 C11 47.2(6) . . . . no C1 C2 C10 C12 67.1(6) . . . . no C1 C2 C3 Fe1 60.1(3) . . . . no C3 C2 C10 C11 134.8(4) . . . . no Fe1 C2 C10 C12 170.6(4) . . . . no C1 C2 C10 C13 -177.1(5) . . . . no Fe1 C2 C10 C13 -73.5(5) . . . . no C10 C2 C3 Fe1 -128.5(4) . . . . no C10 C2 C3 C4 170.0(4) . . . . no C1 C2 C3 C4 -1.4(5) . . . . no C1 C2 C10 C11 -56.3(7) . . . . no Fe1 C2 C3 C4 -61.5(3) . . . . no C3 C2 C10 C13 14.1(6) . . . . no C3 C2 C10 C12 -101.8(5) . . . . no C2 C3 C4 Fe1 61.5(3) . . . . no C2 C3 C4 C5 2.3(5) . . . . no C2 C3 C4 C14 -167.6(4) . . . . no Fe1 C3 C4 C5 -59.2(3) . . . . no Fe1 C3 C4 C14 131.0(5) . . . . no C14 C4 C5 Fe1 -131.6(5) . . . . no C5 C4 C14 C15 34.3(6) . . . . no Fe1 C4 C14 C15 -62.8(6) . . . . no C14 C4 C5 C1 167.5(4) . . . . no C3 C4 C5 C1 -2.3(5) . . . . no Fe1 C4 C14 C16 -179.4(4) . . . . no C5 C4 C14 C17 159.1(4) . . . . no C5 C4 C14 C16 -82.3(6) . . . . no Fe1 C4 C5 C1 -60.9(3) . . . . no C3 C4 C5 Fe1 58.5(3) . . . . no C3 C4 C14 C15 -157.9(4) . . . . no C3 C4 C14 C16 85.5(5) . . . . no C3 C4 C14 C17 -33.1(6) . . . . no Fe1 C4 C14 C17 61.9(6) . . . . no Fe1 C18 C37 P3 -54.7(3) . . 2_555 2_555 no P1 C18 C37 C38 -176.6(3) . . 2_555 2_555 no Fe1 C18 C37 C38 127.4(4) . . 2_555 2_555 no P1 C18 C37 P3 1.3(6) . . 2_555 2_555 no P1 C18 C37 Fe1 56.0(3) . . 2_555 . no C23 C19 C20 C28 170.2(5) . . . . no C20 C19 C23 C22 -1.9(5) . . . . no Fe2 C19 C24 C25 -46.7(6) . . . . no C24 C19 C23 Fe2 -131.3(4) . . . . no Fe2 C19 C23 C22 -61.4(3) . . . . no C20 C19 C24 C26 -32.3(7) . . . . no C23 C19 C24 C27 -76.7(5) . . . . no C24 C19 C20 Fe2 134.7(5) . . . . no C24 C19 C20 C21 -166.4(5) . . . . no C20 C19 C23 Fe2 59.5(3) . . . . no C24 C19 C23 C22 167.3(4) . . . . no C20 C19 C24 C25 -154.6(5) . . . . no Fe2 C19 C20 C21 58.9(3) . . . . no C23 C19 C20 Fe2 -58.9(3) . . . . no Fe2 C19 C24 C26 75.6(6) . . . . no Fe2 C19 C24 C27 -163.5(4) . . . . no C23 C19 C24 C26 162.5(4) . . . . no C24 C19 C20 C28 3.7(9) . . . . no C23 C19 C20 C21 0.0(5) . . . . no C23 C19 C24 C25 40.2(5) . . . . no C20 C19 C24 C27 88.6(6) . . . . no Fe2 C19 C20 C28 -131.0(5) . . . . no Fe2 C20 C21 C22 61.8(3) . . . . no Fe2 C20 C28 C29 -164.1(4) . . . . no C19 C20 C28 C30 62.7(6) . . . . no C19 C20 C21 Fe2 -60.0(3) . . . . no C21 C20 C28 C30 -128.3(4) . . . . no C19 C20 C21 C22 1.8(5) . . . . no C21 C20 C28 C31 -7.8(6) . . . . no C21 C20 C28 C29 