# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name W.-H.Zhang _publ_contact_author_address ; Prof T. S. Andy Hor Department of Chemistry National University of Singapore 3 Science Drive 3 117543 Singapore ; _publ_contact_author_email chmwhz@gmail.com loop_ _publ_author_name W.-H.Zhang T.S.A.Hor data_Cpd2 _database_code_depnum_ccdc_archive 'CCDC 823889' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H56 Cl6 Fe2 Ni2 O4 P4' _chemical_formula_weight 1502.83 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5328(4) _cell_length_b 33.6751(15) _cell_length_c 18.5393(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.6450(10) _cell_angle_gamma 90.00 _cell_volume 6517.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2835 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 20.44 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 1.398 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7302 _exptl_absorpt_correction_T_max 0.8964 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45546 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.1039 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.39 _reflns_number_total 14762 _reflns_number_gt 9567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0855P)^2^+11.3285P] 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 14762 _refine_ls_number_parameters 794 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1290 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.2079 _refine_ls_wR_factor_gt 0.1810 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl6 Cl -0.1809(2) 0.11430(12) 0.77607(19) 0.0514(9) Uani 0.824(11) 1 d PD A 1 Cl3 Cl 0.0375(4) 0.17784(17) 0.70143(19) 0.0841(15) Uani 0.824(11) 1 d PD A 1 Cl4 Cl 0.1601(3) 0.09665(9) 0.8071(4) 0.095(2) Uani 0.824(11) 1 d PD A 1 Cl5 Cl 0.0252(5) 0.17742(18) 0.8946(2) 0.0898(18) Uani 0.824(11) 1 d PD A 1 Cl3A Cl 0.0742(18) 0.1644(5) 0.6991(6) 0.068(3) Uani 0.176(11) 1 d PD A 2 Cl4A Cl 0.1343(13) 0.0995(3) 0.8522(8) 0.068(3) Uani 0.176(11) 1 d PD A 2 Cl5A Cl -0.0129(16) 0.1926(4) 0.8698(8) 0.068(3) Uani 0.176(11) 1 d PD A 2 Cl6A Cl -0.1830(10) 0.1162(5) 0.7681(11) 0.068(3) Uani 0.176(11) 1 d PD A 2 Ni1 Ni 0.55595(7) 0.12873(2) 0.29794(4) 0.0271(2) Uani 1 1 d . . . Ni2 Ni 0.00821(10) 0.14263(3) 0.79611(5) 0.0490(3) Uani 1 1 d D . . Fe1 Fe 0.80320(8) 0.05788(3) 0.50078(4) 0.0248(2) Uani 1 1 d . . . Fe2 Fe 0.29282(8) 0.19707(3) 0.09620(4) 0.0278(2) Uani 1 1 d . . . Cl1 Cl 0.72945(14) 0.16733(5) 0.27386(9) 0.0350(4) Uani 1 1 d . . . Cl2 Cl 0.39066(14) 0.08540(5) 0.32071(8) 0.0329(4) Uani 1 1 d . . . P1 P 0.63990(14) 0.14733(5) 0.48457(8) 0.0215(3) Uani 1 1 d . . . P2 P 0.71371(13) 0.03936(5) 0.32185(8) 0.0203(3) Uani 1 1 d . . . P3 P 0.49821(14) 0.11788(5) 0.10963(8) 0.0248(3) Uani 1 1 d . . . P4 P 0.33546(14) 0.20587(5) 0.28024(8) 0.0244(3) Uani 1 1 d . . . O1 O 0.5916(4) 0.14238(12) 0.4056(2) 0.0267(9) Uani 1 1 d . . . O2 O 0.6760(4) 0.08202(12) 0.3099(2) 0.0248(9) Uani 1 1 d . . . O3 O 0.5143(4) 0.11602(13) 0.19093(19) 0.0282(9) Uani 1 1 d . . . O4 O 0.4380(4) 0.17466(13) 0.2878(2) 0.0284(10) Uani 1 1 d . . . C1 C 0.7756(5) 0.11735(18) 0.5104(3) 0.0253(13) Uani 1 1 d . . . C2 C 0.8226(6) 0.10016(19) 0.5802(3) 0.0330(15) Uani 1 1 d . . . H2 H 0.7791 0.1006 0.6244 0.040 Uiso 1 1 calc R . . C3 C 0.9449(7) 0.0831(2) 0.5739(4) 0.047(2) Uani 1 1 d . . . H3 H 0.9997 0.0687 0.6129 0.057 Uiso 1 1 calc R . . C4 C 0.9727(6) 0.0887(2) 0.5032(4) 0.0426(18) Uani 1 1 d . . . H4 H 1.0504 0.0792 0.4839 0.051 Uiso 1 1 calc R . . C5 C 0.8697(6) 0.10997(18) 0.4632(3) 0.0307(14) Uani 1 1 d . . . H5 H 0.8640 0.1181 0.4116 0.037 Uiso 1 1 calc R . . C6 C 0.7254(5) 0.02438(17) 0.4148(3) 0.0227(12) Uani 1 1 d . . . C7 C 0.8305(6) 0.00408(18) 0.4567(3) 0.0263(13) Uani 1 1 d . . . H7 H 0.9097 -0.0051 0.4385 0.032 Uiso 1 1 calc R . . C8 C 0.8002(7) -0.00085(19) 0.5280(3) 0.0366(16) Uani 1 1 d . . . H8 H 0.8559 -0.0136 0.5687 0.044 Uiso 1 1 calc R . . C9 C 0.6799(7) 0.0161(2) 0.5323(3) 0.0377(16) Uani 1 1 d . . . H9 H 0.6357 0.0173 0.5761 0.045 Uiso 1 1 calc R . . C10 C 0.6332(6) 0.03174(19) 0.4621(3) 0.0292(14) Uani 1 1 d . . . H10 H 0.5506 0.0457 0.4490 0.035 Uiso 1 1 calc R . . C11 C 0.4439(6) 0.1641(2) 0.0730(3) 0.0305(14) Uani 1 1 d . . . C12 C 0.3552(6) 0.1719(2) 0.0080(3) 0.0366(16) Uani 1 1 d . . . H12 H 0.3093 0.1518 -0.0245 0.044 Uiso 1 1 calc R . . C13 C 0.3468(7) 0.2134(2) -0.0004(4) 0.0453(19) Uani 1 1 d . . . H13 H 0.2927 0.2276 -0.0400 0.054 Uiso 1 1 calc R . . C14 C 0.4269(7) 0.2311(2) 0.0565(4) 0.0481(19) Uani 1 1 d . . . H14 H 0.4379 0.2601 0.0641 0.058 Uiso 1 1 calc R . . C15 C 0.4886(6) 0.2010(2) 0.1027(3) 0.0324(15) Uani 1 1 d . . . H15 H 0.5499 0.2052 0.1474 0.039 Uiso 1 1 calc R . . C16 C 0.2363(6) 0.20279(19) 0.1951(3) 0.0282(14) Uani 1 1 d . . . C17 C 0.1853(6) 0.2345(2) 0.1489(3) 0.0355(16) Uani 1 1 d . . . H17 H 0.2002 0.2632 0.1573 0.043 Uiso 1 1 calc R . . C18 C 0.1089(6) 0.2168(2) 0.0883(3) 0.0429(18) Uani 1 1 d . . . H18 H 0.0626 0.2313 0.0463 0.051 Uiso 1 1 calc R . . C19 C 0.1107(6) 0.1754(2) 0.0974(4) 0.0408(17) Uani 1 1 d . . . H19 H 0.0668 0.1558 0.0628 0.049 Uiso 1 1 calc R . . C20 C 0.1904(6) 0.1662(2) 0.1637(3) 0.0331(15) Uani 1 1 d . . . H20 H 0.2103 0.1394 0.1838 0.040 Uiso 1 1 calc R . . C1A C 0.6936(5) 0.19664(18) 0.5070(3) 0.0247(13) Uani 1 1 d . . . C2A C 0.7637(6) 0.2054(2) 0.5743(3) 0.0347(15) Uani 1 1 d . . . H2A H 0.7853 0.1851 0.6086 0.042 Uiso 1 1 calc R . . C3A C 0.8010(7) 0.2440(2) 0.5905(4) 0.0481(19) Uani 1 1 d . . . H3A H 0.8461 0.2499 0.6364 0.058 Uiso 1 1 calc R . . C4A C 0.7736(6) 0.2738(2) 0.5406(4) 0.0443(18) Uani 1 1 d . . . H4A H 0.7996 0.3000 0.5522 0.053 Uiso 1 1 calc R . . C5A C 0.7075(7) 0.2651(2) 0.4733(4) 0.0498(19) Uani 1 1 d . . . H5A H 0.6904 0.2854 0.4386 0.060 Uiso 1 1 calc R . . C6A C 0.6659(6) 0.2269(2) 0.4560(4) 0.0375(16) Uani 1 1 d . . . H6A H 0.6193 0.2214 0.4102 0.045 Uiso 1 1 calc R . . C1B C 0.5161(6) 0.13486(19) 0.5388(3) 0.0276(13) Uani 1 1 d . . . C2B C 0.5049(7) 0.1526(3) 0.6057(4) 0.051(2) Uani 1 1 d . . . H2B H 0.5654 0.1714 0.6259 0.061 Uiso 1 1 calc R . . C3B C 0.4016(8) 0.1418(3) 0.6421(4) 0.073(3) Uani 1 1 d . . . H3B H 0.3919 0.1541 0.6866 0.088 Uiso 1 1 calc R . . C4B C 0.3148(8) 0.1137(3) 0.6144(4) 0.061(2) Uani 1 1 d . . . H4B H 0.2473 0.1064 0.6401 0.073 Uiso 1 1 calc R . . C5B C 0.3271(7) 0.0962(2) 0.5483(4) 0.0469(19) Uani 1 1 d . . . H5B H 0.2678 0.0768 0.5291 0.056 Uiso 1 1 calc R . . C6B C 0.4254(6) 0.1070(2) 0.5104(3) 0.0325(15) Uani 1 1 d . . . H6B H 0.4315 0.0954 0.4648 0.039 Uiso 1 1 calc R . . C1C C 0.8705(5) 0.03268(18) 0.2957(3) 0.0248(13) Uani 1 1 d . . . C2C C 0.9508(6) 0.0653(2) 0.2970(3) 0.0342(15) Uani 1 1 d . . . H2C H 0.9204 0.0907 0.3068 0.041 Uiso 1 1 calc R . . C3C C 1.0770(7) 0.0602(3) 0.2837(4) 0.0469(19) Uani 1 1 d . . . H3C H 1.1321 0.0822 0.2844 0.056 Uiso 1 1 calc R . . C4C C 1.1201(7) 0.0231(3) 0.2696(4) 0.049(2) Uani 1 1 d . . . H4C H 1.2060 0.0197 0.2622 0.059 Uiso 1 1 calc R . . C5C C 1.0414(7) -0.0093(3) 0.2660(4) 0.050(2) Uani 1 1 d . . . H5C H 1.0722 -0.0345 0.2548 0.060 Uiso 1 1 calc R . . C6C C 0.9138(6) -0.0046(2) 0.2793(4) 0.0400(17) Uani 1 1 d . . . H6C H 0.8584 -0.0266 0.2770 0.048 Uiso 1 1 calc R . . C1D C 0.6052(5) 0.00518(17) 0.2713(3) 0.0234(12) Uani 1 1 d . . . C2D C 0.5779(7) 0.0099(2) 0.1962(3) 0.0445(18) Uani 1 1 d . . . H2D H 0.6173 0.0304 0.1727 0.053 Uiso 1 1 calc R . . C3D C 0.4925(8) -0.0156(2) 0.1561(4) 0.0475(19) Uani 1 1 d . . . H3D H 0.4745 -0.0126 0.1054 0.057 Uiso 1 1 calc R . . C4D C 0.4354(7) -0.0448(2) 0.1896(4) 0.051(2) Uani 1 1 d . . . H4D H 0.3777 -0.0618 0.1618 0.061 Uiso 1 1 calc R . . C5D C 0.4596(9) -0.0501(3) 0.2636(4) 0.073(3) Uani 1 1 d . . . H5D H 0.4181 -0.0703 0.2864 0.088 Uiso 1 1 calc R . . C6D C 0.5465(8) -0.0250(3) 0.3041(4) 0.054(2) Uani 1 1 d . . . H6D H 0.5654 -0.0288 0.3546 0.065 Uiso 1 1 calc R . . C1E C 0.3837(6) 0.0808(2) 0.0719(3) 0.0290(14) Uani 1 1 d . . . C2E C 0.3001(6) 0.0655(2) 0.1161(3) 0.0368(16) Uani 1 1 d . . . H2E H 0.3046 0.0740 0.1647 0.044 Uiso 1 1 calc R . . C3E C 0.2095(7) 0.0376(3) 0.0887(4) 0.051(2) Uani 1 1 d . . . H3E H 0.1536 0.0270 0.1192 0.061 Uiso 1 1 calc R . . C4E C 0.2005(7) 0.0255(3) 0.0186(4) 0.058(2) Uani 1 1 d . . . H4E H 0.1369 0.0072 0.0001 0.069 Uiso 1 1 calc R . . C5E C 0.2843(9) 0.0400(3) -0.0253(4) 0.063(2) Uani 1 1 d . . . H5E H 0.2794 0.0310 -0.0735 0.075 Uiso 1 1 calc R . . C6E C 0.3757(8) 0.0676(3) 0.0002(4) 0.053(2) Uani 1 1 d . . . H6E H 0.4325 0.0775 -0.0305 0.064 Uiso 1 1 calc R . . C1F C 0.6478(6) 0.10944(19) 0.0758(3) 0.0274(13) Uani 1 1 d . . . C2F C 0.7504(6) 0.0943(2) 0.1212(4) 0.0353(15) Uani 1 1 d . . . H2F H 0.7424 0.0893 0.1703 0.042 Uiso 1 1 calc R . . C3F C 0.8656(7) 0.0864(3) 0.0953(4) 0.052(2) Uani 1 1 d . . . H3F H 0.9351 0.0758 0.1264 0.063 Uiso 1 1 calc R . . C4F C 0.8771(7) 0.0945(2) 0.0229(4) 0.052(2) Uani 1 1 d . . . H4F H 0.9546 0.0890 0.0049 0.062 Uiso 1 1 calc R . . C5F C 0.7771(7) 0.1103(3) -0.0224(4) 0.048(2) Uani 1 1 d . . . H5F H 0.7858 0.1160 -0.0711 0.057 Uiso 1 1 calc R . . C6F C 0.6631(7) 0.1180(2) 0.0040(3) 0.0420(18) Uani 1 1 d . . . H6F H 0.5945 0.1291 -0.0271 0.050 Uiso 1 1 calc R . . C1G C 0.4086(6) 0.25414(18) 0.2902(3) 0.0270(13) Uani 1 1 d . . . C2G C 0.5348(6) 0.2584(2) 0.2777(3) 0.0355(15) Uani 1 1 d . . . H2G H 0.5790 0.2365 0.2619 0.043 Uiso 1 1 calc R . . C3G C 0.5962(7) 0.2949(2) 0.2884(4) 0.0484(19) Uani 1 1 d . . . H3G H 0.6817 0.2977 0.2798 0.058 Uiso 1 1 calc R . . C4G C 0.5309(8) 0.3270(2) 0.3120(4) 0.0458(18) Uani 1 1 d . . . H4G H 0.5727 0.3516 0.3202 0.055 Uiso 1 1 calc R . . C5G C 0.4040(8) 0.3231(2) 0.3236(3) 0.0446(19) Uani 1 1 d . . . H5G H 0.3597 0.3451 0.3390 0.053 Uiso 1 1 calc R . . C6G C 0.3428(7) 0.2869(2) 0.3126(3) 0.0374(16) Uani 1 1 d . . . H6G H 0.2567 0.2843 0.3202 0.045 Uiso 1 1 calc R . . C1H C 0.2292(6) 0.20112(19) 0.3479(3) 0.0285(14) Uani 1 1 d . . . C2H C 0.2786(7) 0.1902(2) 0.4174(4) 0.0455(19) Uani 1 1 d . . . H2H H 0.3666 0.1847 0.4286 0.055 Uiso 1 1 calc R . . C3H C 0.1991(9) 0.1872(3) 0.4711(4) 0.057(2) Uani 1 1 d . . . H3H H 0.2340 0.1799 0.5186 0.069 Uiso 1 1 calc R . . C4H C 0.0730(8) 0.1946(2) 0.4563(4) 0.050(2) Uani 1 1 d . . . H4H H 0.0204 0.1923 0.4933 0.060 Uiso 1 1 calc R . . C5H C 0.0207(8) 0.2056(3) 0.3875(5) 0.078(3) Uani 1 1 d . . . H5H H -0.0676 0.2106 0.3769 0.094 Uiso 1 1 calc R . . C6H C 0.1005(7) 0.2094(3) 0.3331(4) 0.069(3) Uani 1 1 d . . . H6H H 0.0658 0.2177 0.2862 0.083 Uiso 1 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 Cl6 0.0413(15) 0.075(2) 0.0407(16) -0.0159(13) 0.0164(11) -0.0310(14) Cl3 0.066(2) 0.111(3) 0.068(2) 0.049(2) -0.0179(15) -0.046(2) Cl4 0.066(2) 0.059(2) 0.148(6) -0.012(2) -0.026(2) 0.0093(16) Cl5 0.095(3) 0.116(4) 0.058(2) -0.044(2) 0.0052(19) -0.042(3) Cl3A 0.072(6) 0.081(7) 0.047(5) -0.021(4) -0.003(4) -0.001(5) Cl4A 0.072(6) 0.081(7) 0.047(5) -0.021(4) -0.003(4) -0.001(5) Cl5A 0.072(6) 0.081(7) 0.047(5) -0.021(4) -0.003(4) -0.001(5) Cl6A 0.072(6) 0.081(7) 0.047(5) -0.021(4) -0.003(4) -0.001(5) Ni1 0.0221(4) 0.0328(5) 0.0258(4) -0.0002(3) 0.0011(3) 0.0015(3) Ni2 0.0490(6) 0.0521(7) 0.0434(5) -0.0001(5) -0.0033(4) -0.0130(5) Fe1 0.0228(4) 0.0228(5) 0.0267(4) 0.0018(4) -0.0049(3) -0.0018(4) Fe2 0.0276(5) 0.0328(5) 0.0221(4) 0.0024(4) -0.0005(3) 0.0045(4) Cl1 0.0263(8) 0.0342(9) 0.0455(9) 0.0029(7) 0.0091(7) -0.0041(7) Cl2 0.0227(7) 0.0465(10) 0.0299(8) -0.0038(7) 0.0044(6) -0.0129(7) P1 0.0183(7) 0.0253(8) 0.0199(7) -0.0029(6) -0.0015(5) -0.0011(6) P2 0.0148(7) 0.0209(8) 0.0250(7) 0.0004(6) 0.0017(5) -0.0008(6) P3 0.0253(8) 0.0315(9) 0.0176(7) -0.0009(6) 0.0029(6) 0.0011(7) P4 0.0219(8) 0.0289(9) 0.0220(7) -0.0002(6) 0.0011(6) 0.0073(7) O1 0.025(2) 0.033(2) 0.021(2) -0.0024(18) -0.0003(16) 0.0015(19) O2 0.021(2) 0.024(2) 0.028(2) -0.0011(18) 0.0014(16) 0.0019(17) O3 0.029(2) 0.038(3) 0.0174(19) -0.0032(18) 0.0025(16) 0.002(2) O4 0.021(2) 0.033(3) 0.030(2) 0.0015(19) 0.0017(17) 0.0119(19) C1 0.022(3) 0.024(3) 0.028(3) -0.006(3) -0.002(2) -0.002(2) C2 0.043(4) 0.024(3) 0.027(3) -0.002(3) -0.015(3) 0.000(3) C3 0.045(4) 0.032(4) 0.054(5) 0.000(3) -0.033(4) 0.001(3) C4 0.023(3) 0.029(4) 0.072(5) -0.004(4) -0.006(3) -0.002(3) C5 0.028(3) 0.022(3) 0.040(4) 0.000(3) -0.004(3) -0.002(3) C6 0.022(3) 0.022(3) 0.024(3) -0.004(2) 0.001(2) -0.002(2) C7 0.025(3) 0.024(3) 0.027(3) -0.001(3) -0.005(2) 0.001(3) C8 0.048(4) 0.026(4) 0.031(3) 0.009(3) -0.012(3) -0.006(3) C9 0.047(4) 0.038(4) 0.027(3) 0.007(3) 0.001(3) -0.009(3) C10 0.018(3) 0.032(4) 0.037(3) -0.009(3) 0.003(2) -0.007(3) C11 0.033(3) 0.032(4) 0.026(3) -0.003(3) 0.004(3) 0.002(3) C12 0.043(4) 0.050(5) 0.018(3) 0.001(3) 0.009(3) 0.007(3) C13 0.055(5) 0.050(5) 0.032(4) 0.022(3) 0.012(3) 0.011(4) C14 0.046(4) 0.044(5) 0.058(5) 0.017(4) 0.020(4) 0.001(4) C15 0.032(3) 0.035(4) 0.030(3) 0.005(3) 0.006(3) 0.003(3) C16 0.027(3) 0.034(4) 0.023(3) -0.003(3) 0.001(2) 0.007(3) C17 0.034(4) 0.038(4) 0.034(3) 0.001(3) 0.002(3) 0.017(3) C18 0.029(4) 0.067(6) 0.030(3) 0.004(3) -0.007(3) 0.017(4) C19 0.024(3) 0.057(5) 0.039(4) -0.004(3) -0.004(3) -0.011(3) C20 0.034(4) 0.037(4) 0.030(3) 0.001(3) 0.009(3) -0.001(3) C1A 0.015(3) 0.031(3) 0.028(3) -0.004(3) 0.002(2) 0.001(2) C2A 0.030(3) 0.033(4) 0.038(4) -0.001(3) -0.007(3) -0.006(3) C3A 0.036(4) 0.045(5) 0.059(5) -0.014(4) -0.009(3) -0.008(4) C4A 0.030(4) 0.025(4) 0.077(5) -0.012(4) 0.005(4) -0.005(3) C5A 0.047(5) 0.033(4) 0.068(5) 0.015(4) 0.004(4) -0.002(4) C6A 0.038(4) 0.033(4) 0.040(4) 0.002(3) 0.000(3) 0.003(3) C1B 0.023(3) 0.036(4) 0.023(3) -0.003(3) 0.001(2) -0.005(3) C2B 0.044(4) 0.077(6) 0.032(4) -0.020(4) 0.011(3) -0.020(4) C3B 0.052(5) 0.140(10) 0.031(4) -0.023(5) 0.016(4) -0.025(6) C4B 0.045(5) 0.100(8) 0.039(4) 0.007(5) 0.016(4) -0.022(5) C5B 0.028(4) 0.054(5) 0.060(5) -0.001(4) 0.007(3) -0.015(3) C6B 0.024(3) 0.040(4) 0.033(3) -0.005(3) 0.003(3) 0.000(3) C1C 0.018(3) 0.030(3) 0.026(3) 0.002(3) -0.001(2) 0.001(2) C2C 0.027(3) 0.037(4) 0.039(4) -0.002(3) 0.007(3) -0.006(3) C3C 0.025(4) 0.062(5) 0.055(5) 0.007(4) 0.008(3) -0.007(4) C4C 0.024(4) 0.079(6) 0.046(4) 0.012(4) 0.012(3) 0.008(4) C5C 0.045(4) 0.056(5) 0.052(4) 0.006(4) 0.023(4) 0.024(4) C6C 0.035(4) 0.040(4) 0.047(4) 0.002(3) 0.013(3) 0.004(3) C1D 0.018(3) 0.021(3) 0.030(3) 0.000(2) -0.001(2) -0.001(2) C2D 0.063(5) 0.040(4) 0.029(3) 0.001(3) 0.001(3) -0.015(4) C3D 0.065(5) 0.043(5) 0.031(4) -0.005(3) -0.004(3) 0.001(4) C4D 0.046(5) 0.045(5) 0.057(5) -0.018(4) -0.005(4) -0.017(4) C5D 0.078(6) 0.090(7) 0.050(5) -0.001(5) 0.000(4) -0.061(6) C6D 0.063(5) 0.062(6) 0.035(4) 0.006(4) 0.002(4) -0.032(4) C1E 0.025(3) 0.036(4) 0.025(3) -0.003(3) 0.002(2) 0.003(3) C2E 0.036(4) 0.044(4) 0.031(3) -0.009(3) 0.005(3) -0.003(3) C3E 0.040(4) 0.068(6) 0.047(4) -0.015(4) 0.014(3) -0.009(4) C4E 0.038(4) 0.070(6) 0.062(5) -0.024(4) -0.001(4) -0.026(4) C5E 0.072(6) 0.077(7) 0.038(4) -0.025(4) 0.006(4) -0.023(5) C6E 0.060(5) 0.069(6) 0.030(4) -0.012(4) 0.008(3) -0.029(4) C1F 0.026(3) 0.028(3) 0.029(3) 0.003(3) 0.010(2) 0.002(3) C2F 0.026(3) 0.044(4) 0.038(4) -0.006(3) 0.011(3) 0.003(3) C3F 0.038(4) 0.067(6) 0.054(5) 0.004(4) 0.010(3) 0.006(4) C4F 0.037(4) 0.065(6) 0.058(5) -0.023(4) 0.026(4) -0.005(4) C5F 0.042(4) 0.071(6) 0.033(4) -0.007(4) 0.016(3) -0.005(4) C6F 0.039(4) 0.061(5) 0.027(3) -0.001(3) 0.008(3) -0.007(4) C1G 0.030(3) 0.027(3) 0.021(3) 0.004(2) -0.004(2) 0.005(3) C2G 0.035(4) 0.035(4) 0.036(4) -0.003(3) 0.003(3) 0.004(3) C3G 0.041(4) 0.048(5) 0.053(5) 0.002(4) -0.005(3) -0.009(4) C4G 0.062(5) 0.032(4) 0.040(4) 0.003(3) -0.004(4) -0.007(4) C5G 0.078(6) 0.029(4) 0.029(3) 0.005(3) 0.012(4) 0.015(4) C6G 0.045(4) 0.042(4) 0.025(3) 0.002(3) 0.005(3) 0.008(3) C1H 0.024(3) 0.031(4) 0.031(3) -0.003(3) 0.006(2) 0.003(3) C2H 0.040(4) 0.060(5) 0.038(4) 0.005(4) 0.013(3) 0.018(4) C3H 0.078(6) 0.060(6) 0.039(4) 0.010(4) 0.026(4) 0.013(5) C4H 0.057(5) 0.040(5) 0.058(5) -0.012(4) 0.029(4) -0.018(4) C5H 0.023(4) 0.140(10) 0.074(6) -0.024(6) 0.018(4) 0.000(5) C6H 0.026(4) 0.144(10) 0.037(4) -0.001(5) 0.002(3) 0.012(5) _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 Cl6 Ni2 2.195(2) . ? Cl3 Ni2 2.174(3) . ? Cl4 Ni2 2.216(3) . ? Cl5 Ni2 2.156(3) . ? Cl3A Ni2 2.141(7) . ? Cl4A Ni2 2.143(7) . ? Cl5A Ni2 2.198(7) . ? Cl6A Ni2 2.200(7) . ? Ni1 O4 1.977(4) . ? Ni1 O2 2.012(4) . ? Ni1 O3 2.020(4) . ? Ni1 O1 2.033(4) . ? Ni1 Cl1 2.3336(17) . ? Ni1 Cl2 2.3525(16) . ? Fe1 C7 2.024(6) . ? Fe1 C6 2.034(5) . ? Fe1 C1 2.035(6) . ? Fe1 C10 2.038(6) . ? Fe1 C2 2.039(6) . ? Fe1 C8 2.042(6) . ? Fe1 C5 2.045(6) . ? Fe1 C9 2.051(7) . ? Fe1 C4 2.061(7) . ? Fe1 C3 2.061(6) . ? Fe2 C16 2.011(6) . ? Fe2 C13 2.026(6) . ? Fe2 C12 2.027(6) . ? Fe2 C17 2.029(6) . ? Fe2 C14 2.032(7) . ? Fe2 C11 2.032(6) . ? Fe2 C18 2.035(6) . ? Fe2 C20 2.042(6) . ? Fe2 C15 2.054(6) . ? Fe2 C19 2.056(6) . ? P1 O1 1.494(4) . ? P1 C1 1.763(6) . ? P1 C1A 1.785(6) . ? P1 C1B 1.799(6) . ? P2 O2 1.499(4) . ? P2 C6 1.784(6) . ? P2 C1D 1.796(6) . ? P2 C1C 1.796(6) . ? P3 O3 1.495(4) . ? P3 C11 1.764(7) . ? P3 C1F 1.794(6) . ? P3 C1E 1.811(6) . ? P4 O4 1.500(4) . ? P4 C16 1.776(6) . ? P4 C1H 1.797(6) . ? P4 C1G 1.798(6) . ? C1 C5 1.429(8) . ? C1 C2 1.444(8) . ? C2 C3 1.430(10) . ? C3 C4 1.392(11) . ? C4 C5 1.423(9) . ? C6 C10 1.414(8) . ? C6 C7 1.438(8) . ? C7 C8 1.409(8) . ? C8 C9 1.403(10) . ? C9 C10 1.428(9) . ? C11 C15 1.414(9) . ? C11 C12 1.447(8) . ? C12 C13 1.407(10) . ? C13 C14 1.395(11) . ? C14 C15 1.427(9) . ? C16 C20 1.420(9) . ? C16 C17 1.428(9) . ? C17 C18 1.422(9) . ? C18 C19 1.404(11) . ? C19 C20 1.427(9) . ? C1A C2A 1.394(8) . ? C1A C6A 1.396(9) . ? C2A C3A 1.377(10) . ? C3A C4A 1.370(10) . ? C4A C5A 1.376(10) . ? C5A C6A 1.382(10) . ? C1B C6B 1.392(8) . ? C1B C2B 1.395(9) . ? C2B C3B 1.403(10) . ? C3B C4B 1.366(12) . ? C4B C5B 1.382(11) . ? C5B C6B 1.375(9) . ? C1C C6C 1.384(9) . ? C1C C2C 1.385(8) . ? C2C C3C 1.394(9) . ? C3C C4C 1.369(11) . ? C4C C5C 1.366(11) . ? C5C C6C 1.408(9) . ? C1D C6D 1.373(9) . ? C1D C2D 1.393(8) . ? C2D C3D 1.388(10) . ? C3D C4D 1.345(10) . ? C4D C5D 1.372(11) . ? C5D C6D 1.389(10) . ? C1E C2E 1.380(9) . ? C1E C6E 1.393(9) . ? C2E C3E 1.387(10) . ? C3E C4E 1.354(10) . ? C4E C5E 1.368(11) . ? C5E C6E 1.376(11) . ? C1F C2F 1.375(9) . ? C1F C6F 1.393(8) . ? C2F C3F 1.390(9) . ? C3F C4F 1.391(10) . ? C4F C5F 1.364(11) . ? C5F C6F 1.380(9) . ? C1G C2G 1.386(9) . ? C1G C6G 1.395(9) . ? C2G C3G 1.391(10) . ? C3G C4G 1.384(11) . ? C4G C5G 1.388(11) . ? C5G C6G 1.382(10) . ? C1H C2H 1.374(9) . ? C1H C6H 1.375(9) . ? C2H C3H 1.388(10) . ? C3H C4H 1.343(11) . ? C4H C5H 1.372(12) . ? C5H C6H 1.401(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ni1 O2 179.12(16) . . ? O4 Ni1 O3 91.19(16) . . ? O2 Ni1 O3 89.65(16) . . ? O4 Ni1 O1 87.04(16) . . ? O2 Ni1 O1 92.12(16) . . ? O3 Ni1 O1 177.98(16) . . ? O4 Ni1 Cl1 92.55(13) . . ? O2 Ni1 Cl1 87.70(12) . . ? O3 Ni1 Cl1 90.20(13) . . ? O1 Ni1 Cl1 90.84(12) . . ? O4 Ni1 Cl2 91.80(13) . . ? O2 Ni1 Cl2 87.97(12) . . ? O3 Ni1 Cl2 88.60(13) . . ? O1 Ni1 Cl2 90.50(12) . . ? Cl1 Ni1 Cl2 175.51(7) . . ? Cl3A Ni2 Cl4A 113.0(4) . . ? Cl3A Ni2 Cl5 121.7(5) . . ? Cl4A Ni2 Cl5 88.9(3) . . ? Cl3A Ni2 Cl3 16.0(4) . . ? Cl4A Ni2 Cl3 128.1(4) . . ? Cl5 Ni2 Cl3 112.49(15) . . ? Cl3A Ni2 Cl6 113.3(5) . . ? Cl4A Ni2 Cl6 106.1(4) . . ? Cl5 Ni2 Cl6 110.53(13) . . ? Cl3 Ni2 Cl6 108.86(11) . . ? Cl3A Ni2 Cl5A 109.4(4) . . ? Cl4A Ni2 Cl5A 109.0(3) . . ? Cl5 Ni2 Cl5A 20.2(3) . . ? Cl3 Ni2 Cl5A 97.0(4) . . ? Cl6 Ni2 Cl5A 105.9(5) . . ? Cl3A Ni2 Cl6A 109.2(4) . . ? Cl4A Ni2 Cl6A 109.2(4) . . ? Cl5 Ni2 Cl6A 113.0(6) . . ? Cl3 Ni2 Cl6A 104.7(6) . . ? Cl6 Ni2 Cl6A 4.2(6) . . ? Cl5A Ni2 Cl6A 107.0(4) . . ? Cl3A Ni2 Cl4 90.3(4) . . ? Cl4A Ni2 Cl4 24.2(4) . . ? Cl5 Ni2 Cl4 108.89(14) . . ? Cl3 Ni2 Cl4 106.10(15) . . ? Cl6 Ni2 Cl4 109.86(14) . . ? Cl5A Ni2 Cl4 127.5(4) . . ? Cl6A Ni2 Cl4 111.5(5) . . ? C7 Fe1 C6 41.5(2) . . ? C7 Fe1 C1 161.1(2) . . ? C6 Fe1 C1 124.6(2) . . ? C7 Fe1 C10 68.7(2) . . ? C6 Fe1 C10 40.7(2) . . ? C1 Fe1 C10 109.1(2) . . ? C7 Fe1 C2 155.6(2) . . ? C6 Fe1 C2 160.8(2) . . ? C1 Fe1 C2 41.5(2) . . ? C10 Fe1 C2 123.7(3) . . ? C7 Fe1 C8 40.6(2) . . ? C6 Fe1 C8 68.8(2) . . ? C1 Fe1 C8 157.6(3) . . ? C10 Fe1 C8 68.1(3) . . ? C2 Fe1 C8 120.1(3) . . ? C7 Fe1 C5 123.8(3) . . ? C6 Fe1 C5 109.2(2) . . ? C1 Fe1 C5 41.0(2) . . ? C10 Fe1 C5 125.1(3) . . ? C2 Fe1 C5 69.0(3) . . ? C8 Fe1 C5 158.7(3) . . ? C7 Fe1 C9 68.3(3) . . ? C6 Fe1 C9 68.8(2) . . ? C1 Fe1 C9 123.1(3) . . ? C10 Fe1 C9 40.9(2) . . ? C2 Fe1 C9 106.2(3) . . ? C8 Fe1 C9 40.1(3) . . ? C5 Fe1 C9 160.6(3) . . ? C7 Fe1 C4 106.9(3) . . ? C6 Fe1 C4 123.7(3) . . ? C1 Fe1 C4 68.6(3) . . ? C10 Fe1 C4 160.7(3) . . ? C2 Fe1 C4 68.2(3) . . ? C8 Fe1 C4 121.6(3) . . ? C5 Fe1 C4 40.5(2) . . ? C9 Fe1 C4 156.8(3) . . ? C7 Fe1 C3 120.3(3) . . ? C6 Fe1 C3 157.7(3) . . ? C1 Fe1 C3 68.6(3) . . ? C10 Fe1 C3 159.2(3) . . ? C2 Fe1 C3 40.8(3) . . ? C8 Fe1 C3 105.7(3) . . ? C5 Fe1 C3 67.6(3) . . ? C9 Fe1 C3 121.8(3) . . ? C4 Fe1 C3 39.5(3) . . ? C16 Fe2 C13 158.8(3) . . ? C16 Fe2 C12 160.5(3) . . ? C13 Fe2 C12 40.6(3) . . ? C16 Fe2 C17 41.4(2) . . ? C13 Fe2 C17 119.9(3) . . ? C12 Fe2 C17 155.4(3) . . ? C16 Fe2 C14 125.5(3) . . ? C13 Fe2 C14 40.2(3) . . ? C12 Fe2 C14 68.2(3) . . ? C17 Fe2 C14 106.5(3) . . ? C16 Fe2 C11 125.5(2) . . ? C13 Fe2 C11 69.0(3) . . ? C12 Fe2 C11 41.8(2) . . ? C17 Fe2 C11 160.7(2) . . ? C14 Fe2 C11 68.3(3) . . ? C16 Fe2 C18 68.9(2) . . ? C13 Fe2 C18 103.0(3) . . ? C12 Fe2 C18 119.1(3) . . ? C17 Fe2 C18 41.0(3) . . ? C14 Fe2 C18 119.4(3) . . ? C11 Fe2 C18 158.1(3) . . ? C16 Fe2 C20 41.0(3) . . ? C13 Fe2 C20 155.9(3) . . ? C12 Fe2 C20 122.4(3) . . ? C17 Fe2 C20 69.3(3) . . ? C14 Fe2 C20 163.5(3) . . ? C11 Fe2 C20 110.1(3) . . ? C18 Fe2 C20 68.6(3) . . ? C16 Fe2 C15 110.9(2) . . ? C13 Fe2 C15 68.7(3) . . ? C12 Fe2 C15 69.1(3) . . ? C17 Fe2 C15 123.5(3) . . ? C14 Fe2 C15 40.9(3) . . ? C11 Fe2 C15 40.5(2) . . ? C18 Fe2 C15 157.2(3) . . ? C20 Fe2 C15 127.2(3) . . ? C16 Fe2 C19 68.5(3) . . ? C13 Fe2 C19 118.6(3) . . ? C12 Fe2 C19 105.3(3) . . ? C17 Fe2 C19 68.5(3) . . ? C14 Fe2 C19 154.0(3) . . ? C11 Fe2 C19 124.5(3) . . ? C18 Fe2 C19 40.1(3) . . ? C20 Fe2 C19 40.7(3) . . ? C15 Fe2 C19 162.5(3) . . ? O1 P1 C1 111.1(3) . . ? O1 P1 C1A 112.9(3) . . ? C1 P1 C1A 104.4(3) . . ? O1 P1 C1B 110.1(2) . . ? C1 P1 C1B 109.6(3) . . ? C1A P1 C1B 108.5(3) . . ? O2 P2 C6 113.4(2) . . ? O2 P2 C1D 113.5(2) . . ? C6 P2 C1D 106.3(3) . . ? O2 P2 C1C 108.4(3) . . ? C6 P2 C1C 106.1(3) . . ? C1D P2 C1C 108.9(3) . . ? O3 P3 C11 114.3(3) . . ? O3 P3 C1F 111.0(3) . . ? C11 P3 C1F 105.1(3) . . ? O3 P3 C1E 109.9(3) . . ? C11 P3 C1E 107.1(3) . . ? C1F P3 C1E 109.1(3) . . ? O4 P4 C16 111.9(3) . . ? O4 P4 C1H 112.3(3) . . ? C16 P4 C1H 105.6(3) . . ? O4 P4 C1G 109.3(3) . . ? C16 P4 C1G 109.7(3) . . ? C1H P4 C1G 107.9(3) . . ? P1 O1 Ni1 168.9(3) . . ? P2 O2 Ni1 156.3(3) . . ? P3 O3 Ni1 164.1(3) . . ? P4 O4 Ni1 173.0(3) . . ? C5 C1 C2 107.2(5) . . ? C5 C1 P1 122.4(4) . . ? C2 C1 P1 130.0(5) . . ? C5 C1 Fe1 69.9(3) . . ? C2 C1 Fe1 69.4(3) . . ? P1 C1 Fe1 131.3(3) . . ? C3 C2 C1 107.0(6) . . ? C3 C2 Fe1 70.4(4) . . ? C1 C2 Fe1 69.1(3) . . ? C4 C3 C2 109.1(6) . . ? C4 C3 Fe1 70.2(4) . . ? C2 C3 Fe1 68.8(3) . . ? C3 C4 C5 108.5(6) . . ? C3 C4 Fe1 70.3(4) . . ? C5 C4 Fe1 69.1(4) . . ? C4 C5 C1 108.1(6) . . ? C4 C5 Fe1 70.3(4) . . ? C1 C5 Fe1 69.1(4) . . ? C10 C6 C7 106.9(5) . . ? C10 C6 P2 125.8(4) . . ? C7 C6 P2 127.3(4) . . ? C10 C6 Fe1 69.8(3) . . ? C7 C6 Fe1 68.9(3) . . ? P2 C6 Fe1 124.7(3) . . ? C8 C7 C6 108.0(5) . . ? C8 C7 Fe1 70.4(4) . . ? C6 C7 Fe1 69.6(3) . . ? C9 C8 C7 108.9(5) . . ? C9 C8 Fe1 70.3(4) . . ? C7 C8 Fe1 69.0(3) . . ? C8 C9 C10 107.6(6) . . ? C8 C9 Fe1 69.6(4) . . ? C10 C9 Fe1 69.1(3) . . ? C6 C10 C9 108.6(6) . . ? C6 C10 Fe1 69.5(3) . . ? C9 C10 Fe1 70.0(4) . . ? C15 C11 C12 108.1(6) . . ? C15 C11 P3 123.5(5) . . ? C12 C11 P3 128.4(5) . . ? C15 C11 Fe2 70.6(4) . . ? C12 C11 Fe2 68.9(4) . . ? P3 C11 Fe2 128.6(3) . . ? C13 C12 C11 107.3(6) . . ? C13 C12 Fe2 69.7(4) . . ? C11 C12 Fe2 69.3(3) . . ? C14 C13 C12 108.6(6) . . ? C14 C13 Fe2 70.1(4) . . ? C12 C13 Fe2 69.7(4) . . ? C13 C14 C15 109.4(7) . . ? C13 C14 Fe2 69.7(4) . . ? C15 C14 Fe2 70.4(4) . . ? C11 C15 C14 106.8(6) . . ? C11 C15 Fe2 68.9(4) . . ? C14 C15 Fe2 68.7(4) . . ? C20 C16 C17 108.7(5) . . ? C20 C16 P4 122.9(5) . . ? C17 C16 P4 128.3(5) . . ? C20 C16 Fe2 70.7(3) . . ? C17 C16 Fe2 70.0(3) . . ? P4 C16 Fe2 127.3(3) . . ? C18 C17 C16 106.8(6) . . ? C18 C17 Fe2 69.7(4) . . ? C16 C17 Fe2 68.6(3) . . ? C19 C18 C17 108.9(6) . . ? C19 C18 Fe2 70.8(4) . . ? C17 C18 Fe2 69.3(4) . . ? C18 C19 C20 108.4(6) . . ? C18 C19 Fe2 69.1(4) . . ? C20 C19 Fe2 69.1(4) . . ? C16 C20 C19 107.1(6) . . ? C16 C20 Fe2 68.3(4) . . ? C19 C20 Fe2 70.2(4) . . ? C2A C1A C6A 119.3(6) . . ? C2A C1A P1 121.3(5) . . ? C6A C1A P1 119.4(5) . . ? C3A C2A C1A 119.8(6) . . ? C4A C3A C2A 121.1(7) . . ? C3A C4A C5A 119.4(7) . . ? C4A C5A C6A 121.1(7) . . ? C5A C6A C1A 119.4(6) . . ? C6B C1B C2B 119.3(6) . . ? C6B C1B P1 117.2(4) . . ? C2B C1B P1 123.4(5) . . ? C1B C2B C3B 118.7(7) . . ? C4B C3B C2B 121.4(7) . . ? C3B C4B C5B 119.4(7) . . ? C6B C5B C4B 120.5(7) . . ? C5B C6B C1B 120.6(6) . . ? C6C C1C C2C 120.4(6) . . ? C6C C1C P2 121.0(5) . . ? C2C C1C P2 118.5(5) . . ? C1C C2C C3C 119.6(7) . . ? C4C C3C C2C 119.6(7) . . ? C5C C4C C3C 121.7(7) . . ? C4C C5C C6C 119.2(7) . . ? C1C C6C C5C 119.4(7) . . ? C6D C1D C2D 118.9(6) . . ? C6D C1D P2 122.4(5) . . ? C2D C1D P2 118.7(5) . . ? C3D C2D C1D 119.7(6) . . ? C4D C3D C2D 120.2(7) . . ? C3D C4D C5D 121.4(7) . . ? C4D C5D C6D 118.9(7) . . ? C1D C6D C5D 120.8(7) . . ? C2E C1E C6E 119.0(6) . . ? C2E C1E P3 118.2(5) . . ? C6E C1E P3 122.7(5) . . ? C1E C2E C3E 119.8(6) . . ? C4E C3E C2E 120.9(7) . . ? C3E C4E C5E 119.6(7) . . ? C4E C5E C6E 121.0(7) . . ? C5E C6E C1E 119.6(7) . . ? C2F C1F C6F 118.7(6) . . ? C2F C1F P3 120.0(5) . . ? C6F C1F P3 121.3(5) . . ? C1F C2F C3F 120.7(6) . . ? C2F C3F C4F 119.2(7) . . ? C5F C4F C3F 120.7(7) . . ? C4F C5F C6F 119.5(7) . . ? C5F C6F C1F 121.2(7) . . ? C2G C1G C6G 119.5(6) . . ? C2G C1G P4 118.9(5) . . ? C6G C1G P4 121.5(5) . . ? C1G C2G C3G 120.4(7) . . ? C4G C3G C2G 119.7(7) . . ? C3G C4G C5G 120.3(7) . . ? C6G C5G C4G 120.0(7) . . ? C5G C6G C1G 120.1(7) . . ? C2H C1H C6H 118.8(6) . . ? C2H C1H P4 119.0(5) . . ? C6H C1H P4 122.1(5) . . ? C1H C2H C3H 120.1(7) . . ? C4H C3H C2H 121.0(8) . . ? C3H C4H C5H 120.3(7) . . ? C4H C5H C6H 119.2(7) . . ? C1H C6H C5H 120.5(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.928 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.133 data_Cpd3 _database_code_depnum_ccdc_archive 'CCDC 823890' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H60 Cl6 Cr2 Fe2 O5 P4' _chemical_formula_weight 1521.45 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1220(4) _cell_length_b 15.5622(5) _cell_length_c 39.1918(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.4650(10) _cell_angle_gamma 90.00 _cell_volume 6777.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6876 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 23.51 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6174 _exptl_absorpt_correction_T_max 0.7920 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47443 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15537 _reflns_number_gt 11705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0701P)^2^+8.0278P] 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 15537 _refine_ls_number_parameters 815 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1496 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.63087(4) 0.23867(3) 0.128920(11) 0.01964(10) Uani 1 1 d . . . Cr2 Cr 0.90693(5) 0.25068(4) 0.380361(15) 0.04360(16) Uani 1 1 d . . . Fe1 Fe 0.46399(4) 0.27984(3) 0.016178(11) 0.02923(11) Uani 1 1 d . . . Fe2 Fe 0.75440(4) 0.19398(3) 0.245481(11) 0.02961(11) Uani 1 1 d . . . Cl1 Cl 0.80640(7) 0.31442(5) 0.11865(2) 0.03437(19) Uani 1 1 d . . . Cl2 Cl 0.45743(6) 0.16048(5) 0.14032(2) 0.03167(18) Uani 1 1 d . . . Cl3 Cl 0.76918(12) 0.21834(8) 0.41593(4) 0.0892(4) Uani 1 1 d . . . Cl4 Cl 1.06078(15) 0.30854(16) 0.40738(5) 0.1513(8) Uani 1 1 d . . . Cl5 Cl 0.96480(12) 0.13205(9) 0.35552(3) 0.0714(4) Uani 1 1 d . . . Cl6 Cl 0.83230(19) 0.33809(9) 0.34101(4) 0.1069(6) Uani 1 1 d . . . P1 P 0.48141(7) 0.40112(5) 0.086198(19) 0.02306(17) Uani 1 1 d . . . P2 P 0.61099(7) 0.11825(5) 0.057355(19) 0.02446(17) Uani 1 1 d . . . P3 P 0.82242(7) 0.09985(5) 0.17097(2) 0.02514(18) Uani 1 1 d . . . P4 P 0.57090(7) 0.33280(5) 0.204553(19) 0.02390(17) Uani 1 1 d . . . O1 O 0.52781(19) 0.32528(13) 0.10609(5) 0.0283(5) Uani 1 1 d . . . O2 O 0.65194(19) 0.17856(13) 0.08530(5) 0.0291(5) Uani 1 1 d . . . O3 O 0.72305(17) 0.14613(13) 0.15206(5) 0.0271(5) Uani 1 1 d . . . O4 O 0.61941(19) 0.30430(13) 0.17144(5) 0.0277(5) Uani 1 1 d . . . C1 C 0.5113(3) 0.38862(19) 0.04228(8) 0.0292(7) Uani 1 1 d . . . C2 C 0.4342(3) 0.4087(2) 0.01273(8) 0.0370(8) Uani 1 1 d . . . H2 H 0.3551 0.4378 0.0128 0.044 Uiso 1 1 calc R . . C3 C 0.4934(4) 0.3796(2) -0.01636(9) 0.0482(10) Uani 1 1 d . . . H3 H 0.4611 0.3838 -0.0402 0.058 Uiso 1 1 calc R . . C4 C 0.6047(4) 0.3422(2) -0.00590(9) 0.0464(10) Uani 1 1 d . . . H4 H 0.6633 0.3159 -0.0211 0.056 Uiso 1 1 calc R . . C5 C 0.6164(3) 0.3473(2) 0.03026(9) 0.0346(8) Uani 1 1 d . . . H5 H 0.6851 0.3255 0.0447 0.042 Uiso 1 1 calc R . . C6 C 0.4827(3) 0.15776(19) 0.03360(8) 0.0283(7) Uani 1 1 d . . . C7 C 0.4600(3) 0.1580(2) -0.00275(8) 0.0371(8) Uani 1 1 d . . . H7 H 0.5130 0.1342 -0.0201 0.045 Uiso 1 1 calc R . . C8 C 0.3460(3) 0.1983(2) -0.00917(9) 0.0429(9) Uani 1 1 d . . . H8 H 0.3071 0.2088 -0.0320 0.051 Uiso 1 1 calc R . . C9 C 0.2994(3) 0.2225(2) 0.02216(9) 0.0384(9) Uani 1 1 d . . . H9 H 0.2224 0.2530 0.0251 0.046 Uiso 1 1 calc R . . C10 C 0.3824(3) 0.19800(19) 0.04883(9) 0.0299(7) Uani 1 1 d . . . H10 H 0.3730 0.2073 0.0736 0.036 Uiso 1 1 calc R . . C11 C 0.8673(3) 0.1523(2) 0.20985(8) 0.0318(8) Uani 1 1 d . . . C12 C 0.8996(3) 0.1153(3) 0.24267(8) 0.0393(9) Uani 1 1 d . . . H12 H 0.9022 0.0532 0.2482 0.047 Uiso 1 1 calc R . . C13 C 0.9267(3) 0.1837(3) 0.26545(9) 0.0485(11) Uani 1 1 d . . . H13 H 0.9502 0.1777 0.2900 0.058 Uiso 1 1 calc R . . C14 C 0.9121(3) 0.2623(3) 0.24742(9) 0.0430(9) Uani 1 1 d . . . H14 H 0.9237 0.3206 0.2572 0.052 Uiso 1 1 calc R . . C15 C 0.8763(3) 0.2430(2) 0.21306(8) 0.0326(8) Uani 1 1 d . . . H15 H 0.8589 0.2855 0.1947 0.039 Uiso 1 1 calc R . . C16 C 0.5939(3) 0.2536(2) 0.23664(8) 0.0298(7) Uani 1 1 d . . . C17 C 0.6347(3) 0.2627(2) 0.27201(8) 0.0375(9) Uani 1 1 d . . . H17 H 0.6511 0.3175 0.2842 0.045 Uiso 1 1 calc R . . C18 C 0.6467(3) 0.1794(2) 0.28614(9) 0.0427(9) Uani 1 1 d . . . H18 H 0.6746 0.1659 0.3099 0.051 Uiso 1 1 calc R . . C19 C 0.6151(3) 0.1189(3) 0.26052(10) 0.0441(9) Uani 1 1 d . . . H19 H 0.6176 0.0557 0.2633 0.053 Uiso 1 1 calc R . . C20 C 0.5821(3) 0.1633(2) 0.22985(9) 0.0335(8) Uani 1 1 d . . . H20 H 0.5564 0.1368 0.2078 0.040 Uiso 1 1 calc R . . C1A C 0.3229(3) 0.4106(2) 0.08956(8) 0.0278(7) Uani 1 1 d . . . C2A C 0.2591(3) 0.4815(2) 0.07599(9) 0.0379(8) Uani 1 1 d . . . H2A H 0.3006 0.5258 0.0652 0.045 Uiso 1 1 calc R . . C3A C 0.1367(3) 0.4862(3) 0.07838(11) 0.0522(11) Uani 1 1 d . . . H3A H 0.0947 0.5348 0.0700 0.063 Uiso 1 1 calc R . . C4A C 0.0750(3) 0.4195(3) 0.09317(11) 0.0546(11) Uani 1 1 d . . . H4A H -0.0093 0.4222 0.0941 0.066 Uiso 1 1 calc R . . C5A C 0.1356(3) 0.3498(2) 0.10646(10) 0.0443(10) Uani 1 1 d . . . H5A H 0.0928 0.3049 0.1165 0.053 Uiso 1 1 calc R . . C6A C 0.2600(3) 0.3450(2) 0.10519(8) 0.0335(8) Uani 1 1 d . . . H6A H 0.3017 0.2977 0.1148 0.040 Uiso 1 1 calc R . . C1B C 0.5524(3) 0.49925(19) 0.10065(8) 0.0289(7) Uani 1 1 d . . . C2B C 0.4947(3) 0.5599(2) 0.12015(9) 0.0400(9) Uani 1 1 d . . . H2B H 0.4128 0.5534 0.1245 0.048 Uiso 1 1 calc R . . C3B C 0.5588(4) 0.6308(2) 0.13323(11) 0.0544(11) Uani 1 1 d . . . H3B H 0.5205 0.6711 0.1470 0.065 Uiso 1 1 calc R . . C4B C 0.6756(4) 0.6416(2) 0.12615(11) 0.0556(11) Uani 1 1 d . . . H4B H 0.7179 0.6895 0.1351 0.067 Uiso 1 1 calc R . . C5B C 0.7338(4) 0.5835(3) 0.10607(11) 0.0538(11) Uani 1 1 d . . . H5B H 0.8148 0.5922 0.1010 0.065 Uiso 1 1 calc R . . C6B C 0.6722(3) 0.5124(2) 0.09334(10) 0.0411(9) Uani 1 1 d . . . H6B H 0.7117 0.4726 0.0797 0.049 Uiso 1 1 calc R . . C1C C 0.7299(3) 0.1055(2) 0.02836(8) 0.0335(8) Uani 1 1 d . . . C2C C 0.8216(4) 0.1654(3) 0.02792(12) 0.0549(11) Uani 1 1 d . . . H2C H 0.8237 0.2112 0.0436 0.066 Uiso 1 1 calc R . . C3C C 0.9106(4) 0.1576(3) 0.00435(14) 0.0765(15) Uani 1 1 d . . . H3C H 0.9727 0.1985 0.0038 0.092 Uiso 1 1 calc R . . C4C C 0.9077(4) 0.0896(3) -0.01834(12) 0.0725(15) Uani 1 1 d . . . H4C H 0.9673 0.0850 -0.0345 0.087 Uiso 1 1 calc R . . C5C C 0.8198(4) 0.0297(3) -0.01742(11) 0.0656(13) Uani 1 1 d . . . H5C H 0.8203 -0.0175 -0.0324 0.079 Uiso 1 1 calc R . . C6C C 0.7294(4) 0.0376(3) 0.00545(9) 0.0491(10) Uani 1 1 d . . . H6C H 0.6672 -0.0033 0.0055 0.059 Uiso 1 1 calc R . . C1D C 0.5724(3) 0.01353(19) 0.07233(7) 0.0284(7) Uani 1 1 d . . . C2D C 0.6612(3) -0.0442(2) 0.08342(9) 0.0422(9) Uani 1 1 d . . . H2D H 0.7429 -0.0291 0.0824 0.051 Uiso 1 1 calc R . . C3D C 0.6297(4) -0.1232(3) 0.09580(10) 0.0556(11) Uani 1 1 d . . . H3D H 0.6901 -0.1622 0.1031 0.067 Uiso 1 1 calc R . . C4D C 0.5105(4) -0.1461(2) 0.09758(10) 0.0537(11) Uani 1 1 d . . . H4D H 0.4898 -0.2005 0.1059 0.064 Uiso 1 1 calc R . . C5D C 0.4219(4) -0.0892(2) 0.08721(10) 0.0478(10) Uani 1 1 d . . . H5D H 0.3405 -0.1043 0.0887 0.057 Uiso 1 1 calc R . . C6D C 0.4527(3) -0.0103(2) 0.07460(9) 0.0380(9) Uani 1 1 d . . . H6D H 0.3917 0.0283 0.0674 0.046 Uiso 1 1 calc R . . C1E C 0.9557(3) 0.0934(2) 0.14684(8) 0.0302(7) Uani 1 1 d . . . C2E C 0.9471(3) 0.1038(3) 0.11169(9) 0.0476(10) Uani 1 1 d . . . H2E H 0.8717 0.1129 0.1005 0.057 Uiso 1 1 calc R . . C3E C 1.0499(4) 0.1007(3) 0.09314(11) 0.0616(13) Uani 1 1 d . . . H3E H 1.0449 0.1085 0.0693 0.074 Uiso 1 1 calc R . . C4E C 1.1585(4) 0.0865(3) 0.10957(11) 0.0580(12) Uani 1 1 d . . . H4E H 1.2279 0.0830 0.0968 0.070 Uiso 1 1 calc R . . C5E C 1.1686(4) 0.0773(3) 0.14326(12) 0.0682(14) Uani 1 1 d . . . H5E H 1.2449 0.0686 0.1540 0.082 Uiso 1 1 calc R . . C6E C 1.0681(3) 0.0806(3) 0.16263(10) 0.0545(12) Uani 1 1 d . . . H6E H 1.0758 0.0741 0.1865 0.065 Uiso 1 1 calc R . . C1F C 0.7720(3) -0.0076(2) 0.18053(8) 0.0336(8) Uani 1 1 d . . . C2F C 0.8525(4) -0.0721(3) 0.18945(13) 0.0643(13) Uani 1 1 d . . . H2F H 0.9357 -0.0613 0.1908 0.077 Uiso 1 1 calc R . . C3F C 0.8077(5) -0.1543(3) 0.19644(15) 0.0824(17) Uani 1 1 d . . . H3F H 0.8615 -0.1986 0.2028 0.099 Uiso 1 1 calc R . . C4F C 0.6885(5) -0.1705(3) 0.19422(11) 0.0630(13) Uani 1 1 d . . . H4F H 0.6598 -0.2256 0.1993 0.076 Uiso 1 1 calc R . . C5F C 0.6091(4) -0.1066(3) 0.18459(10) 0.0505(10) Uani 1 1 d . . . H5F H 0.5262 -0.1183 0.1828 0.061 Uiso 1 1 calc R . . C6F C 0.6507(3) -0.0251(2) 0.17756(9) 0.0380(8) Uani 1 1 d . . . H6F H 0.5961 0.0184 0.1707 0.046 Uiso 1 1 calc R . . C1G C 0.4119(3) 0.3563(2) 0.20159(8) 0.0297(7) Uani 1 1 d . . . C2G C 0.3276(3) 0.2966(3) 0.21158(12) 0.0595(12) Uani 1 1 d . . . H2G H 0.3530 0.2436 0.2209 0.071 Uiso 1 1 calc R . . C3G C 0.2072(4) 0.3151(3) 0.20786(15) 0.0788(16) Uani 1 1 d . . . H3G H 0.1503 0.2749 0.2149 0.095 Uiso 1 1 calc R . . C4G C 0.1689(3) 0.3925(3) 0.19373(11) 0.0582(12) Uani 1 1 d . . . H4G H 0.0862 0.4045 0.1910 0.070 Uiso 1 1 calc R . . C5G C 0.2505(3) 0.4506(3) 0.18390(11) 0.0513(11) Uani 1 1 d . . . H5G H 0.2243 0.5032 0.1745 0.062 Uiso 1 1 calc R . . C6G C 0.3734(3) 0.4333(2) 0.18761(9) 0.0406(9) Uani 1 1 d . . . H6G H 0.4297 0.4740 0.1806 0.049 Uiso 1 1 calc R . . C1H C 0.6487(3) 0.4292(2) 0.21787(8) 0.0292(7) Uani 1 1 d . . . C2H C 0.7371(3) 0.4617(2) 0.19778(9) 0.0398(9) Uani 1 1 d . . . H2H H 0.7538 0.4350 0.1770 0.048 Uiso 1 1 calc R . . C3H C 0.8012(4) 0.5343(3) 0.20844(11) 0.0549(11) Uani 1 1 d . . . H3H H 0.8623 0.5561 0.1951 0.066 Uiso 1 1 calc R . . C4H C 0.7750(4) 0.5741(3) 0.23859(12) 0.0593(12) Uani 1 1 d . . . H4H H 0.8178 0.6237 0.2455 0.071 Uiso 1 1 calc R . . C5H C 0.6873(3) 0.5425(2) 0.25872(10) 0.0489(10) Uani 1 1 d . . . H5H H 0.6714 0.5697 0.2795 0.059 Uiso 1 1 calc R . . C6H C 0.6219(3) 0.4701(2) 0.24837(9) 0.0373(8) Uani 1 1 d . . . H6H H 0.5604 0.4489 0.2618 0.045 Uiso 1 1 calc R . . C1S C 0.0026(6) 0.5201(7) 0.0005(3) 0.083(3) Uani 0.50 1 d PDU A -1 H1SA H 0.0191 0.5226 0.0250 0.124 Uiso 0.50 1 calc PR A -1 H1SB H -0.0580 0.4766 -0.0046 0.124 Uiso 0.50 1 calc PR A -1 H1SC H -0.0265 0.5755 -0.0076 0.124 Uiso 0.50 1 calc PR A -1 O1S O 0.1129(6) 0.4982(5) -0.01642(18) 0.089(2) Uani 0.50 1 d PDU A -1 H1S H 0.1161 0.4455 -0.0193 0.134 Uiso 0.50 1 calc PR A -1 O2S O 0.0943(5) 0.3858(6) -0.0205(2) 0.111(2) Uani 0.50 1 d PDU B 2 H2S H 0.0908 0.3467 -0.0349 0.166 Uiso 0.50 1 calc PR B 2 C2S C -0.0134(8) 0.3849(9) -0.0012(3) 0.122(3) Uani 0.50 1 d PDU B 2 H2SA H 0.0053 0.3624 0.0215 0.183 Uiso 0.50 1 calc PR B 2 H2SB H -0.0736 0.3488 -0.0127 0.183 Uiso 0.50 1 calc PR B 2 H2SC H -0.0444 0.4430 0.0006 0.183 Uiso 0.50 1 calc PR B 2 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 Cr1 0.0172(2) 0.0213(2) 0.0204(2) 0.00050(18) 0.00122(17) -0.00016(17) Cr2 0.0344(3) 0.0593(4) 0.0374(3) -0.0074(3) 0.0054(2) -0.0072(3) Fe1 0.0393(3) 0.0250(2) 0.0232(2) 0.00010(17) -0.00150(18) -0.00036(19) Fe2 0.0237(2) 0.0402(3) 0.0249(2) 0.00288(19) 0.00096(17) 0.00422(18) Cl1 0.0243(4) 0.0390(4) 0.0405(4) 0.0001(3) 0.0088(3) -0.0084(3) Cl2 0.0213(3) 0.0327(4) 0.0409(4) 0.0084(3) 0.0000(3) -0.0053(3) Cl3 0.0865(8) 0.0611(7) 0.1253(11) 0.0157(7) 0.0655(8) 0.0148(6) Cl4 0.0715(10) 0.252(2) 0.1304(13) -0.1029(14) 0.0031(9) -0.0467(12) Cl5 0.0773(8) 0.0901(9) 0.0469(6) -0.0051(6) 0.0046(5) 0.0264(7) Cl6 0.1761(17) 0.0606(8) 0.0824(10) 0.0059(7) -0.0136(10) 0.0060(10) P1 0.0246(4) 0.0193(4) 0.0253(4) 0.0016(3) 0.0005(3) -0.0012(3) P2 0.0269(4) 0.0236(4) 0.0231(4) -0.0034(3) 0.0037(3) 0.0006(3) P3 0.0194(4) 0.0284(4) 0.0277(4) 0.0021(3) 0.0014(3) 0.0034(3) P4 0.0212(4) 0.0274(4) 0.0232(4) -0.0013(3) 0.0027(3) 0.0012(3) O1 0.0294(11) 0.0258(11) 0.0295(11) 0.0033(9) -0.0017(9) 0.0039(9) O2 0.0295(11) 0.0304(11) 0.0272(11) -0.0061(9) -0.0008(9) 0.0014(9) O3 0.0202(10) 0.0305(11) 0.0303(11) 0.0037(9) -0.0019(8) 0.0037(8) O4 0.0283(11) 0.0321(11) 0.0231(10) -0.0038(9) 0.0040(8) -0.0010(9) C1 0.0376(17) 0.0209(15) 0.0291(16) 0.0035(12) 0.0025(13) -0.0061(13) C2 0.056(2) 0.0245(16) 0.0299(17) 0.0065(13) -0.0045(15) -0.0021(15) C3 0.085(3) 0.0345(19) 0.0256(17) 0.0081(15) 0.0016(18) -0.0080(19) C4 0.065(2) 0.041(2) 0.0344(19) 0.0032(16) 0.0190(17) -0.0106(18) C5 0.0339(17) 0.0313(17) 0.0392(18) -0.0011(14) 0.0084(14) -0.0061(14) C6 0.0332(16) 0.0227(15) 0.0288(16) -0.0035(12) -0.0009(13) -0.0007(12) C7 0.049(2) 0.0297(17) 0.0319(17) -0.0068(14) -0.0051(15) 0.0009(15) C8 0.051(2) 0.0341(19) 0.041(2) -0.0056(15) -0.0188(16) -0.0002(16) C9 0.0299(17) 0.0308(18) 0.054(2) -0.0018(16) -0.0103(15) -0.0004(14) C10 0.0292(16) 0.0222(15) 0.0384(17) 0.0018(13) 0.0034(13) -0.0037(12) C11 0.0211(14) 0.0455(19) 0.0288(16) -0.0014(14) -0.0002(12) 0.0065(13) C12 0.0273(16) 0.057(2) 0.0330(18) 0.0040(16) -0.0030(14) 0.0138(15) C13 0.0276(17) 0.085(3) 0.0324(18) -0.0071(19) -0.0090(14) 0.0098(18) C14 0.0264(17) 0.061(2) 0.042(2) -0.0177(17) 0.0022(15) -0.0075(16) C15 0.0247(15) 0.0391(18) 0.0342(17) -0.0031(14) 0.0040(13) -0.0029(13) C16 0.0221(14) 0.0399(18) 0.0279(16) 0.0016(13) 0.0062(12) 0.0045(13) C17 0.0326(17) 0.053(2) 0.0274(17) 0.0004(15) 0.0079(13) 0.0129(15) C18 0.0401(19) 0.062(2) 0.0266(17) 0.0142(16) 0.0101(14) 0.0078(17) C19 0.0345(18) 0.047(2) 0.051(2) 0.0201(17) 0.0073(16) 0.0010(16) C20 0.0241(15) 0.0359(18) 0.0404(18) 0.0048(15) 0.0013(13) -0.0004(13) C1A 0.0280(15) 0.0286(16) 0.0267(15) -0.0047(12) -0.0023(12) 0.0022(12) C2A 0.0336(18) 0.0336(18) 0.046(2) 0.0088(15) -0.0015(15) 0.0033(14) C3A 0.039(2) 0.046(2) 0.071(3) 0.008(2) -0.0052(19) 0.0165(17) C4A 0.0253(18) 0.065(3) 0.074(3) 0.002(2) 0.0057(18) 0.0014(18) C5A 0.0333(18) 0.046(2) 0.054(2) -0.0035(18) 0.0100(16) -0.0098(16) C6A 0.0304(16) 0.0324(17) 0.0379(18) -0.0028(14) 0.0038(14) 0.0006(13) C1B 0.0344(16) 0.0238(15) 0.0281(16) 0.0049(12) -0.0047(13) -0.0029(13) C2B 0.047(2) 0.0333(18) 0.0395(19) -0.0049(15) 0.0031(16) -0.0045(15) C3B 0.074(3) 0.035(2) 0.053(2) -0.0112(18) 0.000(2) -0.0051(19) C4B 0.075(3) 0.031(2) 0.059(3) 0.0011(18) -0.017(2) -0.0214(19) C5B 0.043(2) 0.044(2) 0.073(3) 0.004(2) -0.010(2) -0.0184(17) C6B 0.0381(19) 0.0327(18) 0.052(2) 0.0022(16) 0.0017(16) -0.0070(15) C1C 0.0347(17) 0.0351(18) 0.0309(17) 0.0040(14) 0.0054(14) 0.0046(14) C2C 0.043(2) 0.048(2) 0.076(3) -0.004(2) 0.023(2) -0.0013(18) C3C 0.055(3) 0.076(3) 0.101(4) 0.026(3) 0.035(3) 0.004(2) C4C 0.065(3) 0.101(4) 0.055(3) 0.013(3) 0.034(2) 0.031(3) C5C 0.058(3) 0.090(3) 0.050(2) -0.023(2) 0.012(2) 0.019(2) C6C 0.044(2) 0.062(3) 0.042(2) -0.0159(18) 0.0071(17) 0.0080(18) C1D 0.0371(17) 0.0249(15) 0.0234(15) -0.0013(12) 0.0034(13) 0.0005(13) C2D 0.044(2) 0.0370(19) 0.045(2) 0.0060(16) -0.0029(16) 0.0029(16) C3D 0.074(3) 0.040(2) 0.053(2) 0.0144(18) -0.005(2) 0.016(2) C4D 0.078(3) 0.0296(19) 0.054(2) 0.0116(17) 0.008(2) -0.0021(19) C5D 0.047(2) 0.035(2) 0.063(2) 0.0037(18) 0.0162(19) -0.0071(16) C6D 0.0394(18) 0.0270(17) 0.048(2) 0.0011(15) 0.0093(16) 0.0026(14) C1E 0.0213(14) 0.0338(17) 0.0358(17) -0.0024(14) 0.0057(13) 0.0004(12) C2E 0.0328(19) 0.070(3) 0.040(2) -0.0069(19) 0.0056(15) 0.0083(18) C3E 0.053(2) 0.090(3) 0.044(2) -0.006(2) 0.0213(19) 0.016(2) C4E 0.034(2) 0.071(3) 0.071(3) -0.003(2) 0.0250(19) 0.0051(19) C5E 0.0236(19) 0.109(4) 0.072(3) 0.003(3) 0.0051(19) 0.004(2) C6E 0.0290(19) 0.092(3) 0.043(2) 0.003(2) 0.0015(16) 0.0003(19) C1F 0.0344(17) 0.0351(18) 0.0315(17) 0.0078(14) 0.0028(13) 0.0006(14) C2F 0.049(2) 0.040(2) 0.102(4) 0.021(2) -0.017(2) 0.0056(18) C3F 0.086(4) 0.042(3) 0.117(4) 0.030(3) -0.023(3) 0.005(2) C4F 0.093(3) 0.036(2) 0.060(3) 0.0184(19) 0.001(2) -0.015(2) C5F 0.054(2) 0.054(2) 0.045(2) -0.0028(18) 0.0165(18) -0.0210(19) C6F 0.0377(18) 0.0351(18) 0.0419(19) -0.0001(15) 0.0104(15) 0.0008(15) C1G 0.0251(15) 0.0351(17) 0.0290(16) -0.0023(13) 0.0026(12) 0.0046(13) C2G 0.0297(19) 0.060(3) 0.089(3) 0.025(2) 0.007(2) 0.0038(18) C3G 0.029(2) 0.088(4) 0.121(4) 0.032(3) 0.017(2) -0.001(2) C4G 0.0263(19) 0.083(3) 0.065(3) -0.005(2) -0.0010(18) 0.0146(19) C5G 0.044(2) 0.046(2) 0.062(3) -0.0087(19) -0.0151(19) 0.0179(17) C6G 0.0363(18) 0.0357(19) 0.049(2) -0.0018(16) -0.0067(16) 0.0031(15) C1H 0.0260(15) 0.0294(16) 0.0321(16) -0.0039(13) 0.0010(13) 0.0015(12) C2H 0.0375(18) 0.041(2) 0.0417(19) -0.0041(16) 0.0078(15) -0.0097(15) C3H 0.047(2) 0.048(2) 0.071(3) -0.005(2) 0.011(2) -0.0150(18) C4H 0.042(2) 0.046(2) 0.090(3) -0.021(2) -0.005(2) -0.0117(18) C5H 0.045(2) 0.048(2) 0.052(2) -0.0241(18) -0.0092(18) 0.0042(17) C6H 0.0307(17) 0.0409(19) 0.0402(19) -0.0072(15) 0.0012(14) 0.0039(14) C1S 0.085(4) 0.084(4) 0.078(4) 0.004(3) -0.010(3) -0.007(3) O1S 0.078(3) 0.108(3) 0.081(3) 0.006(3) -0.001(3) 0.012(3) O2S 0.105(4) 0.114(4) 0.112(4) 0.020(3) -0.017(3) 0.008(3) C2S 0.131(4) 0.115(4) 0.119(5) 0.001(3) -0.007(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.960(2) . ? Cr1 O4 1.963(2) . ? Cr1 O3 1.967(2) . ? Cr1 O2 1.971(2) . ? Cr1 Cl1 2.3303(9) . ? Cr1 Cl2 2.3399(8) . ? Cr2 Cl4 2.1689(17) . ? Cr2 Cl3 2.1743(14) . ? Cr2 Cl6 2.1927(17) . ? Cr2 Cl5 2.1964(14) . ? Fe1 C6 2.026(3) . ? Fe1 C1 2.035(3) . ? Fe1 C2 2.036(3) . ? Fe1 C7 2.036(3) . ? Fe1 C3 2.044(3) . ? Fe1 C10 2.045(3) . ? Fe1 C5 2.050(3) . ? Fe1 C8 2.051(3) . ? Fe1 C9 2.059(3) . ? Fe1 C4 2.063(4) . ? Fe2 C11 2.024(3) . ? Fe2 C16 2.028(3) . ? Fe2 C17 2.029(3) . ? Fe2 C12 2.033(3) . ? Fe2 C20 2.043(3) . ? Fe2 C13 2.045(3) . ? Fe2 C15 2.045(3) . ? Fe2 C18 2.047(3) . ? Fe2 C19 2.047(4) . ? Fe2 C14 2.050(4) . ? P1 O1 1.494(2) . ? P1 C1 1.778(3) . ? P1 C1A 1.780(3) . ? P1 C1B 1.799(3) . ? P2 O2 1.498(2) . ? P2 C6 1.780(3) . ? P2 C1D 1.790(3) . ? P2 C1C 1.791(3) . ? P3 O3 1.489(2) . ? P3 C11 1.781(3) . ? P3 C1E 1.795(3) . ? P3 C1F 1.808(3) . ? P4 O4 1.494(2) . ? P4 C16 1.772(3) . ? P4 C1H 1.798(3) . ? P4 C1G 1.805(3) . ? C1 C5 1.432(5) . ? C1 C2 1.445(4) . ? C2 C3 1.415(5) . ? C3 C4 1.413(6) . ? C4 C5 1.420(5) . ? C6 C10 1.432(4) . ? C6 C7 1.436(4) . ? C7 C8 1.427(5) . ? C8 C9 1.405(5) . ? C9 C10 1.417(5) . ? C11 C15 1.421(5) . ? C11 C12 1.441(4) . ? C12 C13 1.413(5) . ? C13 C14 1.419(6) . ? C14 C15 1.420(5) . ? C16 C20 1.434(5) . ? C16 C17 1.447(4) . ? C17 C18 1.412(5) . ? C18 C19 1.411(5) . ? C19 C20 1.421(5) . ? C1A C6A 1.394(4) . ? C1A C2A 1.403(4) . ? C2A C3A 1.371(5) . ? C3A C4A 1.386(6) . ? C4A C5A 1.369(6) . ? C5A C6A 1.389(5) . ? C1B C2B 1.389(5) . ? C1B C6B 1.390(5) . ? C2B C3B 1.399(5) . ? C3B C4B 1.350(6) . ? C4B C5B 1.378(6) . ? C5B C6B 1.384(5) . ? C1C C2C 1.382(5) . ? C1C C6C 1.387(5) . ? C2C C3C 1.388(6) . ? C3C C4C 1.382(7) . ? C4C C5C 1.353(7) . ? C5C C6C 1.381(6) . ? C1D C6D 1.389(5) . ? C1D C2D 1.391(5) . ? C2D C3D 1.373(5) . ? C3D C4D 1.378(6) . ? C4D C5D 1.372(6) . ? C5D C6D 1.373(5) . ? C1E C6E 1.385(5) . ? C1E C2E 1.386(5) . ? C2E C3E 1.382(5) . ? C3E C4E 1.362(6) . ? C4E C5E 1.328(6) . ? C5E C6E 1.379(6) . ? C1F C6F 1.376(5) . ? C1F C2F 1.381(5) . ? C2F C3F 1.403(6) . ? C3F C4F 1.349(7) . ? C4F C5F 1.372(6) . ? C5F C6F 1.382(5) . ? C1G C6G 1.377(5) . ? C1G C2G 1.388(5) . ? C2G C3G 1.371(6) . ? C3G C4G 1.386(6) . ? C4G C5G 1.349(6) . ? C5G C6G 1.394(5) . ? C1H C2H 1.382(5) . ? C1H C6H 1.397(5) . ? C2H C3H 1.390(5) . ? C3H C4H 1.376(6) . ? C4H C5H 1.372(6) . ? C5H C6H 1.392(5) . ? C1S O1S 1.459(5) . ? O2S C2S 1.444(5) . ? 