107.7(5) . . . . no C19 C20 C28 C31 -176.7(5) . . . . no C28 C20 C21 Fe2 128.5(4) . . . . no C28 C20 C21 C22 -169.7(4) . . . . no Fe2 C20 C28 C30 -40.2(6) . . . . no Fe2 C20 C28 C31 80.4(5) . . . . no C19 C20 C28 C29 -61.2(6) . . . . no Fe2 C21 C22 C23 58.2(3) . . . . no Fe2 C21 C22 C32 -132.6(5) . . . . no C20 C21 C22 C32 166.2(4) . . . . no C20 C21 C22 Fe2 -61.2(3) . . . . no C20 C21 C22 C23 -3.0(5) . . . . no Fe2 C22 C32 C33 72.1(6) . . . . no C32 C22 C23 Fe2 132.8(5) . . . . no Fe2 C22 C23 C19 61.0(3) . . . . no Fe2 C22 C32 C34 -169.6(4) . . . . no Fe2 C22 C32 C35 -51.3(6) . . . . no C21 C22 C32 C33 168.5(4) . . . . no C21 C22 C32 C34 -73.2(6) . . . . no C32 C22 C23 C19 -166.3(4) . . . . no C21 C22 C32 C35 45.2(6) . . . . no C21 C22 C23 Fe2 -57.9(3) . . . . no C23 C22 C32 C34 94.0(5) . . . . no C23 C22 C32 C35 -147.7(5) . . . . no C21 C22 C23 C19 3.0(5) . . . . no C23 C22 C32 C33 -24.4(6) . . . . no P4 C36 C44 C45 -179.7(3) . . 2_445 2_445 no Fe2 C36 C44 C45 -123.7(4) . . 2_445 2_445 no P4 C36 C44 P6 -0.8(6) . . 2_445 2_445 no Fe2 C36 C44 P6 55.2(3) . . 2_445 2_445 no P4 C36 C44 Fe2 -56.0(3) . . 2_445 . no P3 C37 C38 C43 140.4(4) . . . . no Fe1 C37 C38 C39 54.6(7) 2_555 . . . no P3 C37 C38 C39 -39.3(6) . . . . no C18 C37 C38 C39 142.8(5) 2_555 . . . no C18 C37 C38 C43 -37.4(6) 2_555 . . . no Fe1 C37 C38 C43 -125.6(4) 2_555 . . . no C43 C38 C39 C40 2.4(7) . . . . no C37 C38 C43 C42 177.5(4) . . . . no C39 C38 C43 C42 -2.8(7) . . . . no C37 C38 C39 C40 -177.9(5) . . . . no C38 C39 C40 C41 -0.3(8) . . . . no C39 C40 C41 C42 -1.6(8) . . . . no C40 C41 C42 C43 1.2(8) . . . . no C41 C42 C43 C38 1.0(7) . . . . no P6 C44 C45 C50 29.5(6) . . . . no Fe2 C44 C45 C46 118.5(5) 2_445 . . . no P6 C44 C45 C46 -150.8(4) . . . . no C36 C44 C45 C46 30.3(7) 2_445 . . . no C36 C44 C45 C50 -149.3(5) 2_445 . . . no Fe2 C44 C45 C50 -61.2(6) 2_445 . . . no C44 C45 C46 C47 -179.4(4) . . . . no C50 C45 C46 C47 0.3(7) . . . . no C44 C45 C50 C49 179.1(4) . . . . no C46 C45 C50 C49 -0.6(7) . . . . no C45 C46 C47 C48 0.6(7) . . . . no C46 C47 C48 C49 -1.2(7) . . . . no C47 C48 C49 C50 0.9(7) . . . . no C48 C49 C50 C45 0.0(7) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br1 Cu3 4.1757(8) . . no Br1 P1 3.6366(14) . . no Br1 P3 3.6703(13) . . no Br1 N2 3.555(4) . . no Br1 C18 3.684(5) . . no Br1 C33 3.673(5) . . no Br1 C36 3.688(5) . . no Br2 C52 3.565(6) . 