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 O1 Cr1 O4 88.38(9) . . ? O1 Cr1 O3 175.53(9) . . ? O4 Cr1 O3 92.36(9) . . ? O1 Cr1 O2 91.12(9) . . ? O4 Cr1 O2 175.79(9) . . ? O3 Cr1 O2 88.47(9) . . ? O1 Cr1 Cl1 92.93(7) . . ? O4 Cr1 Cl1 88.22(7) . . ? O3 Cr1 Cl1 91.50(6) . . ? O2 Cr1 Cl1 87.63(7) . . ? O1 Cr1 Cl2 88.51(7) . . ? O4 Cr1 Cl2 91.39(7) . . ? O3 Cr1 Cl2 87.06(6) . . ? O2 Cr1 Cl2 92.78(7) . . ? Cl1 Cr1 Cl2 178.50(4) . . ? Cl4 Cr2 Cl3 110.24(7) . . ? Cl4 Cr2 Cl6 110.65(9) . . ? Cl3 Cr2 Cl6 109.80(7) . . ? Cl4 Cr2 Cl5 108.98(7) . . ? Cl3 Cr2 Cl5 108.52(6) . . ? Cl6 Cr2 Cl5 108.60(6) . . ? C6 Fe1 C1 126.14(12) . . ? C6 Fe1 C2 163.70(13) . . ? C1 Fe1 C2 41.58(13) . . ? C6 Fe1 C7 41.40(12) . . ? C1 Fe1 C7 163.51(13) . . ? C2 Fe1 C7 153.15(13) . . ? C6 Fe1 C3 154.86(15) . . ? C1 Fe1 C3 68.73(13) . . ? C2 Fe1 C3 40.59(14) . . ? C7 Fe1 C3 118.78(14) . . ? C6 Fe1 C10 41.17(12) . . ? C1 Fe1 C10 108.38(13) . . ? C2 Fe1 C10 125.43(14) . . ? C7 Fe1 C10 69.19(13) . . ? C3 Fe1 C10 161.88(15) . . ? C6 Fe1 C5 108.52(13) . . ? C1 Fe1 C5 41.04(13) . . ? C2 Fe1 C5 69.13(14) . . ? C7 Fe1 C5 125.44(14) . . ? C3 Fe1 C5 68.07(15) . . ? C10 Fe1 C5 122.31(13) . . ? C6 Fe1 C8 68.76(13) . . ? C1 Fe1 C8 154.70(14) . . ? C2 Fe1 C8 118.57(14) . . ? C7 Fe1 C8 40.88(14) . . ? C3 Fe1 C8 106.47(15) . . ? C10 Fe1 C8 68.06(14) . . ? C5 Fe1 C8 162.15(15) . . ? C6 Fe1 C9 68.53(13) . . ? C1 Fe1 C9 121.01(14) . . ? C2 Fe1 C9 106.97(14) . . ? C7 Fe1 C9 68.41(14) . . ? C3 Fe1 C9 124.54(16) . . ? C10 Fe1 C9 40.39(13) . . ? C5 Fe1 C9 157.02(14) . . ? C8 Fe1 C9 39.97(15) . . ? C6 Fe1 C4 120.91(15) . . ? C1 Fe1 C4 68.60(14) . . ? C2 Fe1 C4 68.46(15) . . ? C7 Fe1 C4 106.88(15) . . ? C3 Fe1 C4 40.24(16) . . ? C10 Fe1 C4 156.96(14) . . ? C5 Fe1 C4 40.38(14) . . ? C8 Fe1 C4 124.68(15) . . ? C9 Fe1 C4 161.06(15) . . ? C11 Fe2 C16 126.58(12) . . ? C11 Fe2 C17 164.28(14) . . ? C16 Fe2 C17 41.80(12) . . ? C11 Fe2 C12 41.59(13) . . ? C16 Fe2 C12 163.99(13) . . ? C17 Fe2 C12 152.29(13) . . ? C11 Fe2 C20 108.66(13) . . ? C16 Fe2 C20 41.25(13) . . ? C17 Fe2 C20 69.45(14) . . ? C12 Fe2 C20 125.44(14) . . ? C11 Fe2 C13 68.91(13) . . ? C16 Fe2 C13 154.79(15) . . ? C17 Fe2 C13 118.03(15) . . ? C12 Fe2 C13 40.56(15) . . ? C20 Fe2 C13 161.42(16) . . ? C11 Fe2 C15 40.86(13) . . ? C16 Fe2 C15 108.97(13) . . ? C17 Fe2 C15 126.07(14) . . ? C12 Fe2 C15 69.04(14) . . ? C20 Fe2 C15 122.62(13) . . ? C13 Fe2 C15 68.40(14) . . ? C11 Fe2 C18 154.53(15) . . ? C16 Fe2 C18 69.11(13) . . ? C17 Fe2 C18 40.55(14) . . ? C12 Fe2 C18 117.92(14) . . ? C20 Fe2 C18 68.58(14) . . ? C13 Fe2 C18 105.27(15) . . ? C15 Fe2 C18 161.91(15) . . ? C11 Fe2 C19 121.01(15) . . ? C16 Fe2 C19 68.84(14) . . ? C17 Fe2 C19 68.40(15) . . ? C12 Fe2 C19 106.50(15) . . ? C20 Fe2 C19 40.67(13) . . ? C13 Fe2 C19 123.58(16) . . ? C15 Fe2 C19 157.20(14) . . ? C18 Fe2 C19 40.31(15) . . ? C11 Fe2 C14 68.70(14) . . ? C16 Fe2 C14 120.96(15) . . ? C17 Fe2 C14 106.67(15) . . ? C12 Fe2 C14 68.56(15) . . ? C20 Fe2 C14 157.27(15) . . ? C13 Fe2 C14 40.57(16) . . ? C15 Fe2 C14 40.58(13) . . ? C18 Fe2 C14 123.84(15) . . ? C19 Fe2 C14 160.44(15) . . ? O1 P1 C1 110.12(13) . . ? O1 P1 C1A 110.35(14) . . ? C1 P1 C1A 107.93(15) . . ? O1 P1 C1B 111.66(13) . . ? C1 P1 C1B 107.45(14) . . ? C1A P1 C1B 109.23(15) . . ? O2 P2 C6 112.19(13) . . ? O2 P2 C1D 113.59(13) . . ? C6 P2 C1D 106.73(15) . . ? O2 P2 C1C 108.88(14) . . ? C6 P2 C1C 107.66(15) . . ? C1D P2 C1C 107.53(15) . . ? O3 P3 C11 112.24(14) . . ? O3 P3 C1E 112.15(14) . . ? C11 P3 C1E 105.61(15) . . ? O3 P3 C1F 108.67(14) . . ? C11 P3 C1F 108.93(16) . . ? C1E P3 C1F 109.14(15) . . ? O4 P4 C16 111.29(14) . . ? O4 P4 C1H 108.22(14) . . ? C16 P4 C1H 108.76(15) . . ? O4 P4 C1G 113.19(13) . . ? C16 P4 C1G 107.36(15) . . ? C1H P4 C1G 107.89(15) . . ? P1 O1 Cr1 164.42(14) . . ? P2 O2 Cr1 152.54(14) . . ? P3 O3 Cr1 160.80(14) . . ? P4 O4 Cr1 158.55(14) . . ? C5 C1 C2 107.3(3) . . ? C5 C1 P1 123.9(2) . . ? C2 C1 P1 128.6(3) . . ? C5 C1 Fe1 70.01(18) . . ? C2 C1 Fe1 69.22(18) . . ? P1 C1 Fe1 121.51(16) . . ? C3 C2 C1 107.3(3) . . ? C3 C2 Fe1 70.0(2) . . ? C1 C2 Fe1 69.20(18) . . ? C4 C3 C2 109.3(3) . . ? C4 C3 Fe1 70.6(2) . . ? C2 C3 Fe1 69.39(19) . . ? C3 C4 C5 108.0(3) . . ? C3 C4 Fe1 69.1(2) . . ? C5 C4 Fe1 69.29(19) . . ? C4 C5 C1 108.2(3) . . ? C4 C5 Fe1 70.3(2) . . ? C1 C5 Fe1 68.94(18) . . ? C10 C6 C7 107.8(3) . . ? C10 C6 P2 123.7(2) . . ? C7 C6 P2 128.5(3) . . ? C10 C6 Fe1 70.12(17) . . ? C7 C6 Fe1 69.65(18) . . ? P2 C6 Fe1 124.65(16) . . ? C8 C7 C6 107.0(3) . . ? C8 C7 Fe1 70.11(19) . . ? C6 C7 Fe1 68.95(18) . . ? C9 C8 C7 108.8(3) . . ? C9 C8 Fe1 70.34(19) . . ? C7 C8 Fe1 69.00(19) . . ? C8 C9 C10 108.6(3) . . ? C8 C9 Fe1 69.7(2) . . ? C10 C9 Fe1 69.27(18) . . ? C9 C10 C6 107.7(3) . . ? C9 C10 Fe1 70.34(19) . . ? C6 C10 Fe1 68.72(18) . . ? C15 C11 C12 107.7(3) . . ? C15 C11 P3 123.2(2) . . ? C12 C11 P3 129.1(3) . . ? C15 C11 Fe2 70.35(18) . . ? C12 C11 Fe2 69.53(18) . . ? P3 C11 Fe2 125.30(16) . . ? C13 C12 C11 107.5(3) . . ? C13 C12 Fe2 70.2(2) . . ? C11 C12 Fe2 68.87(18) . . ? C12 C13 C14 108.6(3) . . ? C12 C13 Fe2 69.29(19) . . ? C14 C13 Fe2 69.9(2) . . ? C13 C14 C15 108.1(3) . . ? C13 C14 Fe2 69.5(2) . . ? C15 C14 Fe2 69.53(19) . . ? C14 C15 C11 108.1(3) . . ? C14 C15 Fe2 69.9(2) . . ? C11 C15 Fe2 68.79(18) . . ? C20 C16 C17 107.2(3) . . ? C20 C16 P4 122.7(2) . . ? C17 C16 P4 129.9(3) . . ? C20 C16 Fe2 69.96(18) . . ? C17 C16 Fe2 69.14(18) . . ? P4 C16 Fe2 122.61(16) . . ? C18 C17 C16 107.8(3) . . ? C18 C17 Fe2 70.4(2) . . ? C16 C17 Fe2 69.06(18) . . ? C19 C18 C17 108.5(3) . . ? C19 C18 Fe2 69.9(2) . . ? C17 C18 Fe2 69.03(19) . . ? C18 C19 C20 108.9(3) . . ? C18 C19 Fe2 69.8(2) . . ? C20 C19 Fe2 69.52(19) . . ? C19 C20 C16 107.5(3) . . ? C19 C20 Fe2 69.82(19) . . ? C16 C20 Fe2 68.78(17) . . ? C6A C1A C2A 119.2(3) . . ? C6A C1A P1 119.3(2) . . ? C2A C1A P1 121.5(2) . . ? C3A C2A C1A 120.2(3) . . ? C2A C3A C4A 120.0(4) . . ? C5A C4A C3A 120.5(4) . . ? C4A C5A C6A 120.3(4) . . ? C5A C6A C1A 119.7(3) . . ? C2B C1B C6B 118.9(3) . . ? C2B C1B P1 122.9(3) . . ? C6B C1B P1 118.1(3) . . ? C1B C2B C3B 119.8(4) . . ? C4B C3B C2B 120.2(4) . . ? C3B C4B C5B 121.0(4) . . ? C4B C5B C6B 119.6(4) . . ? C5B C6B C1B 120.5(4) . . ? C2C C1C C6C 119.2(3) . . ? C2C C1C P2 119.9(3) . . ? C6C C1C P2 120.9(3) . . ? C1C C2C C3C 119.8(4) . . ? C4C C3C C2C 119.8(5) . . ? C5C C4C C3C 120.5(4) . . ? C4C C5C C6C 120.2(4) . . ? C5C C6C C1C 120.4(4) . . ? C6D C1D C2D 118.5(3) . . ? C6D C1D P2 120.5(2) . . ? C2D C1D P2 120.9(3) . . ? C3D C2D C1D 120.0(4) . . ? C2D C3D C4D 120.6(4) . . ? C5D C4D C3D 120.0(4) . . ? C4D C5D C6D 119.7(4) . . ? C5D C6D C1D 121.1(3) . . ? C6E C1E C2E 118.9(3) . . ? C6E C1E P3 121.5(3) . . ? C2E C1E P3 119.6(2) . . ? C3E C2E C1E 119.7(3) . . ? C4E C3E C2E 119.6(4) . . ? C5E C4E C3E 121.5(4) . . ? C4E C5E C6E 120.5(4) . . ? C5E C6E C1E 119.8(4) . . ? C6F C1F C2F 120.0(3) . . ? C6F C1F P3 118.5(3) . . ? C2F C1F P3 121.4(3) . . ? C1F C2F C3F 118.7(4) . . ? C4F C3F C2F 120.9(4) . . ? C3F C4F C5F 120.1(4) . . ? C4F C5F C6F 120.2(4) . . ? C1F C6F C5F 120.0(3) . . ? C6G C1G C2G 119.5(3) . . ? C6G C1G P4 119.3(3) . . ? C2G C1G P4 121.2(3) . . ? C3G C2G C1G 119.9(4) . . ? C2G C3G C4G 120.5(4) . . ? C5G C4G C3G 119.8(4) . . ? C4G C5G C6G 120.6(4) . . ? C1G C6G C5G 119.7(3) . . ? C2H C1H C6H 120.3(3) . . ? C2H C1H P4 119.0(2) . . ? C6H C1H P4 120.7(3) . . ? C1H C2H C3H 119.6(3) . . ? C4H C3H C2H 120.0(4) . . ? C5H C4H C3H 120.9(4) . . ? C4H C5H C6H 119.9(4) . . ? C5H C6H C1H 119.3(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.399 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.100 data_Cpd4 _database_code_depnum_ccdc_archive 'CCDC 823891' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H62 Cl12 Fe4 O4 P4' _chemical_formula_weight 1751.89 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3325(7) _cell_length_b 18.2129(10) _cell_length_c 32.9846(18) _cell_angle_alpha 74.7150(10) _cell_angle_beta 84.3700(10) _cell_angle_gamma 78.4280(10) _cell_volume 7560.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6192 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.83 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 1.308 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5279 _exptl_absorpt_correction_T_max 0.8803 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99083 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 0.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 34647 _reflns_number_gt 24774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0894P)^2^+18.7584P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 34647 _refine_ls_number_parameters 1799 _refine_ls_number_restraints 473 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.2151 _refine_ls_wR_factor_gt 0.1997 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.004 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1D C 0.4420(10) 0.5849(8) 0.4065(3) 0.039(2) Uani 0.482(11) 1 d PGDU A 1 C2D C 0.4142(12) 0.6627(7) 0.4064(4) 0.040(2) Uani 0.482(11) 1 d PGU A 1 H2DA H 0.4405 0.7003 0.3849 0.048 Uiso 0.482(11) 1 calc PR A 1 C3D C 0.3477(12) 0.6849(6) 0.4379(5) 0.048(2) Uani 0.482(11) 1 d PGU A 1 H3DA H 0.3289 0.7376 0.4378 0.058 Uiso 0.482(11) 1 calc PR A 1 C4D C 0.3088(10) 0.6293(7) 0.4696(4) 0.059(3) Uani 0.482(11) 1 d PGU A 1 H4DA H 0.2638 0.6443 0.4910 0.071 Uiso 0.482(11) 1 calc PR A 1 C5D C 0.3366(10) 0.5515(6) 0.4697(3) 0.062(3) Uani 0.482(11) 1 d PGU A 1 H5DA H 0.3103 0.5139 0.4912 0.075 Uiso 0.482(11) 1 calc PR A 1 C6D C 0.4032(10) 0.5293(6) 0.4382(4) 0.052(2) Uani 0.482(11) 1 d PGU A 1 H6DA H 0.4219 0.4767 0.4382 0.063 Uiso 0.482(11) 1 calc PR A 1 C1X C 0.4546(12) 0.5840(10) 0.4103(4) 0.036(2) Uani 0.518(11) 1 d PDU A 2 C2X C 0.4549(12) 0.5298(9) 0.4497(4) 0.053(2) Uani 0.518(11) 1 d PU A 2 H2XA H 0.4926 0.4794 0.4528 0.063 Uiso 0.518(11) 1 calc PR A 2 C3X C 0.3988(12) 0.5515(10) 0.4842(5) 0.060(3) Uani 0.518(11) 1 d PU A 2 H3XA H 0.4000 0.5158 0.5107 0.072 Uiso 0.518(11) 1 calc PR A 2 C4X C 0.3453(12) 0.6204(10) 0.4798(5) 0.057(3) Uani 0.518(11) 1 d PU A 2 H4XA H 0.3051 0.6331 0.5029 0.068 Uiso 0.518(11) 1 calc PR A 2 C5X C 0.3456(15) 0.6715(11) 0.4451(6) 0.051(2) Uani 0.518(11) 1 d PU A 2 H5XA H 0.3090 0.7218 0.4439 0.061 Uiso 0.518(11) 1 calc PR A 2 C6X C 0.3987(14) 0.6558(10) 0.4080(6) 0.040(2) Uani 0.518(11) 1 d PU A 2 H6XA H 0.3953 0.6942 0.3825 0.048 Uiso 0.518(11) 1 calc PR A 2 C1H C 1.0608(4) 0.57572(19) 0.40766(13) 0.0298(19) Uani 0.512(13) 1 d PGDU B 1 C2H C 1.0886(4) 0.5199(2) 0.38489(10) 0.034(2) Uani 0.512(13) 1 d PGU B 1 H2HA H 1.0624 0.5284 0.3583 0.041 Uiso 0.512(13) 1 calc PR B 1 C3H C 1.1550(4) 0.4514(2) 0.40151(13) 0.041(2) Uani 0.512(13) 1 d PGU B 1 H3HA H 1.1738 0.4137 0.3861 0.049 Uiso 0.512(13) 1 calc PR B 1 C4H C 1.1936(5) 0.4388(3) 0.44090(17) 0.047(2) Uani 0.512(13) 1 d PGU B 1 H4HA H 1.2385 0.3925 0.4521 0.056 Uiso 0.512(13) 1 calc PR B 1 C5H C 1.1658(8) 0.4946(4) 0.4637(2) 0.049(2) Uani 0.512(13) 1 d PGU B 1 H5HA H 1.1919 0.4860 0.4903 0.058 Uiso 0.512(13) 1 calc PR B 1 C6H C 1.0994(7) 0.5631(3) 0.44705(19) 0.043(2) Uani 0.512(13) 1 d PGU B 1 H6HA H 1.0806 0.6008 0.4624 0.051 Uiso 0.512(13) 1 calc PR B 1 C1Y C 1.0479(4) 0.5697(2) 0.41049(12) 0.030(2) Uani 0.488(13) 1 d PGDU B 2 C2Y C 1.1003(4) 0.5234(2) 0.38491(9) 0.033(2) Uani 0.488(13) 1 d PGU B 2 H2YA H 1.0961 0.5406 0.3555 0.040 Uiso 0.488(13) 1 calc PR B 2 C3Y C 1.1587(3) 0.4518(2) 0.40278(13) 0.041(2) Uani 0.488(13) 1 d PGU B 2 H3YA H 1.1942 0.4206 0.3855 0.050 Uiso 0.488(13) 1 calc PR B 2 C4Y C 1.1648(6) 0.4265(3) 0.44622(14) 0.048(2) Uani 0.488(13) 1 d PGU B 2 H4YA H 1.2044 0.3781 0.4583 0.058 Uiso 0.488(13) 1 calc PR B 2 C5Y C 1.1124(8) 0.4728(4) 0.47180(10) 0.048(2) Uani 0.488(13) 1 d PGU B 2 H5YA H 1.1166 0.4556 0.5012 0.058 Uiso 0.488(13) 1 calc PR B 2 C6Y C 1.0540(7) 0.5443(4) 0.45394(12) 0.040(2) Uani 0.488(13) 1 d PGU B 2 H6YA H 1.0185 0.5756 0.4712 0.048 Uiso 0.488(13) 1 calc PR B 2 Fe1 Fe 0.74838(5) 0.62720(4) 0.35905(2) 0.01919(15) Uani 1 1 d . . . Fe2 Fe 0.64663(6) 0.39990(4) 0.33659(2) 0.02838(18) Uani 1 1 d . A . Fe3 Fe 0.85029(6) 0.82299(4) 0.41125(2) 0.02767(17) Uani 1 1 d . B . Fe4 Fe 0.54505(5) 0.22254(4) 0.13921(2) 0.02194(16) Uani 1 1 d . . . Fe5 Fe 0.28777(6) 0.43540(5) 0.07300(2) 0.02989(18) Uani 1 1 d . . . Fe6 Fe 0.80017(6) -0.00031(4) 0.19262(3) 0.03103(18) Uani 1 1 d . . . Fe7 Fe 0.09762(8) 0.79279(5) 0.12840(3) 0.0454(2) Uani 1 1 d . . . Fe8 Fe 0.35844(7) 0.12533(5) 0.42026(3) 0.0423(2) Uani 1 1 d . . . Cl1 Cl 0.74734(11) 0.55643(8) 0.43015(4) 0.0326(3) Uani 1 1 d . . . Cl2 Cl 0.75233(10) 0.69905(8) 0.28921(4) 0.0323(3) Uani 1 1 d . . . Cl3 Cl 0.42659(10) 0.16343(8) 0.18899(4) 0.0347(3) Uani 1 1 d . . . Cl4 Cl 0.66783(10) 0.28207(8) 0.09225(4) 0.0347(3) Uani 1 1 d . . . Cl5 Cl -0.03974(15) 0.77274(11) 0.16847(6) 0.0614(5) Uani 1 1 d . . . Cl6 Cl 0.0682(2) 0.90225(12) 0.08216(6) 0.0843(8) Uani 1 1 d . . . Cl7 Cl 0.1483(2) 0.69773(13) 0.09863(9) 0.0954(9) Uani 1 1 d . . . Cl8 Cl 0.2210(2) 0.7946(2) 0.16769(8) 0.1117(11) Uani 1 1 d . . . Cl9 Cl 0.33577(13) 0.24834(9) 0.41834(5) 0.0461(4) Uani 1 1 d . . . Cl10 Cl 0.32635(19) 0.11577(15) 0.35795(7) 0.0791(7) Uani 1 1 d . . . Cl11 Cl 0.51732(15) 0.06857(11) 0.43236(6) 0.0608(5) Uani 1 1 d . . . Cl12 Cl 0.2526(2) 0.07190(12) 0.46880(9) 0.0862(8) Uani 1 1 d . . . P1 P 0.86696(10) 0.46881(7) 0.32113(4) 0.0234(3) Uani 1 1 d . . . P2 P 0.52315(10) 0.56018(8) 0.36423(4) 0.0263(3) Uani 1 1 d D . . P3 P 0.62703(10) 0.80156(7) 0.38005(4) 0.0230(3) Uani 1 1 d . . . P4 P 0.97601(10) 0.66331(7) 0.38465(4) 0.0218(3) Uani 1 1 d D . . P5 P 0.41801(10) 0.39394(7) 0.16173(4) 0.0236(3) Uani 1 1 d . . . P6 P 0.39284(11) 0.26503(8) 0.05368(4) 0.0275(3) Uani 1 1 d . . . P7 P 0.61783(11) 0.04132(8) 0.12397(4) 0.0292(3) Uani 1 1 d . . . P8 P 0.74525(10) 0.18224(8) 0.20392(4) 0.0250(3) Uani 1 1 d . . . O1 O 0.8224(3) 0.5313(2) 0.34309(11) 0.0270(8) Uani 1 1 d . . . O2 O 0.6127(3) 0.6007(2) 0.35178(11) 0.0267(8) Uani 1 1 d . A . O3 O 0.6712(3) 0.7210(2) 0.37638(11) 0.0276(8) Uani 1 1 d . . . O4 O 0.8849(3) 0.6524(2) 0.36467(11) 0.0249(7) Uani 1 1 d . B . O5 O 0.4893(3) 0.3251(2) 0.15205(11) 0.0283(8) Uani 1 1 d . . . O6 O 0.4475(3) 0.2424(2) 0.09373(11) 0.0311(8) Uani 1 1 d . . . O7 O 0.6053(3) 0.1251(2) 0.12370(12) 0.0328(9) Uani 1 1 d . . . O8 O 0.6409(3) 0.1971(2) 0.18665(12) 0.0291(8) Uani 1 1 d . . . C1 C 0.7721(4) 0.4320(3) 0.30217(17) 0.0285(11) Uani 1 1 d . . . C2 C 0.7689(4) 0.3530(3) 0.30375(19) 0.0348(13) Uani 1 1 d . . . H2 H 0.8215 0.3072 0.3152 0.042 Uiso 1 1 calc R . . C3 C 0.6775(5) 0.3525(4) 0.2856(2) 0.0424(15) Uani 1 1 d . . . H3 H 0.6541 0.3059 0.2828 0.051 Uiso 1 1 calc R . . C4 C 0.6237(5) 0.4293(4) 0.27314(19) 0.0391(14) Uani 1 1 d . . . H4 H 0.5564 0.4457 0.2601 0.047 Uiso 1 1 calc R . . C5 C 0.6816(4) 0.4787(3) 0.28273(16) 0.0299(12) Uani 1 1 d . . . H5 H 0.6625 0.5357 0.2774 0.036 Uiso 1 1 calc R . . C6 C 0.5582(4) 0.4578(3) 0.37573(17) 0.0299(12) Uani 1 1 d . A . C7 C 0.5057(5) 0.4030(3) 0.36628(19) 0.0378(14) Uani 1 1 d . . . H7 H 0.4394 0.4152 0.3526 0.045 Uiso 1 1 calc R A . C8 C 0.5656(5) 0.3286(3) 0.3803(2) 0.0420(15) Uani 1 1 d . A . H8 H 0.5491 0.2797 0.3774 0.050 Uiso 1 1 calc R . . C9 C 0.6542(5) 0.3355(3) 0.39785(19) 0.0417(15) Uani 1 1 d . . . H9 H 0.7102 0.2923 0.4092 0.050 Uiso 1 1 calc R A . C10 C 0.6514(5) 0.4147(3) 0.39572(18) 0.0354(13) Uani 1 1 d . A . H10 H 0.7038 0.4364 0.4058 0.042 Uiso 1 1 calc R . . C11 C 0.7229(4) 0.8582(3) 0.37748(17) 0.0293(11) Uani 1 1 d . . . C12 C 0.7293(5) 0.9121(3) 0.4017(2) 0.0392(14) Uani 1 1 d . . . H12 H 0.6783 0.9273 0.4233 0.047 Uiso 1 1 calc R . . C13 C 0.8207(5) 0.9407(4) 0.3879(3) 0.0538(19) Uani 1 1 d . . . H13 H 0.8462 0.9782 0.3993 0.065 Uiso 1 1 calc R . . C14 C 0.8720(5) 0.9056(4) 0.3572(2) 0.0500(18) Uani 1 1 d . . . H14 H 0.9391 0.9145 0.3430 0.060 Uiso 1 1 calc R . . C15 C 0.8115(4) 0.8545(3) 0.34941(18) 0.0332(12) Uani 1 1 d . . . H15 H 0.8283 0.8221 0.3289 0.040 Uiso 1 1 calc R . . C16 C 0.9393(4) 0.7165(3) 0.42348(16) 0.0253(11) Uani 1 1 d . B . C17 C 0.9916(4) 0.7720(3) 0.43292(18) 0.0341(13) Uani 1 1 d . . . H17 H 1.0579 0.7855 0.4200 0.041 Uiso 1 1 calc R B . C18 C 0.9305(5) 0.8031(4) 0.46445(19) 0.0414(15) Uani 1 1 d . B . H18 H 0.9460 0.8434 0.4768 0.050 Uiso 1 1 calc R . . C19 C 0.8414(5) 0.7686(4) 0.47418(18) 0.0382(14) Uani 1 1 d . . . H19 H 0.7847 0.7805 0.4945 0.046 Uiso 1 1 calc R B . C20 C 0.8477(4) 0.7147(3) 0.44925(16) 0.0285(11) Uani 1 1 d . B . H20 H 0.7962 0.6823 0.4494 0.034 Uiso 1 1 calc R . . C21 C 0.3013(4) 0.4200(3) 0.13518(17) 0.0291(11) Uani 1 1 d . . . C22 C 0.2474(5) 0.4963(4) 0.11746(19) 0.0396(14) Uani 1 1 d . . . H22 H 0.2678 0.5457 0.1175 0.048 Uiso 1 1 calc R . . C23 C 0.1589(5) 0.4877(5) 0.0998(2) 0.055(2) Uani 1 1 d . . . H23 H 0.1071 0.5305 0.0847 0.066 Uiso 1 1 calc R . . C24 C 0.1575(5) 0.4089(5) 0.1068(2) 0.0539(19) Uani 1 1 d . . . H24 H 0.1047 0.3870 0.0971 0.065 Uiso 1 1 calc R . . C25 C 0.2448(4) 0.3652(4) 0.12858(17) 0.0357(13) Uani 1 1 d . . . H25 H 0.2634 0.3081 0.1375 0.043 Uiso 1 1 calc R . . C26 C 0.3643(4) 0.3674(3) 0.03607(16) 0.0303(12) Uani 1 1 d . . . C27 C 0.2786(5) 0.4181(4) 0.01503(18) 0.0416(15) Uani 1 1 d . . . H27 H 0.2204 0.4022 0.0051 0.050 Uiso 1 1 calc R . . C28 C 0.2917(6) 0.4953(4) 0.0106(2) 0.0523(19) Uani 1 1 d . . . H28 H 0.2433 0.5427 -0.0023 0.063 Uiso 1 1 calc R . . C29 C 0.3845(5) 0.4931(4) 0.0291(2) 0.0440(15) Uani 1 1 d . . . H29 H 0.4121 0.5386 0.0311 0.053 Uiso 1 1 calc R . . C30 C 0.4303(4) 0.4145(3) 0.04439(17) 0.0330(12) Uani 1 1 d . . . H30 H 0.4957 0.3954 0.0588 0.040 Uiso 1 1 calc R . . C31 C 0.6719(4) -0.0181(3) 0.17176(17) 0.0290(11) Uani 1 1 d . . . C32 C 0.7484(5) -0.0868(3) 0.17718(19) 0.0365(13) Uani 1 1 d . . . H32 H 0.7786 -0.1133 0.1550 0.044 Uiso 1 1 calc R . . C33 C 0.7725(5) -0.1100(3) 0.2199(2) 0.0448(15) Uani 1 1 d . . . H33 H 0.8242 -0.1553 0.2329 0.054 Uiso 1 1 calc R . . C34 C 0.7116(5) -0.0565(4) 0.2412(2) 0.0432(15) Uani 1 1 d . . . H34 H 0.7137 -0.0581 0.2714 0.052 Uiso 1 1 calc R . . C35 C 0.6496(4) 0.0005(3) 0.21138(17) 0.0331(12) Uani 1 1 d . . . H35 H 0.5997 0.0452 0.2171 0.040 Uiso 1 1 calc R . . C36 C 0.8332(4) 0.1039(3) 0.19092(19) 0.0338(12) Uani 1 1 d . . . C37 C 0.9001(5) 0.0434(4) 0.2183(2) 0.0428(15) Uani 1 1 d . . . H37 H 0.9066 0.0375 0.2487 0.051 Uiso 1 1 calc R . . C38 C 0.9551(5) -0.0064(4) 0.1938(3) 0.0540(19) Uani 1 1 d . . . H38 H 1.0059 -0.0539 0.2043 0.065 Uiso 1 1 calc R . . C39 C 0.9236(5) 0.0226(4) 0.1522(3) 0.055(2) Uani 1 1 d . . . H39 H 0.9483 -0.0012 0.1285 0.067 Uiso 1 1 calc R . . C40 C 0.8500(5) 0.0907(4) 0.1502(2) 0.0387(14) Uani 1 1 d . . . H40 H 0.8146 0.1230 0.1247 0.046 Uiso 1 1 calc R . . C1A C 0.9421(4) 0.3892(3) 0.35657(18) 0.0309(12) Uani 1 1 d . . . C2A C 1.0115(5) 0.3328(4) 0.3424(2) 0.0458(15) Uani 1 1 d . . . H2A H 1.0224 0.3370 0.3134 0.055 Uiso 1 1 calc R . . C3A C 1.0647(6) 0.2705(4) 0.3705(3) 0.067(2) Uani 1 1 d . . . H3A H 1.1098 0.2314 0.3607 0.080 Uiso 1 1 calc R . . C4A C 1.0511(6) 0.2656(4) 0.4138(3) 0.061(2) Uani 1 1 d . . . H4A H 1.0882 0.2238 0.4331 0.073 Uiso 1 1 calc R . . C5A C 0.9833(5) 0.3221(4) 0.4278(2) 0.0549(19) Uani 1 1 d . . . H5A H 0.9735 0.3186 0.4568 0.066 Uiso 1 1 calc R . . C6A C 0.9291(4) 0.3845(4) 0.39947(19) 0.0372(13) Uani 1 1 d . . . H6A H 0.8838 0.4234 0.4093 0.045 Uiso 1 1 calc R . . C1B C 0.9466(4) 0.5044(3) 0.27574(17) 0.0280(11) Uani 1 1 d . . . C2B C 0.9685(5) 0.4685(4) 0.2429(2) 0.0413(14) Uani 1 1 d . . . H2B H 0.9414 0.4242 0.2441 0.050 Uiso 1 1 calc R . . C3B C 1.0299(5) 0.4974(4) 0.2085(2) 0.0475(16) Uani 1 1 d . . . H3B H 1.0456 0.4725 0.1865 0.057 Uiso 1 1 calc R . . C4B C 1.0681(5) 0.5637(4) 0.20686(19) 0.0409(14) Uani 1 1 d . . . H4B H 1.1098 0.5835 0.1835 0.049 Uiso 1 1 calc R . . C5B C 1.0459(4) 0.6009(3) 0.23888(19) 0.0351(13) Uani 1 1 d . . . H5B H 1.0719 0.6459 0.2373 0.042 Uiso 1 1 calc R . . C6B C 0.9852(4) 0.5713(3) 0.27331(17) 0.0289(11) Uani 1 1 d . . . H6B H 0.9698 0.5964 0.2953 0.035 Uiso 1 1 calc R . . C1C C 0.4388(4) 0.5900(3) 0.32168(17) 0.0288(11) Uani 1 1 d . A . C2C C 0.3426(4) 0.5685(4) 0.3270(2) 0.0413(14) Uani 1 1 d . . . H2C H 0.3201 0.5407 0.3534 0.050 Uiso 1 1 calc R A . C3C C 0.2800(5) 0.5886(4) 0.2927(2) 0.0505(17) Uani 1 1 d . A . H3C H 0.2160 0.5730 0.2957 0.061 Uiso 1 1 calc R . . C4C C 0.3120(5) 0.6310(4) 0.2548(3) 0.0547(19) Uani 1 1 d . . . H4C H 0.2688 0.6454 0.2320 0.066 Uiso 1 1 calc R A . C5C C 0.4059(5) 0.6529(4) 0.2492(2) 0.0437(15) Uani 1 1 d . A . H5C H 0.4271 0.6814 0.2227 0.052 Uiso 1 1 calc R . . C6C C 0.4698(4) 0.6329(3) 0.28280(18) 0.0336(12) Uani 1 1 d . . . H6C H 0.5339 0.6484 0.2792 0.040 Uiso 1 1 calc R A . C1E C 0.5448(4) 0.8537(3) 0.33747(16) 0.0276(11) Uani 1 1 d . . . C2E C 0.5108(4) 0.8133(4) 0.31279(18) 0.0355(13) Uani 1 1 d . . . H2E H 0.5313 0.7592 0.3183 0.043 Uiso 1 1 calc R . . C3E C 0.4467(5) 0.8521(4) 0.28021(19) 0.0443(15) Uani 1 1 d . . . H3E H 0.4237 0.8245 0.2637 0.053 Uiso 1 1 calc R . . C4E C 0.4171(5) 0.9310(5) 0.2722(2) 0.0527(19) Uani 1 1 d . . . H4E H 0.3740 0.9573 0.2500 0.063 Uiso 1 1 calc R . . C5E C 0.4497(6) 0.9721(4) 0.2964(2) 0.0527(19) Uani 1 1 d . . . H5E H 0.4276 1.0260 0.2909 0.063 Uiso 1 1 calc R . . C6E C 0.5156(5) 0.9339(4) 0.32894(19) 0.0394(14) Uani 1 1 d . . . H6E H 0.5398 0.9620 0.3449 0.047 Uiso 1 1 calc R . . C1F C 0.5561(4) 0.7985(3) 0.42967(16) 0.0285(11) Uani 1 1 d . . . C2F C 0.4945(5) 0.8643(3) 0.43772(19) 0.0398(14) Uani 1 1 d . . . H2F H 0.4848 0.9108 0.4166 0.048 Uiso 1 1 calc R . . C3F C 0.4473(6) 0.8605(4) 0.4775(2) 0.0523(18) Uani 1 1 d . . . H3F H 0.4054 0.9048 0.4835 0.063 Uiso 1 1 calc R . . C4F C 0.4615(5) 0.7921(4) 0.5082(2) 0.0481(16) Uani 1 1 d . . . H4F H 0.4296 0.7902 0.5350 0.058 Uiso 1 1 calc R . . C5F C 0.5218(5) 0.7267(4) 0.49992(19) 0.0426(15) Uani 1 1 d . . . H5F H 0.5305 0.6801 0.5210 0.051 Uiso 1 1 calc R . . C6F C 0.5698(4) 0.7292(3) 0.46035(17) 0.0322(12) Uani 1 1 d . . . H6F H 0.6110 0.6846 0.4545 0.039 Uiso 1 1 calc R . . C1G C 1.0554(4) 0.7151(3) 0.34459(17) 0.0265(11) Uani 1 1 d . B . C2G C 1.0205(4) 0.7454(3) 0.30410(17) 0.0296(11) Uani 1 1 d . . . H2G H 0.9567 0.7376 0.2979 0.036 Uiso 1 1 calc R B . C3G C 1.0793(5) 0.7870(4) 0.2731(2) 0.0437(15) Uani 1 1 d . B . H3G H 1.0566 0.8066 0.2455 0.052 Uiso 1 1 calc R . . C4G C 1.1725(5) 0.7995(4) 0.2830(2) 0.0528(18) Uani 1 1 d . . . H4G H 1.2115 0.8294 0.2622 0.063 Uiso 1 1 calc R B . C5G C 1.2084(5) 0.7690(5) 0.3227(2) 0.0528(18) Uani 1 1 d . B . H5G H 1.2716 0.7778 0.3290 0.063 Uiso 1 1 calc R . . C6G C 1.1512(4) 0.7252(4) 0.3535(2) 0.0411(14) Uani 1 1 d . . . H6G H 1.1769 0.7022 0.3803 0.049 Uiso 1 1 calc R B . C1I C 0.3825(4) 0.3754(3) 0.21711(16) 0.0275(11) Uani 1 1 d . . . C2I C 0.2939(5) 0.4177(4) 0.2313(2) 0.0438(15) Uani 1 1 d . . . H2I H 0.2539 0.4578 0.2121 0.053 Uiso 1 1 calc R . . C3I C 0.2645(6) 0.4008(4) 0.2736(2) 0.0526(18) Uani 1 1 d . . . H3I H 0.2049 0.4299 0.2833 0.063 Uiso 1 1 calc R . . C4I C 0.3221(5) 0.3417(4) 0.30158(19) 0.0458(16) Uani 1 1 d . . . H4I H 0.3020 0.3303 0.3303 0.055 Uiso 1 1 calc R . . C5I C 0.4103(5) 0.2989(4) 0.28719(19) 0.0447(15) Uani 1 1 d . . . H5I H 0.4493 0.2579 0.3063 0.054 Uiso 1 1 calc R . . C6I C 0.4410(5) 0.3159(3) 0.24527(19) 0.0372(13) Uani 1 1 d . . . H6I H 0.5013 0.2873 0.2358 0.045 Uiso 1 1 calc R . . C1J C 0.4767(4) 0.4787(3) 0.14485(17) 0.0283(11) Uani 1 1 d . . . C2J C 0.5564(5) 0.4789(3) 0.11476(19) 0.0366(13) Uani 1 1 d . . . H2J H 0.5851 0.4332 0.1065 0.044 Uiso 1 1 calc R . . C3J C 0.5945(6) 0.5469(4) 0.0965(2) 0.0505(17) Uani 1 1 d . . . H3J H 0.6487 0.5470 0.0760 0.061 Uiso 1 1 calc R . . C4J C 0.5524(6) 0.6133(4) 0.1086(2) 0.0542(19) Uani 1 1 d . . . H4J H 0.5777 0.6592 0.0962 0.065 Uiso 1 1 calc R . . C5J C 0.4732(6) 0.6132(4) 0.1388(2) 0.0567(19) Uani 1 1 d . . . H5J H 0.4448 0.6592 0.1468 0.068 Uiso 1 1 calc R . . C6J C 0.4353(5) 0.5467(4) 0.1574(2) 0.0458(16) Uani 1 1 d . . . H6J H 0.3821 0.5469 0.1783 0.055 Uiso 1 1 calc R . . C1K C 0.4709(5) 0.2333(3) 0.01115(17) 0.0338(13) Uani 1 1 d . . . C2K C 0.4427(5) 0.1852(4) -0.0105(2) 0.0474(16) Uani 1 1 d . . . H2K H 0.3812 0.1662 -0.0028 0.057 Uiso 1 1 calc R . . C3K C 0.5056(6) 0.1654(4) -0.0433(2) 0.0564(19) Uani 1 1 d . . . H3K H 0.4860 0.1336 -0.0583 0.068 Uiso 1 1 calc R . . C4K C 0.5953(6) 0.1916(4) -0.0541(2) 0.0557(19) Uani 1 1 d . . . H4K H 0.6376 0.1775 -0.0763 0.067 Uiso 1 1 calc R . . C5K C 0.6245(6) 0.2381(5) -0.0332(2) 0.0575(19) Uani 1 1 d . . . H5K H 0.6870 0.2556 -0.0407 0.069 Uiso 1 1 calc R . . C6K C 0.5618(5) 0.2596(4) -0.0007(2) 0.0470(16) Uani 1 1 d . . . H6K H 0.5815 0.2926 0.0135 0.056 Uiso 1 1 calc R . . C1L C 0.2774(4) 0.2270(3) 0.06123(18) 0.0330(12) Uani 1 1 d . . . C2L C 0.2124(5) 0.2385(4) 0.0284(2) 0.0445(15) Uani 1 1 d . . . H2L H 0.2278 0.2688 0.0016 0.053 Uiso 1 1 calc R . . C3L C 0.1255(5) 0.2054(5) 0.0354(3) 0.0569(19) Uani 1 1 d . . . H3L H 0.0824 0.2124 0.0132 0.068 Uiso 1 1 calc R . . C4L C 0.1026(6) 0.1620(5) 0.0753(3) 0.063(2) Uani 1 1 d . . . H4L H 0.0436 0.1395 0.0800 0.075 Uiso 1 1 calc R . . C5L C 0.1642(6) 0.1514(4) 0.1078(3) 0.0572(19) Uani 1 1 d . . . H5L H 0.1466 0.1228 0.1348 0.069 Uiso 1 1 calc R . . C6L C 0.2529(5) 0.1830(4) 0.1010(2) 0.0406(14) Uani 1 1 d . . . H6L H 0.2962 0.1747 0.1232 0.049 Uiso 1 1 calc R . . C1M C 0.4983(5) 0.0127(3) 0.1185(2) 0.0400(14) Uani 1 1 d . . . C2M C 0.4629(6) 0.0263(4) 0.0787(3) 0.0555(19) Uani 1 1 d . . . H2M H 0.5011 0.0484 0.0547 0.067 Uiso 1 1 calc R . . C3M C 0.3691(7) 0.0063(5) 0.0751(3) 0.072(3) Uani 1 1 d . . . H3M H 0.3434 0.0162 0.0483 0.087 Uiso 1 1 calc R . . C4M C 0.3153(7) -0.0264(5) 0.1085(4) 0.077(3) Uani 1 1 d . . . H4M H 0.2539 -0.0414 0.1050 0.093 Uiso 1 1 calc R . . C5M C 0.3494(7) -0.0386(6) 0.1489(4) 0.085(3) Uani 1 1 d . . . H5M H 0.3099 -0.0599 0.1727 0.102 Uiso 1 1 calc R . . C6M C 0.4422(6) -0.0189(5) 0.1534(3) 0.065(2) Uani 1 1 d . . . H6M H 0.4665 -0.0272 0.1804 0.078 Uiso 1 1 calc R . . C1N C 0.7008(5) 0.0230(3) 0.08012(18) 0.0374(13) Uani 1 1 d . . . C2N C 0.7197(6) -0.0498(4) 0.0720(2) 0.0486(17) Uani 1 1 d . . . H2N H 0.6889 -0.0899 0.0893 0.058 Uiso 1 1 calc R . . C3N C 0.7843(7) -0.0627(4) 0.0380(2) 0.064(2) Uani 1 1 d . . . H3N H 0.7963 -0.1113 0.0318 0.077 Uiso 1 1 calc R . . C4N C 0.8312(8) -0.0039(5) 0.0131(2) 0.076(3) Uani 1 1 d . . . H4N H 0.8763 -0.0129 -0.0096 0.091 Uiso 1 1 calc R . . C5N C 0.8114(7) 0.0683(4) 0.0217(2) 0.065(2) Uani 1 1 d . . . H5N H 0.8429 0.1082 0.0046 0.078 Uiso 1 1 calc R . . C6N C 0.7465(6) 0.0821(4) 0.0548(2) 0.0471(16) Uani 1 1 d . . . H6N H 0.7331 0.1314 0.0602 0.056 Uiso 1 1 calc R . . C1P C 0.8062(4) 0.2656(3) 0.18609(18) 0.0331(12) Uani 1 1 d . . . C2P C 0.9103(5) 0.2573(5) 0.1787(3) 0.059(2) Uani 1 1 d . . . H2P H 0.9511 0.2077 0.1828 0.071 Uiso 1 1 calc R . . C3P C 0.9549(7) 0.3225(6) 0.1650(3) 0.081(3) Uani 1 1 d . . . H3P H 1.0264 0.3172 0.1605 0.097 Uiso 1 1 calc R . . C4P C 0.8952(8) 0.3943(5) 0.1579(3) 0.076(3) Uani 1 1 d . . . H4P H 0.9258 0.4382 0.1474 0.092 Uiso 1 1 calc R . . C5P C 0.7917(7) 0.4035(4) 0.1660(3) 0.065(2) Uani 1 1 d . . . H5P H 0.7515 0.4533 0.1620 0.078 Uiso 1 1 calc R . . C6P C 0.7466(5) 0.3383(4) 0.1803(2) 0.0461(16) Uani 1 1 d . . . H6P H 0.6754 0.3438 0.1860 0.055 Uiso 1 1 calc R . . C1Q C 0.7322(4) 0.1601(3) 0.26027(17) 