2_455 no Br2 Br4 3.8428(7) . . no Br2 C39 3.667(5) . . no Br4 Br2 3.8428(7) . . no Br4 P6 3.8236(12) . . no Br4 N1 3.592(5) . . no Br1 H33B 2.8600 . . no Br1 H48 2.9400 . 1_655 no Br1 H36A 2.8400 . . no Br1 H18A 3.1400 . . no Br2 H52A 3.0000 . 2_455 no Br3 H5A 3.2200 . . no Br3 H7B 3.0400 . . no Br4 H41 3.1300 . 2_455 no Br4 H42 3.1700 . 2_455 no Br4 H52C 3.2300 . 2_455 no Br4 H54B 3.1000 . 2_445 no Cu1 P2 4.1823(15) . . no Cu1 C7 4.193(6) . . no Cu2 C39 3.965(5) . . no Cu2 C11 3.923(5) . 2_555 no Cu2 C13 4.179(5) . 2_555 no Cu3 C25 3.817(5) . . no Cu3 P5 3.8855(15) . . no Cu3 Br1 4.1757(8) . . no Cu4 C50 3.549(5) . . no Cu4 C30 4.018(5) . 2_445 no Cu4 C52 4.027(6) . 2_455 no Cu1 H15C 3.5800 . . no Cu1 H5A 3.6600 . . no Cu1 H7B 3.6700 . . no Cu2 H13A 3.3300 . 2_555 no Cu2 H39 3.4700 . . no Cu2 H11A 3.0300 . 2_555 no Cu3 H25A 3.5600 . . no Cu3 H25C 3.1700 . . no Cu4 H50 2.9800 . . no Cu4 H30A 3.0600 . 2_445 no Cu4 H31C 3.5600 . 2_445 no Cu4 H52C 3.2300 . 2_455 no Fe1 C39 3.909(5) . 2_555 no Fe2 C50 3.868(5) . 2_445 no Fe1 H7C 3.4300 . . no Fe1 H11A 3.4700 . . no Fe2 H25C 3.4300 . . no P1 Br1 3.6366(14) . . no P1 Cu2 4.1647(14) . . no P1 P3 3.7305(16) . . no P1 C5 3.335(5) . . no P1 C37 2.775(5) . 2_555 no P1 P3 3.2068(18) . 2_555 no P2 Cu1 4.1823(15) . . no P2 C18 2.963(5) . . no P2 C37 3.013(5) . 2_555 no P2 C1 3.459(5) . . no P2 Cu2 3.8342(14) . 2_555 no P3 Cu1 3.9533(13) . . no P3 P1 3.7305(16) . . no P3 Br1 3.6703(13) . . no P4 C19 3.666(5) . . no P4 C44 2.769(5) . 2_445 no P4 Cu4 4.1852(14) . . no P4 P6 3.1820(18) . 2_445 no P4 C23 3.327(5) . . no P5 C53 3.480(5) . 2_445 no P5 P5 3.7236(17) . 2_445 no P5 C44 3.030(5) . 2_445 no P5 C36 2.980(5) . . no P5 Cu4 3.9503(15) . 2_445 no P5 C54 3.650(6) . 2_445 no P5 Cu3 3.8855(15) . . no P5 C19 3.459(5) . . no P6 Br4 3.8236(12) . . no P6 Cu3 4.2690(13) . . no P6 C30 3.607(5) . 2_445 no P1 H7C 3.0600 . . no P1 H18A 2.3500 . . no P2 H49 3.0400 . 2_455 no P2 H7C 2.9100 . . no P2 H9C 3.2000 . . no P3 H39 3.0200 . . no P3 H11A 2.8700 . 2_555 no P4 H25C 3.0400 . . no P4 H36A 2.3600 . . no P5 H54B 3.1100 . 2_445 no P5 H25C 3.0800 . . no P5 H26A 3.1300 . . no P6 H50 2.8400 . . no P6 H30A 2.9700 . 2_445 no N1 Br4 3.592(5) . . no N1 C52 3.423(8) . 2_455 no N2 Br1 3.555(4) . . no N1 H52C 2.7700 . 2_455 no N1 H50 2.7800 . . no N2 H11A 2.9000 . 