0.0286(11) Uani 1 1 d . . . C2Q C 0.8121(5) 0.1626(3) 0.28427(19) 0.0373(13) Uani 1 1 d . . . H2Q H 0.8743 0.1754 0.2711 0.045 Uiso 1 1 calc R . . C3Q C 0.7977(6) 0.1457(4) 0.3277(2) 0.0490(17) Uani 1 1 d . . . H3Q H 0.8507 0.1473 0.3441 0.059 Uiso 1 1 calc R . . C4Q C 0.7077(6) 0.1267(4) 0.3472(2) 0.0513(18) Uani 1 1 d . . . H4Q H 0.7001 0.1145 0.3767 0.062 Uiso 1 1 calc R . . C5Q C 0.6271(6) 0.1252(4) 0.32365(19) 0.0448(15) Uani 1 1 d . . . H5Q H 0.5646 0.1134 0.3370 0.054 Uiso 1 1 calc R . . C6Q C 0.6408(5) 0.1415(3) 0.28041(19) 0.0370(13) Uani 1 1 d . . . H6Q H 0.5874 0.1399 0.2643 0.044 Uiso 1 1 calc R . . C1S C 0.8956(6) 0.3346(4) 0.05060(17) 0.067(2) Uani 1 1 d D . . H1S1 H 0.8305 0.3500 0.0654 0.081 Uiso 1 1 calc R . . H1S2 H 0.9371 0.2922 0.0703 0.081 Uiso 1 1 calc R . . Cl1A Cl 0.95961(18) 0.41289(15) 0.03477(8) 0.0846(7) Uani 1 1 d D . . Cl1B Cl 0.87158(17) 0.30241(15) 0.00763(9) 0.0809(7) Uani 1 1 d D . . C2S C 0.2049(7) 0.1553(4) 0.2559(4) 0.102(3) Uani 1 1 d DU . . H2S1 H 0.2703 0.1629 0.2406 0.122 Uiso 1 1 calc R . . H2S2 H 0.2184 0.1319 0.2856 0.122 Uiso 1 1 calc R . . Cl2A Cl 0.1228(4) 0.2446(3) 0.25080(18) 0.1860(19) Uani 1 1 d DU . . Cl2B Cl 0.1507(4) 0.0930(3) 0.23606(15) 0.1592(16) Uani 1 1 d DU . . C3S C 0.1161(8) 0.3419(5) 0.8983(3) 0.098(3) Uani 1 1 d D . . H3SA H 0.1191 0.3624 0.8676 0.117 Uiso 0.39(3) 1 calc PR C 1 H3SB H 0.0533 0.3203 0.9065 0.117 Uiso 0.39(3) 1 calc PR C 1 H3SC H 0.0465 0.3307 0.9015 0.117 Uiso 0.61(3) 1 d PR C 2 H3SD H 0.1311 0.3617 0.8681 0.117 Uiso 0.61(3) 1 d PR C 2 Cl3A Cl 0.1165(2) 0.41543(14) 0.92323(9) 0.0844(7) Uani 1 1 d DU C . Cl3B Cl 0.2242(6) 0.2698(6) 0.9138(4) 0.058(3) Uani 0.39(3) 1 d PDU C 1 Cl3C Cl 0.1955(18) 0.2592(6) 0.9149(3) 0.151(5) Uani 0.61(3) 1 d P C 2 C4S C 0.3185(6) 0.2668(3) 0.8115(3) 0.087(3) Uani 1 1 d D . . H4S1 H 0.2583 0.2481 0.8271 0.104 Uiso 1 1 calc R . . H4S2 H 0.3213 0.2581 0.7833 0.104 Uiso 1 1 calc R . . Cl4A Cl 0.4285(2) 0.21375(16) 0.83703(9) 0.0945(8) Uani 1 1 d D . . Cl4B Cl 0.3045(3) 0.36622(14) 0.80711(8) 0.0986(9) Uani 1 1 d D . . C5S C 0.1832(11) 0.8950(7) 0.5216(6) 0.292(18) Uani 1 1 d D . . H5SA H 0.2412 0.8848 0.5396 0.350 Uiso 0.782(19) 1 calc PR D 1 H5SB H 0.1959 0.9349 0.4961 0.350 Uiso 0.782(19) 1 calc PR D 1 H5SC H 0.1422 0.9401 0.5033 0.350 Uiso 0.218(19) 1 calc PR D 2 H5SD H 0.2545 0.9025 0.5193 0.350 Uiso 0.218(19) 1 calc PR D 2 Cl5A Cl 0.1751(4) 0.8104(3) 0.50769(17) 0.1719(17) Uani 1 1 d DU D . Cl5B Cl 0.0715(9) 0.9286(7) 0.5479(5) 0.285(7) Uani 0.782(19) 1 d PDU D 1 Cl5C Cl 0.135(2) 0.8813(14) 0.5736(5) 0.176(15) Uani 0.218(19) 1 d PDU D 2 C6S C 0.8185(16) 0.0313(13) 0.6403(11) 0.32(2) Uani 1 1 d . . . H6S1 H 0.7678 -0.0024 0.6442 0.390 Uiso 1 1 calc R . . H6S2 H 0.8141 0.0488 0.6662 0.390 Uiso 1 1 calc R . . Cl6A Cl 0.9275(5) -0.0243(5) 0.6400(4) 0.320(5) Uani 1 1 d . . . Cl6B Cl 0.7769(7) 0.1043(4) 0.6058(3) 0.264(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1D 0.031(4) 0.053(4) 0.036(4) -0.011(4) 0.007(4) -0.014(4) C2D 0.032(5) 0.057(4) 0.039(4) -0.022(4) 0.005(4) -0.014(4) C3D 0.040(4) 0.068(5) 0.041(5) -0.025(4) 0.007(4) -0.010(4) C4D 0.048(5) 0.082(5) 0.041(5) -0.015(4) 0.013(4) -0.004(5) C5D 0.052(5) 0.080(4) 0.044(5) -0.003(4) 0.014(4) -0.011(5) C6D 0.044(5) 0.065(4) 0.041(4) -0.003(4) 0.010(4) -0.013(4) C1X 0.029(4) 0.051(4) 0.032(4) -0.015(3) 0.005(3) -0.017(3) C2X 0.044(5) 0.065(4) 0.042(4) -0.004(4) 0.011(4) -0.014(4) C3X 0.052(5) 0.078(5) 0.042(4) -0.006(4) 0.012(4) -0.011(4) C4X 0.045(5) 0.082(5) 0.040(4) -0.020(4) 0.009(4) -0.005(4) C5X 0.042(4) 0.069(5) 0.043(4) -0.024(4) 0.007(4) -0.007(4) C6X 0.032(4) 0.056(4) 0.039(4) -0.020(4) 0.004(3) -0.013(4) C1H 0.031(4) 0.029(3) 0.029(4) -0.005(3) -0.008(3) -0.005(3) C2H 0.034(4) 0.031(4) 0.038(4) -0.010(3) -0.005(3) -0.001(3) C3H 0.037(4) 0.034(4) 0.048(4) -0.008(3) -0.004(4) 0.002(3) C4H 0.043(4) 0.038(4) 0.049(4) -0.001(3) -0.009(4) 0.007(4) C5H 0.048(5) 0.048(4) 0.041(4) -0.002(3) -0.016(4) 0.005(4) C6H 0.046(5) 0.044(4) 0.035(4) -0.009(3) -0.011(4) 0.004(4) C1Y 0.030(4) 0.031(4) 0.031(4) -0.009(3) -0.011(3) -0.002(3) C2Y 0.034(4) 0.030(4) 0.037(4) -0.010(3) -0.006(3) -0.002(3) C3Y 0.038(4) 0.034(4) 0.048(4) -0.008(4) -0.005(4) 0.003(4) C4Y 0.043(4) 0.040(4) 0.050(4) 0.001(4) -0.010(4) 0.006(4) C5Y 0.052(5) 0.044(4) 0.040(4) 0.000(4) -0.015(4) 0.004(4) C6Y 0.044(5) 0.040(4) 0.033(4) -0.004(3) -0.011(4) 0.002(4) Fe1 0.0203(3) 0.0212(3) 0.0173(3) -0.0043(3) -0.0010(3) -0.0074(3) Fe2 0.0293(4) 0.0239(4) 0.0347(4) -0.0070(3) -0.0017(3) -0.0116(3) Fe3 0.0261(4) 0.0252(4) 0.0346(4) -0.0110(3) -0.0046(3) -0.0053(3) Fe4 0.0216(4) 0.0216(3) 0.0227(4) -0.0070(3) -0.0005(3) -0.0026(3) Fe5 0.0255(4) 0.0349(4) 0.0272(4) -0.0092(3) -0.0021(3) 0.0015(3) Fe6 0.0303(4) 0.0268(4) 0.0350(4) -0.0093(3) -0.0019(3) -0.0009(3) Fe7 0.0533(6) 0.0348(5) 0.0408(5) -0.0036(4) 0.0079(4) -0.0040(4) Fe8 0.0457(5) 0.0400(5) 0.0438(5) -0.0177(4) 0.0074(4) -0.0087(4) Cl1 0.0490(8) 0.0302(7) 0.0178(6) -0.0014(5) -0.0006(5) -0.0120(6) Cl2 0.0334(7) 0.0394(7) 0.0200(6) 0.0028(5) -0.0040(5) -0.0099(6) Cl3 0.0304(7) 0.0420(8) 0.0317(7) -0.0052(6) 0.0026(5) -0.0136(6) Cl4 0.0306(7) 0.0362(7) 0.0357(7) -0.0074(6) 0.0089(6) -0.0096(6) Cl5 0.0514(10) 0.0610(11) 0.0585(11) -0.0090(9) 0.0152(8) 0.0037(9) Cl6 0.121(2) 0.0562(12) 0.0474(11) 0.0094(9) 0.0152(12) 0.0106(12) Cl7 0.1078(19) 0.0565(12) 0.122(2) -0.0423(13) 0.0634(17) -0.0206(12) Cl8 0.102(2) 0.164(3) 0.0627(15) 0.0152(16) -0.0210(14) -0.060(2) Cl9 0.0499(9) 0.0384(8) 0.0513(9) -0.0125(7) -0.0042(7) -0.0083(7) Cl10 0.0857(16) 0.0982(17) 0.0715(14) -0.0500(13) -0.0111(12) -0.0164(13) Cl11 0.0567(11) 0.0603(11) 0.0622(11) -0.0253(9) -0.0027(9) 0.0100(9) Cl12 0.0908(17) 0.0520(12) 0.1059(18) -0.0149(11) 0.0489(14) -0.0221(11) P1 0.0236(6) 0.0223(6) 0.0262(7) -0.0080(5) 0.0001(5) -0.0069(5) P2 0.0231(7) 0.0289(7) 0.0273(7) -0.0050(5) 0.0038(5) -0.0107(5) P3 0.0215(6) 0.0231(6) 0.0241(6) -0.0062(5) -0.0012(5) -0.0027(5) P4 0.0206(6) 0.0247(6) 0.0211(6) -0.0063(5) -0.0053(5) -0.0038(5) P5 0.0226(6) 0.0243(6) 0.0242(6) -0.0084(5) 0.0006(5) -0.0022(5) P6 0.0284(7) 0.0328(7) 0.0226(6) -0.0099(6) -0.0029(5) -0.0036(6) P7 0.0368(8) 0.0222(7) 0.0296(7) -0.0094(6) -0.0029(6) -0.0030(6) P8 0.0221(6) 0.0240(6) 0.0295(7) -0.0071(5) -0.0032(5) -0.0041(5) O1 0.034(2) 0.0244(18) 0.0250(18) -0.0096(15) 0.0016(15) -0.0072(15) O2 0.0231(18) 0.033(2) 0.0284(19) -0.0082(15) -0.0003(14) -0.0138(15) O3 0.0263(19) 0.0274(19) 0.0296(19) -0.0084(15) -0.0020(15) -0.0037(15) O4 0.0215(18) 0.0293(19) 0.0268(18) -0.0091(15) -0.0038(14) -0.0070(14) O5 0.030(2) 0.0260(18) 0.0288(19) -0.0084(15) 0.0004(15) -0.0030(15) O6 0.034(2) 0.033(2) 0.0254(19) -0.0084(16) -0.0068(16) -0.0014(16) O7 0.040(2) 0.0228(18) 0.035(2) -0.0116(16) 0.0010(17) 0.0003(16) O8 0.0253(19) 0.0307(19) 0.032(2) -0.0086(16) -0.0049(15) -0.0047(15) C1 0.029(3) 0.030(3) 0.031(3) -0.012(2) 0.002(2) -0.012(2) C2 0.033(3) 0.030(3) 0.047(3) -0.019(3) 0.001(3) -0.009(2) C3 0.043(4) 0.044(4) 0.054(4) -0.028(3) -0.004(3) -0.018(3) C4 0.036(3) 0.050(4) 0.036(3) -0.013(3) -0.010(3) -0.013(3) C5 0.035(3) 0.031(3) 0.025(3) -0.006(2) -0.002(2) -0.009(2) C6 0.029(3) 0.029(3) 0.033(3) -0.006(2) 0.003(2) -0.013(2) C7 0.035(3) 0.036(3) 0.044(3) -0.004(3) 0.006(3) -0.024(3) C8 0.047(4) 0.030(3) 0.051(4) -0.004(3) 0.006(3) -0.026(3) C9 0.050(4) 0.031(3) 0.037(3) 0.006(3) -0.001(3) -0.011(3) C10 0.035(3) 0.036(3) 0.033(3) -0.002(2) 0.000(2) -0.012(3) C11 0.031(3) 0.022(3) 0.035(3) -0.006(2) -0.007(2) -0.002(2) C12 0.035(3) 0.030(3) 0.055(4) -0.017(3) -0.008(3) 0.000(2) C13 0.046(4) 0.024(3) 0.091(6) -0.007(3) -0.020(4) -0.006(3) C14 0.037(4) 0.038(4) 0.065(5) 0.011(3) -0.008(3) -0.014(3) C15 0.029(3) 0.034(3) 0.031(3) 0.004(2) -0.008(2) -0.004(2) C16 0.024(3) 0.029(3) 0.023(2) -0.009(2) -0.009(2) 0.001(2) C17 0.028(3) 0.043(3) 0.035(3) -0.015(3) -0.009(2) -0.006(2) C18 0.046(4) 0.046(4) 0.040(3) -0.022(3) -0.013(3) -0.005(3) C19 0.042(3) 0.043(3) 0.031(3) -0.015(3) -0.002(3) -0.002(3) C20 0.035(3) 0.029(3) 0.022(3) -0.007(2) -0.002(2) -0.005(2) C21 0.023(3) 0.035(3) 0.029(3) -0.014(2) 0.003(2) -0.001(2) C22 0.037(3) 0.041(3) 0.039(3) -0.018(3) -0.001(3) 0.009(3) C23 0.029(3) 0.086(6) 0.043(4) -0.025(4) -0.003(3) 0.018(3) C24 0.028(3) 0.099(6) 0.041(4) -0.024(4) 0.005(3) -0.022(4) C25 0.026(3) 0.056(4) 0.028(3) -0.014(3) 0.004(2) -0.013(3) C26 0.033(3) 0.035(3) 0.019(2) -0.007(2) 0.001(2) 0.003(2) C27 0.044(4) 0.051(4) 0.025(3) -0.011(3) -0.011(3) 0.009(3) C28 0.071(5) 0.036(4) 0.033(3) 0.003(3) -0.003(3) 0.015(3) C29 0.050(4) 0.030(3) 0.044(4) -0.002(3) 0.007(3) -0.003(3) C30 0.032(3) 0.036(3) 0.028(3) -0.007(2) 0.007(2) -0.007(2) C31 0.031(3) 0.025(3) 0.031(3) -0.007(2) -0.001(2) -0.007(2) C32 0.045(3) 0.025(3) 0.041(3) -0.010(2) -0.004(3) -0.004(2) C33 0.050(4) 0.027(3) 0.050(4) 0.002(3) -0.007(3) -0.004(3) C34 0.041(4) 0.048(4) 0.035(3) 0.001(3) -0.001(3) -0.009(3) C35 0.034(3) 0.032(3) 0.031(3) -0.006(2) 0.004(2) -0.007(2) C36 0.025(3) 0.032(3) 0.045(3) -0.015(3) -0.003(2) -0.003(2) C37 0.032(3) 0.038(3) 0.061(4) -0.015(3) -0.020(3) -0.001(3) C38 0.030(3) 0.037(4) 0.093(6) -0.021(4) -0.007(3) 0.007(3) C39 0.040(4) 0.043(4) 0.084(6) -0.026(4) 0.022(4) -0.007(3) C40 0.035(3) 0.040(3) 0.042(3) -0.013(3) 0.009(3) -0.011(3) C1A 0.025(3) 0.023(3) 0.043(3) -0.003(2) -0.004(2) -0.006(2) C2A 0.040(4) 0.042(4) 0.054(4) -0.014(3) -0.003(3) 0.000(3) C3A 0.052(5) 0.039(4) 0.097(7) -0.009(4) -0.002(4) 0.009(3) C4A 0.043(4) 0.054(5) 0.072(5) 0.004(4) -0.009(4) -0.001(3) C5A 0.046(4) 0.060(5) 0.049(4) 0.009(3) -0.013(3) -0.013(3) C6A 0.030(3) 0.043(3) 0.040(3) -0.006(3) -0.006(2) -0.012(3) C1B 0.024(3) 0.028(3) 0.033(3) -0.009(2) 0.000(2) -0.005(2) C2B 0.043(4) 0.048(4) 0.044(3) -0.026(3) 0.007(3) -0.018(3) C3B 0.045(4) 0.064(4) 0.039(3) -0.024(3) 0.015(3) -0.016(3) C4B 0.035(3) 0.051(4) 0.032(3) -0.003(3) 0.007(3) -0.010(3) C5B 0.028(3) 0.034(3) 0.041(3) -0.004(3) -0.001(2) -0.008(2) C6B 0.021(3) 0.031(3) 0.036(3) -0.010(2) 0.000(2) -0.005(2) C1C 0.018(2) 0.034(3) 0.037(3) -0.013(2) -0.001(2) -0.007(2) C2C 0.029(3) 0.041(3) 0.053(4) -0.006(3) -0.002(3) -0.013(3) C3C 0.030(3) 0.054(4) 0.073(5) -0.017(4) -0.012(3) -0.013(3) C4C 0.041(4) 0.062(5) 0.066(5) -0.024(4) -0.023(3) -0.001(3) C5C 0.041(4) 0.056(4) 0.034(3) -0.010(3) -0.007(3) -0.008(3) C6C 0.027(3) 0.044(3) 0.035(3) -0.015(3) 0.000(2) -0.013(2) C1E 0.020(2) 0.036(3) 0.025(3) -0.008(2) 0.000(2) 0.000(2) C2E 0.030(3) 0.046(3) 0.030(3) -0.007(3) -0.003(2) -0.008(3) C3E 0.033(3) 0.068(5) 0.036(3) -0.017(3) -0.008(3) -0.009(3) C4E 0.038(4) 0.077(5) 0.027(3) 0.000(3) -0.002(3) 0.010(3) C5E 0.055(4) 0.046(4) 0.038(4) 0.002(3) -0.001(3) 0.015(3) C6E 0.042(3) 0.039(3) 0.032(3) -0.005(3) -0.002(3) 0.002(3) C1F 0.029(3) 0.034(3) 0.027(3) -0.012(2) -0.001(2) -0.009(2) C2F 0.053(4) 0.031(3) 0.034(3) -0.010(2) 0.006(3) -0.005(3) C3F 0.061(5) 0.052(4) 0.042(4) -0.022(3) 0.017(3) -0.004(3) C4F 0.053(4) 0.064(4) 0.031(3) -0.018(3) 0.015(3) -0.020(3) C5F 0.054(4) 0.044(4) 0.031(3) -0.005(3) 0.000(3) -0.016(3) C6F 0.034(3) 0.038(3) 0.026(3) -0.009(2) -0.003(2) -0.007(2) C1G 0.022(3) 0.029(3) 0.031(3) -0.012(2) -0.002(2) -0.005(2) C2G 0.029(3) 0.030(3) 0.030(3) -0.006(2) -0.003(2) -0.010(2) C3G 0.047(4) 0.046(4) 0.037(3) -0.008(3) 0.002(3) -0.010(3) C4G 0.048(4) 0.062(4) 0.053(4) -0.014(4) 0.018(3) -0.030(4) C5G 0.032(3) 0.077(5) 0.062(5) -0.030(4) 0.009(3) -0.031(3) C6G 0.029(3) 0.059(4) 0.042(3) -0.024(3) -0.001(3) -0.009(3) C1I 0.029(3) 0.027(3) 0.027(3) -0.006(2) 0.000(2) -0.008(2) C2I 0.042(4) 0.044(4) 0.036(3) -0.006(3) 0.009(3) 0.004(3) C3I 0.048(4) 0.062(5) 0.042(4) -0.018(3) 0.019(3) -0.001(3) C4I 0.054(4) 0.060(4) 0.028(3) -0.012(3) 0.007(3) -0.024(3) C5I 0.052(4) 0.052(4) 0.026(3) -0.005(3) -0.007(3) -0.006(3) C6I 0.034(3) 0.038(3) 0.037(3) -0.008(3) -0.007(2) -0.002(3) C1J 0.030(3) 0.027(3) 0.030(3) -0.009(2) -0.001(2) -0.008(2) C2J 0.038(3) 0.036(3) 0.041(3) -0.016(3) 0.001(3) -0.010(3) C3J 0.052(4) 0.060(4) 0.045(4) -0.011(3) 0.011(3) -0.030(4) C4J 0.077(5) 0.038(4) 0.054(4) -0.005(3) -0.005(4) -0.032(4) C5J 0.080(5) 0.036(4) 0.061(5) -0.020(3) 0.003(4) -0.020(4) C6J 0.054(4) 0.037(3) 0.050(4) -0.019(3) 0.010(3) -0.014(3) C1K 0.038(3) 0.035(3) 0.025(3) -0.008(2) -0.001(2) 0.001(2) C2K 0.048(4) 0.047(4) 0.050(4) -0.023(3) 0.004(3) -0.002(3) C3K 0.064(5) 0.057(4) 0.060(5) -0.043(4) -0.001(4) -0.002(4) C4K 0.067(5) 0.062(5) 0.036(4) -0.027(3) 0.011(3) 0.005(4) C5K 0.053(4) 0.070(5) 0.048(4) -0.020(4) 0.021(3) -0.013(4) C6K 0.048(4) 0.059(4) 0.035(3) -0.018(3) 0.006(3) -0.008(3) C1L 0.027(3) 0.038(3) 0.039(3) -0.019(3) -0.002(2) -0.005(2) C2L 0.032(3) 0.061(4) 0.047(4) -0.024(3) -0.009(3) -0.006(3) C3L 0.035(4) 0.076(5) 0.068(5) -0.036(4) -0.011(3) -0.001(3) C4L 0.037(4) 0.070(5) 0.096(7) -0.041(5) 0.003(4) -0.021(4) C5L 0.045(4) 0.054(4) 0.071(5) -0.011(4) 0.003(4) -0.014(3) C6L 0.042(4) 0.043(3) 0.038(3) -0.011(3) -0.003(3) -0.006(3) C1M 0.049(4) 0.029(3) 0.048(4) -0.020(3) -0.010(3) -0.004(3) C2M 0.062(5) 0.046(4) 0.064(5) -0.018(3) -0.024(4) -0.008(3) C3M 0.068(6) 0.054(5) 0.105(7) -0.036(5) -0.042(5) 0.007(4) C4M 0.060(5) 0.062(5) 0.128(9) -0.039(6) -0.027(6) -0.021(4) C5M 0.064(6) 0.103(7) 0.102(8) -0.031(6) 0.001(5) -0.045(5) C6M 0.059(5) 0.079(6) 0.065(5) -0.014(4) -0.003(4) -0.038(4) C1N 0.052(4) 0.029(3) 0.031(3) -0.011(2) -0.002(3) -0.002(3) C2N 0.076(5) 0.029(3) 0.041(4) -0.015(3) 0.000(3) -0.005(3) C3N 0.095(6) 0.036(4) 0.053(4) -0.018(3) 0.009(4) 0.008(4) C4N 0.107(7) 0.060(5) 0.042(4) -0.012(4) 0.028(4) 0.013(5) C5N 0.094(6) 0.053(4) 0.040(4) -0.012(3) 0.026(4) -0.007(4) C6N 0.066(5) 0.036(3) 0.034(3) -0.010(3) 0.007(3) 0.000(3) C1P 0.038(3) 0.032(3) 0.031(3) -0.003(2) -0.006(2) -0.014(2) C2P 0.032(4) 0.059(5) 0.076(5) 0.006(4) -0.002(3) -0.016(3) C3P 0.059(5) 0.091(7) 0.089(7) 0.017(5) -0.016(5) -0.051(5) C4P 0.092(7) 0.070(6) 0.071(5) 0.020(4) -0.036(5) -0.057(5) C5P 0.081(6) 0.038(4) 0.079(6) 0.000(4) -0.029(5) -0.024(4) C6P 0.051(4) 0.033(3) 0.059(4) -0.011(3) -0.013(3) -0.013(3) C1Q 0.034(3) 0.021(2) 0.030(3) -0.005(2) -0.005(2) -0.004(2) C2Q 0.034(3) 0.037(3) 0.041(3) -0.009(3) -0.007(3) -0.005(3) C3Q 0.064(5) 0.045(4) 0.038(4) -0.007(3) -0.021(3) -0.005(3) C4Q 0.079(5) 0.038(4) 0.031(3) 0.002(3) -0.012(3) -0.007(3) C5Q 0.059(4) 0.039(3) 0.035(3) -0.007(3) 0.008(3) -0.011(3) C6Q 0.039(3) 0.031(3) 0.041(3) -0.008(3) -0.001(3) -0.008(3) C1S 0.053(5) 0.067(5) 0.080(6) -0.014(4) 0.001(4) -0.013(4) Cl1A 0.0689(14) 0.0991(18) 0.0906(17) -0.0068(13) -0.0205(12) -0.0408(13) Cl1B 0.0580(13) 0.0862(16) 0.1080(19) -0.0456(14) -0.0102(12) -0.0036(11) C2S 0.100(4) 0.106(4) 0.100(4) -0.027(2) -0.005(2) -0.017(2) Cl2A 0.187(3) 0.196(3) 0.190(3) -0.090(3) -0.038(3) 0.000(3) Cl2B 0.160(3) 0.167(3) 0.160(3) -0.056(2) -0.021(2) -0.025(2) C3S 0.106(8) 0.099(8) 0.096(8) -0.045(6) -0.035(6) 0.005(6) Cl3A 0.0821(15) 0.0725(14) 0.1008(17) -0.0273(12) -0.0277(13) -0.0006(11) Cl3B 0.061(5) 0.051(4) 0.055(4) -0.007(2) 0.004(2) -0.005(2) Cl3C 0.311(13) 0.057(4) 0.060(4) -0.006(3) -0.029(7) 0.024(6) C4S 0.159(10) 0.070(6) 0.041(4) 0.003(4) -0.023(5) -0.056(6) Cl4A 0.117(2) 0.0854(17) 0.0868(17) -0.0111(14) -0.0190(15) -0.0390(16) Cl4B 0.168(3) 0.0693(14) 0.0609(14) 0.0076(11) -0.0260(16) -0.0497(17) C5S 0.21(2) 0.123(14) 0.54(5) -0.13(2) 0.23(3) -0.077(14) Cl5A 0.152(3) 0.180(3) 0.189(3) -0.043(3) -0.007(3) -0.045(3) Cl5B 0.288(8) 0.280(8) 0.296(8) -0.075(4) -0.017(4) -0.066(4) Cl5C 0.181(15) 0.177(15) 0.177(15) -0.048(5) -0.015(4) -0.038(5) C6S 0.124(16) 0.158(18) 0.58(6) 0.07(3) 0.09(2) -0.045(14) Cl6A 0.115(4) 0.310(9) 0.561(17) -0.130(10) 0.005(7) -0.080(5) Cl6B 0.353(10) 0.155(5) 0.307(9) -0.050(5) -0.060(8) -0.087(6) _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 C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C1D P2 1.776(7) . ? C2D C3D 1.3900 . ? C3D C4D 1.3900 . ? C4D C5D 1.3900 . ? C5D C6D 1.3900 . ? C1X C6X 1.357(18) . ? C1X C2X 1.408(19) . ? C1X P2 1.803(8) . ? C2X C3X 1.402(19) . ? C3X C4X 1.29(2) . ? C4X C5X 1.27(2) . ? C5X C6X 1.420(18) . ? C1H C2H 1.3900 . ? C1H C6H 1.3900 . ? C1H P4 1.790(3) . ? C2H C3H 1.3900 . ? C3H C4H 1.3900 . ? C4H C5H 1.3900 . ? C5H C6H 1.3900 . ? C1Y C2Y 1.3900 . ? C1Y C6Y 1.3900 . ? C1Y P4 1.814(3) . ? C2Y C3Y 1.3900 . ? C3Y C4Y 1.3900 . ? C4Y C5Y 1.3900 . ? C5Y C6Y 1.3900 . ? Fe1 O1 1.998(3) . ? Fe1 O3 2.000(4) . ? Fe1 O4 2.002(3) . ? Fe1 O2 2.015(3) . ? Fe1 Cl2 2.3316(14) . ? Fe1 Cl1 2.3596(14) . ? Fe2 C6 2.022(6) . ? Fe2 C1 2.024(5) . ? Fe2 C7 2.030(6) . ? Fe2 C2 2.035(6) . ? Fe2 C10 2.047(6) . ? Fe2 C5 2.049(5) . ? Fe2 C8 2.051(6) . ? Fe2 C9 2.053(6) . ? Fe2 C4 2.056(6) . ? Fe2 C3 2.056(6) . ? Fe3 C16 2.022(5) . ? Fe3 C11 2.023(5) . ? Fe3 C12 2.029(6) . ? Fe3 C17 2.034(6) . ? Fe3 C20 2.044(5) . ? Fe3 C14 2.047(6) . ? Fe3 C13 2.048(6) . ? Fe3 C19 2.054(6) . ? Fe3 C15 2.056(6) . ? Fe3 C18 2.057(6) . ? Fe4 O7 1.970(4) . ? Fe4 O6 1.995(4) . ? Fe4 O5 2.005(4) . ? Fe4 O8 2.017(4) . ? Fe4 Cl4 2.3630(14) . ? Fe4 Cl3 2.3644(15) . ? Fe5 C21 2.017(5) . ? Fe5 C26 2.025(5) . ? Fe5 C23 2.031(6) . ? Fe5 C22 2.034(6) . ? Fe5 C27 2.037(6) . ? Fe5 C24 2.041(6) . ? Fe5 C25 2.043(6) . ? Fe5 C30 2.047(6) . ? Fe5 C29 2.059(6) . ? Fe5 C28 2.060(6) . ? Fe6 C31 2.018(5) . ? Fe6 C36 2.019(6) . ? Fe6 C37 2.032(6) . ? Fe6 C32 2.035(6) . ? Fe6 C35 2.040(6) . ? Fe6 C40 2.046(6) . ? Fe6 C38 2.050(7) . ? Fe6 C39 2.051(7) . ? Fe6 C33 2.055(6) . ? Fe6 C34 2.064(6) . ? Fe7 Cl6 2.158(2) . ? Fe7 Cl7 2.171(2) . ? Fe7 Cl5 2.185(2) . ? Fe7 Cl8 2.202(3) . ? Fe8 Cl9 2.1845(18) . ? Fe8 Cl11 2.187(2) . ? Fe8 Cl12 2.188(2) . ? Fe8 Cl10 2.197(2) . ? P1 O1 1.501(4) . ? P1 C1 1.778(5) . ? P1 C1A 1.796(5) . ? P1 C1B 1.801(5) . ? P2 O2 1.495(4) . ? P2 C6 1.776(6) . ? P2 C1C 1.787(6) . ? P3 O3 1.498(4) . ? P3 C11 1.780(6) . ? P3 C1F 1.801(5) . ? P3 C1E 1.805(5) . ? P4 O4 1.507(3) . ? P4 C16 1.778(5) . ? P4 C1G 1.796(5) . ? P5 O5 1.500(4) . ? P5 C21 1.779(6) . ? P5 C1I 1.801(5) . ? P5 C1J 1.802(5) . ? P6 O6 1.493(4) . ? P6 C26 1.775(6) . ? P6 C1L 1.781(6) . ? P6 C1K 1.813(6) . ? P7 O7 1.499(4) . ? P7 C31 1.785(6) . ? P7 C1N 1.794(6) . ? P7 C1M 1.812(7) . ? P8 O8 1.502(4) . ? P8 C36 1.773(6) . ? P8 C1Q 1.794(6) . ? P8 C1P 1.800(6) . ? C1 C5 1.429(8) . ? C1 C2 1.435(7) . ? C2 C3 1.411(8) . ? C3 C4 1.412(9) . ? C4 C5 1.408(8) . ? C6 C7 1.438(8) . ? C6 C10 1.446(8) . ? C7 C8 1.414(9) . ? C8 C9 1.407(9) . ? C9 C10 1.419(8) . ? C11 C15 1.429(8) . ? C11 C12 1.438(8) . ? C12 C13 1.408(9) . ? C13 C14 1.391(11) . ? C14 C15 1.432(9) . ? C16 C20 1.419(7) . ? C16 C17 1.448(8) . ? C17 C18 1.423(8) . ? C18 C19 1.423(9) . ? C19 C20 1.424(8) . ? C21 C22 1.430(8) . ? C21 C25 1.434(8) . ? C22 C23 1.419(10) . ? C23 C24 1.395(11) . ? C24 C25 1.413(9) . ? C26 C27 1.426(8) . ? C26 C30 1.435(8) . ? C27 C28 1.420(10) . ? C28 C29 1.422(10) . ? C29 C30 1.416(8) . ? C31 C35 1.423(8) . ? C31 C32 1.430(8) . ? C32 C33 1.411(9) . ? C33 C34 1.426(9) . ? C34 C35 1.416(8) . ? C36 C40 1.415(8) . ? C36 C37 1.438(8) . ? C37 C38 1.421(10) . ? C38 C39 1.406(11) . ? C39 C40 1.409(9) . ? C1A C2A 1.384(8) . ? C1A C6A 1.390(8) . ? C2A C3A 1.379(10) . ? C3A C4A 1.403(12) . ? C4A C5A 1.374(11) . ? C5A C6A 1.389(9) . ? C1B C2B 1.385(8) . ? C1B C6B 1.395(7) . ? C2B C3B 1.382(9) . ? C3B C4B 1.387(9) . ? C4B C5B 1.378(9) . ? C5B C6B 1.381(8) . ? C1C C6C 1.387(8) . ? C1C C2C 1.397(8) . ? C2C C3C 1.397(9) . ? C3C C4C 1.364(11) . ? C4C C5C 1.370(9) . ? C5C C6C 1.391(8) . ? C1E C2E 1.391(8) . ? C1E C6E 1.393(8) . ? C2E C3E 1.386(8) . ? C3E C4E 1.373(10) . ? C4E C5E 1.377(11) . ? C5E C6E 1.399(9) . ? C1F C2F 1.383(8) . ? C1F C6F 1.385(8) . ? C2F C3F 1.390(9) . ? C3F C4F 1.373(10) . ? C4F C5F 1.373(9) . ? C5F C6F 1.390(8) . ? C1G C2G 1.391(7) . ? C1G C6G 1.395(8) . ? C2G C3G 1.381(8) . ? C3G C4G 1.392(10) . ? C4G C5G 1.373(10) . ? C5G C6G 1.383(9) . ? C1I C6I 1.385(8) . ? C1I C2I 1.387(8) . ? C2I C3I 1.383(9) . ? C3I C4I 1.372(10) . ? C4I C5I 1.392(9) . ? C5I C6I 1.374(8) . ? C1J C2J 1.381(8) . ? C1J C6J 1.401(8) . ? C2J C3J 1.398(9) . ? C3J C4J 1.370(10) . ? C4J C5J 1.380(11) . ? C5J C6J 1.376(9) . ? C1K C6K 1.375(9) . ? C1K C2K 1.389(9) . ? C2K C3K 1.384(9) . ? C3K C4K 1.357(11) . ? C4K C5K 1.355(11) . ? C5K C6K 1.385(9) . ? C1L C6L 1.392(8) . ? C1L C2L 1.400(8) . ? C2L C3L 1.383(10) . ? C3L C4L 1.386(12) . ? C4L C5L 1.366(11) . ? C5L C6L 1.390(9) . ? C1M C6M 1.368(10) . ? C1M C2M 1.381(9) . ? C2M C3M 1.394(11) . ? C3M C4M 1.323(13) . ? C4M C5M 1.396(14) . ? C5M C6M 1.388(11) . ? C1N C6N 1.385(9) . ? C1N C2N 1.392(8) . ? C2N C3N 1.386(10) . ? C3N C4N 1.384(12) . ? C4N C5N 1.385(11) . ? C5N C6N 1.371(9) . ? C1P C2P 1.370(9) . ? C1P C6P 1.377(8) . ? C2P C3P 1.384(10) . ? C3P C4P 1.363(13) . ? C4P C5P 1.364(12) . ? C5P C6P 1.390(9) . ? C1Q C6Q 1.389(8) . ? C1Q C2Q 1.402(8) . ? C2Q C3Q 1.387(9) . ? C3Q C4Q 1.367(10) . ? C4Q C5Q 1.395(10) . ? C5Q C6Q 1.380(9) . ? C1S Cl1A 1.744(4) . ? C1S Cl1B 1.748(4) . ? C2S Cl2B 1.746(5) . ? C2S Cl2A 1.746(5) . ? C3S Cl3C 1.652(15) . ? C3S Cl3A 1.749(5) . ? C3S Cl3B 1.759(5) . ? C4S Cl4A 1.743(5) . ? C4S Cl4B 1.750(4) . ? C5S Cl5B 1.734(5) . ? C5S Cl5A 1.744(5) . ? C5S Cl5C 1.744(5) . ? C6S Cl6B 1.55(2) . ? C6S Cl6A 1.60(2) . ? 