2_555 no C1 P2 3.459(5) . . no C1 C3 2.313(7) . . no C1 C4 2.344(7) . . no C1 C10 2.743(7) . . no C2 C5 2.313(7) . . no C2 C6 2.774(7) . . no C2 C4 2.352(7) . . no C2 P3 3.489(5) . 2_555 no C3 C37 3.345(6) . 2_555 no C3 C5 2.260(7) . . no C3 P3 3.616(5) . 2_555 no C3 C1 2.313(7) . . no C3 C10 2.593(7) . . no C3 C14 2.630(7) . . no C4 C18 3.269(6) . . no C4 C2 2.352(7) . . no C4 C37 3.504(6) . 2_555 no C4 C1 2.344(7) . . no C5 C14 2.607(7) . . no C5 C6 2.560(7) . . no C5 Cu1 4.212(5) . . no C5 C18 3.505(6) . . no C5 C3 2.260(7) . . no C5 C2 2.313(7) . . no C5 P1 3.335(5) . . no C7 Cu1 4.193(6) . . no C7 C52 3.587(8) . 2_455 no C8 C34 3.583(7) . 2_556 no C9 C11 3.200(8) . . no C9 C10 3.528(8) . . no C10 C9 3.528(8) . . no C11 C9 3.200(8) . . no C11 Cu2 3.923(5) . 2_555 no C13 Cu2 4.179(5) . 2_555 no C15 C33 3.406(7) . . no C17 C38 3.538(7) . 2_555 no C18 C38 2.495(7) . 2_555 no C18 P2 2.963(5) . . no C18 C5 3.505(6) . . no C18 P3 2.732(5) . 2_555 no C18 C4 3.269(6) . . no C18 Cu1 3.352(5) . . no C19 C28 2.740(7) . . no C19 P5 3.459(5) . . no C19 C22 2.345(7) . . no C19 P4 3.666(5) . . no C19 C21 2.319(7) . . no C20 C23 2.313(7) . . no C20 P6 3.509(5) . 2_445 no C20 C24 2.766(7) . . no C20 C22 2.347(7) . . no C21 C32 2.634(7) . . no C21 P6 3.622(5) . 2_445 no C21 C23 2.262(7) . . no C21 C44 3.339(6) . 2_445 no C21 C28 2.589(7) . . no C21 C19 2.319(7) . . no C22 C20 2.347(7) . . no C22 C36 3.265(6) . . no C22 C19 2.345(7) . . no C22 C44 3.483(6) . 2_445 no C23 C36 3.476(6) . . no C23 C32 2.620(7) . . no C23 C21 2.262(7) . . no C23 C24 2.548(7) . . no C23 P4 3.327(5) . . no C23 C20 2.313(7) . . no C25 Cu3 3.817(5) . . no C26 C28 3.538(7) . . no C26 C30 3.290(7) . . no C26 C29 3.593(7) . . no C28 C26 3.538(7) . . no C29 C26 3.593(7) . . no C30 P6 3.607(5) . 2_445 no C30 Cu4 4.018(5) . 2_445 no C30 C26 3.290(7) . . no C33 Br1 3.673(5) . . no C33 C15 3.406(7) . . no C34 C8 3.583(7) . 2_556 no C35 C45 3.366(7) . 2_445 no C35 C46 3.406(6) . 2_445 no C36 P6 2.728(5) . 2_445 no C36 P5 2.980(5) . . no C36 Cu3 3.610(5) . . no C36 C45 2.515(7) . 2_445 no C36 Br1 3.688(5) . . no C36 C23 3.476(6) . . no C36 C22 3.265(6) . . no C38 C17 3.538(7) . 2_555 no C39 Br2 3.667(5) . . no C39 Cu2 3.965(5) . . no C45 C35 3.366(7) . 2_445 no C46 C53 3.558(7) . 2_445 no C46 C35 3.406(6) . 2_445 no C46 C54 3.361(8) . 2_445 no C50 Cu4 3.549(5) . . no C51 C51 3.452(7) . 