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 C2D C1D C6D 120.0 . . ? C2D C1D P2 118.1(8) . . ? C6D C1D P2 121.9(8) . . ? C3D C2D C1D 120.0 . . ? C2D C3D C4D 120.0 . . ? C5D C4D C3D 120.0 . . ? C4D C5D C6D 120.0 . . ? C5D C6D C1D 120.0 . . ? C6X C1X C2X 117.2(10) . . ? C6X C1X P2 120.4(11) . . ? C2X C1X P2 122.4(11) . . ? C3X C2X C1X 119.8(14) . . ? C4X C3X C2X 120.2(14) . . ? C5X C4X C3X 121.8(15) . . ? C4X C5X C6X 122.7(15) . . ? C1X C6X C5X 118.2(13) . . ? C2H C1H C6H 120.0 . . ? C2H C1H P4 118.3(2) . . ? C6H C1H P4 121.7(2) . . ? C1H C2H C3H 120.0 . . ? C4H C3H C2H 120.0 . . ? C5H C4H C3H 120.0 . . ? C4H C5H C6H 120.0 . . ? C5H C6H C1H 120.0 . . ? C2Y C1Y C6Y 120.0 . . ? C2Y C1Y P4 117.2(2) . . ? C6Y C1Y P4 122.7(2) . . ? C1Y C2Y C3Y 120.0 . . ? C2Y C3Y C4Y 120.0 . . ? C5Y C4Y C3Y 120.0 . . ? C4Y C5Y C6Y 120.0 . . ? C5Y C6Y C1Y 120.0 . . ? O1 Fe1 O3 178.06(15) . . ? O1 Fe1 O4 88.21(15) . . ? O3 Fe1 O4 93.11(15) . . ? O1 Fe1 O2 90.43(15) . . ? O3 Fe1 O2 88.28(15) . . ? O4 Fe1 O2 178.22(15) . . ? O1 Fe1 Cl2 91.56(11) . . ? O3 Fe1 Cl2 89.90(11) . . ? O4 Fe1 Cl2 88.44(11) . . ? O2 Fe1 Cl2 90.45(11) . . ? O1 Fe1 Cl1 89.04(11) . . ? O3 Fe1 Cl1 89.53(11) . . ? O4 Fe1 Cl1 90.18(11) . . ? O2 Fe1 Cl1 90.95(11) . . ? Cl2 Fe1 Cl1 178.48(6) . . ? C6 Fe2 C1 125.6(2) . . ? C6 Fe2 C7 41.6(2) . . ? C1 Fe2 C7 162.5(2) . . ? C6 Fe2 C2 162.9(2) . . ? C1 Fe2 C2 41.4(2) . . ? C7 Fe2 C2 154.0(2) . . ? C6 Fe2 C10 41.6(2) . . ? C1 Fe2 C10 108.6(2) . . ? C7 Fe2 C10 69.6(2) . . ? C2 Fe2 C10 124.7(2) . . ? C6 Fe2 C5 108.5(2) . . ? C1 Fe2 C5 41.1(2) . . ? C7 Fe2 C5 124.5(2) . . ? C2 Fe2 C5 68.9(2) . . ? C10 Fe2 C5 123.5(2) . . ? C6 Fe2 C8 68.8(2) . . ? C1 Fe2 C8 156.2(2) . . ? C7 Fe2 C8 40.5(2) . . ? C2 Fe2 C8 119.6(2) . . ? C10 Fe2 C8 68.2(2) . . ? C5 Fe2 C8 160.3(2) . . ? C6 Fe2 C9 68.9(2) . . ? C1 Fe2 C9 122.1(2) . . ? C7 Fe2 C9 68.5(3) . . ? C2 Fe2 C9 107.1(3) . . ? C10 Fe2 C9 40.5(2) . . ? C5 Fe2 C9 158.8(2) . . ? C8 Fe2 C9 40.1(3) . . ? C6 Fe2 C4 121.4(2) . . ? C1 Fe2 C4 68.4(2) . . ? C7 Fe2 C4 106.5(3) . . ? C2 Fe2 C4 68.2(3) . . ? C10 Fe2 C4 158.3(2) . . ? C5 Fe2 C4 40.1(2) . . ? C8 Fe2 C4 123.4(3) . . ? C9 Fe2 C4 159.5(3) . . ? C6 Fe2 C3 155.7(2) . . ? C1 Fe2 C3 68.4(2) . . ? C7 Fe2 C3 119.2(2) . . ? C2 Fe2 C3 40.3(2) . . ? C10 Fe2 C3 160.6(3) . . ? C5 Fe2 C3 67.7(2) . . ? C8 Fe2 C3 106.4(3) . . ? C9 Fe2 C3 123.6(3) . . ? C4 Fe2 C3 40.1(3) . . ? C16 Fe3 C11 126.9(2) . . ? C16 Fe3 C12 163.9(2) . . ? C11 Fe3 C12 41.6(2) . . ? C16 Fe3 C17 41.8(2) . . ? C11 Fe3 C17 164.5(2) . . ? C12 Fe3 C17 152.1(2) . . ? C16 Fe3 C20 40.8(2) . . ? C11 Fe3 C20 109.0(2) . . ? C12 Fe3 C20 125.6(2) . . ? C17 Fe3 C20 69.2(2) . . ? C16 Fe3 C14 121.6(3) . . ? C11 Fe3 C14 68.7(2) . . ? C12 Fe3 C14 68.4(3) . . ? C17 Fe3 C14 106.8(3) . . ? C20 Fe3 C14 157.7(3) . . ? C16 Fe3 C13 155.1(3) . . ? C11 Fe3 C13 68.2(2) . . ? C12 Fe3 C13 40.4(3) . . ? C17 Fe3 C13 118.4(3) . . ? C20 Fe3 C13 161.8(3) . . ? C14 Fe3 C13 39.7(3) . . ? C16 Fe3 C19 68.9(2) . . ? C11 Fe3 C19 120.6(2) . . ? C12 Fe3 C19 106.0(3) . . ? C17 Fe3 C19 68.8(2) . . ? C20 Fe3 C19 40.7(2) . . ? C14 Fe3 C19 160.1(3) . . ? C13 Fe3 C19 123.9(3) . . ? C16 Fe3 C15 109.2(2) . . ? C11 Fe3 C15 41.0(2) . . ? C12 Fe3 C15 69.3(2) . . ? C17 Fe3 C15 126.0(2) . . ? C20 Fe3 C15 122.8(2) . . ? C14 Fe3 C15 40.8(3) . . ? C13 Fe3 C15 67.8(3) . . ? C19 Fe3 C15 157.0(2) . . ? C16 Fe3 C18 69.0(2) . . ? C11 Fe3 C18 154.2(2) . . ? C12 Fe3 C18 117.6(3) . . ? C17 Fe3 C18 40.7(2) . . ? C20 Fe3 C18 68.4(2) . . ? C14 Fe3 C18 123.7(3) . . ? C13 Fe3 C18 105.8(3) . . ? C19 Fe3 C18 40.5(3) . . ? C15 Fe3 C18 162.0(3) . . ? O7 Fe4 O6 87.06(16) . . ? O7 Fe4 O5 176.38(16) . . ? O6 Fe4 O5 92.52(15) . . ? O7 Fe4 O8 91.35(16) . . ? O6 Fe4 O8 176.95(16) . . ? O5 Fe4 O8 89.23(15) . . ? O7 Fe4 Cl4 88.17(12) . . ? O6 Fe4 Cl4 92.38(12) . . ? O5 Fe4 Cl4 88.26(11) . . ? O8 Fe4 Cl4 90.18(11) . . ? O7 Fe4 Cl3 92.75(12) . . ? O6 Fe4 Cl3 90.35(12) . . ? O5 Fe4 Cl3 90.84(11) . . ? O8 Fe4 Cl3 87.12(11) . . ? Cl4 Fe4 Cl3 177.17(6) . . ? C21 Fe5 C26 127.1(2) . . ? C21 Fe5 C23 68.8(2) . . ? C26 Fe5 C23 153.6(3) . . ? C21 Fe5 C22 41.3(2) . . ? C26 Fe5 C22 164.7(2) . . ? C23 Fe5 C22 40.9(3) . . ? C21 Fe5 C27 163.9(2) . . ? C26 Fe5 C27 41.1(2) . . ? C23 Fe5 C27 117.9(3) . . ? C22 Fe5 C27 152.6(2) . . ? C21 Fe5 C24 68.4(2) . . ? C26 Fe5 C24 120.4(3) . . ? C23 Fe5 C24 40.1(3) . . ? C22 Fe5 C24 68.4(3) . . ? C27 Fe5 C24 106.5(3) . . ? C21 Fe5 C25 41.4(2) . . ? C26 Fe5 C25 108.2(2) . . ? C23 Fe5 C25 68.5(3) . . ? C22 Fe5 C25 69.5(3) . . ? C27 Fe5 C25 125.0(3) . . ? C24 Fe5 C25 40.5(3) . . ? C21 Fe5 C30 109.5(2) . . ? C26 Fe5 C30 41.2(2) . . ? C23 Fe5 C30 162.5(3) . . ? C22 Fe5 C30 126.3(3) . . ? C27 Fe5 C30 68.8(2) . . ? C24 Fe5 C30 156.9(3) . . ? C25 Fe5 C30 122.5(2) . . ? C21 Fe5 C29 121.3(3) . . ? C26 Fe5 C29 68.8(2) . . ? C23 Fe5 C29 124.5(3) . . ? C22 Fe5 C29 107.1(3) . . ? C27 Fe5 C29 68.5(3) . . ? C24 Fe5 C29 160.9(3) . . ? C25 Fe5 C29 157.2(3) . . ? C30 Fe5 C29 40.3(2) . . ? C21 Fe5 C28 155.0(3) . . ? C26 Fe5 C28 68.5(2) . . ? C23 Fe5 C28 105.9(3) . . ? C22 Fe5 C28 118.6(3) . . ? C27 Fe5 C28 40.5(3) . . ? C24 Fe5 C28 124.1(3) . . ? C25 Fe5 C28 161.4(3) . . ? C30 Fe5 C28 67.9(3) . . ? C29 Fe5 C28 40.4(3) . . ? C31 Fe6 C36 125.5(2) . . ? C31 Fe6 C37 163.3(2) . . ? C36 Fe6 C37 41.6(2) . . ? C31 Fe6 C32 41.3(2) . . ? C36 Fe6 C32 162.4(2) . . ? C37 Fe6 C32 154.0(2) . . ? C31 Fe6 C35 41.1(2) . . ? C36 Fe6 C35 108.5(2) . . ? C37 Fe6 C35 125.5(3) . . ? C32 Fe6 C35 69.1(2) . . ? C31 Fe6 C40 108.5(2) . . ? C36 Fe6 C40 40.7(2) . . ? C37 Fe6 C40 68.6(3) . . ? C32 Fe6 C40 124.8(2) . . ? C35 Fe6 C40 122.8(2) . . ? C31 Fe6 C38 155.0(3) . . ? C36 Fe6 C38 69.0(2) . . ? C37 Fe6 C38 40.7(3) . . ? C32 Fe6 C38 118.9(3) . . ? C35 Fe6 C38 161.8(3) . . ? C40 Fe6 C38 67.8(3) . . ? C31 Fe6 C39 121.0(3) . . ? C36 Fe6 C39 68.5(3) . . ? C37 Fe6 C39 68.2(3) . . ? C32 Fe6 C39 106.5(3) . . ? C35 Fe6 C39 157.3(3) . . ? C40 Fe6 C39 40.2(3) . . ? C38 Fe6 C39 40.1(3) . . ? C31 Fe6 C33 68.4(2) . . ? C36 Fe6 C33 156.4(3) . . ? C37 Fe6 C33 119.9(3) . . ? C32 Fe6 C33 40.3(3) . . ? C35 Fe6 C33 68.3(2) . . ? C40 Fe6 C33 160.7(3) . . ? C38 Fe6 C33 106.4(3) . . ? C39 Fe6 C33 123.6(3) . . ? C31 Fe6 C34 68.4(2) . . ? C36 Fe6 C34 121.9(3) . . ? C37 Fe6 C34 107.6(3) . . ? C32 Fe6 C34 68.4(3) . . ? C35 Fe6 C34 40.4(2) . . ? C40 Fe6 C34 157.8(3) . . ? C38 Fe6 C34 124.5(3) . . ? C39 Fe6 C34 160.6(3) . . ? C33 Fe6 C34 40.5(3) . . ? Cl6 Fe7 Cl7 111.22(11) . . ? Cl6 Fe7 Cl5 110.68(9) . . ? Cl7 Fe7 Cl5 109.20(9) . . ? Cl6 Fe7 Cl8 108.77(12) . . ? Cl7 Fe7 Cl8 107.76(14) . . ? Cl5 Fe7 Cl8 109.14(10) . . ? Cl9 Fe8 Cl11 111.34(8) . . ? Cl9 Fe8 Cl12 108.38(8) . . ? Cl11 Fe8 Cl12 111.16(10) . . ? Cl9 Fe8 Cl10 107.70(9) . . ? Cl11 Fe8 Cl10 107.35(9) . . ? Cl12 Fe8 Cl10 110.87(12) . . ? O1 P1 C1 113.0(2) . . ? O1 P1 C1A 110.0(2) . . ? C1 P1 C1A 107.6(3) . . ? O1 P1 C1B 111.1(2) . . ? C1 P1 C1B 105.8(2) . . ? C1A P1 C1B 109.1(3) . . ? O2 P2 C6 113.3(2) . . ? O2 P2 C1D 115.8(5) . . ? C6 P2 C1D 108.2(5) . . ? O2 P2 C1C 108.6(2) . . ? C6 P2 C1C 107.6(3) . . ? C1D P2 C1C 102.5(5) . . ? O2 P2 C1X 110.9(6) . . ? C6 P2 C1X 107.2(6) . . ? C1D P2 C1X 6.9(10) . . ? C1C P2 C1X 109.1(6) . . ? O3 P3 C11 112.6(2) . . ? O3 P3 C1F 110.0(2) . . ? C11 P3 C1F 107.4(3) . . ? O3 P3 C1E 111.5(2) . . ? C11 P3 C1E 105.4(2) . . ? C1F P3 C1E 109.7(2) . . ? O4 P4 C16 112.3(2) . . ? O4 P4 C1H 115.0(2) . . ? C16 P4 C1H 108.1(2) . . ? O4 P4 C1G 109.0(2) . . ? C16 P4 C1G 108.3(2) . . ? C1H P4 C1G 103.7(3) . . ? O4 P4 C1Y 109.7(2) . . ? C16 P4 C1Y 107.2(2) . . ? C1H P4 C1Y 7.0 . . ? C1G P4 C1Y 110.3(3) . . ? O5 P5 C21 114.2(2) . . ? O5 P5 C1I 110.5(2) . . ? C21 P5 C1I 106.2(2) . . ? O5 P5 C1J 110.3(2) . . ? C21 P5 C1J 104.7(3) . . ? C1I P5 C1J 110.7(2) . . ? O6 P6 C26 109.6(2) . . ? O6 P6 C1L 110.5(3) . . ? C26 P6 C1L 109.7(3) . . ? O6 P6 C1K 112.6(2) . . ? C26 P6 C1K 105.0(3) . . ? C1L P6 C1K 109.2(3) . . ? O7 P7 C31 110.1(2) . . ? O7 P7 C1N 109.3(3) . . ? C31 P7 C1N 109.5(3) . . ? O7 P7 C1M 113.1(3) . . ? C31 P7 C1M 108.4(3) . . ? C1N P7 C1M 106.4(3) . . ? O8 P8 C36 115.2(2) . . ? O8 P8 C1Q 108.9(2) . . ? C36 P8 C1Q 106.5(3) . . ? O8 P8 C1P 111.7(2) . . ? C36 P8 C1P 106.1(3) . . ? C1Q P8 C1P 108.0(3) . . ? P1 O1 Fe1 166.2(2) . . ? P2 O2 Fe1 155.9(2) . . ? P3 O3 Fe1 165.9(2) . . ? P4 O4 Fe1 160.2(2) . . ? P5 O5 Fe4 162.9(2) . . ? P6 O6 Fe4 167.4(3) . . ? P7 O7 Fe4 157.4(3) . . ? P8 O8 Fe4 153.0(2) . . ? C5 C1 C2 107.5(5) . . ? C5 C1 P1 124.2(4) . . ? C2 C1 P1 128.3(4) . . ? C5 C1 Fe2 70.4(3) . . ? C2 C1 Fe2 69.7(3) . . ? P1 C1 Fe2 124.3(3) . . ? C3 C2 C1 107.4(5) . . ? C3 C2 Fe2 70.6(4) . . ? C1 C2 Fe2 68.9(3) . . ? C2 C3 C4 108.7(5) . . ? C2 C3 Fe2 69.0(3) . . ? C4 C3 Fe2 69.9(3) . . ? C5 C4 C3 108.4(5) . . ? C5 C4 Fe2 69.6(3) . . ? C3 C4 Fe2 69.9(4) . . ? C4 C5 C1 108.0(5) . . ? C4 C5 Fe2 70.2(3) . . ? C1 C5 Fe2 68.5(3) . . ? C7 C6 C10 107.4(5) . . ? C7 C6 P2 128.7(4) . . ? C10 C6 P2 123.9(4) . . ? C7 C6 Fe2 69.5(3) . . ? C10 C6 Fe2 70.1(3) . . ? P2 C6 Fe2 123.9(3) . . ? C8 C7 C6 107.5(5) . . ? C8 C7 Fe2 70.5(3) . . ? C6 C7 Fe2 68.9(3) . . ? C9 C8 C7 109.0(5) . . ? C9 C8 Fe2 70.0(3) . . ? C7 C8 Fe2 68.9(3) . . ? C8 C9 C10 108.8(6) . . ? C8 C9 Fe2 69.9(3) . . ? C10 C9 Fe2 69.5(3) . . ? C9 C10 C6 107.2(5) . . ? C9 C10 Fe2 70.0(4) . . ? C6 C10 Fe2 68.3(3) . . ? C15 C11 C12 108.2(5) . . ? C15 C11 P3 122.6(4) . . ? C12 C11 P3 129.2(5) . . ? C15 C11 Fe3 70.7(3) . . ? C12 C11 Fe3 69.4(3) . . ? P3 C11 Fe3 124.6(3) . . ? C13 C12 C11 106.7(6) . . ? C13 C12 Fe3 70.5(4) . . ? C11 C12 Fe3 69.0(3) . . ? C14 C13 C12 109.8(6) . . ? C14 C13 Fe3 70.1(4) . . ? C12 C13 Fe3 69.1(3) . . ? C13 C14 C15 108.5(6) . . ? C13 C14 Fe3 70.2(4) . . ? C15 C14 Fe3 69.9(3) . . ? C11 C15 C14 106.7(6) . . ? C11 C15 Fe3 68.3(3) . . ? C14 C15 Fe3 69.2(4) . . ? C20 C16 C17 107.8(5) . . ? C20 C16 P4 124.6(4) . . ? C17 C16 P4 127.5(4) . . ? C20 C16 Fe3 70.4(3) . . ? C17 C16 Fe3 69.5(3) . . ? P4 C16 Fe3 122.7(3) . . ? C18 C17 C16 107.3(5) . . ? C18 C17 Fe3 70.5(3) . . ? C16 C17 Fe3 68.7(3) . . ? C17 C18 C19 108.5(5) . . ? C17 C18 Fe3 68.8(3) . . ? C19 C18 Fe3 69.6(3) . . ? C18 C19 C20 108.1(5) . . ? C18 C19 Fe3 69.9(3) . . ? C20 C19 Fe3 69.3(3) . . ? C16 C20 C19 108.3(5) . . ? C16 C20 Fe3 68.7(3) . . ? C19 C20 Fe3 70.0(3) . . ? C22 C21 C25 108.5(5) . . ? C22 C21 P5 127.4(5) . . ? C25 C21 P5 124.1(4) . . ? C22 C21 Fe5 70.0(3) . . ? C25 C21 Fe5 70.3(3) . . ? P5 C21 Fe5 126.1(3) . . ? C23 C22 C21 106.7(6) . . ? C23 C22 Fe5 69.5(4) . . ? C21 C22 Fe5 68.7(3) . . ? C24 C23 C22 108.8(6) . . ? C24 C23 Fe5 70.4(4) . . ? C22 C23 Fe5 69.7(3) . . ? C23 C24 C25 109.5(6) . . ? C23 C24 Fe5 69.6(4) . . ? C25 C24 Fe5 69.8(3) . . ? C24 C25 C21 106.5(6) . . ? C24 C25 Fe5 69.7(4) . . ? C21 C25 Fe5 68.3(3) . . ? C27 C26 C30 107.6(5) . . ? C27 C26 P6 131.3(5) . . ? C30 C26 P6 121.0(4) . . ? C27 C26 Fe5 69.9(3) . . ? C30 C26 Fe5 70.2(3) . . ? P6 C26 Fe5 122.6(3) . . ? C28 C27 C26 107.8(6) . . ? C28 C27 Fe5 70.6(4) . . ? C26 C27 Fe5 69.0(3) . . ? C27 C28 C29 108.5(5) . . ? C27 C28 Fe5 68.9(3) . . ? C29 C28 Fe5 69.8(4) . . ? C30 C29 C28 108.0(6) . . ? C30 C29 Fe5 69.4(3) . . ? C28 C29 Fe5 69.8(4) . . ? C29 C30 C26 108.1(5) . . ? C29 C30 Fe5 70.3(3) . . ? C26 C30 Fe5 68.5(3) . . ? C35 C31 C32 108.3(5) . . ? C35 C31 P7 123.7(4) . . ? C32 C31 P7 127.9(4) . . ? C35 C31 Fe6 70.3(3) . . ? C32 C31 Fe6 70.0(3) . . ? P7 C31 Fe6 121.7(3) . . ? C33 C32 C31 107.5(5) . . ? C33 C32 Fe6 70.6(4) . . ? C31 C32 Fe6 68.7(3) . . ? C32 C33 C34 108.6(5) . . ? C32 C33 Fe6 69.1(3) . . ? C34 C33 Fe6 70.1(3) . . ? C35 C34 C33 107.9(6) . . ? C35 C34 Fe6 68.9(3) . . ? C33 C34 Fe6 69.4(4) . . ? C34 C35 C31 107.8(5) . . ? C34 C35 Fe6 70.7(3) . . ? C31 C35 Fe6 68.7(3) . . ? C40 C36 C37 107.3(5) . . ? C40 C36 P8 124.8(5) . . ? C37 C36 P8 127.9(5) . . ? C40 C36 Fe6 70.6(3) . . ? C37 C36 Fe6 69.7(3) . . ? P8 C36 Fe6 125.2(3) . . ? C38 C37 C36 107.5(6) . . ? C38 C37 Fe6 70.3(4) . . ? C36 C37 Fe6 68.7(3) . . ? C39 C38 C37 108.2(6) . . ? C39 C38 Fe6 70.0(4) . . ? C37 C38 Fe6 68.9(4) . . ? C38 C39 C40 108.5(6) . . ? C38 C39 Fe6 69.9(4) . . ? C40 C39 Fe6 69.7(4) . . ? C39 C40 C36 108.5(6) . . ? C39 C40 Fe6 70.1(4) . . ? C36 C40 Fe6 68.6(3) . . ? C2A C1A C6A 119.5(5) . . ? C2A C1A P1 122.0(5) . . ? C6A C1A P1 118.5(4) . . ? C3A C2A C1A 120.7(7) . . ? C2A C3A C4A 119.7(7) . . ? C5A C4A C3A 119.6(7) . . ? C4A C5A C6A 120.5(7) . . ? C5A C6A C1A 119.9(6) . . ? C2B C1B C6B 119.3(5) . . ? C2B C1B P1 122.0(4) . . ? C6B C1B P1 118.7(4) . . ? C3B C2B C1B 120.6(6) . . ? C2B C3B C4B 119.2(6) . . ? C5B C4B C3B 121.1(5) . . ? C4B C5B C6B 119.3(5) . . ? C5B C6B C1B 120.4(5) . . ? C6C C1C C2C 119.6(5) . . ? C6C C1C P2 120.0(4) . . ? C2C C1C P2 120.4(4) . . ? C1C C2C C3C 119.6(6) . . ? C4C C3C C2C 119.8(6) . . ? C3C C4C C5C 121.2(6) . . ? C4C C5C C6C 119.9(6) . . ? C1C C6C C5C 119.9(5) . . ? C2E C1E C6E 119.7(5) . . ? C2E C1E P3 119.5(4) . . ? C6E C1E P3 120.8(4) . . ? C3E C2E C1E 120.4(6) . . ? C4E C3E C2E 119.6(6) . . ? C3E C4E C5E 120.9(6) . . ? C4E C5E C6E 120.2(6) . . ? C1E C6E C5E 119.1(6) . . ? C2F C1F C6F 121.0(5) . . ? C2F C1F P3 121.0(4) . . ? C6F C1F P3 117.9(4) . . ? C1F C2F C3F 119.0(6) . . ? C4F C3F C2F 120.2(6) . . ? C5F C4F C3F 120.7(6) . . ? C4F C5F C6F 120.0(6) . . ? C1F C6F C5F 119.1(5) . . ? C2G C1G C6G 119.7(5) . . ? C2G C1G P4 119.2(4) . . ? C6G C1G P4 121.1(4) . . ? C3G C2G C1G 120.1(5) . . ? C2G C3G C4G 119.3(6) . . ? C5G C4G C3G 121.1(6) . . ? C4G C5G C6G 119.7(6) . . ? C5G C6G C1G 119.9(6) . . ? C6I C1I C2I 120.0(5) . . ? C6I C1I P5 119.7(4) . . ? C2I C1I P5 120.2(4) . . ? C3I C2I C1I 119.9(6) . . ? C4I C3I C2I 120.2(6) . . ? C3I C4I C5I 119.7(6) . . ? C6I C5I C4I 120.5(6) . . ? C5I C6I C1I 119.6(6) . . ? C2J C1J C6J 119.6(5) . . ? C2J C1J P5 118.3(4) . . ? C6J C1J P5 121.6(4) . . ? C1J C2J C3J 120.2(6) . . ? C4J C3J C2J 119.7(6) . . ? C3J C4J C5J 120.3(6) . . ? C6J C5J C4J 120.9(7) . . ? C5J C6J C1J 119.4(6) . . ? C6K C1K C2K 118.7(6) . . ? C6K C1K P6 117.8(5) . . ? C2K C1K P6 123.4(5) . . ? C3K C2K C1K 119.8(7) . . ? C4K C3K C2K 120.3(7) . . ? C5K C4K C3K 120.8(6) . . ? C4K C5K C6K 119.7(7) . . ? C1K C6K C5K 120.7(7) . . ? C6L C1L C2L 119.4(6) . . ? C6L C1L P6 118.4(5) . . ? C2L C1L P6 122.2(5) . . ? C3L C2L C1L 120.2(7) . . ? C2L C3L C4L 119.4(7) . . ? C5L C4L C3L 121.1(7) . . ? C4L C5L C6L 120.0(7) . . ? C5L C6L C1L 119.9(6) . . ? C6M C1M C2M 120.8(7) . . ? C6M C1M P7 120.2(5) . . ? C2M C1M P7 119.0(6) . . ? C1M C2M C3M 118.3(8) . . ? C4M C3M C2M 121.7(9) . . ? C3M C4M C5M 120.3(8) . . ? C6M C5M C4M 119.1(9) . . ? C1M C6M C5M 119.7(8) . . ? C6N C1N C2N 120.5(6) . . ? C6N C1N P7 119.1(4) . . ? C2N C1N P7 120.4(5) . . ? C3N C2N C1N 119.4(7) . . ? C4N C3N C2N 120.0(7) . . ? C3N C4N C5N 119.8(7) . . ? C6N C5N C4N 120.8(7) . . ? C5N C6N C1N 119.5(6) . . ? C2P C1P C6P 120.2(6) . . ? C2P C1P P8 120.9(5) . . ? C6P C1P P8 118.9(5) . . ? C1P C2P C3P 119.5(8) . . ? C4P C3P C2P 120.0(8) . . ? C3P C4P C5P 121.1(7) . . ? C4P C5P C6P 119.1(8) . . ? C1P C6P C5P 120.0(7) . . ? C6Q C1Q C2Q 119.5(5) . . ? C6Q C1Q P8 119.4(4) . . ? C2Q C1Q P8 121.1(4) . . ? C3Q C2Q C1Q 118.8(6) . . ? C4Q C3Q C2Q 121.2(6) . . ? C3Q C4Q C5Q 120.6(6) . . ? C6Q C5Q C4Q 118.7(6) . . ? C5Q C6Q C1Q 121.2(6) . . ? Cl1A C1S Cl1B 111.5(3) . . ? Cl2B C2S Cl2A 110.8(5) . . ? Cl3C C3S Cl3A 117.3(8) . . ? Cl3C C3S Cl3B 15.0(9) . . ? Cl3A C3S Cl3B 107.6(6) . . ? Cl4A C4S Cl4B 112.6(3) . . ? Cl5B C5S Cl5A 111.4(5) . . ? Cl5B C5S Cl5C 43.2(9) . . ? Cl5A C5S Cl5C 104.9(6) . . ? Cl6B C6S Cl6A 127.5(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.535 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.125 data_Cpd5 _database_code_depnum_ccdc_archive 'CCDC 823892' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68.50 H57 Cl4 Fe3 O8 P4' _chemical_formula_weight 1441.37 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.3426(11) _cell_length_b 19.6446(12) _cell_length_c 20.0689(12) _cell_angle_alpha 74.9240(10) _cell_angle_beta 87.5210(10) _cell_angle_gamma 65.0060(10) _cell_volume 6310.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6395 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.12 _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5830 _exptl_absorpt_correction_T_max 0.6885 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81628 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.50 _reflns_number_total 28928 _reflns_number_gt 21063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0827P)^2^+5.6254P] 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 28928 _refine_ls_number_parameters 1576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1615 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.53636(3) 0.75525(3) 0.43075(3) 0.01852(12) Uani 1 1 d . . . Fe2 Fe 0.76665(3) 0.74359(4) 0.29763(3) 0.02701(14) Uani 1 1 d . . . Fe3 Fe 0.30168(3) 0.76680(4) 0.55871(3) 0.02969(15) Uani 1 1 d . . . Fe4 Fe 0.03209(3) 0.75771(3) 0.92505(3) 0.02135(13) Uani 1 1 d . . . Fe5 Fe 0.23894(3) 0.75213(4) 1.07389(3) 0.02879(14) Uani 1 1 d . . . Fe6 Fe -0.18893(4) 0.78432(4) 0.77637(3) 0.02963(15) Uani 1 1 d . . . Cl1 Cl 0.59192(6) 0.61878(5) 0.46457(5) 0.0311(2) Uani 1 1 d . . . Cl2 Cl 0.48357(6) 0.89190(5) 0.40109(5) 0.0293(2) Uani 1 1 d . . . Cl3 Cl -0.02198(6) 0.89393(5) 0.89732(5) 0.0310(2) Uani 1 1 d . . . Cl4 Cl 0.08652(7) 0.62256(6) 0.95096(7) 0.0407(3) Uani 1 1 d . . . P1 P 0.58991(6) 0.74593(6) 0.26293(5) 0.0205(2) Uani 1 1 d . . . P2 P 0.72228(6) 0.75668(6) 0.46048(5) 0.0239(2) Uani 1 1 d . . . P3 P 0.48985(6) 0.73651(6) 0.60163(5) 0.0234(2) Uani 1 1 d . . . P4 P 0.34356(6) 0.77443(6) 0.39242(5) 0.0226(2) Uani 1 1 d . . . P5 P 0.21628(6) 0.76888(6) 0.90253(5) 0.0240(2) Uani 1 1 d . . . P6 P 0.06829(6) 0.72953(6) 1.10296(6) 0.0263(2) Uani 1 1 d . . . P7 P -0.16722(6) 0.79012(5) 0.94261(5) 0.0218(2) Uani 1 1 d . . . P8 P 0.00675(6) 0.74906(6) 0.75618(6) 0.0265(2) Uani 1 1 d . . . O1 O 0.56282(16) 0.75668(15) 0.33257(13) 0.0233(6) Uani 1 1 d . . . O2 O 0.64601(16) 0.74728(15) 0.45716(14) 0.0258(6) Uani 1 1 d . . . O3 O 0.50742(16) 0.75783(16) 0.52759(13) 0.0266(6) Uani 1 1 d . . . O4 O 0.42955(16) 0.75874(15) 0.40522(14) 0.0259(6) Uani 1 1 d . . . O5 O 0.14453(16) 0.75042(16) 0.90752(15) 0.0279(6) Uani 1 1 d . . . O6 O 0.04582(16) 0.75107(16) 1.02710(14) 0.0287(6) Uani 1 1 d . . . O7 O -0.07728(15) 0.76099(15) 0.94245(15) 0.0272(6) Uani 1 1 d . . . O8 O 0.01736(16) 0.76434(16) 0.82349(15) 0.0282(6) Uani 1 1 d . . . C1 C 0.6968(2) 0.6994(2) 0.2661(2) 0.0268(9) Uani 1 1 d . . . C2 C 0.7506(3) 0.7095(3) 0.2145(3) 0.0394(11) Uani 1 1 d . . . H2 H 0.7347 0.7426 0.1663 0.047 Uiso 1 1 calc R . . C3 C 0.8305(3) 0.6634(3) 0.2447(3) 0.0506(14) Uani 1 1 d . . . H3 H 0.8802 0.6598 0.2213 0.061 Uiso 1 1 calc R . . C4 C 0.8275(3) 0.6252(3) 0.3139(3) 0.0497(14) Uani 1 1 d . . . H4 H 0.8747 0.5904 0.3474 0.060 Uiso 1 1 calc R . . C5 C 0.7458(3) 0.6459(3) 0.3280(2) 0.0354(10) Uani 1 1 d . . . H5 H 0.7258 0.6277 0.3726 0.042 Uiso 1 1 calc R . . C6 C 0.7511(2) 0.7917(2) 0.3776(2) 0.0269(9) Uani 1 1 d . . . C7 C 0.8296(3) 0.7767(3) 0.3539(3) 0.0406(11) Uani 1 1 d . . . H7 H 0.8818 0.7427 0.3814 0.049 Uiso 1 1 calc R . . C8 C 0.8185(3) 0.8198(3) 0.2837(3) 0.0449(12) Uani 1 1 d . . . H8 H 0.8624 0.8197 0.2532 0.054 Uiso 1 1 calc R . . C9 C 0.7355(3) 0.8608(3) 0.2633(2) 0.0383(11) Uani 1 1 d . . . H9 H 0.7111 0.8948 0.2167 0.046 Uiso 1 1 calc R . . C10 C 0.6927(3) 0.8441(2) 0.3219(2) 0.0290(9) Uani 1 1 d . . . H10 H 0.6333 0.8647 0.3233 0.035 Uiso 1 1 calc R . . C11 C 0.4099(2) 0.7080(2) 0.6136(2) 0.0314(10) Uani 1 1 d . . . C12 C 0.3468(3) 0.7279(3) 0.6595(2) 0.0466(13) Uani 1 1 d . . . H12 H 0.3397 0.7603 0.6918 0.056 Uiso 1 1 calc R . . C13 C 0.2959(3) 0.6926(4) 0.6495(3) 0.0623(18) Uani 1 1 d . . . H13 H 0.2462 0.6975 0.6733 0.075 Uiso 1 1 calc R . . C14 C 0.3267(3) 0.6509(3) 0.5992(3) 0.0578(16) Uani 1 1 d . . . H14 H 0.3025 0.6218 0.5818 0.069 Uiso 1 1 calc R . . C15 C 0.3978(3) 0.6595(3) 0.5769(3) 0.0386(11) Uani 1 1 d . . . H15 H 0.4322 0.6370 0.5417 0.046 Uiso 1 1 calc R . . C16 C 0.2831(2) 0.8158(2) 0.4554(2) 0.0264(9) Uani 1 1 d . . . C17 C 0.2119(3) 0.8090(3) 0.4831(2) 0.0374(11) Uani 1 1 d . . . H17 H 0.1851 0.7796 0.4697 0.045 Uiso 1 1 calc R . . C18 C 0.1874(3) 0.8522(3) 0.5332(2) 0.0438(12) Uani 1 1 d . . . H18 H 0.1408 0.8574 0.5616 0.053 Uiso 1 1 calc R . . C19 C 0.2422(3) 0.8853(3) 0.5369(2) 0.0387(11) Uani 1 1 d . . . H19 H 0.2403 0.9174 0.5682 0.046 Uiso 1 1 calc R . . C20 C 0.3003(2) 0.8639(2) 0.4885(2) 0.0276(9) Uani 1 1 d . . . H20 H 0.3462 0.8782 0.4803 0.033 Uiso 1 1 calc R . . C21 C 0.2299(2) 0.8039(2) 0.9716(2) 0.0269(9) Uani 1 1 d . . . C22 C 0.3030(3) 0.7941(3) 1.0041(2) 0.0341(10) Uani 1 1 d . . . H22 H 0.3585 0.7640 0.9927 0.041 Uiso 1 1 calc R . . C23 C 0.2818(3) 0.8357(3) 1.0549(2) 0.0413(11) Uani 1 1 d . . . H23 H 0.3201 0.8386 1.0861 0.050 Uiso 1 1 calc R . . C24 C 0.1970(3) 0.8702(3) 1.0553(2) 0.0402(11) Uani 1 1 d . . . H24 H 0.1659 0.9014 1.0870 0.048 Uiso 1 1 calc R . . C25 C 0.1639(3) 0.8520(2) 1.0039(2) 0.0293(9) Uani 1 1 d . . . H25 H 0.1058 0.8687 0.9926 0.035 Uiso 1 1 calc R . . C26 C 0.1732(2) 0.6960(2) 1.1221(2) 0.0301(9) Uani 1 1 d . . . C27 C 0.2126(3) 0.7124(3) 1.1715(2) 0.0404(11) Uani 1 1 d . . . H27 H 0.1861 0.7441 1.2041 0.049 Uiso 1 1 calc R . . C28 C 0.2973(3) 0.6742(3) 1.1655(3) 0.0473(13) Uani 1 1 d . . . H28 H 0.3401 0.6757 1.1927 0.057 Uiso 1 1 calc R . . C29 C 0.3093(3) 0.6354(3) 1.1142(3) 0.0458(13) Uani 1 1 d . . . H29 H 0.3623 0.6052 1.0985 0.055 Uiso 1 1 calc R . . C30 C 0.2332(3) 0.6482(2) 1.0862(2) 0.0357(10) Uani 1 1 d . . . H30 H 0.2238 0.6275 1.0490 0.043 Uiso 1 1 calc R . . C31 C -0.2154(2) 0.8306(2) 0.8585(2) 0.0257(9) Uani 1 1 d . . . C32 C -0.2855(2) 0.8271(3) 0.8325(2) 0.0327(10) Uani 1 1 d . . . H32 H -0.3154 0.7983 0.8586 0.039 Uiso 1 1 calc R . . C33 C -0.3034(3) 0.8723(3) 0.7628(3) 0.0427(12) Uani 1 1 d . . . H33 H -0.3478 0.8796 0.7314 0.051 Uiso 1 1 calc R . . C34 C -0.2462(3) 0.9041(3) 0.7448(3) 0.0419(12) Uani 1 1 d . . . H34 H -0.2441 0.9373 0.6989 0.050 Uiso 1 1 calc R . . C35 C -0.1916(3) 0.8786(2) 0.8035(2) 0.0302(9) Uani 1 1 d . . . H35 H -0.1452 0.8913 0.8061 0.036 Uiso 1 1 calc R . . C36 C -0.0765(3) 0.7262(3) 0.7503(2) 0.0325(10) Uani 1 1 d . . . C37 C -0.1340(3) 0.7517(3) 0.6927(3) 0.0413(12) Uani 1 1 d . . . H37 H -0.1355 0.7870 0.6469 0.050 Uiso 1 1 calc R . . C38 C -0.1876(3) 0.7171(3) 0.7129(3) 0.0529(15) Uani 1 1 d . . . H38 H -0.2344 0.7249 0.6841 0.064 Uiso 1 1 calc R . . C39 C -0.1648(3) 0.6713(3) 0.7811(4) 0.0532(16) Uani 1 1 d . . . H39 H -0.1932 0.6415 0.8087 0.064 Uiso 1 1 calc R . . C40 C -0.0959(3) 0.6753(3) 0.8052(3) 0.0400(11) Uani 1 1 d . . . H40 H -0.0668 0.6483 0.8516 0.048 Uiso 1 1 calc R . . C1A C 0.5572(2) 0.8380(2) 0.1993(2) 0.0260(9) Uani 1 1 d . . . C2A C 0.5150(3) 0.9059(2) 0.2202(2) 0.0300(9) Uani 1 1 d . . . H2A H 0.5003 0.9025 0.2660 0.036 Uiso 1 1 calc R . . C3A C 0.4946(3) 0.9783(3) 0.1738(3) 0.0431(12) Uani 1 1 d . . . H3A H 0.4667 1.0240 0.1881 0.052 Uiso 1 1 calc R . . C4A C 0.5158(4) 0.9827(3) 0.1065(3) 0.0555(15) Uani 1 1 d . . . H4A H 0.5032 1.0316 0.0752 0.067 Uiso 1 1 calc R . . C5A C 0.5549(4) 0.9163(3) 0.0848(3) 0.0520(14) Uani 1 1 d . . . H5A H 0.5673 0.9203 0.0384 0.062 Uiso 1 1 calc R . . C6A C 0.5762(3) 0.8440(3) 0.1301(2) 0.0368(10) Uani 1 1 d . . . H6A H 0.6033 0.7988 0.1149 0.044 Uiso 1 1 calc R . . C1B C 0.5547(2) 0.6824(2) 0.2378(2) 0.0249(8) Uani 1 1 d . . . C2B C 0.5257(3) 0.6939(3) 0.1710(2) 0.0417(11) Uani 1 1 d . . . H2B H 0.5181 0.7397 0.1366 0.050 Uiso 1 1 calc R . . C3B C 0.5081(3) 0.6374(4) 0.1556(3) 0.0522(14) Uani 1 1 d . . . H3B H 0.4891 0.6448 0.1103 0.063 Uiso 1 1 calc R . . C4B C 0.5178(3) 0.5717(3) 0.2048(3) 0.0459(12) Uani 1 1 d . . . H4B H 0.5066 0.5335 0.1933 0.055 Uiso 1 1 calc R . . C5B C 0.5441(3) 0.5607(3) 0.2715(3) 0.0479(13) Uani 1 1 d . . . H5B H 0.5489 0.5158 0.3058 0.057 Uiso 1 1 calc R . . C6B C 0.5633(3) 0.6155(3) 0.2884(2) 0.0401(11) Uani 1 1 d . . . H6B H 0.5822 0.6074 0.3339 0.048 Uiso 1 1 calc R . . C1C C 0.7103(2) 0.8288(2) 0.5050(2) 0.0265(9) Uani 1 1 d . . . C2C C 0.7662(3) 0.8607(3) 0.5002(2) 0.0380(11) Uani 1 1 d . . . H2C H 0.8121 0.8426 0.4755 0.046 Uiso 1 1 calc R . . C3C C 0.7538(3) 0.9187(3) 0.5318(3) 0.0428(12) Uani 1 1 d . . . H3C H 0.7914 0.9401 0.5288 0.051 Uiso 1 1 calc R . . C4C C 0.6860(3) 0.9457(3) 0.5680(2) 0.0418(12) Uani 1 1 d . . . H4C H 0.6779 0.9849 0.5899 0.050 Uiso 1 1 calc R . . C5C C 0.6305(3) 0.9152(3) 0.5717(2) 0.0389(11) Uani 1 1 d . . . H5C H 0.5840 0.9345 0.5954 0.047 Uiso 1 1 calc R . . C6C C 0.6423(3) 0.8565(2) 0.5411(2) 0.0318(9) Uani 1 1 d . . . H6C H 0.6045 0.8353 0.5446 0.038 Uiso 1 1 calc R . . C1D C 0.8042(2) 0.6647(3) 0.5034(2) 0.0330(10) Uani 1 1 d . . . C2D C 0.8769(3) 0.6603(3) 0.5256(3) 0.0509(13) Uani 1 1 d . . . H2D H 0.8842 0.7057 0.5222 0.061 Uiso 1 1 calc R . . C3D C 0.9392(3) 0.5864(4) 0.5533(3) 0.0662(18) Uani 1 1 d . . . H3D H 0.9890 0.5823 0.5686 0.079 Uiso 1 1 calc R . . C4D C 0.9293(3) 0.5206(4) 0.5587(3) 0.0635(18) Uani 1 1 d . . . H4D H 0.9722 0.4716 0.5774 0.076 Uiso 1 1 calc R . . C5D C 0.8582(3) 0.5248(3) 0.5374(3) 0.0536(15) Uani 1 1 d . . . H5D H 0.8517 0.4790 0.5414 0.064 Uiso 1 1 calc R . . C6D C 0.7945(3) 0.5972(3) 0.5096(2) 0.0394(11) Uani 1 1 d . . . H6D H 0.7450 0.6002 0.4950 0.047 Uiso 1 1 calc R . . C1E C 0.4643(2) 0.8184(2) 0.63681(19) 0.0258(9) Uani 1 1 d . . . C2E C 0.4406(3) 0.8924(2) 0.5920(2) 0.0315(9) Uani 1 1 d . . . H2E H 0.4370 0.8995 0.5439 0.038 Uiso 1 1 calc R . . C3E C 0.4224(3) 0.9556(3) 0.6184(2) 0.0427(12) Uani 1 1 d . . . H3E H 0.4053 1.0059 0.5882 0.051 Uiso 1 1 calc R . . C4E C 0.4293(3) 0.9449(3) 0.6891(3) 0.0505(14) Uani 1 1 d . . . H4E H 0.4186 0.9877 0.7069 0.061 Uiso 1 1 calc R . . C5E C 0.4519(4) 0.8718(3) 0.7335(3) 0.0593(16) Uani 1 1 d . . . H5E H 0.4553 0.8649 0.7816 0.071 Uiso 1 1 calc R . . C6E C 0.4694(3) 0.8087(3) 0.7076(2) 0.0470(13) Uani 1 1 d . . . H6E H 0.4849 0.7588 0.7381 0.056 Uiso 1 1 calc R . . C1F C 0.5754(3) 0.6555(2) 0.6538(2) 0.0282(9) Uani 1 1 d . . . C2F C 0.6524(3) 0.6489(2) 0.6400(2) 0.0318(10) Uani 1 1 d . . . H2F H 0.6597 0.6856 0.6030 0.038 Uiso 1 1 calc R . . C3F C 0.7189(3) 0.5883(3) 0.6807(3) 0.0399(11) Uani 1 1 d . . . H3F H 0.7712 0.5836 0.6713 0.048 Uiso 1 1 calc R . . C4F C 0.7076(3) 0.5355(3) 0.7346(3) 0.0514(14) Uani 1 1 d . . . H4F H 0.7524 0.4954 0.7632 0.062 Uiso 1 1 calc R . . C5F C 0.6308(3) 0.5403(3) 0.7478(3) 0.0592(16) Uani 1 1 d . . . H5F H 0.6242 0.5023 0.7839 0.071 Uiso 1 1 calc R . . C6F C 0.5642(3) 0.6006(3) 0.7077(3) 0.0474(13) Uani 1 1 d . . . H6F H 0.5121 0.6046 0.7169 0.057 Uiso 1 1 calc R . . C1G C 0.3350(2) 0.6866(2) 0.3923(2) 0.0284(9) Uani 1 1 d . . . C2G C 0.2619(3) 0.6870(3) 0.3754(3) 0.0474(13) Uani 1 1 d . . . H2G H 0.2153 0.7342 0.3627 0.057 Uiso 1 1 calc R . . C3G C 0.2582(4) 0.6176(3) 0.3772(3) 0.0542(14) Uani 1 1 d . . . H3G H 0.2093 0.6175 0.3652 0.065 Uiso 1 1 calc R . . C4G C 0.3268(4) 0.5487(3) 0.3968(3) 0.0556(15) Uani 1 1 d . . . H4G H 0.3241 0.5014 0.3993 0.067 Uiso 1 1 calc R . . C5G C 0.3977(3) 0.5482(3) 0.4125(3) 0.0539(14) Uani 1 1 d . . . H5G H 0.4440 0.5006 0.4251 0.065 Uiso 1 1 calc R . . C6G C 0.4033(3) 0.6167(3) 0.4101(3) 0.0389(11) Uani 1 1 d . . . H6G H 0.4532 0.6159 0.4206 0.047 Uiso 1 1 calc R . . C1H C 0.3006(2) 0.8426(2) 0.3102(2) 0.0247(8) Uani 1 1 d . . . C2H C 0.3518(3) 0.8575(3) 0.2618(2) 0.0344(10) Uani 1 1 d . . . H2H H 0.4079 0.8331 0.2727 0.041 Uiso 1 1 calc R . . C3H C 0.3202(3) 0.9087(3) 0.1969(2) 0.0419(11) Uani 1 1 d . . . H3H H 0.3548 0.9187 0.1639 0.050 Uiso 1 1 calc R . . C4H C 0.2380(3) 0.9448(2) 0.1811(2) 0.0356(10) Uani 1 1 d . . . H4H H 0.2168 0.9798 0.1373 0.043 Uiso 1 1 calc R . . C5H C 0.1869(3) 0.9303(3) 0.2283(2) 0.0394(11) Uani 1 1 d . . . H5H H 0.1309 0.9548 0.2168 0.047 Uiso 1 1 calc R . . C6H C 0.2177(3) 0.8795(3) 0.2928(2) 0.0389(11) Uani 1 1 d . . . H6H H 0.1824 0.8698 0.3253 0.047 Uiso 1 1 calc R . . C1I C 0.3074(2) 0.6832(3) 0.9033(2) 0.0312(10) Uani 1 1 d . . . C2I C 0.3794(3) 0.6887(3) 0.8855(3) 0.0495(13) Uani 1 1 d . . . H2I H 0.3800 0.7379 0.8695 0.059 Uiso 1 1 calc R . . C3I C 0.4498(3) 0.6220(4) 0.8915(3) 0.0629(18) Uani 1 1 d . . . H3I H 0.4983 0.6259 0.8797 0.075 Uiso 1 1 calc R . . C4I C 0.4494(3) 0.5516(4) 0.9140(3) 0.0625(18) Uani 1 1 d . . . H4I H 0.4980 0.5068 0.9183 0.075 Uiso 1 1 calc R . . C5I C 0.3784(3) 0.5434(3) 0.9313(3) 0.0564(15) Uani 1 1 d . . . H5I H 0.3790 0.4937 0.9467 0.068 Uiso 1 1 calc R . . C6I C 0.3064(3) 0.6104(3) 0.9253(2) 0.0400(11) Uani 1 1 d . . . H6I H 0.2578 0.6063 0.9360 0.048 Uiso 1 1 calc R . . C1J C 0.2087(2) 0.8428(2) 0.8248(2) 0.0284(9) Uani 1 1 d . . . C2J C 0.2456(3) 0.8924(3) 0.8226(3) 0.0456(12) Uani 1 1 d . . . H2J H 0.2747 0.8876 0.8623 0.055 Uiso 1 1 calc R . . C3J C 0.2395(4) 0.9483(3) 0.7626(3) 0.0557(15) Uani 1 1 d . . . H3J H 0.2647 0.9814 0.7614 0.067 Uiso 1 1 calc R . . C4J C 0.1971(4) 0.9559(3) 0.7047(3) 0.0564(15) Uani 1 1 d . . . H4J H 0.1934 0.9941 0.6638 0.068 Uiso 1 1 calc R . . C5J C 0.1603(4) 0.9083(4) 0.7063(3) 0.0577(15) Uani 1 1 d . . . H5J H 0.1308 0.9140 0.6664 0.069 Uiso 1 1 calc R . . C6J C 0.1658(3) 0.8513(3) 0.7662(2) 0.0457(12) Uani 1 1 d . . . H6J H 0.1403 0.8185 0.7668 0.055 Uiso 1 1 calc R . . C1K C 0.0204(2) 0.8130(2) 1.1373(2) 0.0306(9) Uani 1 1 d . . . C2K C 0.0199(3) 0.8071(3) 1.2080(2) 0.0426(12) Uani 1 1 d . . . H2K H 0.0393 0.7580 1.2404 0.051 Uiso 1 1 calc R . . C3K C -0.0095(3) 0.8749(3) 1.2303(3) 0.0525(14) Uani 1 1 d . . . H3K H -0.0100 0.8714 1.2779 0.063 Uiso 1 1 calc R . . C4K C -0.0376(3) 0.9462(3) 1.1834(3) 0.0555(15) Uani 1 1 d . . . H4K H -0.0557 0.9915 1.1988 0.067 Uiso 1 1 calc R . . C5K C -0.0396(3) 0.9519(3) 1.1139(3) 0.0508(14) Uani 1 1 d . . . H5K H -0.0606 1.0014 1.0821 0.061 Uiso 1 1 calc R . . C6K C -0.0110(3) 0.8856(3) 1.0898(3) 0.0382(11) Uani 1 1 d . . . H6K H -0.0130 0.8900 1.0421 0.046 Uiso 1 1 calc R . . C1L C 0.0461(3) 0.6500(2) 1.1502(2) 0.0327(10) Uani 1 1 d . . . C2L C 0.0762(3) 0.6117(3) 1.2189(3) 0.0503(14) Uani 1 1 d . . . H2L H 0.1062 0.6289 1.2418 0.060 Uiso 1 1 calc R . . C3L C 0.0617(3) 0.5484(3) 1.2531(3) 0.0613(17) Uani 1 1 d . . . H3L H 0.0804 0.5237 1.2999 0.074 Uiso 1 1 calc R . . C4L C 0.0210(4) 0.5213(3) 1.2203(3) 0.0597(17) Uani 1 1 d . . . H4L H 0.0125 0.4776 1.2441 0.072 Uiso 1 1 calc R . . C5L C -0.0076(4) 0.5574(3) 1.1529(3) 0.0567(15) Uani 1 1 d . . . H5L H -0.0353 0.5381 1.1301 0.068 Uiso 1 1 calc R . . C6L C 0.0040(3) 0.6231(3) 1.1173(3) 0.0445(12) Uani 1 1 d . . . H6L H -0.0169 0.6487 1.0711 0.053 Uiso 1 1 calc R . . C1M C -0.2129(2) 0.8654(2) 0.9868(2) 0.0266(9) Uani 1 1 d . . . C2M C -0.1753(3) 0.8578(3) 1.0488(3) 0.0437(12) Uani 1 1 d . . . H2M H -0.1271 0.8137 1.0673 0.052 Uiso 1 1 calc R . . C3M C -0.2091(3) 0.9158(4) 1.0833(3) 0.0542(15) Uani 1 1 d . . . H3M H -0.1838 0.9110 1.1251 0.065 Uiso 1 1 calc R . . C4M C -0.2800(3) 0.9806(3) 1.0558(3) 0.0477(13) Uani 1 1 d . . . H4M H -0.3025 1.0202 1.0787 0.057 Uiso 1 1 calc R . . C5M C -0.3173(3) 0.9873(3) 0.9957(3) 0.0456(13) Uani 1 1 d . . . H5M H -0.3660 1.0310 0.9778 0.055 Uiso 1 1 calc R . . C6M C -0.2839(3) 0.9301(2) 0.9604(2) 0.0373(11) Uani 1 1 d . . . H6M H -0.3097 0.9354 0.9186 0.045 Uiso 1 1 calc R . . C1N C -0.1905(3) 0.7109(2) 0.9868(2) 0.0317(10) Uani 1 1 d . . . C2N C -0.2626(3) 0.7230(3) 1.0178(3) 0.0439(12) Uani 1 1 d . . . H2N H -0.3014 0.7738 1.0153 0.053 Uiso 1 1 calc R . . C3N C -0.2769(4) 0.6585(4) 1.0529(3) 0.0686(19) Uani 1 1 d . . . H3N H -0.3253 0.6662 1.0745 0.082 Uiso 1 1 calc R . . C4N C -0.2212(5) 0.5851(4) 1.0558(4) 0.074(2) Uani 1 1 d . . . H4N H -0.2308 0.5421 1.0799 0.089 Uiso 1 1 calc R . . C5N C -0.1503(4) 0.5732(3) 1.0234(4) 0.0721(19) Uani 1 1 d . . . H5N H -0.1129 0.5222 1.0246 0.087 Uiso 1 1 calc R . . C6N C -0.1336(3) 0.6348(3) 0.9896(3) 0.0487(13) Uani 1 1 d . . . H6N H -0.0848 0.6261 0.9687 0.058 Uiso 1 1 calc R . . C1P C -0.0107(2) 0.8343(3) 0.6861(2) 0.0353(10) Uani 1 1 d . . . C2P C -0.0297(3) 0.9039(3) 0.7022(3) 0.0524(15) Uani 1 1 d . . . H2P H -0.0310 0.9055 0.7487 0.063 Uiso 1 1 calc R . . C3P C -0.0466(4) 0.9707(3) 0.6498(4) 0.077(2) Uani 1 1 d . . . H3P H -0.0588 1.0179 0.6608 0.093 Uiso 1 1 calc R . . C4P C -0.0458(3) 0.9696(4) 0.5818(4) 0.080(3) Uani 1 1 d . . . H4P H -0.0582 1.0159 0.5466 0.097 Uiso 1 1 calc R . . C5P C -0.0274(3) 0.9018(5) 0.5648(3) 0.071(2) Uani 1 1 d . . . H5P H -0.0278 0.9015 0.5180 0.085 Uiso 1 1 calc R . . C6P C -0.0078(3) 0.8324(4) 0.6169(3) 0.0529(14) Uani 1 1 d . . . H6P H 0.0072 0.7850 0.6055 0.063 Uiso 1 1 calc R . . C1U C 0.0934(3) 0.6666(2) 0.7419(2) 0.0317(10) Uani 1 1 d . . . C2U C 0.1630(3) 0.6365(3) 0.7834(2) 0.0376(11) Uani 1 1 d . . . H2U H 0.1660 0.6599 0.8179 0.045 Uiso 1 1 calc R . . C3U C 0.2297(3) 0.5709(3) 0.7745(3) 0.0482(13) Uani 1 1 d . . . H3U H 0.2779 0.5499 0.8027 0.058 Uiso 1 1 calc R . . C4U C 0.2237(4) 0.5374(3) 0.7236(4) 0.0668(18) Uani 1 1 d . . . H4U H 0.2680 0.4928 0.7178 0.080 Uiso 1 1 calc R . . C5U C 0.1548(4) 0.5679(4) 0.6817(4) 0.077(2) Uani 1 1 d . . . H5U H 0.1520 0.5456 0.6463 0.092 Uiso 1 1 calc R . . C6U C 0.0890(4) 0.6320(3) 0.6918(3) 0.0628(17) Uani 1 1 d . . . H6U H 0.0407 0.6523 0.6641 0.075 Uiso 1 1 calc R . . Cl5 Cl 0.03851(11) 0.74594(15) 0.43938(11) 0.0887(6) Uani 1 1 d . . . O9 O -0.0399(4) 0.7873(6) 0.4617(5) 0.180(4) Uani 1 1 d . . . O10 O 0.0966(5) 0.6975(5) 0.4994(3) 0.154(3) Uani 1 1 d . . . O11 O 0.0633(4) 0.8062(5) 0.4016(3) 0.134(3) Uani 1 1 d . . . O12 O 0.0330(3) 0.7004(5) 0.3933(4) 0.141(3) Uani 1 1 d . . . Cl6 Cl 0.50471(7) 0.19566(7) 0.04504(7) 0.0456(3) Uani 1 1 d . . . O13 O 0.4372(2) 0.1835(3) 0.0673(3) 0.0998(19) Uani 1 1 d . . . O14 O 0.5707(2) 0.1530(3) 0.09438(19) 0.0706(13) Uani 1 1 d . . . O15 O 0.4898(3) 0.2753(2) 0.0232(3) 0.0799(14) Uani 1 1 d . . . O16 O 0.5302(3) 0.1658(3) -0.0150(2) 0.0904(16) Uani 1 1 d . . . Cl8 Cl 0.36944(11) 0.30873(10) 0.18235(10) 0.0774(5) Uani 1 1 d . . . Cl7 Cl 0.2848(2) 0.45954(12) 0.08704(13) 0.1493(13) Uani 1 1 d . . . C1S C 0.3271(4) 0.3604(4) 0.0980(3) 0.0735(19) Uani 1 1 d . . . H1S1 H 0.3689 0.3467 0.0656 0.088 Uiso 1 1 calc R . . H1S2 H 0.2855 0.3450 0.0873 0.088 Uiso 1 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 Fe1 0.0200(3) 0.0171(3) 0.0158(3) -0.0026(2) 0.0042(2) -0.0066(2) Fe2 0.0212(3) 0.0332(3) 0.0282(3) -0.0121(3) 0.0075(2) -0.0113(3) Fe3 0.0231(3) 0.0329(3) 0.0269(3) 0.0015(3) 0.0057(2) -0.0121(3) Fe4 0.0183(3) 0.0133(3) 0.0287(3) -0.0023(2) 0.0044(2) -0.0054(2) Fe5 0.0212(3) 0.0303(3) 0.0279(3) -0.0040(3) 0.0017(2) -0.0066(2) Fe6 0.0259(3) 0.0306(3) 0.0388(4) -0.0184(3) 0.0084(3) -0.0133(3) Cl1 0.0322(5) 0.0184(5) 0.0349(6) 0.0002(4) -0.0014(4) -0.0074(4) Cl2 0.0389(6) 0.0174(4) 0.0258(5) -0.0051(4) 0.0089(4) -0.0074(4) Cl3 0.0360(5) 0.0146(4) 0.0359(6) -0.0017(4) -0.0031(4) -0.0070(4) Cl4 0.0403(6) 0.0146(5) 0.0581(7) -0.0054(5) 0.0180(5) -0.0071(4) P1 0.0224(5) 0.0210(5) 0.0176(5) -0.0063(4) 0.0052(4) -0.0083(4) P2 0.0207(5) 0.0258(5) 0.0241(5) -0.0082(4) 0.0020(4) -0.0080(4) P3 0.0236(5) 0.0212(5) 0.0165(5) 0.0008(4) 0.0041(4) -0.0049(4) P4 0.0216(5) 0.0178(5) 0.0253(5) -0.0030(4) 0.0014(4) -0.0072(4) P5 0.0192(5) 0.0237(5) 0.0288(6) -0.0072(4) 0.0059(4) -0.0092(4) P6 0.0211(5) 0.0199(5) 0.0274(6) 0.0013(4) 0.0036(4) -0.0034(4) P7 0.0192(5) 0.0155(5) 0.0284(5) -0.0041(4) 0.0067(4) -0.0066(4) P8 0.0236(5) 0.0225(5) 0.0338(6) -0.0108(4) 0.0090(4) -0.0090(4) O1 0.0291(14) 0.0221(13) 0.0187(13) -0.0059(11) 0.0070(11) -0.0110(12) O2 0.0233(14) 0.0248(14) 0.0271(15) -0.0056(12) 0.0035(11) -0.0092(12) O3 0.0297(15) 0.0278(15) 0.0178(14) -0.0046(11) 0.0064(11) -0.0093(12) O4 0.0229(14) 0.0231(14) 0.0297(15) -0.0047(12) 0.0015(12) -0.0093(12) O5 0.0221(14) 0.0249(14) 0.0380(17) -0.0100(13) 0.0064(12) -0.0107(12) O6 0.0256(15) 0.0234(14) 0.0306(16) -0.0014(12) 0.0003(12) -0.0077(12) O7 0.0177(13) 0.0245(14) 0.0391(17) -0.0080(13) 0.0074(12) -0.0096(11) O8 0.0282(15) 0.0237(14) 0.0324(16) -0.0082(12) 0.0052(12) -0.0107(12) C1 0.023(2) 0.030(2) 0.031(2) -0.0173(18) 0.0059(17) -0.0102(17) C2 0.031(2) 0.054(3) 0.038(3) -0.027(2) 0.014(2) -0.016(2) C3 0.030(3) 0.057(3) 0.070(4) -0.043(3) 0.021(2) -0.010(2) C4 0.030(3) 0.036(3) 0.075(4) -0.023(3) -0.001(2) -0.001(2) C5 0.032(2) 0.029(2) 0.042(3) -0.012(2) -0.003(2) -0.0081(19) C6 0.025(2) 0.033(2) 0.029(2) -0.0103(18) 0.0022(17) -0.0167(18) C7 0.032(2) 0.060(3) 0.045(3) -0.022(2) 0.012(2) -0.029(2) C8 0.044(3) 0.061(3) 0.048(3) -0.019(3) 0.021(2) -0.038(3) C9 0.051(3) 0.033(2) 0.037(3) -0.007(2) 0.012(2) -0.026(2) C10 0.037(2) 0.025(2) 0.032(2) -0.0119(18) 0.0061(18) -0.0164(18) C11 0.026(2) 0.034(2) 0.020(2) 0.0079(17) 0.0027(17) -0.0083(18) C12 0.039(3) 0.063(3) 0.023(2) 0.007(2) 0.005(2) -0.019(2) C13 0.047(3) 0.070(4) 0.049(3) 0.024(3) 0.010(3) -0.030(3) C14 0.045(3) 0.038(3) 0.076(4) 0.016(3) -0.004(3) -0.022(2) C15 0.035(2) 0.028(2) 0.043(3) 0.006(2) 0.000(2) -0.012(2) C16 0.0213(19) 0.025(2) 0.026(2) -0.0002(17) -0.0020(16) -0.0073(16) C17 0.023(2) 0.046(3) 0.039(3) -0.007(2) 0.0019(19) -0.013(2) C18 0.021(2) 0.052(3) 0.037(3) -0.006(2) 0.0085(19) 0.000(2) C19 0.037(3) 0.036(3) 0.034(3) -0.011(2) 0.007(2) -0.007(2) C20 0.027(2) 0.024(2) 0.025(2) -0.0001(17) 0.0030(17) -0.0082(17) C21 0.030(2) 0.022(2) 0.029(2) -0.0041(17) 0.0044(17) -0.0132(17) C22 0.028(2) 0.046(3) 0.035(2) -0.009(2) 0.0076(18) -0.022(2) C23 0.048(3) 0.048(3) 0.039(3) -0.015(2) 0.002(2) -0.029(2) C24 0.048(3) 0.034(2) 0.039(3) -0.015(2) 0.008(2) -0.015(2) C25 0.033(2) 0.023(2) 0.028(2) -0.0046(17) 0.0012(18) -0.0095(18) C26 0.025(2) 0.021(2) 0.030(2) 0.0036(17) 0.0046(17) -0.0038(17) C27 0.030(2) 0.051(3) 0.028(2) -0.001(2) 0.0009(19) -0.011(2) C28 0.033(3) 0.057(3) 0.034(3) 0.006(2) -0.009(2) -0.012(2) C29 0.026(2) 0.034(3) 0.052(3) 0.007(2) 0.002(2) 0.000(2) C30 0.032(2) 0.021(2) 0.039(3) 0.0031(19) 0.006(2) -0.0053(18) C31 0.0197(19) 0.0204(19) 0.036(2) -0.0116(17) 0.0051(17) -0.0056(16) C32 0.023(2) 0.036(2) 0.042(3) -0.017(2) 0.0069(19) -0.0118(18) C33 0.027(2) 0.051(3) 0.044(3) -0.021(2) -0.007(2) -0.004(2) C34 0.050(3) 0.033(3) 0.035(3) -0.011(2) 0.002(2) -0.009(2) C35 0.035(2) 0.023(2) 0.033(2) -0.0110(18) 0.0065(19) -0.0102(18) C36 0.030(2) 0.033(2) 0.041(3) -0.022(2) 0.0129(19) -0.0136(19) C37 0.035(2) 0.054(3) 0.048(3) -0.034(3) 0.012(2) -0.021(2) C38 0.041(3) 0.069(4) 0.080(4) -0.058(4) 0.018(3) -0.031(3) C39 0.042(3) 0.037(3) 0.102(5) -0.042(3) 0.032(3) -0.025(2) C40 0.036(2) 0.026(2) 0.062(3) -0.021(2) 0.019(2) -0.012(2) C1A 0.029(2) 0.031(2) 0.019(2) -0.0024(17) 0.0014(16) -0.0162(18) C2A 0.032(2) 0.024(2) 0.028(2) -0.0034(17) -0.0007(18) -0.0081(18) C3A 0.049(3) 0.027(2) 0.045(3) -0.002(2) -0.010(2) -0.012(2) C4A 0.078(4) 0.047(3) 0.041(3) 0.013(2) -0.016(3) -0.038(3) C5A 0.079(4) 0.063(4) 0.024(2) 0.003(2) 0.009(2) -0.049(3) C6A 0.044(3) 0.045(3) 0.025(2) -0.008(2) 0.0088(19) -0.024(2) C1B 0.0231(19) 0.023(2) 0.027(2) -0.0096(17) 0.0065(16) -0.0075(16) C2B 0.047(3) 0.051(3) 0.032(3) -0.003(2) -0.005(2) -0.029(2) C3B 0.059(3) 0.078(4) 0.041(3) -0.019(3) -0.005(3) -0.047(3) C4B 0.050(3) 0.049(3) 0.056(3) -0.027(3) 0.007(3) -0.030(3) C5B 0.062(3) 0.035(3) 0.053(3) -0.010(2) 0.002(3) -0.027(3) C6B 0.054(3) 0.038(3) 0.033(3) -0.011(2) 0.001(2) -0.022(2) C1C 0.029(2) 0.026(2) 0.022(2) -0.0086(16) -0.0016(16) -0.0079(17) C2C 0.029(2) 0.043(3) 0.045(3) -0.018(2) 0.001(2) -0.014(2) C3C 0.039(3) 0.040(3) 0.054(3) -0.016(2) -0.009(2) -0.018(2) C4C 0.049(3) 0.034(3) 0.039(3) -0.016(2) -0.013(2) -0.009(2) C5C 0.038(3) 0.039(3) 0.035(3) -0.016(2) 0.005(2) -0.009(2) C6C 0.032(2) 0.031(2) 0.031(2) -0.0096(19) 0.0048(18) -0.0118(19) C1D 0.025(2) 0.038(2) 0.026(2) -0.0073(19) 0.0021(17) -0.0038(19) C2D 0.039(3) 0.052(3) 0.057(3) -0.022(3) -0.004(2) -0.009(2) C3D 0.034(3) 0.074(4) 0.066(4) -0.016(3) -0.017(3) 0.000(3) C4D 0.046(3) 0.057(4) 0.046(3) -0.005(3) 0.002(3) 0.012(3) C5D 0.049(3) 0.039(3) 0.043(3) 0.004(2) 0.008(2) 0.000(2) C6D 0.036(3) 0.033(2) 0.036(3) -0.001(2) 0.000(2) -0.006(2) C1E 0.027(2) 0.025(2) 0.0165(19) -0.0017(16) 0.0051(16) -0.0054(17) C2E 0.036(2) 0.029(2) 0.024(2) -0.0064(18) 0.0027(18) -0.0089(19) C3E 0.050(3) 0.032(2) 0.034(3) -0.007(2) 0.000(2) -0.007(2) C4E 0.061(3) 0.043(3) 0.042(3) -0.026(2) 0.005(3) -0.009(3) C5E 0.086(4) 0.048(3) 0.023(3) -0.018(2) 0.002(3) -0.006(3) C6E 0.064(3) 0.030(2) 0.018(2) 0.0021(18) 0.002(2) 0.002(2) C1F 0.033(2) 0.021(2) 0.021(2) 0.0007(16) 0.0002(17) -0.0068(17) C2F 0.031(2) 0.026(2) 0.032(2) -0.0034(18) 0.0023(18) -0.0091(18) C3F 0.025(2) 0.038(3) 0.050(3) -0.013(2) -0.005(2) -0.005(2) C4F 0.042(3) 0.034(3) 0.051(3) -0.002(2) -0.012(2) 0.006(2) C5F 0.059(4) 0.031(3) 0.055(3) 0.020(2) -0.004(3) -0.007(2) C6F 0.038(3) 0.039(3) 0.046(3) 0.010(2) 0.001(2) -0.010(2) C1G 0.031(2) 0.023(2) 0.032(2) -0.0042(17) 0.0006(18) -0.0136(18) C2G 0.044(3) 0.036(3) 0.060(3) -0.004(2) -0.011(2) -0.019(2) C3G 0.066(4) 0.049(3) 0.063(4) -0.009(3) -0.007(3) -0.041(3) C4G 0.084(4) 0.032(3) 0.059(4) -0.005(2) -0.003(3) -0.036(3) C5G 0.057(3) 0.026(2) 0.071(4) -0.010(3) 0.003(3) -0.013(2) C6G 0.033(2) 0.026(2) 0.054(3) -0.009(2) 0.002(2) -0.0103(19) C1H 0.029(2) 0.0192(19) 0.023(2) -0.0063(16) -0.0012(16) -0.0065(16) C2H 0.033(2) 0.034(2) 0.034(2) -0.0031(19) 0.0006(19) -0.015(2) C3H 0.047(3) 0.048(3) 0.027(2) 0.001(2) 0.002(2) -0.024(2) C4H 0.049(3) 0.024(2) 0.029(2) 0.0006(18) -0.013(2) -0.014(2) C5H 0.033(2) 0.029(2) 0.041(3) -0.001(2) -0.009(2) -0.0018(19) C6H 0.028(2) 0.037(3) 0.036(3) -0.001(2) 0.0040(19) -0.0037(19) C1I 0.019(2) 0.036(2) 0.035(2) -0.0151(19) -0.0004(17) -0.0049(18) C2I 0.029(2) 0.056(3) 0.069(4) -0.033(3) 0.012(2) -0.015(2) C3I 0.024(3) 0.085(5) 0.090(5) -0.056(4) 0.011(3) -0.015(3) C4I 0.033(3) 0.067(4) 0.070(4) -0.044(3) -0.007(3) 0.012(3) C5I 0.056(4) 0.034(3) 0.059(4) -0.020(3) -0.002(3) 0.005(2) C6I 0.036(3) 0.033(2) 0.045(3) -0.015(2) 0.007(2) -0.007(2) C1J 0.026(2) 0.031(2) 0.032(2) -0.0118(18) 0.0113(17) -0.0143(18) C2J 0.050(3) 0.050(3) 0.044(3) -0.005(2) 0.001(2) -0.033(3) C3J 0.070(4) 0.049(3) 0.058(4) -0.006(3) 0.017(3) -0.041(3) C4J 0.076(4) 0.051(3) 0.037(3) -0.002(2) 0.021(3) -0.030(3) C5J 0.076(4) 0.080(4) 0.026(3) -0.010(3) 0.008(3) -0.043(4) C6J 0.061(3) 0.057(3) 0.031(3) -0.014(2) 0.011(2) -0.036(3) C1K 0.023(2) 0.029(2) 0.035(2) -0.0047(18) 0.0077(18) -0.0090(17) C2K 0.037(3) 0.047(3) 0.036(3) -0.007(2) 0.009(2) -0.013(2) C3K 0.052(3) 0.067(4) 0.048(3) -0.031(3) 0.019(3) -0.026(3) C4K 0.050(3) 0.052(3) 0.078(4) -0.039(3) 0.027(3) -0.023(3) C5K 0.045(3) 0.026(2) 0.074(4) -0.011(2) 0.011(3) -0.010(2) C6K 0.034(2) 0.028(2) 0.042(3) -0.004(2) 0.012(2) -0.0076(19) C1L 0.027(2) 0.020(2) 0.036(2) 0.0015(18) 0.0091(18) -0.0020(17) C2L 0.046(3) 0.040(3) 0.040(3) 0.012(2) -0.001(2) -0.007(2) C3L 0.050(3) 0.042(3) 0.055(4) 0.018(3) 0.009(3) -0.004(3) C4L 0.059(4) 0.020(2) 0.075(4) 0.004(3) 0.035(3) -0.006(2) C5L 0.071(4) 0.035(3) 0.071(4) -0.014(3) 0.028(3) -0.031(3) C6L 0.054(3) 0.029(2) 0.044(3) -0.005(2) 0.018(2) -0.016(2) C1M 0.025(2) 0.025(2) 0.030(2) -0.0089(17) 0.0120(17) -0.0115(17) C2M 0.029(2) 0.054(3) 0.049(3) -0.027(3) 0.006(2) -0.011(2) C3M 0.049(3) 0.079(4) 0.051(3) -0.041(3) 0.017(3) -0.031(3) C4M 0.055(3) 0.049(3) 0.059(3) -0.038(3) 0.033(3) -0.029(3) C5M 0.051(3) 0.023(2) 0.051(3) -0.010(2) 0.020(2) -0.006(2) C6M 0.040(3) 0.026(2) 0.036(3) -0.0071(19) 0.008(2) -0.007(2) C1N 0.033(2) 0.026(2) 0.038(3) -0.0044(19) 0.0052(19) -0.0170(19) C2N 0.048(3) 0.044(3) 0.047(3) -0.013(2) 0.017(2) -0.028(2) C3N 0.090(5) 0.084(5) 0.066(4) -0.019(4) 0.033(4) -0.072(4) C4N 0.105(6) 0.051(4) 0.079(5) 0.008(3) 0.006(4) -0.059(4) C5N 0.076(4) 0.032(3) 0.107(5) 0.000(3) -0.002(4) -0.032(3) C6N 0.045(3) 0.027(2) 0.072(4) -0.005(2) 0.006(3) -0.018(2) C1P 0.022(2) 0.039(3) 0.036(3) -0.001(2) 0.0069(18) -0.0109(19) C2P 0.050(3) 0.030(3) 0.057(3) -0.003(2) 0.029(3) -0.006(2) C3P 0.073(4) 0.030(3) 0.089(5) 0.008(3) 0.047(4) -0.002(3) C4P 0.039(3) 0.060(4) 0.078(5) 0.036(4) 0.022(3) 0.005(3) C5P 0.044(3) 0.112(6) 0.039(3) 0.013(4) 0.000(3) -0.036(4) C6P 0.044(3) 0.077(4) 0.039(3) -0.003(3) 0.007(2) -0.035(3) C1U 0.029(2) 0.023(2) 0.043(3) -0.0134(19) 0.0153(19) -0.0098(18) C2U 0.034(2) 0.032(2) 0.038(3) -0.005(2) 0.015(2) -0.010(2) C3U 0.035(3) 0.037(3) 0.054(3) -0.003(2) 0.013(2) -0.005(2) C4U 0.052(4) 0.032(3) 0.108(5) -0.030(3) 0.035(4) -0.006(3) C5U 0.062(4) 0.057(4) 0.112(6) -0.061(4) 0.007(4) -0.003(3) C6U 0.051(3) 0.058(4) 0.081(4) -0.046(3) 0.002(3) -0.008(3) Cl5 0.0576(10) 0.158(2) 0.0814(13) -0.0460(13) 0.0064(9) -0.0665(12) O9 0.071(4) 0.295(10) 0.284(10) -0.210(9) 0.077(5) -0.111(6) O10 0.190(7) 0.233(9) 0.092(5) -0.028(5) -0.002(5) -0.147(7) O11 0.091(4) 0.205(8) 0.114(5) -0.017(5) -0.023(4) -0.082(5) O12 0.060(3) 0.190(7) 0.134(6) -0.031(5) -0.003(3) -0.023(4) Cl6 0.0334(6) 0.0446(7) 0.0597(8) -0.0113(6) -0.0005(6) -0.0186(5) O13 0.038(2) 0.076(3) 0.182(6) -0.018(3) 0.029(3) -0.031(2) O14 0.058(3) 0.108(4) 0.041(2) 0.001(2) -0.0063(19) -0.042(3) O15 0.070(3) 0.051(3) 0.124(4) -0.027(3) 0.027(3) -0.030(2) O16 0.113(4) 0.086(3) 0.061(3) -0.034(3) -0.020(3) -0.021(3) Cl8 0.0734(11) 0.0738(11) 0.0842(12) -0.0194(9) -0.0163(9) -0.0296(9) Cl7 0.270(4) 0.0540(11) 0.0967(17) -0.0142(11) -0.038(2) -0.0420(17) C1S 0.077(5) 0.065(4) 0.071(4) -0.026(4) -0.008(4) -0.017(4) _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 Fe1 O3 2.000(3) . ? Fe1 O1 2.005(3) . ? Fe1 O4 2.015(3) . ? Fe1 O2 2.033(3) . ? Fe1 Cl1 2.3433(11) . ? Fe1 Cl2 2.3495(10) . ? Fe2 C6 2.018(4) . ? Fe2 C1 2.022(4) . ? Fe2 C2 2.028(5) . ? Fe2 C10 2.038(4) . ? Fe2 C7 2.039(5) . ? Fe2 C3 2.047(5) . ? Fe2 C8 2.047(5) . ? Fe2 C5 2.048(5) . ? Fe2 C9 2.049(4) . ? Fe2 C4 2.050(5) . ? Fe3 C11 2.019(4) . ? Fe3 C16 2.022(4) . ? Fe3 C17 2.028(5) . ? Fe3 C18 2.036(4) . ? Fe3 C12 2.041(5) . ? Fe3 C19 2.042(5) . ? Fe3 C20 2.046(4) . ? Fe3 C13 2.047(5) . ? Fe3 C15 2.049(5) . ? Fe3 C14 2.058(5) . ? Fe4 O7 1.998(3) . ? Fe4 O5 2.028(3) . ? Fe4 O8 2.031(3) . ? Fe4 O6 2.038(3) . ? Fe4 Cl4 2.3244(11) . ? Fe4 Cl3 2.3419(10) . ? Fe5 C26 2.018(4) . ? Fe5 C21 2.019(4) . ? Fe5 C22 2.025(4) . ? Fe5 C27 2.031(5) . ? Fe5 C30 2.040(5) . ? Fe5 C25 2.042(4) . ? Fe5 C24 2.044(5) . ? Fe5 C28 2.048(5) . ? Fe5 C23 2.049(5) . ? Fe5 C29 2.050(5) . ? Fe6 C36 2.014(4) . ? Fe6 C37 2.028(5) . ? Fe6 C31 2.029(4) . ? Fe6 C35 2.043(4) . ? Fe6 C32 2.043(4) . ? Fe6 C40 2.046(5) . ? Fe6 C39 2.049(5) . ? Fe6 C33 2.052(5) . ? Fe6 C38 2.053(5) . ? Fe6 C34 2.059(5) . ? P1 O1 1.500(3) . ? P1 C1 1.775(4) . ? P1 C1A 1.792(4) . ? P1 C1B 1.807(4) . ? P2 O2 1.493(3) . ? P2 C6 1.776(4) . ? P2 C1C 1.797(4) . ? P2 C1D 1.809(4) . ? P3 O3 1.495(3) . ? P3 C11 1.765(4) . ? P3 C1E 1.797(4) . ? P3 C1F 1.805(4) . ? P4 O4 1.494(3) . ? P4 C16 1.772(4) . ? P4 C1H 1.791(4) . ? P4 C1G 1.798(4) . ? P5 O5 1.499(3) . ? P5 C21 1.769(4) . ? P5 C1J 1.797(4) . ? P5 C1I 1.799(4) . ? P6 O6 1.496(3) . ? P6 C26 1.773(4) . ? P6 C1L 1.800(4) . ? P6 C1K 1.804(4) . ? P7 O7 1.501(3) . ? P7 C31 1.761(4) . ? P7 C1N 1.789(4) . ? P7 C1M 1.802(4) . ? P8 O8 1.495(3) . ? P8 C36 1.781(4) . ? P8 C1P 1.801(5) . ? P8 C1U 1.806(4) . ? C1 C2 1.433(6) . ? C1 C5 1.440(6) . ? C2 C3 1.416(7) . ? C3 C4 1.408(8) . ? C4 C5 1.415(7) . ? C6 C10 1.425(6) . ? C6 C7 1.429(6) . ? C7 C8 1.414(7) . ? C8 C9 1.408(7) . ? C9 C10 1.429(6) . ? C11 C12 1.433(6) . ? C11 C15 1.434(7) . ? C12 C13 1.424(8) . ? C13 C14 1.415(9) . ? C14 C15 1.423(7) . ? C16 C20 1.426(6) . ? C16 C17 1.441(6) . ? C17 C18 1.421(7) . ? C18 C19 1.422(7) . ? C19 C20 1.413(6) . ? C21 C22 1.434(6) . ? C21 C25 1.436(6) . ? C22 C23 1.409(6) . ? C23 C24 1.411(7) . ? C24 C25 1.412(6) . ? C26 C30 1.422(6) . ? C26 C27 1.426(7) . ? C27 C28 1.428(6) . ? C28 C29 1.391(7) . ? C29 C30 1.423(7) . ? C31 C35 1.436(6) . ? C31 C32 1.442(6) . ? C32 C33 1.414(7) . ? C33 C34 1.424(7) . ? C34 C35 1.419(6) . ? C36 C40 1.426(6) . ? C36 C37 1.434(7) . ? C37 C38 1.409(7) . ? C38 C39 1.397(8) . ? C39 C40 1.413(7) . ? C1A C2A 1.394(6) . ? C1A C6A 1.403(6) . ? C2A C3A 1.386(6) . ? C3A C4A 1.380(7) . ? C4A C5A 1.373(8) . ? C5A C6A 1.373(7) . ? C1B C6B 1.389(6) . ? C1B C2B 1.391(6) . ? C2B C3B 1.387(7) . ? C3B C4B 1.353(7) . ? C4B C5B 1.373(7) . ? C5B C6B 1.386(6) . ? C1C C6C 1.390(6) . ? C1C C2C 1.399(6) . ? C2C C3C 1.377(6) . ? C3C C4C 1.386(7) . ? C4C C5C 1.372(7) . ? C5C C6C 1.379(6) . ? C1D C2D 1.384(7) . ? C1D C6D 1.386(7) . ? C2D C3D 1.398(8) . ? C3D C4D 1.358(9) . ? C4D C5D 1.353(8) . ? C5D C6D 1.391(6) . ? C1E C6E 1.385(6) . ? C1E C2E 1.390(6) . ? C2E C3E 1.382(6) . ? C3E C4E 1.383(7) . ? C4E C5E 1.375(7) . ? C5E C6E 1.376(7) . ? C1F C2F 1.386(6) . ? C1F C6F 1.391(6) . ? C2F C3F 1.386(6) . ? C3F C4F 1.367(7) . ? C4F C5F 1.390(8) . ? C5F C6F 1.382(7) . ? C1G C6G 1.383(6) . ? C1G C2G 1.394(6) . ? C2G C3G 1.384(7) . ? C3G C4G 1.376(8) . ? C4G C5G 1.346(8) . ? C5G C6G 1.382(7) . ? C1H C2H 1.385(6) . ? C1H C6H 1.395(6) . ? C2H C3H 1.390(6) . ? C3H C4H 1.378(6) . ? C4H C5H 1.366(7) . ? C5H C6H 1.381(6) . ? C1I C6I 1.391(6) . ? C1I C2I 1.394(6) . ? C2I C3I 1.379(7) . ? C3I C4I 1.341(9) . ? C4I C5I 1.397(8) . ? C5I C6I 1.397(6) . ? C1J C6J 1.378(6) . ? C1J C2J 1.392(6) . ? C2J C3J 1.375(7) . ? C3J C4J 1.366(8) . ? C4J C5J 1.360(8) . ? C5J C6J 1.387(7) . ? C1K C6K 1.387(6) . ? C1K C2K 1.393(6) . ? C2K C3K 1.394(7) . ? C3K C4K 1.363(8) . ? C4K C5K 1.370(8) . ? C5K C6K 1.391(7) . ? C1L C6L 1.372(7) . ? C1L C2L 1.395(6) . ? C2L C3L 1.382(7) . ? C3L C4L 1.353(9) . ? C4L C5L 1.364(8) . ? C5L C6L 1.401(7) . ? C1M C6M 1.380(6) . ? C1M C2M 1.392(6) . ? C2M C3M 1.392(7) . ? C3M C4M 1.383(8) . ? C4M C5M 1.361(7) . ? C5M C6M 1.392(6) . ? C1N C2N 1.390(6) . ? C1N C6N 1.404(6) . ? C2N C3N 1.403(7) . ? C3N C4N 1.359(9) . ? C4N C5N 1.385(9) . ? C5N C6N 1.372(7) . ? C1P C2P 1.383(7) . ? C1P C6P 1.397(7) . ? C2P C3P 1.376(7) . ? C3P C4P 1.371(10) . ? C4P C5P 1.360(10) . ? C5P C6P 1.400(8) . ? C1U C2U 1.366(6) . ? C1U C6U 1.373(7) . ? C2U C3U 1.400(6) . ? C3U C4U 1.382(8) . ? C4U C5U 1.361(9) . ? C5U C6U 1.383(7) . ? Cl5 O9 1.441(6) . ? Cl5 O11 1.463(7) . ? Cl5 O10 1.467(7) . ? Cl5 O12 1.477(8) . ? Cl6 O13 1.391(4) . ? Cl6 O14 1.400(4) . ? Cl6 O15 1.417(4) . ? Cl6 O16 1.450(5) . ? Cl8 C1S 1.747(7) . ? Cl7 C1S 1.720(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe1 O1 177.99(11) . . ? O3 Fe1 O4 91.92(11) . . ? O1 Fe1 O4 87.61(11) . . ? O3 Fe1 O2 88.35(11) . . ? O1 Fe1 O2 92.20(11) . . ? O4 Fe1 O2 177.84(11) . . ? O3 Fe1 Cl1 90.13(8) . . ? O1 Fe1 Cl1 91.82(8) . . ? O4 Fe1 Cl1 89.88(8) . . ? O2 Fe1 Cl1 87.97(8) . . ? O3 Fe1 Cl2 88.15(8) . . ? O1 Fe1 Cl2 89.91(8) . . ? O4 Fe1 Cl2 91.94(8) . . ? O2 Fe1 Cl2 90.21(8) . . ? Cl1 Fe1 Cl2 177.53(4) . . ? C6 Fe2 C1 127.34(16) . . ? C6 Fe2 C2 165.08(17) . . ? C1 Fe2 C2 41.45(17) . . ? C6 Fe2 C10 41.15(16) . . ? C1 Fe2 C10 108.04(16) . . ? C2 Fe2 C10 126.28(18) . . ? C6 Fe2 C7 41.24(16) . . ? C1 Fe2 C7 165.27(18) . . ? C2 Fe2 C7 151.82(18) . . ? C10 Fe2 C7 69.21(19) . . ? C6 Fe2 C3 153.5(2) . . ? C1 Fe2 C3 68.92(18) . . ? C2 Fe2 C3 40.68(19) . . ? C10 Fe2 C3 163.3(2) . . ? C7 Fe2 C3 118.0(2) . . ? C6 Fe2 C8 68.38(18) . . ? C1 Fe2 C8 153.2(2) . . ? C2 Fe2 C8 117.9(2) . . ? C10 Fe2 C8 68.24(19) . . ? C7 Fe2 C8 40.5(2) . . ? C3 Fe2 C8 106.6(2) . . ? C6 Fe2 C5 108.83(18) . . ? C1 Fe2 C5 41.43(17) . . ? C2 Fe2 C5 69.2(2) . . ? C10 Fe2 C5 121.24(18) . . ? C7 Fe2 C5 126.6(2) . . ? C3 Fe2 C5 68.1(2) . . ? C8 Fe2 C5 163.4(2) . . ? C6 Fe2 C9 68.91(18) . . ? C1 Fe2 C9 119.41(19) . . ? C2 Fe2 C9 106.5(2) . . ? C10 Fe2 C9 40.94(17) . . ? C7 Fe2 C9 68.6(2) . . ? C3 Fe2 C9 125.0(2) . . ? C8 Fe2 C9 40.2(2) . . ? C5 Fe2 C9 155.65(18) . . ? C6 Fe2 C4 120.2(2) . . ? C1 Fe2 C4 68.96(18) . . ? C2 Fe2 C4 68.5(2) . . ? C10 Fe2 C4 155.6(2) . . ? C7 Fe2 C4 107.2(2) . . ? C3 Fe2 C4 40.2(2) . . ? C8 Fe2 C4 125.6(2) . . ? C5 Fe2 C4 40.40(19) . . ? C9 Fe2 C4 162.1(2) . . ? C11 Fe3 C16 125.94(16) . . ? C11 