2_455 no C52 N1 3.423(8) . 2_455 no C52 C7 3.587(8) . 2_455 no C52 Br2 3.565(6) . 2_455 no C52 Cu4 4.027(6) . 2_455 no C53 P5 3.480(5) . 2_445 no C53 C46 3.558(7) . 2_445 no C54 C46 3.361(8) . 2_445 no C54 P5 3.650(6) . 2_445 no C1 H12C 3.0600 . . no C1 H5A 2.1300 . . no C2 H3A 2.1300 . . no C3 H17C 2.7500 . . no C3 H13B 2.5800 . . no C3 H13A 2.8500 . . no C3 H16A 3.0400 . . no C4 H3A 2.1200 . . no C4 H5A 2.0900 . . no C5 H7B 2.6100 . . no C5 H15A 2.7400 . . no C5 H8B 2.7600 . . no C5 H16C 2.9900 . . no C7 H5A 2.7200 . . no C7 H52B 2.6500 . 2_455 no C8 H34A 3.0900 . 2_556 no C9 H12C 3.0000 . . no C9 H11C 2.3600 . . no C10 H9A 3.0200 . . no C11 H9C 2.8800 . . no C11 H9A 2.7300 . . no C12 H9A 2.9200 . . no C13 H3A 2.5200 . . no C15 H33C 2.9700 . . no C15 H5A 2.8300 . . no C15 H33A 3.1000 . . no C16 H33A 2.8800 . 2_556 no C17 H3A 2.8600 . . no C18 H43 2.7100 . 2_555 no C18 H15C 2.9200 . . no C19 H29B 3.0800 . . no C19 H23A 2.1300 . . no C19 H30B 3.0600 . . no C20 H21A 2.1300 . . no C21 H35C 2.7900 . . no C21 H34B 2.9300 . . no C21 H31C 2.7300 . . no C21 H31B 2.6700 . . no C22 H23A 2.1000 . . no C22 H21A 2.1100 . . no C23 H25A 2.6000 . . no C23 H33B 2.9700 . . no C23 H27C 2.8300 . . no C23 H33A 2.7700 . . no C24 H29B 3.0800 . . no C25 H23A 2.6500 . . no C26 H29B 2.8400 . . no C26 H30B 2.4700 . . no C26 H54A 2.9600 . 2_445 no C26 H13C 3.0400 . 1_445 no C27 H29B 3.0300 . . no C28 H26C 3.0200 . . no C29 H27A 2.9400 . . no C29 H26C 2.8200 . . no C30 H26C 2.8200 . . no C30 H40 3.0100 . 2_445 no C30 H26A 2.9800 . . no C31 H21A 2.5100 . . no C31 H9B 3.1000 . 1_545 no C33 H23A 2.7300 . . no C33 H15B 2.9900 . . no C34 H8A 2.9500 . 2_556 no C35 H21A 2.9900 . . no C36 H46 2.7200 . 2_445 no C36 H35B 3.0200 . . no C37 H18A 2.0300 . 2_555 no C38 H17A 2.7100 . 2_555 no C39 H17A 3.0900 . 2_555 no C43 H18A 2.7000 . 2_555 no C43 H17A 2.9100 . 2_555 no C44 H36A 2.0300 . 2_445 no C45 H35B 2.7500 . 2_445 no C46 H54C 2.7900 . 2_445 no C46 H36A 2.7100 . 2_445 no C46 H35B 2.6000 . 2_445 no C48 H43 3.0900 . 2_455 no C49 H43 3.0100 . 2_455 no C49 H42 3.0100 . 2_455 no C49 H9C 3.0100 . 2_455 no C53 H46 2.8700 . 2_445 no C53 H11B 3.0500 . 2_555 no C53 H26A 3.0700 . 2_445 no C54 H26A 3.0100 . 2_445 no C54 H46 3.0300 . 