Fe3 C17 162.99(18) . . ? C16 Fe3 C17 41.70(16) . . ? C11 Fe3 C18 155.5(2) . . ? C16 Fe3 C18 69.23(17) . . ? C17 Fe3 C18 40.94(19) . . ? C11 Fe3 C12 41.33(17) . . ? C16 Fe3 C12 163.22(19) . . ? C17 Fe3 C12 153.53(18) . . ? C18 Fe3 C12 118.8(2) . . ? C11 Fe3 C19 121.3(2) . . ? C16 Fe3 C19 68.99(17) . . ? C17 Fe3 C19 69.1(2) . . ? C18 Fe3 C19 40.8(2) . . ? C12 Fe3 C19 106.7(2) . . ? C11 Fe3 C20 109.01(17) . . ? C16 Fe3 C20 41.03(16) . . ? C17 Fe3 C20 69.25(18) . . ? C18 Fe3 C20 68.48(18) . . ? C12 Fe3 C20 125.4(2) . . ? C19 Fe3 C20 40.46(17) . . ? C11 Fe3 C13 68.79(19) . . ? C16 Fe3 C13 155.1(2) . . ? C17 Fe3 C13 118.4(2) . . ? C18 Fe3 C13 105.5(2) . . ? C12 Fe3 C13 40.8(2) . . ? C19 Fe3 C13 123.7(2) . . ? C20 Fe3 C13 161.5(2) . . ? C11 Fe3 C15 41.29(19) . . ? C16 Fe3 C15 108.28(18) . . ? C17 Fe3 C15 124.5(2) . . ? C18 Fe3 C15 160.6(2) . . ? C12 Fe3 C15 69.2(2) . . ? C19 Fe3 C15 157.80(19) . . ? C20 Fe3 C15 123.08(17) . . ? C13 Fe3 C15 68.2(2) . . ? C11 Fe3 C14 68.9(2) . . ? C16 Fe3 C14 120.9(2) . . ? C17 Fe3 C14 105.9(2) . . ? C18 Fe3 C14 123.0(2) . . ? C12 Fe3 C14 68.7(3) . . ? C19 Fe3 C14 160.1(2) . . ? C20 Fe3 C14 157.6(2) . . ? C13 Fe3 C14 40.3(2) . . ? C15 Fe3 C14 40.55(19) . . ? O7 Fe4 O5 178.02(11) . . ? O7 Fe4 O8 91.82(12) . . ? O5 Fe4 O8 87.81(11) . . ? O7 Fe4 O6 87.64(11) . . ? O5 Fe4 O6 92.73(11) . . ? O8 Fe4 O6 179.46(11) . . ? O7 Fe4 Cl4 89.72(8) . . ? O5 Fe4 Cl4 88.34(8) . . ? O8 Fe4 Cl4 89.83(8) . . ? O6 Fe4 Cl4 90.16(8) . . ? O7 Fe4 Cl3 90.74(8) . . ? O5 Fe4 Cl3 91.20(8) . . ? O8 Fe4 Cl3 89.43(8) . . ? O6 Fe4 Cl3 90.58(8) . . ? Cl4 Fe4 Cl3 179.15(5) . . ? C26 Fe5 C21 126.11(17) . . ? C26 Fe5 C22 163.52(18) . . ? C21 Fe5 C22 41.53(17) . . ? C26 Fe5 C27 41.24(19) . . ? C21 Fe5 C27 163.18(17) . . ? C22 Fe5 C27 153.49(19) . . ? C26 Fe5 C30 41.03(17) . . ? C21 Fe5 C30 108.48(18) . . ? C22 Fe5 C30 125.38(18) . . ? C27 Fe5 C30 69.1(2) . . ? C26 Fe5 C25 108.49(17) . . ? C21 Fe5 C25 41.42(16) . . ? C22 Fe5 C25 69.34(18) . . ? C27 Fe5 C25 124.82(18) . . ? C30 Fe5 C25 122.61(18) . . ? C26 Fe5 C24 121.17(18) . . ? C21 Fe5 C24 68.82(18) . . ? C22 Fe5 C24 68.47(19) . . ? C27 Fe5 C24 106.7(2) . . ? C30 Fe5 C24 157.34(19) . . ? C25 Fe5 C24 40.43(18) . . ? C26 Fe5 C28 68.83(19) . . ? C21 Fe5 C28 155.00(19) . . ? C22 Fe5 C28 118.64(19) . . ? C27 Fe5 C28 40.98(18) . . ? C30 Fe5 C28 68.4(2) . . ? C25 Fe5 C28 161.3(2) . . ? C24 Fe5 C28 123.9(2) . . ? C26 Fe5 C23 155.23(19) . . ? C21 Fe5 C23 68.74(18) . . ? C22 Fe5 C23 40.46(18) . . ? C27 Fe5 C23 119.0(2) . . ? C30 Fe5 C23 161.51(19) . . ? C25 Fe5 C23 68.23(19) . . ? C24 Fe5 C23 40.32(19) . . ? C28 Fe5 C23 106.0(2) . . ? C26 Fe5 C29 68.38(18) . . ? C21 Fe5 C29 121.69(19) . . ? C22 Fe5 C29 107.20(19) . . ? C27 Fe5 C29 68.1(2) . . ? C30 Fe5 C29 40.72(19) . . ? C25 Fe5 C29 158.1(2) . . ? C24 Fe5 C29 160.1(2) . . ? C28 Fe5 C29 39.7(2) . . ? C23 Fe5 C29 124.0(2) . . ? C36 Fe6 C37 41.56(18) . . ? C36 Fe6 C31 124.77(17) . . ? C37 Fe6 C31 160.77(18) . . ? C36 Fe6 C35 107.33(17) . . ? C37 Fe6 C35 122.39(19) . . ? C31 Fe6 C35 41.29(16) . . ? C36 Fe6 C32 162.40(19) . . ? C37 Fe6 C32 154.98(18) . . ? C31 Fe6 C32 41.49(16) . . ? C35 Fe6 C32 69.38(17) . . ? C36 Fe6 C40 41.13(18) . . ? C37 Fe6 C40 69.0(2) . . ? C31 Fe6 C40 109.67(19) . . ? C35 Fe6 C40 124.00(19) . . ? C32 Fe6 C40 125.42(19) . . ? C36 Fe6 C39 68.37(18) . . ? C37 Fe6 C39 67.8(2) . . ? C31 Fe6 C39 124.4(2) . . ? C35 Fe6 C39 160.6(2) . . ? C32 Fe6 C39 108.65(19) . . ? C40 Fe6 C39 40.4(2) . . ? C36 Fe6 C33 155.9(2) . . ? C37 Fe6 C33 119.2(2) . . ? C31 Fe6 C33 68.66(17) . . ? C35 Fe6 C33 68.43(19) . . ? C32 Fe6 C33 40.41(19) . . ? C40 Fe6 C33 160.5(2) . . ? C39 Fe6 C33 123.4(2) . . ? C36 Fe6 C38 68.65(19) . . ? C37 Fe6 C38 40.4(2) . . ? C31 Fe6 C38 158.4(2) . . ? C35 Fe6 C38 158.1(2) . . ? C32 Fe6 C38 120.96(19) . . ? C40 Fe6 C38 68.0(2) . . ? C39 Fe6 C38 39.8(2) . . ? C33 Fe6 C38 106.0(2) . . ? C36 Fe6 C34 120.9(2) . . ? C37 Fe6 C34 105.1(2) . . ? C31 Fe6 C34 68.72(17) . . ? C35 Fe6 C34 40.49(18) . . ? C32 Fe6 C34 68.57(19) . . ? C40 Fe6 C34 158.4(2) . . ? C39 Fe6 C34 158.3(2) . . ? C33 Fe6 C34 40.6(2) . . ? C38 Fe6 C34 121.7(2) . . ? O1 P1 C1 110.29(18) . . ? O1 P1 C1A 110.91(17) . . ? C1 P1 C1A 107.49(19) . . ? O1 P1 C1B 110.58(17) . . ? C1 P1 C1B 106.09(18) . . ? C1A P1 C1B 111.32(19) . . ? O2 P2 C6 113.00(17) . . ? O2 P2 C1C 110.87(18) . . ? C6 P2 C1C 104.34(19) . . ? O2 P2 C1D 110.44(19) . . ? C6 P2 C1D 108.14(19) . . ? C1C P2 C1D 109.8(2) . . ? O3 P3 C11 113.68(18) . . ? O3 P3 C1E 109.46(17) . . ? C11 P3 C1E 108.0(2) . . ? O3 P3 C1F 112.01(17) . . ? C11 P3 C1F 105.43(19) . . ? C1E P3 C1F 108.03(19) . . ? O4 P4 C16 111.34(18) . . ? O4 P4 C1H 111.56(18) . . ? C16 P4 C1H 106.33(18) . . ? O4 P4 C1G 111.01(18) . . ? C16 P4 C1G 109.3(2) . . ? C1H P4 C1G 107.13(19) . . ? O5 P5 C21 113.33(18) . . ? O5 P5 C1J 112.12(18) . . ? C21 P5 C1J 105.79(19) . . ? O5 P5 C1I 110.56(18) . . ? C21 P5 C1I 106.72(19) . . ? C1J P5 C1I 108.0(2) . . ? O6 P6 C26 112.80(18) . . ? O6 P6 C1L 111.9(2) . . ? C26 P6 C1L 104.40(19) . . ? O6 P6 C1K 110.94(18) . . ? C26 P6 C1K 105.2(2) . . ? C1L P6 C1K 111.2(2) . . ? O7 P7 C31 112.45(18) . . ? O7 P7 C1N 108.83(18) . . ? C31 P7 C1N 109.6(2) . . ? O7 P7 C1M 113.25(18) . . ? C31 P7 C1M 105.62(19) . . ? C1N P7 C1M 106.9(2) . . ? O8 P8 C36 113.92(18) . . ? O8 P8 C1P 109.8(2) . . ? C36 P8 C1P 106.5(2) . . ? O8 P8 C1U 111.64(19) . . ? C36 P8 C1U 105.0(2) . . ? C1P P8 C1U 109.8(2) . . ? P1 O1 Fe1 172.06(18) . . ? P2 O2 Fe1 166.02(18) . . ? P3 O3 Fe1 163.74(19) . . ? P4 O4 Fe1 168.81(18) . . ? P5 O5 Fe4 161.11(18) . . ? P6 O6 Fe4 168.26(18) . . ? P7 O7 Fe4 161.56(18) . . ? P8 O8 Fe4 165.26(18) . . ? C2 C1 C5 107.2(4) . . ? C2 C1 P1 130.0(3) . . ? C5 C1 P1 122.6(3) . . ? C2 C1 Fe2 69.5(2) . . ? C5 C1 Fe2 70.3(2) . . ? P1 C1 Fe2 122.1(2) . . ? C3 C2 C1 107.8(4) . . ? C3 C2 Fe2 70.4(3) . . ? C1 C2 Fe2 69.1(2) . . ? C4 C3 C2 108.7(4) . . ? C4 C3 Fe2 70.0(3) . . ? C2 C3 Fe2 69.0(2) . . ? C3 C4 C5 108.6(4) . . ? C3 C4 Fe2 69.8(3) . . ? C5 C4 Fe2 69.8(3) . . ? C4 C5 C1 107.7(4) . . ? C4 C5 Fe2 69.8(3) . . ? C1 C5 Fe2 68.3(2) . . ? C10 C6 C7 108.4(4) . . ? C10 C6 P2 121.6(3) . . ? C7 C6 P2 130.0(3) . . ? C10 C6 Fe2 70.2(2) . . ? C7 C6 Fe2 70.2(2) . . ? P2 C6 Fe2 126.0(2) . . ? C8 C7 C6 106.9(4) . . ? C8 C7 Fe2 70.1(3) . . ? C6 C7 Fe2 68.6(2) . . ? C9 C8 C7 109.5(4) . . ? C9 C8 Fe2 70.0(3) . . ? C7 C8 Fe2 69.4(3) . . ? C8 C9 C10 107.7(4) . . ? C8 C9 Fe2 69.8(3) . . ? C10 C9 Fe2 69.1(2) . . ? C6 C10 C9 107.4(4) . . ? C6 C10 Fe2 68.7(2) . . ? C9 C10 Fe2 70.0(2) . . ? C12 C11 C15 108.2(4) . . ? C12 C11 P3 127.9(4) . . ? C15 C11 P3 123.9(3) . . ? C12 C11 Fe3 70.2(3) . . ? C15 C11 Fe3 70.5(2) . . ? P3 C11 Fe3 124.8(2) . . ? C13 C12 C11 107.0(5) . . ? C13 C12 Fe3 69.8(3) . . ? C11 C12 Fe3 68.5(2) . . ? C14 C13 C12 109.1(5) . . ? C14 C13 Fe3 70.3(3) . . ? C12 C13 Fe3 69.4(3) . . ? C13 C14 C15 108.1(5) . . ? C13 C14 Fe3 69.4(3) . . ? C15 C14 Fe3 69.4(3) . . ? C14 C15 C11 107.6(5) . . ? C14 C15 Fe3 70.1(3) . . ? C11 C15 Fe3 68.2(2) . . ? C20 C16 C17 107.7(4) . . ? C20 C16 P4 122.6(3) . . ? C17 C16 P4 129.8(3) . . ? C20 C16 Fe3 70.4(2) . . ? C17 C16 Fe3 69.4(2) . . ? P4 C16 Fe3 125.3(2) . . ? C18 C17 C16 107.3(4) . . ? C18 C17 Fe3 69.8(3) . . ? C16 C17 Fe3 68.9(2) . . ? C17 C18 C19 108.5(4) . . ? C17 C18 Fe3 69.2(3) . . ? C19 C18 Fe3 69.8(3) . . ? C20 C19 C18 108.2(4) . . ? C20 C19 Fe3 69.9(2) . . ? C18 C19 Fe3 69.4(3) . . ? C19 C20 C16 108.3(4) . . ? C19 C20 Fe3 69.6(2) . . ? C16 C20 Fe3 68.6(2) . . ? C22 C21 C25 107.4(4) . . ? C22 C21 P5 129.5(3) . . ? C25 C21 P5 123.1(3) . . ? C22 C21 Fe5 69.5(2) . . ? C25 C21 Fe5 70.1(2) . . ? P5 C21 Fe5 127.3(2) . . ? C23 C22 C21 107.8(4) . . ? C23 C22 Fe5 70.7(3) . . ? C21 C22 Fe5 69.0(2) . . ? C22 C23 C24 108.6(4) . . ? C22 C23 Fe5 68.8(3) . . ? C24 C23 Fe5 69.6(3) . . ? C23 C24 C25 108.8(4) . . ? C23 C24 Fe5 70.0(3) . . ? C25 C24 Fe5 69.7(2) . . ? C24 C25 C21 107.5(4) . . ? C24 C25 Fe5 69.9(3) . . ? C21 C25 Fe5 68.4(2) . . ? C30 C26 C27 108.3(4) . . ? C30 C26 P6 123.1(4) . . ? C27 C26 P6 128.6(3) . . ? C30 C26 Fe5 70.3(2) . . ? C27 C26 Fe5 69.9(3) . . ? P6 C26 Fe5 124.0(2) . . ? C26 C27 C28 107.3(4) . . ? C26 C27 Fe5 68.9(2) . . ? C28 C27 Fe5 70.1(3) . . ? C29 C28 C27 108.2(4) . . ? C29 C28 Fe5 70.2(3) . . ? C27 C28 Fe5 68.9(3) . . ? C28 C29 C30 109.3(4) . . ? C28 C29 Fe5 70.1(3) . . ? C30 C29 Fe5 69.3(2) . . ? C26 C30 C29 106.9(4) . . ? C26 C30 Fe5 68.7(2) . . ? C29 C30 Fe5 70.0(3) . . ? C35 C31 C32 107.8(4) . . ? C35 C31 P7 123.4(3) . . ? C32 C31 P7 128.8(3) . . ? C35 C31 Fe6 69.9(2) . . ? C32 C31 Fe6 69.8(2) . . ? P7 C31 Fe6 128.4(2) . . ? C33 C32 C31 107.3(4) . . ? C33 C32 Fe6 70.1(3) . . ? C31 C32 Fe6 68.7(2) . . ? C32 C33 C34 109.0(4) . . ? C32 C33 Fe6 69.5(2) . . ? C34 C33 Fe6 70.0(3) . . ? C35 C34 C33 108.1(4) . . ? C35 C34 Fe6 69.2(3) . . ? C33 C34 Fe6 69.5(3) . . ? C34 C35 C31 107.8(4) . . ? C34 C35 Fe6 70.4(3) . . ? C31 C35 Fe6 68.8(2) . . ? C40 C36 C37 107.7(4) . . ? C40 C36 P8 123.5(4) . . ? C37 C36 P8 128.8(4) . . ? C40 C36 Fe6 70.6(2) . . ? C37 C36 Fe6 69.8(2) . . ? P8 C36 Fe6 126.0(2) . . ? C38 C37 C36 107.6(5) . . ? C38 C37 Fe6 70.8(3) . . ? C36 C37 Fe6 68.7(2) . . ? C39 C38 C37 108.4(5) . . ? C39 C38 Fe6 69.9(3) . . ? C37 C38 Fe6 68.9(3) . . ? C38 C39 C40 109.3(5) . . ? C38 C39 Fe6 70.2(3) . . ? C40 C39 Fe6 69.7(3) . . ? C39 C40 C36 107.1(5) . . ? C39 C40 Fe6 70.0(3) . . ? C36 C40 Fe6 68.2(3) . . ? C2A C1A C6A 119.2(4) . . ? C2A C1A P1 118.6(3) . . ? C6A C1A P1 122.1(3) . . ? C3A C2A C1A 120.3(4) . . ? C4A C3A C2A 119.4(5) . . ? C5A C4A C3A 120.7(5) . . ? C4A C5A C6A 120.6(5) . . ? C5A C6A C1A 119.7(5) . . ? C6B C1B C2B 119.4(4) . . ? C6B C1B P1 116.3(3) . . ? C2B C1B P1 124.1(3) . . ? C3B C2B C1B 119.5(5) . . ? C4B C3B C2B 120.9(5) . . ? C3B C4B C5B 120.2(5) . . ? C4B C5B C6B 120.4(5) . . ? C5B C6B C1B 119.6(4) . . ? C6C C1C C2C 119.6(4) . . ? C6C C1C P2 119.6(3) . . ? C2C C1C P2 120.8(3) . . ? C3C C2C C1C 119.9(4) . . ? C2C C3C C4C 120.1(5) . . ? C5C C4C C3C 120.0(4) . . ? C4C C5C C6C 120.7(4) . . ? C5C C6C C1C 119.7(4) . . ? C2D C1D C6D 120.1(4) . . ? C2D C1D P2 121.9(4) . . ? C6D C1D P2 117.9(3) . . ? C1D C2D C3D 118.1(5) . . ? C4D C3D C2D 121.4(6) . . ? C5D C4D C3D 120.5(5) . . ? C4D C5D C6D 119.9(6) . . ? C1D C6D C5D 120.0(5) . . ? C6E C1E C2E 119.6(4) . . ? C6E C1E P3 121.2(3) . . ? C2E C1E P3 119.3(3) . . ? C3E C2E C1E 119.8(4) . . ? C2E C3E C4E 120.0(4) . . ? C5E C4E C3E 120.2(5) . . ? C4E C5E C6E 120.1(5) . . ? C5E C6E C1E 120.3(4) . . ? C2F C1F C6F 120.3(4) . . ? C2F C1F P3 119.3(3) . . ? C6F C1F P3 120.4(3) . . ? C1F C2F C3F 120.2(4) . . ? C4F C3F C2F 119.5(4) . . ? C3F C4F C5F 120.9(4) . . ? C6F C5F C4F 120.1(5) . . ? C5F C6F C1F 119.1(5) . . ? C6G C1G C2G 119.4(4) . . ? C6G C1G P4 118.5(3) . . ? C2G C1G P4 122.1(3) . . ? C3G C2G C1G 119.9(5) . . ? C4G C3G C2G 119.4(5) . . ? C5G C4G C3G 120.9(5) . . ? C4G C5G C6G 120.8(5) . . ? C5G C6G C1G 119.6(5) . . ? C2H C1H C6H 119.0(4) . . ? C2H C1H P4 118.7(3) . . ? C6H C1H P4 122.2(3) . . ? C1H C2H C3H 119.9(4) . . ? C4H C3H C2H 120.0(4) . . ? C5H C4H C3H 120.7(4) . . ? C4H C5H C6H 119.8(4) . . ? C5H C6H C1H 120.6(4) . . ? C6I C1I C2I 119.8(4) . . ? C6I C1I P5 119.2(3) . . ? C2I C1I P5 121.0(4) . . ? C3I C2I C1I 120.0(5) . . ? C4I C3I C2I 120.3(5) . . ? C3I C4I C5I 121.6(5) . . ? C4I C5I C6I 118.8(5) . . ? C1I C6I C5I 119.4(5) . . ? C6J C1J C2J 118.9(4) . . ? C6J C1J P5 120.1(3) . . ? C2J C1J P5 121.1(4) . . ? C3J C2J C1J 120.2(5) . . ? C4J C3J C2J 120.4(5) . . ? C5J C4J C3J 120.0(5) . . ? C4J C5J C6J 120.6(5) . . ? C1J C6J C5J 119.9(5) . . ? C6K C1K C2K 120.1(4) . . ? C6K C1K P6 116.8(3) . . ? C2K C1K P6 122.9(3) . . ? C1K C2K C3K 119.3(5) . . ? C4K C3K C2K 120.4(5) . . ? C3K C4K C5K 120.2(5) . . ? C4K C5K C6K 121.0(5) . . ? C1K C6K C5K 118.9(5) . . ? C6L C1L C2L 119.5(4) . . ? C6L C1L P6 119.9(3) . . ? C2L C1L P6 120.5(4) . . ? C3L C2L C1L 119.4(6) . . ? C4L C3L C2L 121.0(6) . . ? C3L C4L C5L 120.1(5) . . ? C4L C5L C6L 120.4(6) . . ? C1L C6L C5L 119.6(5) . . ? C6M C1M C2M 119.6(4) . . ? C6M C1M P7 121.3(3) . . ? C2M C1M P7 119.0(3) . . ? C1M C2M C3M 119.9(5) . . ? C4M C3M C2M 119.8(5) . . ? C5M C4M C3M 120.3(4) . . ? C4M C5M C6M 120.6(5) . . ? C1M C6M C5M 119.8(5) . . ? C2N C1N C6N 119.8(4) . . ? C2N C1N P7 122.0(3) . . ? C6N C1N P7 118.2(3) . . ? C1N C2N C3N 119.4(5) . . ? C4N C3N C2N 120.2(6) . . ? C3N C4N C5N 120.3(5) . . ? C6N C5N C4N 121.1(6) . . ? C5N C6N C1N 119.1(5) . . ? C2P C1P C6P 119.7(5) . . ? C2P C1P P8 118.1(4) . . ? C6P C1P P8 122.2(4) . . ? C3P C2P C1P 119.6(6) . . ? C4P C3P C2P 120.9(6) . . ? C5P C4P C3P 120.4(6) . . ? C4P C5P C6P 120.0(6) . . ? C1P C6P C5P 119.3(6) . . ? C2U C1U C6U 119.9(4) . . ? C2U C1U P8 119.4(3) . . ? C6U C1U P8 120.6(4) . . ? C1U C2U C3U 120.0(5) . . ? C4U C3U C2U 118.9(5) . . ? C5U C4U C3U 121.1(5) . . ? C4U C5U C6U 119.3(6) . . ? C1U C6U C5U 120.8(6) . . ? O9 Cl5 O11 105.5(5) . . ? O9 Cl5 O10 110.3(5) . . ? O11 Cl5 O10 107.9(4) . . ? O9 Cl5 O12 110.1(3) . . ? O11 Cl5 O12 110.2(4) . . ? O10 Cl5 O12 112.6(5) . . ? O13 Cl6 O14 111.9(3) . . ? O13 Cl6 O15 113.8(3) . . ? O14 Cl6 O15 111.1(3) . . ? O13 Cl6 O16 108.4(3) . . ? O14 Cl6 O16 105.2(3) . . ? O15 Cl6 O16 105.8(3) . . ? Cl7 C1S Cl8 112.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.138 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.113 data_Cpd6 _database_code_depnum_ccdc_archive 'CCDC 823893' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H66 Cl Fe3 I4 O6 P4' _chemical_formula_weight 1861.73 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' O O 0.0106 0.0060 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.6672(16) _cell_length_b 14.5893(7) _cell_length_c 18.7987(9) _cell_angle_alpha 90.00 _cell_angle_beta 121.3280(10) _cell_angle_gamma 90.00 _cell_volume 7184.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3652 _exptl_absorpt_coefficient_mu 2.493 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3162 _exptl_absorpt_correction_T_max 0.5218 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20457 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6314 _reflns_number_gt 5452 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1222P)^2^+93.7319P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6314 _refine_ls_number_parameters 418 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.2056 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.29103(13) 0.2500 0.0388(4) Uani 1 2 d S . . Fe2 Fe 0.51294(4) 0.25764(6) 0.51440(6) 0.0290(3) Uani 1 1 d . . . I1 I 0.5000 0.48135(6) 0.2500 0.0601(3) Uani 1 2 d S . . P1 P 0.41503(6) 0.28652(11) 0.32032(10) 0.0256(4) Uani 1 1 d . . . P2 P 0.40357(6) 0.23835(12) 0.04584(11) 0.0290(4) Uani 1 1 d . . . O1 O 0.44704(17) 0.2666(3) 0.2833(3) 0.0295(10) Uani 1 1 d . . . O2 O 0.44280(19) 0.2662(4) 0.1322(3) 0.0340(11) Uani 1 1 d . . . C1 C 0.4535(3) 0.3298(5) 0.4235(4) 0.0320(15) Uani 1 1 d . . . C2 C 0.4479(3) 0.3185(6) 0.4945(5) 0.0435(19) Uani 1 1 d . . . H2 H 0.4192 0.2879 0.4948 0.052 Uiso 1 1 calc R . . C3 C 0.4905(4) 0.3608(6) 0.5634(5) 0.051(2) Uani 1 1 d . . . H3 H 0.4972 0.3626 0.6209 0.061 Uiso 1 1 calc R . . C4 C 0.5227(3) 0.3960(5) 0.5382(5) 0.047(2) Uani 1 1 d . . . H4 H 0.5557 0.4275 0.5744 0.057 Uiso 1 1 calc R . . C5 C 0.4998(3) 0.3789(4) 0.4506(4) 0.0339(15) Uani 1 1 d . . . H5 H 0.5139 0.3967 0.4157 0.041 Uiso 1 1 calc R . . C6 C 0.5203(3) 0.1391(5) 0.4632(5) 0.0356(16) Uani 1 1 d . . . H6 H 0.5013 0.1235 0.4032 0.043 Uiso 1 1 calc R . . C7 C 0.5678(3) 0.1882(5) 0.5066(4) 0.0303(14) Uani 1 1 d . . . C8 C 0.5810(3) 0.1964(5) 0.5926(5) 0.0386(17) Uani 1 1 d . . . H8 H 0.6118 0.2266 0.6382 0.046 Uiso 1 1 calc R . . C9 C 0.5428(3) 0.1539(6) 0.5995(5) 0.048(2) Uani 1 1 d . . . H9 H 0.5416 0.1501 0.6510 0.058 Uiso 1 1 calc R . . C10 C 0.5052(3) 0.1180(5) 0.5204(6) 0.047(2) Uani 1 1 d . . . H10 H 0.4736 0.0854 0.5077 0.057 Uiso 1 1 calc R . . C1V C 0.3666(3) 0.3706(5) 0.2609(4) 0.0306(14) Uani 1 1 d . . . C2V C 0.3161(3) 0.3480(6) 0.2099(6) 0.051(2) Uani 1 1 d . . . H2V H 0.3054 0.2874 0.2088 0.061 Uiso 1 1 calc R . . C3V C 0.2802(3) 0.4147(7) 0.1594(6) 0.060(2) Uani 1 1 d . . . H3V H 0.2456 0.3989 0.1245 0.072 Uiso 1 1 calc R . . C4V C 0.2960(4) 0.5024(7) 0.1615(6) 0.055(2) Uani 1 1 d . . . H4V H 0.2725 0.5466 0.1257 0.066 Uiso 1 1 calc R . . C5V C 0.3449(4) 0.5266(6) 0.2145(7) 0.061(2) Uani 1 1 d . . . H5V H 0.3547 0.5883 0.2182 0.073 Uiso 1 1 calc R . . C6V C 0.3809(3) 0.4615(6) 0.2636(6) 0.047(2) Uani 1 1 d . . . H6V H 0.4151 0.4788 0.2989 0.057 Uiso 1 1 calc R . . C1W C 0.3827(3) 0.1847(5) 0.3231(4) 0.0332(15) Uani 1 1 d . . . C2W C 0.3903(3) 0.1044(5) 0.2914(5) 0.0416(18) Uani 1 1 d . . . H2W H 0.4115 0.1040 0.2690 0.050 Uiso 1 1 calc R . . C3W C 0.3661(4) 0.0245(6) 0.2932(6) 0.061(3) Uani 1 1 d . . . H3W H 0.3705 -0.0301 0.2712 0.073 Uiso 1 1 calc R . . C4W C 0.3363(4) 0.0249(8) 0.3265(7) 0.071(3) Uani 1 1 d . . . H4W H 0.3207 -0.0298 0.3282 0.085 Uiso 1 1 calc R . . C5W C 0.3283(4) 0.1035(8) 0.3576(7) 0.068(3) Uani 1 1 d . . . H5W H 0.3076 0.1026 0.3808 0.081 Uiso 1 1 calc R . . C6W C 0.3508(3) 0.1840(7) 0.3550(6) 0.050(2) Uani 1 1 d . . . H6W H 0.3445 0.2386 0.3747 0.060 Uiso 1 1 calc R . . C1Y C 0.3588(3) 0.1580(5) 0.0458(4) 0.0363(16) Uani 1 1 d . . . C2Y C 0.3625(3) 0.0662(6) 0.0358(6) 0.053(2) Uani 1 1 d . . . H2Y H 0.3867 0.0438 0.0239 0.063 Uiso 1 1 calc R . . C3Y C 0.3296(4) 0.0058(7) 0.0435(7) 0.067(3) Uani 1 1 d . . . H3Y H 0.3322 -0.0575 0.0372 0.081 Uiso 1 1 calc R . . C4Y C 0.2944(4) 0.0367(8) 0.0598(6) 0.066(3) Uani 1 1 d . . . H4Y H 0.2726 -0.0048 0.0647 0.079 Uiso 1 1 calc R . . C5Y C 0.2903(4) 0.1305(9) 0.0693(7) 0.074(3) Uani 1 1 d . . . H5Y H 0.2656 0.1526 0.0804 0.089 Uiso 1 1 calc R . . C6Y C 0.3225(4) 0.1904(7) 0.0623(7) 0.061(2) Uani 1 1 d . . . H6Y H 0.3198 0.2537 0.0688 0.073 Uiso 1 1 calc R . . C1Z C 0.3661(3) 0.3343(5) -0.0153(5) 0.0372(16) Uani 1 1 d . . . C2Z C 0.3269(3) 0.3222(7) -0.0976(5) 0.049(2) Uani 1 1 d . . . H2Z H 0.3191 0.2631 -0.1209 0.059 Uiso 1 1 calc R . . C3Z C 0.2996(4) 0.3970(9) -0.1452(7) 0.070(3) Uani 1 1 d . . . H3Z H 0.2730 0.3890 -0.2008 0.084 Uiso 1 1 calc R . . C4Z C 0.3117(5) 0.4832(10) -0.1104(9) 0.083(4) Uani 1 1 d . . . H4Z H 0.2941 0.5342 -0.1435 0.099 Uiso 1 1 calc R . . C5Z C 0.3485(5) 0.4962(7) -0.0289(10) 0.081(4) Uani 1 1 d . . . H5Z H 0.3550 0.5554 -0.0057 0.097 Uiso 1 1 calc R . . C6Z C 0.3769(3) 0.4212(6) 0.0202(7) 0.057(2) Uani 1 1 d . . . H6Z H 0.4028 0.4297 0.0761 0.069 Uiso 1 1 calc R . . I2 I 0.28252(3) 0.79014(5) 0.17351(5) 0.0704(3) Uani 1 1 d . . . I3 I 0.2500 0.7500 0.0000 0.0613(3) Uani 1 2 d S . . O1S O 0.4650(6) 0.1335(12) 0.7178(10) 0.099(6) Uani 0.50 1 d PD A -2 C1S C 0.4266(12) 0.2880(16) 0.6863(18) 0.128(8) Uani 0.50 1 d PD A -2 H1SA H 0.4579 0.3141 0.6939 0.193 Uiso 0.50 1 calc PR A -2 H1SB H 0.4273 0.2910 0.7384 0.193 Uiso 0.50 1 calc PR A -2 H1SC H 0.3976 0.3224 0.6440 0.193 Uiso 0.50 1 calc PR A -2 C2S C 0.4222(8) 0.1887(16) 0.6592(12) 0.128(8) Uani 0.50 1 d PD A -2 H2SA H 0.3908 0.1626 0.6524 0.154 Uiso 0.50 1 calc PR A -2 H2SB H 0.4195 0.1865 0.6049 0.154 Uiso 0.50 1 calc PR A -2 C3S C 0.4806(10) 0.0444(15) 0.7051(13) 0.128(8) Uani 0.50 1 d PD A -2 H3SA H 0.4826 0.0461 0.6548 0.154 Uiso 0.50 1 calc PR A -2 H3SB H 0.4547 -0.0011 0.6963 0.154 Uiso 0.50 1 calc PR A -2 C4S C 0.5320(10) 0.015(3) 0.7786(18) 0.128(8) Uani 0.50 1 d PD A -2 H4SA H 0.5429 -0.0411 0.7646 0.193 Uiso 0.50 1 calc PR A -2 H4SB H 0.5289 0.0042 0.8267 0.193 Uiso 0.50 1 calc PR A -2 H4SC H 0.5570 0.0627 0.7913 0.193 Uiso 0.50 1 calc PR A -2 Cl1 Cl 0.5000 -0.0631(5) 0.7500 0.1063(19) Uani 1 2 d S B 1 O1W O 0.4102(9) 0.1627(16) 0.5807(13) 0.118(8) Uani 0.50 1 d P C 1 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 Fe1 0.0213(7) 0.0702(11) 0.0208(7) 0.000 0.0081(6) 0.000 Fe2 0.0349(6) 0.0265(5) 0.0226(5) 0.0023(4) 0.0128(4) 0.0073(4) I1 0.0806(6) 0.0548(5) 0.0518(5) 0.000 0.0391(5) 0.000 P1 0.0225(8) 0.0268(8) 0.0258(8) 0.0033(7) 0.0113(7) 0.0041(6) P2 0.0239(8) 0.0327(9) 0.0229(9) 0.0002(7) 0.0069(7) -0.0048(7) O1 0.024(2) 0.035(2) 0.030(2) -0.001(2) 0.014(2) 0.0011(19) O2 0.032(3) 0.041(3) 0.022(2) -0.004(2) 0.009(2) -0.003(2) C1 0.039(4) 0.030(3) 0.029(3) 0.002(3) 0.019(3) 0.013(3) C2 0.047(4) 0.057(5) 0.036(4) 0.010(4) 0.028(4) 0.023(4) C3 0.064(5) 0.057(5) 0.029(4) -0.005(4) 0.021(4) 0.026(4) C4 0.055(5) 0.034(4) 0.035(4) -0.007(3) 0.011(4) 0.012(4) C5 0.039(4) 0.020(3) 0.033(4) -0.001(3) 0.012(3) 0.009(3) C6 0.036(4) 0.021(3) 0.043(4) -0.001(3) 0.016(3) 0.003(3) C7 0.031(3) 0.028(3) 0.027(3) 0.005(3) 0.012(3) 0.013(3) C8 0.041(4) 0.040(4) 0.027(4) 0.011(3) 0.013(3) 0.015(3) C9 0.059(5) 0.052(5) 0.039(4) 0.019(4) 0.029(4) 0.019(4) C10 0.055(5) 0.026(4) 0.068(6) 0.012(4) 0.037(5) 0.003(3) C1V 0.028(3) 0.036(4) 0.025(3) 0.004(3) 0.011(3) 0.008(3) C2V 0.042(4) 0.046(5) 0.053(5) 0.007(4) 0.017(4) 0.000(4) C3V 0.036(4) 0.068(6) 0.055(5) 0.010(5) 0.009(4) 0.011(4) C4V 0.051(5) 0.055(5) 0.056(5) 0.017(4) 0.025(5) 0.027(4) C5V 0.060(6) 0.035(4) 0.082(7) 0.012(4) 0.033(5) 0.015(4) C6V 0.038(4) 0.035(4) 0.061(5) -0.001(4) 0.020(4) 0.003(3) C1W 0.024(3) 0.034(4) 0.035(4) 0.007(3) 0.011(3) 0.002(3) C2W 0.028(4) 0.035(4) 0.047(4) 0.004(3) 0.009(3) 0.000(3) C3W 0.049(5) 0.037(5) 0.067(6) 0.010(4) 0.010(5) 0.001(4) C4W 0.046(5) 0.061(7) 0.082(7) 0.035(6) 0.017(5) -0.011(5) C5W 0.051(5) 0.080(8) 0.073(7) 0.034(6) 0.033(5) -0.003(5) C6W 0.036(4) 0.064(5) 0.054(5) 0.014(4) 0.027(4) 0.002(4) C1Y 0.029(3) 0.043(4) 0.026(3) 0.000(3) 0.006(3) -0.011(3) C2Y 0.042(4) 0.045(5) 0.066(6) 0.007(4) 0.025(4) -0.006(4) C3Y 0.070(7) 0.045(5) 0.076(7) 0.003(5) 0.030(6) -0.024(5) C4Y 0.061(6) 0.068(7) 0.061(6) 0.004(5) 0.027(5) -0.031(5) C5Y 0.064(6) 0.095(9) 0.079(7) 0.005(6) 0.047(6) -0.017(6) C6Y 0.068(6) 0.056(6) 0.076(7) -0.005(5) 0.049(6) -0.013(5) C1Z 0.026(3) 0.040(4) 0.041(4) 0.010(3) 0.015(3) 0.003(3) C2Z 0.037(4) 0.063(5) 0.040(4) 0.010(4) 0.014(4) 0.006(4) C3Z 0.052(6) 0.092(9) 0.052(6) 0.033(6) 0.017(5) 0.029(6) C4Z 0.067(7) 0.091(9) 0.102(10) 0.058(8) 0.052(7) 0.045(7) C5Z 0.073(7) 0.045(6) 0.124(11) 0.014(6) 0.050(8) 0.013(5) C6Z 0.045(5) 0.042(5) 0.074(6) -0.001(4) 0.024(5) 0.005(4) I2 0.0821(5) 0.0478(4) 0.0645(5) 0.0042(3) 0.0263(4) 0.0024(3) I3 0.0630(6) 0.0347(4) 0.0646(6) 0.0057(4) 0.0180(5) -0.0058(3) O1S 0.118(14) 0.102(14) 0.116(15) -0.013(12) 0.087(14) -0.005(11) C1S 0.090(10) 0.24(2) 0.071(9) 0.028(13) 0.056(8) 0.005(14) C2S 0.090(10) 0.24(2) 0.071(9) 0.028(13) 0.056(8) 0.005(14) C3S 0.090(10) 0.24(2) 0.071(9) 0.028(13) 0.056(8) 0.005(14) C4S 0.090(10) 0.24(2) 0.071(9) 0.028(13) 0.056(8) 0.005(14) Cl1 0.061(2) 0.198(6) 0.058(2) 0.000 0.030(2) 0.000 O1W 0.159(19) 0.125(16) 0.103(14) -0.011(12) 0.092(15) -0.079(15) _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 Fe1 O2 2.017(5) 2_655 ? Fe1 O2 2.017(5) . ? Fe1 O1 2.053(5) 2_655 ? Fe1 O1 2.053(5) . ? Fe1 I1 2.777(2) . ? Fe2 C1 2.027(7) . ? Fe2 C8 2.031(7) . ? Fe2 C2 2.032(7) . ? Fe2 C7 2.033(7) . ? Fe2 C9 2.041(8) . ? Fe2 C6 2.048(7) . ? Fe2 C5 2.056(7) . ? Fe2 C4 2.056(8) . ? Fe2 C3 2.060(8) . ? Fe2 C10 2.061(8) . ? P1 O1 1.497(5) . ? P1 C1 1.782(7) . ? P1 C1V 1.798(7) . ? P1 C1W 1.802(7) . ? P2 O2 1.490(5) . ? P2 C7 1.782(7) 2_655 ? P2 C1Z 1.796(7) . ? P2 C1Y 1.804(7) . ? C1 C5 1.425(11) . ? C1 C2 1.440(10) . ? C2 C3 1.416(13) . ? C3 C4 1.396(14) . ? C4 C5 1.437(11) . ? C6 C10 1.411(12) . ? C6 C7 1.436(10) . ? C7 C8 1.454(10) . ? C7 P2 1.782(7) 2_655 ? C8 C9 1.390(12) . ? C9 C10 1.425(13) . ? C1V C2V 1.373(11) . ? C1V C6V 1.389(11) . ? C2V C3V 1.404(13) . ? C3V C4V 1.362(15) . ? C4V C5V 1.346(14) . ? C5V C6V 1.382(12) . ? C1W C2W 1.387(11) . ? C1W C6W 1.389(11) . ? C2W C3W 1.394(12) . ? C3W C4W 1.349(16) . ? C4W C5W 1.365(17) . ? C5W C6W 1.375(14) . ? C1Y C2Y 1.365(12) . ? C1Y C6Y 1.387(13) . ? C2Y C3Y 1.402(13) . ? C3Y C4Y 1.343(16) . ? C4Y C5Y 1.395(17) . ? C5Y C6Y 1.375(14) . ? C1Z C6Z 1.390(12) . ? C1Z C2Z 1.392(11) . ? C2Z C3Z 1.384(13) . ? C3Z C4Z 1.377(19) . ? C4Z C5Z 1.363(19) . ? C5Z C6Z 1.404(14) . ? I2 I3 2.9316(8) . ? I3 I2 2.9316(8) 7_565 ? O1S C2S 1.444(5) . ? O1S C3S 1.447(5) . ? C1S C2S 1.518(5) . ? C3S C4S 1.521(5) . ? 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 O2 Fe1 O2 159.3(3) 2_655 . ? O2 Fe1 O1 85.95(19) 2_655 2_655 ? O2 Fe1 O1 90.48(19) . 