2_445 no H3A C13 2.5200 . . no H3A C17 2.8600 . . no H3A H13A 2.4500 . . no H3A H13B 2.0900 . . no H3A H17C 2.2900 . . no H5A Br3 3.2200 . . no H5A Cu1 3.6600 . . no H5A C7 2.7200 . . no H5A C15 2.8300 . . no H5A H7B 2.0900 . . no H5A H15A 2.2800 . . no H7A H8C 2.4300 . . no H7A H9B 2.3200 . . no H7A H52B 2.3100 . 2_455 no H7B Br3 3.0400 . . no H7B Cu1 3.6700 . . no H7B C5 2.6100 . . no H7B H5A 2.0900 . . no H7B H8B 2.4900 . . no H7C Fe1 3.4300 . . no H7C P1 3.0600 . . no H7C P2 2.9100 . . no H7C H9C 2.5000 . . no H7C H52B 2.3500 . 2_455 no H8A H9A 2.4700 . . no H8A H12C 2.3500 . . no H8A C34 2.9500 . 2_556 no H8B C5 2.7600 . . no H8B H7B 2.4900 . . no H8C H7A 2.4300 . . no H8C H9B 2.4700 . . no H9A C10 3.0200 . . no H9A C11 2.7300 . . no H9A C12 2.9200 . . no H9A H8A 2.4700 . . no H9A H11C 1.8800 . . no H9A H12C 2.1800 . . no H9B C31 3.1000 . 1_565 no H9B H7A 2.3200 . . no H9B H8C 2.4700 . . no H9B H21A 2.3400 . 1_565 no H9B H31B 2.3500 . 1_565 no H9C P2 3.2000 . . no H9C C11 2.8800 . . no H9C H7C 2.5000 . . no H9C H11C 2.0800 . . no H9C C49 3.0100 . 2_455 no H11A Fe1 3.4700 . . no H11A H13A 2.5300 . . no H11A Cu2 3.0300 . 2_555 no H11A P3 2.8700 . 2_555 no H11A N2 2.9000 . 2_555 no H11B H12A 2.5200 . . no H11B H13C 2.3300 . . no H11B C53 3.0500 . 2_555 no H11C C9 2.3600 . . no H11C H9A 1.8800 . . no H11C H9C 2.0800 . . no H11C H12C 2.5400 . . no H12A H11B 2.5200 . . no H12A H13C 2.4700 . . no H12B H13B 2.4500 . . no H12C C1 3.0600 . . no H12C C9 3.0000 . . no H12C H8A 2.3500 . . no H12C H9A 2.1800 . . no H12C H11C 2.5400 . . no H13A C3 2.8500 . . no H13A H3A 2.4500 . . no H13A H11A 2.5300 . . no H13A Cu2 3.3300 . 2_555 no H13A H39 2.4900 . 2_555 no H13B C3 2.5800 . . no H13B H3A 2.0900 . . no H13B H12B 2.4500 . . no H13B H27A 2.5800 . 2_556 no H13C C26 3.0400 . 1_665 no H13C H11B 2.3300 . . no H13C H12A 2.4700 . . no H15A C5 2.7400 . . no H15A H5A 2.2800 . . no H15A H16C 2.4600 . . no H15B C33 2.9900 . . no H15B H16B 2.4700 . . no H15B H17B 2.5200 . . no H15B H33C 2.4400 . . no H15C Cu1 3.5800 . . no H15C C18 2.9200 . . no H15C H17A 2.5200 . . no H15C H18A 2.3000 . . no H16A C3 3.0400 . . no H16A H17C 2.5300 . . no H16A H27C 2.4800 . 2_556 no H16B H15B 2.4700 . . no H16B H17B 2.4700 . . no H16C C5 2.9900 . . no H16C H15A 2.4600 . . no H16C H33A 2.4900 . 2_556 no H17A H15C 2.5200 . . no H17A C38 2.7100 . 2_555 no H17A C39 3.0900 . 2_555 no H17A C43 2.9100 . 2_555 no H17B H15B 2.5200 . . no H17B H16B 2.4700 . . no H17C C3 2.7500 . . no H17C H3A 2.2900 . . no H17C H16A 2.5300 . . no H17C H27C 2.5300 . 2_556 no H18A Br1 3.1400 . . no H18A H15C 2.3000 . . no H18A C43 2.7000 . 2_555 no H18A H43 2.3200 . 2_555 no H21A C31 2.5100 . . no H21A C35 2.9900 . . no H21A H9B 2.3400 . 1_545 no H21A H31B 2.2200 . . no H21A H31C 2.2800 . . no H21A H35C 2.3700 . . no H23A C25 2.6500 . . no H23A C33 2.7300 . . no H23A H25A 2.0500 . . no H23A H33A 2.3200 . . no H25A Cu3 3.5600 . . no H25A C23 2.6000 . . no H25A H23A 2.0500 . . no H25A H27C 2.4600 . . no H25B H26B 2.3200 . . no H25B H27B 2.4900 . . no H25C Cu3 3.1700 . . no H25C Fe2 3.4300 . . no H25C P4 3.0400 . . no H25C P5 3.0800 . . no H25C H26A 2.5600 . . no H26A P5 3.1300 . . no H26A C30 2.9800 . . no H26A H25C 2.5600 . . no H26A H30B 2.0300 . . no H26A C53 3.0700 . 2_445 no H26A C54 3.0100 . 2_445 no H26A H54A 2.4000 . 2_445 no H26B H25B 2.3200 . . no H26B H27B 2.4900 . . no H26C C28 3.0200 . . no H26C C29 2.8200 . . no H26C C30 2.8200 . . no H26C H27A 2.5000 . . no H26C H29B 2.0000 . . no H26C H30B 2.1800 . . no H27A C29 2.9400 . . no H27A H26C 2.5000 . . no H27A H29B 2.2700 . . no H27A H13B 2.5800 . 2_556 no H27B H25B 2.4900 . . no H27B H26B 2.4900 . . no H27C C23 2.8300 . . no H27C H25A 2.4600 . . no H27C H16A 2.4800 . 2_556 no H27C H17C 2.5300 . 2_556 no H29A H30C 2.4300 . . no H29A H31A 2.4300 . . no H29B C19 3.0800 . . no H29B C24 3.0800 . . no H29B C26 2.8400 . . no H29B C27 3.0300 . . no H29B H26C 2.0000 . . no H29B H27A 2.2700 . . no H29B H29B 2.5400 . 2_446 no H29C H31B 2.4500 . . no H30A H31C 2.3900 . . no H30A Cu4 3.0600 . 2_445 no H30A P6 2.9700 . 2_445 no H30B C19 3.0600 . . no H30B C26 2.4700 . . no H30B H26A 2.0300 . . no H30B H26C 2.1800 . . no H30C H29A 2.4300 . . no H30C H39 2.5300 . 2_445 no H30C H40 2.4800 . 2_445 no H31A H29A 2.4300 . . no H31A H40 2.3500 . 2_445 no H31B C21 2.6700 . . no H31B H9B 2.3500 . 1_545 no H31B H21A 2.2200 . . no H31B H29C 2.4500 . . no H31C C21 2.7300 . . no H31C H21A 2.2800 . . no H31C H30A 2.3900 . . no H31C Cu4 3.5600 . 2_445 no H31C H50 2.4600 . 2_445 no H33A C15 3.1000 . . no H33A C23 2.7700 . . no H33A H23A 2.3200 . . no H33A H34C 2.4600 . . no H33A C16 2.8800 . 2_556 no H33A H16C 2.4900 . 2_556 no H33B Br1 2.8600 . . no H33B C23 2.9700 . . no H33B H35B 2.5100 . . no H33B H36A 2.5800 . . no H33C C15 2.9700 . . no H33C H15B 2.4400 . . no H33C H34A 2.5300 . . no H33C H35A 2.5100 . . no H34A H33C 2.5300 . . no H34A H35A 2.4300 . . no H34A C8 3.0900 . 2_556 no H34B C21 2.9300 . . no H34B H35C 2.5200 . . no H34C H33A 2.4600 . . no H35A H33C 2.5100 . . no H35A H34A 2.4300 . . no H35B C36 3.0200 . . no H35B H33B 2.5100 . . no H35B H36A 2.4900 . . no H35B C45 2.7500 . 2_445 no H35B C46 2.6000 . 2_445 no H35C C21 2.7900 . . no H35C H21A 2.3700 . . no H35C H34B 2.5200 . . no H36A Br1 2.8400 . . no H36A H33B 2.5800 . . no H36A H35B 2.4900 . . no H36A C46 2.7100 . 2_445 no H36A H46 2.2500 . 2_445 no H39 Cu2 3.4700 . . no H39 P3 3.0200 . . no H39 H13A 2.4900 . 2_555 no H39 H30C 2.5300 . 2_445 no H40 C30 3.0100 . 2_445 no H40 H30C 2.4800 . 2_445 no H40 H31A 2.3500 . 2_445 no H41 H52C 2.5500 . . no H41 Br4 3.1300 . 2_455 no H42 Br4 3.1700 . 2_455 no H42 C49 3.0100 . 2_455 no H43 C18 2.7100 . 2_555 no H43 C48 3.0900 . 2_455 no H43 C49 3.0100 . 2_455 no H43 H18A 2.3200 . 2_555 no H46 C36 2.7200 . 2_445 no H46 C53 2.8700 . 2_445 no H46 C54 3.0300 . 2_445 no H46 H36A 2.2500 . 2_445 no H46 H54C 2.5800 . 2_445 no H48 Br1 2.9400 . 1_455 no H49 P2 3.0400 . 2_455 no H50 Cu4 2.9800 . . no H50 P6 2.8400 . . no H50 N1 2.7800 . . no H50 H31C 2.4600 . 2_445 no H52A Br2 3.0000 . 2_455 no H52B C7 2.6500 . 2_455 no H52B H7A 2.3100 . 2_455 no H52B H7C 2.3500 . 2_455 no H52C H41 2.5500 . . no H52C Br4 3.2300 . 2_455 no H52C Cu4 3.2300 . 2_455 no H52C N1 2.7700 . 2_455 no H54A C26 2.9600 . 2_445 no H54A H26A 2.4000 . 2_445 no H54B Br4 3.1000 . 2_445 no H54B P5 3.1100 . 2_445 no H54C C46 2.7900 . 2_445 no H54C H46 2.5800 . 2_445 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C33 H33B Br1 0.9800 2.8600 3.673(5) 141.00 . yes C36 H36A Br1 0.9500 2.8400 3.688(5) 150.00 . yes # start Validation Reply Form _vrf_PLAT027_ds210 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 62.95 Deg. RESPONSE: due to construction, with CuKa-radiation the Oxford Gemini Ultra Diffractometer does not allow to measure at higher angles than theta ~ 62 Deg. ; _vrf_PLAT051_ds210 ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 10.93 Perc. RESPONSE: The structure contains a solvent accessible void at (0.5,0,0.5), in which three moieties of disordered Dichlormethane are present. Theses molecules have been included in the calculation of _chemical_formula_weight and all other atom dependent values. ; # end Validation Reply Form #===END