2_655 ? O2 Fe1 O1 90.48(19) 2_655 . ? O2 Fe1 O1 85.95(19) . . ? O1 Fe1 O1 160.0(3) 2_655 . ? O2 Fe1 I1 100.33(16) 2_655 . ? O2 Fe1 I1 100.33(16) . . ? O1 Fe1 I1 99.99(14) 2_655 . ? O1 Fe1 I1 99.99(14) . . ? C1 Fe2 C8 166.8(3) . . ? C1 Fe2 C2 41.6(3) . . ? C8 Fe2 C2 150.0(3) . . ? C1 Fe2 C7 127.8(3) . . ? C8 Fe2 C7 41.9(3) . . ? C2 Fe2 C7 166.9(3) . . ? C1 Fe2 C9 152.4(3) . . ? C8 Fe2 C9 39.9(3) . . ? C2 Fe2 C9 117.8(3) . . ? C7 Fe2 C9 68.7(3) . . ? C1 Fe2 C6 108.2(3) . . ? C8 Fe2 C6 69.2(3) . . ? C2 Fe2 C6 128.3(3) . . ? C7 Fe2 C6 41.2(3) . . ? C9 Fe2 C6 68.2(3) . . ? C1 Fe2 C5 40.9(3) . . ? C8 Fe2 C5 128.1(3) . . ? C2 Fe2 C5 68.9(3) . . ? C7 Fe2 C5 107.8(3) . . ? C9 Fe2 C5 165.3(3) . . ? C6 Fe2 C5 119.2(3) . . ? C1 Fe2 C4 68.8(3) . . ? C8 Fe2 C4 107.2(3) . . ? C2 Fe2 C4 68.2(4) . . ? C7 Fe2 C4 118.2(3) . . ? C9 Fe2 C4 127.1(4) . . ? C6 Fe2 C4 153.1(3) . . ? C5 Fe2 C4 40.9(3) . . ? C1 Fe2 C3 68.6(3) . . ? C8 Fe2 C3 117.0(3) . . ? C2 Fe2 C3 40.5(4) . . ? C7 Fe2 C3 151.3(3) . . ? C9 Fe2 C3 108.0(3) . . ? C6 Fe2 C3 166.2(4) . . ? C5 Fe2 C3 67.8(3) . . ? C4 Fe2 C3 39.7(4) . . ? C1 Fe2 C10 118.7(3) . . ? C8 Fe2 C10 68.3(3) . . ? C2 Fe2 C10 108.2(4) . . ? C7 Fe2 C10 68.6(3) . . ? C9 Fe2 C10 40.6(4) . . ? C6 Fe2 C10 40.2(3) . . ? C5 Fe2 C10 152.8(3) . . ? C4 Fe2 C10 165.2(4) . . ? C3 Fe2 C10 128.5(4) . . ? O1 P1 C1 110.6(3) . . ? O1 P1 C1V 111.9(3) . . ? C1 P1 C1V 107.5(3) . . ? O1 P1 C1W 110.9(3) . . ? C1 P1 C1W 108.9(3) . . ? C1V P1 C1W 107.0(3) . . ? O2 P2 C7 111.3(3) . 2_655 ? O2 P2 C1Z 111.7(3) . . ? C7 P2 C1Z 107.5(3) 2_655 . ? O2 P2 C1Y 111.1(3) . . ? C7 P2 C1Y 109.1(3) 2_655 . ? C1Z P2 C1Y 105.8(3) . . ? P1 O1 Fe1 157.2(3) . . ? P2 O2 Fe1 173.7(4) . . ? C5 C1 C2 107.6(7) . . ? C5 C1 P1 122.6(5) . . ? C2 C1 P1 129.6(6) . . ? C5 C1 Fe2 70.6(4) . . ? C2 C1 Fe2 69.4(4) . . ? P1 C1 Fe2 122.0(3) . . ? C3 C2 C1 107.5(8) . . ? C3 C2 Fe2 70.8(4) . . ? C1 C2 Fe2 69.1(4) . . ? C4 C3 C2 109.2(7) . . ? C4 C3 Fe2 70.0(4) . . ? C2 C3 Fe2 68.7(4) . . ? C3 C4 C5 108.3(8) . . ? C3 C4 Fe2 70.3(5) . . ? C5 C4 Fe2 69.5(4) . . ? C1 C5 C4 107.4(7) . . ? C1 C5 Fe2 68.5(4) . . ? C4 C5 Fe2 69.6(4) . . ? C10 C6 C7 108.3(7) . . ? C10 C6 Fe2 70.4(4) . . ? C7 C6 Fe2 68.8(4) . . ? C6 C7 C8 106.6(6) . . ? C6 C7 P2 122.4(5) . 2_655 ? C8 C7 P2 130.5(6) . 2_655 ? C6 C7 Fe2 70.0(4) . . ? C8 C7 Fe2 69.0(4) . . ? P2 C7 Fe2 120.0(3) 2_655 . ? C9 C8 C7 107.9(7) . . ? C9 C8 Fe2 70.4(5) . . ? C7 C8 Fe2 69.1(4) . . ? C8 C9 C10 109.3(7) . . ? C8 C9 Fe2 69.7(4) . . ? C10 C9 Fe2 70.4(4) . . ? C6 C10 C9 107.8(7) . . ? C6 C10 Fe2 69.5(4) . . ? C9 C10 Fe2 68.9(5) . . ? C2V C1V C6V 118.3(7) . . ? C2V C1V P1 122.5(6) . . ? C6V C1V P1 119.1(5) . . ? C1V C2V C3V 120.7(8) . . ? C4V C3V C2V 119.2(8) . . ? C5V C4V C3V 120.7(8) . . ? C4V C5V C6V 120.7(9) . . ? C5V C6V C1V 120.3(8) . . ? C2W C1W C6W 119.6(7) . . ? C2W C1W P1 117.8(6) . . ? C6W C1W P1 122.7(6) . . ? C1W C2W C3W 118.9(8) . . ? C4W C3W C2W 120.5(10) . . ? C3W C4W C5W 121.1(9) . . ? C4W C5W C6W 119.8(9) . . ? C5W C6W C1W 120.0(10) . . ? C2Y C1Y C6Y 119.9(8) . . ? C2Y C1Y P2 121.4(6) . . ? C6Y C1Y P2 118.6(7) . . ? C1Y C2Y C3Y 119.2(9) . . ? C4Y C3Y C2Y 121.2(10) . . ? C3Y C4Y C5Y 119.7(9) . . ? C6Y C5Y C4Y 119.6(11) . . ? C5Y C6Y C1Y 120.3(10) . . ? C6Z C1Z C2Z 120.1(8) . . ? C6Z C1Z P2 119.4(6) . . ? C2Z C1Z P2 120.5(7) . . ? C3Z C2Z C1Z 120.1(10) . . ? C4Z C3Z C2Z 119.3(10) . . ? C5Z C4Z C3Z 121.5(10) . . ? C4Z C5Z C6Z 119.9(11) . . ? C1Z C6Z C5Z 118.9(10) . . ? I2 I3 I2 180.0 . 7_565 ? C2S O1S C3S 128.6(7) . . ? O1S C2S C1S 112.9(13) . . ? O1S C3S C4S 112.3(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.176 _refine_diff_density_min -2.682 _refine_diff_density_rms 0.189 data_Cpd7 _database_code_depnum_ccdc_archive 'CCDC 823894' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H57 Cl6 Cu Fe2 O7 P4' _chemical_formula_weight 1533.99 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.9691(9) _cell_length_b 13.3154(6) _cell_length_c 27.6655(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.9990(10) _cell_angle_gamma 90.00 _cell_volume 6978.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4943 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.11 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3128 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6349 _exptl_absorpt_correction_T_max 0.8121 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19719 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6144 _reflns_number_gt 5351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1141P)^2^+182.6053P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6144 _refine_ls_number_parameters 407 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.1046 _refine_ls_wR_factor_ref 0.2941 _refine_ls_wR_factor_gt 0.2893 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.161 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O2S O 0.4479(9) 1.0364(14) 0.9974(7) 0.064(4) Uiso 0.50 1 d P . . O1S O 0.2865(7) 0.8666(10) 0.9759(4) 0.028(3) Uiso 0.50 1 d P . . O9S O 0.2232(17) 0.178(2) 0.9343(12) 0.123(9) Uiso 0.50 1 d PD . . H9O H 0.22(3) 0.230(7) 0.918(6) 0.184 Uiso 0.50 1 d PD . . C9S C 0.251(5) 0.212(8) 0.981(2) 0.26(4) Uiso 0.50 1 d PD . . Cl3 Cl 0.3528(5) 0.9581(9) 0.9837(5) 0.1005(15) Uiso 0.50 1 d PD A 1 Cl2 Cl 0.5000 1.0000 1.0000 0.1005(15) Uiso 0.50 2 d SPD . 1 C1L C 0.4148(6) 1.0609(11) 0.9916(15) 0.1005(15) Uiso 0.50 1 d PD A 1 C2L C 0.275(4) 0.855(5) 0.964(2) 0.1005(15) Uiso 0.25 1 d PD A 2 Cl4 Cl 0.3493(6) 0.9273(7) 0.9870(5) 0.1005(15) Uiso 0.50 1 d PD A 2 Cl5 Cl 0.2500 0.7500 1.0000 0.1005(15) Uiso 0.50 2 d SPD . 2 C3L C 0.3010(12) 0.9531(17) 0.983(3) 0.1005(15) Uiso 0.25 1 d PD A 3 Cl6 Cl 0.3961(10) 0.9559(15) 0.9902(8) 0.1005(15) Uiso 0.25 1 d PD A 3 Cl7 Cl 0.2728(10) 0.8247(16) 0.9787(8) 0.1005(15) Uiso 0.25 1 d PD A 3 Cu1 Cu 0.5000 0.59752(11) 0.7500 0.0287(4) Uani 1 2 d S . . Fe1 Fe 0.43102(6) 0.59628(9) 0.91732(4) 0.0279(4) Uani 1 1 d . . . Cl1 Cl 0.61856(10) 0.59528(17) 0.77887(8) 0.0342(5) Uani 1 1 d . . . P1 P 0.44294(11) 0.41960(15) 0.83072(7) 0.0226(5) Uani 1 1 d . . . P2 P 0.48524(11) 0.77447(15) 0.84063(7) 0.0236(5) Uani 1 1 d . . . O1 O 0.4798(3) 0.4891(4) 0.79766(19) 0.0248(12) Uani 1 1 d . . . O2 O 0.4771(3) 0.7057(4) 0.7978(2) 0.0281(13) Uani 1 1 d . . . C1 C 0.3936(4) 0.4847(7) 0.8737(3) 0.0292(19) Uani 1 1 d . . . C2 C 0.3844(5) 0.4589(7) 0.9230(3) 0.037(2) Uani 1 1 d . . . H2 H 0.4041 0.4002 0.9403 0.045 Uiso 1 1 calc R . . C3 C 0.3411(6) 0.5351(9) 0.9423(4) 0.048(3) Uani 1 1 d . . . H3 H 0.3271 0.5383 0.9759 0.058 Uiso 1 1 calc R . . C4 C 0.3236(5) 0.6062(8) 0.9063(4) 0.041(2) Uani 1 1 d . . . H4 H 0.2948 0.6666 0.9100 0.050 Uiso 1 1 calc R . . C5 C 0.3555(4) 0.5742(7) 0.8632(4) 0.034(2) Uani 1 1 d . . . H5 H 0.3525 0.6091 0.8319 0.041 Uiso 1 1 calc R . . C6 C 0.4932(5) 0.7096(6) 0.8970(3) 0.0276(18) Uani 1 1 d . . . C7 C 0.4622(5) 0.7352(7) 0.9410(3) 0.037(2) Uani 1 1 d . . . H7 H 0.4316 0.7929 0.9467 0.045 Uiso 1 1 calc R . . C8 C 0.4847(6) 0.6598(8) 0.9757(3) 0.045(3) Uani 1 1 d . . . H8 H 0.4710 0.6562 1.0093 0.054 Uiso 1 1 calc R . . C9 C 0.5281(5) 0.5918(8) 0.9533(4) 0.040(2) Uani 1 1 d . . . H9 H 0.5500 0.5323 0.9686 0.049 Uiso 1 1 calc R . . C10 C 0.5343(4) 0.6218(7) 0.9045(3) 0.0289(18) Uani 1 1 d . . . H10 H 0.5617 0.5877 0.8803 0.035 Uiso 1 1 calc R . . C1W C 0.5619(4) 0.8541(6) 0.8392(3) 0.0286(18) Uani 1 1 d . . . C2W C 0.5859(7) 0.8858(9) 0.7969(4) 0.063(4) Uani 1 1 d . . . H2W H 0.5651 0.8611 0.7681 0.075 Uiso 1 1 calc R . . C3W C 0.6413(8) 0.9547(11) 0.7949(5) 0.079(5) Uani 1 1 d . . . H3W H 0.6553 0.9783 0.7652 0.094 Uiso 1 1 calc R . . C4W C 0.6742(6) 0.9865(9) 0.8364(5) 0.055(3) Uani 1 1 d . . . H4W H 0.7111 1.0322 0.8353 0.066 Uiso 1 1 calc R . . C5W C 0.6537(7) 0.9522(10) 0.8801(5) 0.071(4) Uani 1 1 d . . . H5W H 0.6768 0.9745 0.9086 0.085 Uiso 1 1 calc R . . C6W C 0.5975(6) 0.8827(10) 0.8820(5) 0.061(3) Uani 1 1 d . . . H6W H 0.5847 0.8568 0.9115 0.073 Uiso 1 1 calc R . . C1X C 0.4092(4) 0.8560(7) 0.8413(3) 0.0285(18) Uani 1 1 d . . . C2X C 0.3483(5) 0.8294(8) 0.8164(4) 0.042(2) Uani 1 1 d . . . H2X H 0.3458 0.7695 0.7991 0.051 Uiso 1 1 calc R . . C3X C 0.2893(5) 0.8931(8) 0.8169(4) 0.046(3) Uani 1 1 d . . . H3X H 0.2476 0.8751 0.8000 0.055 Uiso 1 1 calc R . . C4X C 0.2929(6) 0.9793(9) 0.8416(5) 0.051(3) Uani 1 1 d . . . H4X H 0.2534 1.0207 0.8420 0.061 Uiso 1 1 calc R . . C5X C 0.3537(7) 1.0072(9) 0.8663(5) 0.063(3) Uani 1 1 d . . . H5X H 0.3555 1.0677 0.8831 0.076 Uiso 1 1 calc R . . C6X C 0.4125(6) 0.9467(8) 0.8665(4) 0.048(3) Uani 1 1 d . . . H6X H 0.4540 0.9661 0.8833 0.057 Uiso 1 1 calc R . . C1Y C 0.5072(4) 0.3422(6) 0.8624(3) 0.0267(18) Uani 1 1 d . . . C2Y C 0.4878(6) 0.2530(7) 0.8853(4) 0.042(2) Uani 1 1 d . . . H2Y H 0.4412 0.2312 0.8831 0.050 Uiso 1 1 calc R . . C3Y C 0.5389(7) 0.1980(9) 0.9110(4) 0.055(3) Uani 1 1 d . . . H3Y H 0.5261 0.1394 0.9265 0.066 Uiso 1 1 calc R . . C4Y C 0.6069(7) 0.2278(9) 0.9138(4) 0.054(3) Uani 1 1 d . . . H4Y H 0.6403 0.1889 0.9310 0.065 Uiso 1 1 calc R . . C5Y C 0.6278(6) 0.3159(9) 0.8916(4) 0.051(3) Uani 1 1 d . . . H5Y H 0.6748 0.3364 0.8941 0.062 Uiso 1 1 calc R . . C6Y C 0.5777(5) 0.3725(7) 0.8656(3) 0.035(2) Uani 1 1 d . . . H6Y H 0.5911 0.4310 0.8501 0.042 Uiso 1 1 calc R . . C1Z C 0.3807(4) 0.3372(6) 0.7992(3) 0.0262(17) Uani 1 1 d . . . C2Z C 0.3190(5) 0.3109(7) 0.8194(4) 0.037(2) Uani 1 1 d . . . H2Z H 0.3067 0.3409 0.8482 0.044 Uiso 1 1 calc R . . C3Z C 0.2749(5) 0.2402(7) 0.7974(4) 0.041(2) Uani 1 1 d . . . H3Z H 0.2329 0.2229 0.8112 0.050 Uiso 1 1 calc R . . C4Z C 0.2934(5) 0.1945(7) 0.7543(4) 0.041(2) Uani 1 1 d . . . H4Z H 0.2648 0.1452 0.7397 0.049 Uiso 1 1 calc R . . C5Z C 0.3549(6) 0.2241(10) 0.7337(4) 0.057(3) Uani 1 1 d . . . H5Z H 0.3671 0.1963 0.7045 0.069 Uiso 1 1 calc R . . C6Z C 0.3980(6) 0.2944(9) 0.7562(4) 0.049(3) Uani 1 1 d . . . H6Z H 0.4395 0.3134 0.7422 0.059 Uiso 1 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 Cu1 0.0289(8) 0.0264(8) 0.0305(8) 0.000 -0.0009(6) 0.000 Fe1 0.0333(7) 0.0281(7) 0.0226(6) -0.0052(5) 0.0047(5) -0.0073(5) Cl1 0.0210(10) 0.0400(12) 0.0407(12) 0.0103(10) -0.0071(8) -0.0086(9) P1 0.0236(10) 0.0197(10) 0.0244(10) 0.0010(8) -0.0005(8) -0.0073(8) P2 0.0279(11) 0.0196(10) 0.0231(10) -0.0037(8) 0.0001(8) -0.0034(8) O1 0.028(3) 0.023(3) 0.023(3) 0.006(2) 0.005(2) -0.006(2) O2 0.041(3) 0.020(3) 0.023(3) -0.006(2) 0.000(2) -0.002(2) C1 0.027(4) 0.028(4) 0.032(5) -0.005(4) 0.004(3) -0.013(4) C2 0.042(5) 0.037(5) 0.034(5) -0.005(4) 0.008(4) -0.017(4) C3 0.048(6) 0.059(7) 0.041(6) -0.017(5) 0.024(5) -0.018(5) C4 0.036(5) 0.045(6) 0.044(6) -0.019(5) 0.011(4) -0.006(4) C5 0.025(4) 0.033(5) 0.043(5) -0.002(4) -0.002(4) -0.006(4) C6 0.037(5) 0.027(4) 0.018(4) -0.004(3) 0.002(3) -0.010(4) C7 0.053(6) 0.029(5) 0.030(5) -0.008(4) 0.006(4) -0.011(4) C8 0.070(7) 0.041(6) 0.023(5) -0.005(4) -0.003(4) -0.019(5) C9 0.040(5) 0.040(6) 0.040(5) 0.004(4) -0.007(4) -0.010(4) C10 0.027(4) 0.032(5) 0.028(4) -0.002(4) -0.001(3) -0.007(4) C1W 0.027(4) 0.022(4) 0.036(5) 0.002(4) 0.000(3) -0.006(3) C2W 0.086(9) 0.057(7) 0.044(6) -0.014(5) 0.000(6) -0.045(7) C3W 0.102(11) 0.093(11) 0.043(7) -0.015(7) 0.031(7) -0.065(9) C4W 0.042(6) 0.042(6) 0.082(9) -0.008(6) 0.009(6) -0.020(5) C5W 0.061(8) 0.065(8) 0.082(9) 0.013(7) -0.028(7) -0.036(7) C6W 0.053(7) 0.061(8) 0.066(8) 0.017(6) -0.016(6) -0.033(6) C1X 0.027(4) 0.028(4) 0.031(4) -0.002(4) 0.005(3) 0.003(3) C2X 0.042(5) 0.034(5) 0.051(6) -0.011(4) -0.003(4) -0.004(4) C3X 0.034(5) 0.044(6) 0.059(7) 0.007(5) -0.007(5) 0.011(4) C4X 0.037(6) 0.043(6) 0.074(8) 0.010(6) 0.003(5) 0.014(5) C5X 0.061(8) 0.040(6) 0.090(10) -0.021(6) 0.014(7) 0.012(6) C6X 0.044(6) 0.035(6) 0.063(7) -0.017(5) -0.005(5) 0.000(5) C1Y 0.033(4) 0.024(4) 0.023(4) 0.001(3) -0.001(3) -0.002(3) C2Y 0.053(6) 0.033(5) 0.040(5) 0.009(4) -0.002(4) -0.011(4) C3Y 0.078(8) 0.040(6) 0.045(6) 0.018(5) -0.003(6) 0.009(6) C4Y 0.065(8) 0.054(7) 0.041(6) 0.012(5) -0.010(5) 0.021(6) C5Y 0.038(5) 0.060(7) 0.055(7) 0.011(6) -0.004(5) 0.008(5) C6Y 0.032(5) 0.035(5) 0.038(5) 0.008(4) 0.001(4) 0.001(4) C1Z 0.029(4) 0.023(4) 0.026(4) -0.002(3) -0.001(3) -0.010(3) C2Z 0.031(5) 0.035(5) 0.044(5) -0.007(4) 0.005(4) -0.011(4) C3Z 0.027(5) 0.038(5) 0.060(6) -0.007(5) 0.004(4) -0.011(4) C4Z 0.037(5) 0.033(5) 0.051(6) -0.008(4) -0.011(4) -0.010(4) C5Z 0.062(7) 0.068(8) 0.043(6) -0.030(6) 0.008(5) -0.026(6) C6Z 0.041(5) 0.062(7) 0.047(6) -0.020(5) 0.012(5) -0.025(5) _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 O2S C1L 0.72(2) . ? O2S Cl2 1.099(18) . ? O2S Cl6 1.46(2) . ? O2S Cl3 2.10(2) . ? O1S Cl7 0.622(19) . ? O1S C3L 1.20(2) . ? O1S Cl4 1.459(15) . ? O1S Cl3 1.755(15) . ? O1S Cl5 1.840(13) . ? O9S C9S 1.449(11) . ? C9S C9S 1.44(12) 7_557 ? Cl3 C1L 1.811(10) . ? Cl2 O2S 1.099(18) 5_677 ? Cl2 C1L 1.812(10) 5_677 ? Cl2 C1L 1.812(10) . ? C2L Cl4 1.793(10) . ? C2L Cl5 1.797(10) . ? Cl5 C2L 1.797(11) 7_567 ? Cl5 O1S 1.840(13) 7_567 ? C3L Cl7 1.793(10) . ? C3L Cl6 1.805(10) . ? Cu1 O1 2.006(5) 2_656 ? Cu1 O1 2.006(5) . ? Cu1 O2 2.017(6) 2_656 ? Cu1 O2 2.017(6) . ? Cu1 Cl1 2.347(2) 2_656 ? Cu1 Cl1 2.347(2) . ? Fe1 C6 2.014(8) . ? Fe1 C1 2.019(8) . ? Fe1 C10 2.037(8) . ? Fe1 C5 2.039(9) . ? Fe1 C7 2.039(9) . ? Fe1 C2 2.042(9) . ? Fe1 C3 2.043(10) . ? Fe1 C8 2.046(9) . ? Fe1 C4 2.048(10) . ? Fe1 C9 2.049(10) . ? P1 O1 1.499(6) . ? P1 C1 1.777(9) . ? P1 C1Y 1.791(8) . ? P1 C1Z 1.803(8) . ? P2 O2 1.500(6) . ? P2 C6 1.782(8) . ? P2 C1W 1.802(8) . ? P2 C1X 1.805(8) . ? C1 C5 1.417(13) . ? C1 C2 1.426(13) . ? C2 C3 1.426(15) . ? C3 C4 1.401(16) . ? C4 C5 1.432(14) . ? C6 C10 1.414(13) . ? C6 C7 1.422(12) . ? C7 C8 1.438(14) . ? C8 C9 1.390(15) . ? C9 C10 1.420(13) . ? C1W C2W 1.347(15) . ? C1W C6W 1.385(15) . ? C2W C3W 1.399(16) . ? C3W C4W 1.345(18) . ? C4W C5W 1.367(19) . ? C5W C6W 1.415(15) . ? C1X C2X 1.362(13) . ? C1X C6X 1.394(13) . ? C2X C3X 1.404(14) . ? C3X C4X 1.337(16) . ? C4X C5X 1.360(17) . ? C5X C6X 1.376(16) . ? C1Y C6Y 1.396(12) . ? C1Y C2Y 1.403(12) . ? C2Y C3Y 1.381(15) . ? C3Y C4Y 1.347(17) . ? C4Y C5Y 1.393(17) . ? C5Y C6Y 1.385(14) . ? C1Z C2Z 1.370(12) . ? C1Z C6Z 1.373(13) . ? C2Z C3Z 1.379(13) . ? C3Z C4Z 1.400(15) . ? C4Z C5Z 1.381(15) . ? C5Z C6Z 1.371(14) . ? 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 C1L O2S Cl2 171(5) . . ? C1L O2S Cl6 74(2) . . ? Cl2 O2S Cl6 106.3(16) . . ? C1L O2S Cl3 56.7(17) . . ? Cl2 O2S Cl3 123.6(14) . . ? Cl6 O2S Cl3 17.4(9) . . ? Cl7 O1S C3L 159(5) . . ? Cl7 O1S Cl4 144(3) . . ? C3L O1S Cl4 41.8(12) . . ? Cl7 O1S Cl3 155(3) . . ? C3L O1S Cl3 32.5(12) . . ? Cl4 O1S Cl3 10.9(7) . . ? Cl7 O1S Cl5 14(2) . . ? C3L O1S Cl5 147(4) . . ? Cl4 O1S Cl5 135.2(10) . . ? Cl3 O1S Cl5 145.3(9) . . ? C9S C9S O9S 147(10) 7_557 . ? O1S Cl3 C1L 174.8(9) . . ? O1S Cl3 O2S 165.7(10) . . ? C1L Cl3 O2S 19.4(6) . . ? O2S Cl2 O2S 180(2) 5_677 . ? O2S Cl2 C1L 3.6(19) 5_677 5_677 ? O2S Cl2 C1L 176.4(19) . 5_677 ? O2S Cl2 C1L 176.4(19) 5_677 . ? O2S Cl2 C1L 3.6(19) . . ? C1L Cl2 C1L 180.000(6) 5_677 . ? O2S C1L Cl3 104(2) . . ? O2S C1L Cl2 5(3) . . ? Cl3 C1L Cl2 104.3(7) . . ? Cl4 C2L Cl5 116.6(9) . . ? O1S Cl4 C2L 9(2) . . ? C2L Cl5 C2L 180.000(8) . 7_567 ? C2L Cl5 O1S 13.0(13) . . ? C2L Cl5 O1S 167.0(13) 7_567 . ? C2L Cl5 O1S 167.0(13) . 7_567 ? C2L Cl5 O1S 13.0(13) 7_567 7_567 ? O1S Cl5 O1S 180.000(3) . 7_567 ? O1S C3L Cl7 7.0(15) . . ? O1S C3L Cl6 104.9(15) . . ? Cl7 C3L Cl6 108.7(8) . . ? O2S Cl6 C3L 133.8(16) . . ? O1S Cl7 C3L 14(3) . . ? O1 Cu1 O1 87.9(3) 2_656 . ? O1 Cu1 O2 91.6(2) 2_656 2_656 ? O1 Cu1 O2 178.6(2) . 2_656 ? O1 Cu1 O2 178.6(2) 2_656 . ? O1 Cu1 O2 91.6(2) . . ? O2 Cu1 O2 88.9(3) 2_656 . ? O1 Cu1 Cl1 88.86(17) 2_656 2_656 ? O1 Cu1 Cl1 90.09(17) . 2_656 ? O2 Cu1 Cl1 91.23(18) 2_656 2_656 ? O2 Cu1 Cl1 89.81(18) . 2_656 ? O1 Cu1 Cl1 90.09(17) 2_656 . ? O1 Cu1 Cl1 88.86(17) . . ? O2 Cu1 Cl1 89.81(18) 2_656 . ? O2 Cu1 Cl1 91.23(18) . . ? Cl1 Cu1 Cl1 178.55(13) 2_656 . ? C6 Fe1 C1 125.2(3) . . ? C6 Fe1 C10 40.9(4) . . ? C1 Fe1 C10 109.2(3) . . ? C6 Fe1 C5 107.6(4) . . ? C1 Fe1 C5 40.9(4) . . ? C10 Fe1 C5 122.7(4) . . ? C6 Fe1 C7 41.1(4) . . ? C1 Fe1 C7 161.1(4) . . ? C10 Fe1 C7 68.9(4) . . ? C5 Fe1 C7 123.2(4) . . ? C6 Fe1 C2 162.8(4) . . ? C1 Fe1 C2 41.1(4) . . ? C10 Fe1 C2 126.0(4) . . ? C5 Fe1 C2 68.7(4) . . ? C7 Fe1 C2 155.1(4) . . ? C6 Fe1 C3 154.8(4) . . ? C1 Fe1 C3 68.6(4) . . ? C10 Fe1 C3 162.3(4) . . ? C5 Fe1 C3 68.0(4) . . ? C7 Fe1 C3 119.1(4) . . ? C2 Fe1 C3 40.9(4) . . ? C6 Fe1 C8 68.7(4) . . ? C1 Fe1 C8 157.0(4) . . ? C10 Fe1 C8 68.0(4) . . ? C5 Fe1 C8 160.2(4) . . ? C7 Fe1 C8 41.2(4) . . ? C2 Fe1 C8 120.6(4) . . ? C3 Fe1 C8 106.7(4) . . ? C6 Fe1 C4 120.2(4) . . ? C1 Fe1 C4 69.1(4) . . ? C10 Fe1 C4 157.1(4) . . ? C5 Fe1 C4 41.0(4) . . ? C7 Fe1 C4 105.0(4) . . ? C2 Fe1 C4 68.8(4) . . ? C3 Fe1 C4 40.1(5) . . ? C8 Fe1 C4 122.7(4) . . ? C6 Fe1 C9 68.4(4) . . ? C1 Fe1 C9 123.2(4) . . ? C10 Fe1 C9 40.7(4) . . ? C5 Fe1 C9 158.8(4) . . ? C7 Fe1 C9 68.4(4) . . ? C2 Fe1 C9 108.6(4) . . ? C3 Fe1 C9 124.7(5) . . ? C8 Fe1 C9 39.7(4) . . ? C4 Fe1 C9 159.4(4) . . ? O1 P1 C1 112.7(4) . . ? O1 P1 C1Y 109.1(4) . . ? C1 P1 C1Y 108.8(4) . . ? O1 P1 C1Z 113.2(4) . . ? C1 P1 C1Z 105.5(4) . . ? C1Y P1 C1Z 107.4(4) . . ? O2 P2 C6 113.3(4) . . ? O2 P2 C1W 113.1(4) . . ? C6 P2 C1W 105.8(4) . . ? O2 P2 C1X 109.1(4) . . ? C6 P2 C1X 108.3(4) . . ? C1W P2 C1X 107.0(4) . . ? P1 O1 Cu1 163.1(4) . . ? P2 O2 Cu1 159.6(4) . . ? C5 C1 C2 108.2(8) . . ? C5 C1 P1 123.6(7) . . ? C2 C1 P1 128.2(7) . . ? C5 C1 Fe1 70.3(5) . . ? C2 C1 Fe1 70.3(5) . . ? P1 C1 Fe1 125.3(4) . . ? C3 C2 C1 106.8(9) . . ? C3 C2 Fe1 69.6(6) . . ? C1 C2 Fe1 68.6(5) . . ? C4 C3 C2 109.5(9) . . ? C4 C3 Fe1 70.2(6) . . ? C2 C3 Fe1 69.5(5) . . ? C3 C4 C5 107.3(9) . . ? C3 C4 Fe1 69.8(6) . . ? C5 C4 Fe1 69.1(5) . . ? C1 C5 C4 108.2(9) . . ? C1 C5 Fe1 68.8(5) . . ? C4 C5 Fe1 69.8(6) . . ? C10 C6 C7 108.8(8) . . ? C10 C6 P2 123.4(6) . . ? C7 C6 P2 127.8(7) . . ? C10 C6 Fe1 70.5(5) . . ? C7 C6 Fe1 70.4(5) . . ? P2 C6 Fe1 125.7(4) . . ? C6 C7 C8 106.4(9) . . ? C6 C7 Fe1 68.5(5) . . ? C8 C7 Fe1 69.6(5) . . ? C9 C8 C7 108.7(9) . . ? C9 C8 Fe1 70.3(5) . . ? C7 C8 Fe1 69.2(5) . . ? C8 C9 C10 108.7(9) . . ? C8 C9 Fe1 70.1(6) . . ? C10 C9 Fe1 69.2(5) . . ? C6 C10 C9 107.4(8) . . ? C6 C10 Fe1 68.7(5) . . ? C9 C10 Fe1 70.1(5) . . ? C2W C1W C6W 119.0(9) . . ? C2W C1W P2 120.9(7) . . ? C6W C1W P2 120.1(7) . . ? C1W C2W C3W 122.0(10) . . ? C4W C3W C2W 119.2(11) . . ? C3W C4W C5W 120.6(10) . . ? C4W C5W C6W 120.0(12) . . ? C1W C6W C5W 118.9(11) . . ? C2X C1X C6X 119.5(9) . . ? C2X C1X P2 119.7(7) . . ? C6X C1X P2 120.8(7) . . ? C1X C2X C3X 119.6(9) . . ? C4X C3X C2X 120.3(10) . . ? C3X C4X C5X 120.7(10) . . ? C4X C5X C6X 120.5(11) . . ? C5X C6X C1X 119.4(10) . . ? C6Y C1Y C2Y 119.3(8) . . ? C6Y C1Y P1 119.3(7) . . ? C2Y C1Y P1 121.3(7) . . ? C3Y C2Y C1Y 119.2(10) . . ? C4Y C3Y C2Y 121.1(10) . . ? C3Y C4Y C5Y 121.1(10) . . ? C6Y C5Y C4Y 119.0(10) . . ? C5Y C6Y C1Y 120.3(9) . . ? C2Z C1Z C6Z 119.8(8) . . ? C2Z C1Z P1 120.6(7) . . ? C6Z C1Z P1 119.4(7) . . ? C1Z C2Z C3Z 120.3(9) . . ? C2Z C3Z C4Z 120.0(9) . . ? C5Z C4Z C3Z 118.8(9) . . ? C6Z C5Z C4Z 120.3(10) . . ? C5Z C6Z C1Z 120.8(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.735 _refine_diff_density_min -2.642 _refine_diff_density_rms 0.178 data_Cpd8 _database_code_depnum_ccdc_archive 'CCDC 823895' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Cl2 Fe Mn O2 P2' _chemical_formula_weight 712.19 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.066(4) _cell_length_b 16.609(7) _cell_length_c 18.436(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.426(9) _cell_angle_gamma 90.00 _cell_volume 3063(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 929 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.21 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5539 _exptl_absorpt_correction_T_max 0.7959 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21442 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7015 _reflns_number_gt 5807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0586P)^2^+0.4132P] 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 7015 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.74807(3) 0.20585(2) 0.393750(19) 0.01418(10) Uani 1 1 d . . . Fe1 Fe 0.99708(3) 0.33769(2) 0.225042(18) 0.01573(10) Uani 1 1 d . . . Cl1 Cl 0.60094(7) 0.30909(4) 0.41651(3) 0.02486(15) Uani 1 1 d . . . Cl2 Cl 0.75424(8) 0.07779(4) 0.44223(4) 0.03820(19) Uani 1 1 d . . . P1 P 0.73128(6) 0.21325(4) 0.20206(3) 0.01464(13) Uani 1 1 d . . . P2 P 1.06120(6) 0.28795(4) 0.40689(3) 0.01506(14) Uani 1 1 d . . . O1 O 0.73121(17) 0.20375(10) 0.28287(9) 0.0184(4) Uani 1 1 d . . . O2 O 0.93028(16) 0.25358(10) 0.42360(9) 0.0213(4) Uani 1 1 d . . . C1 C 0.8864(2) 0.24666(15) 0.17573(13) 0.0175(5) Uani 1 1 d . . . C2 C 0.9095(3) 0.30698(16) 0.12324(13) 0.0215(5) Uani 1 1 d . . . H2 H 0.8393 0.3385 0.0928 0.026 Uiso 1 1 calc R . . C3 C 1.0496(3) 0.31468(17) 0.12236(14) 0.0264(6) Uani 1 1 d . . . H3 H 1.0955 0.3529 0.0915 0.032 Uiso 1 1 calc R . . C4 C 1.1132(3) 0.25906(16) 0.17343(15) 0.0261(6) Uani 1 1 d . . . H4 H 1.2119 0.2516 0.1849 0.031 Uiso 1 1 calc R . . C5 C 1.0139(2) 0.21715(15) 0.20641(14) 0.0204(5) Uani 1 1 d . . . H5 H 1.0298 0.1744 0.2446 0.024 Uiso 1 1 calc R . . C6 C 1.0322(2) 0.35903(14) 0.33424(12) 0.0154(5) Uani 1 1 d . . . C7 C 1.1246(3) 0.40354(15) 0.29591(13) 0.0212(5) Uani 1 1 d . . . H7 H 1.2242 0.3986 0.3030 0.025 Uiso 1 1 calc R . . C8 C 1.0496(3) 0.45554(15) 0.24587(14) 0.0236(6) Uani 1 1 d . . . H8 H 1.0875 0.4931 0.2111 0.028 Uiso 1 1 calc R . . C9 C 0.9129(3) 0.44427(15) 0.25244(13) 0.0220(5) Uani 1 1 d . . . H9 H 0.8373 0.4726 0.2231 0.026 Uiso 1 1 calc R . . C10 C 0.9002(2) 0.38555(14) 0.30686(13) 0.0174(5) Uani 1 1 d . . . H10 H 0.8145 0.3656 0.3230 0.021 Uiso 1 1 calc R . . C1A C 0.6919(2) 0.11879(14) 0.15762(13) 0.0149(5) Uani 1 1 d . . . C2A C 0.6100(2) 0.06464(14) 0.18989(13) 0.0172(5) Uani 1 1 d . . . H2A H 0.5863 0.0745 0.2375 0.021 Uiso 1 1 calc R . . C3A C 0.5638(2) -0.00338(14) 0.15189(14) 0.0185(5) Uani 1 1 d . . . H3A H 0.5065 -0.0398 0.1731 0.022 Uiso 1 1 calc R . . C4A C 0.6007(2) -0.01875(14) 0.08283(14) 0.0195(5) Uani 1 1 d . . . H4A H 0.5680 -0.0655 0.0570 0.023 Uiso 1 1 calc R . . C5A C 0.6845(2) 0.03356(15) 0.05162(13) 0.0197(5) Uani 1 1 d . . . H5A H 0.7111 0.0223 0.0048 0.024 Uiso 1 1 calc R . . C6A C 0.7298(2) 0.10294(15) 0.08896(13) 0.0180(5) Uani 1 1 d . . . H6A H 0.7867 0.1394 0.0674 0.022 Uiso 1 1 calc R . . C1B C 0.6064(2) 0.28314(13) 0.16374(13) 0.0159(5) Uani 1 1 d . . . C2B C 0.5792(2) 0.29071(15) 0.08837(14) 0.0206(5) Uani 1 1 d . . . H2B H 0.6264 0.2585 0.0573 0.025 Uiso 1 1 calc R . . C3B C 0.4840(3) 0.34475(15) 0.05841(14) 0.0224(5) Uani 1 1 d . . . H3B H 0.4679 0.3510 0.0070 0.027 Uiso 1 1 calc R . . C4B C 0.4123(3) 0.38972(15) 0.10405(15) 0.0230(5) Uani 1 1 d . . . H4B H 0.3456 0.4263 0.0837 0.028 Uiso 1 1 calc R . . C5B C 0.4374(3) 0.38156(15) 0.17910(14) 0.0229(5) Uani 1 1 d . . . H5B H 0.3877 0.4126 0.2099 0.027 Uiso 1 1 calc R . . C6B C 0.5345(2) 0.32847(14) 0.20978(14) 0.0191(5) Uani 1 1 d . . . H6B H 0.5517 0.3231 0.2613 0.023 Uiso 1 1 calc R . . C1C C 1.1366(2) 0.34088(13) 0.48614(13) 0.0147(5) Uani 1 1 d . . . C2C C 1.2665(2) 0.32743(14) 0.51657(13) 0.0172(5) Uani 1 1 d . . . H2C H 1.3220 0.2908 0.4943 0.021 Uiso 1 1 calc R . . C3C C 1.3156(2) 0.36798(15) 0.58009(14) 0.0205(5) Uani 1 1 d . . . H3C H 1.4053 0.3597 0.6007 0.025 Uiso 1 1 calc R . . C4C C 1.2342(3) 0.42011(15) 0.61309(14) 0.0221(5) Uani 1 1 d . . . H4C H 1.2679 0.4469 0.6569 0.026 Uiso 1 1 calc R . . C5C C 1.1038(2) 0.43385(15) 0.58294(13) 0.0197(5) Uani 1 1 d . . . H5C H 1.0484 0.4701 0.6057 0.024 Uiso 1 1 calc R . . C6C C 1.0548(2) 0.39425(14) 0.51920(13) 0.0174(5) Uani 1 1 d . . . H6C H 0.9656 0.4035 0.4981 0.021 Uiso 1 1 calc R . . C1D C 1.1735(3) 0.20901(14) 0.38674(14) 0.0198(5) Uani 1 1 d . . . C2D C 1.2862(3) 0.22160(17) 0.35102(16) 0.0267(6) Uani 1 1 d . . . H2D H 1.3054 0.2739 0.3341 0.032 Uiso 1 1 calc R . . C3D C 1.3702(3) 0.15793(18) 0.34019(17) 0.0352(7) Uani 1 1 d . . . H3D H 1.4464 0.1664 0.3151 0.042 Uiso 1 1 calc R . . C4D C 1.3440(3) 0.08234(18) 0.36553(17) 0.0366(7) Uani 1 1 d . . . H4D H 1.4024 0.0390 0.3579 0.044 Uiso 1 1 calc R . . C5D C 1.2335(3) 0.06908(17) 0.40208(16) 0.0352(7) Uani 1 1 d . . . H5D H 1.2169 0.0170 0.4203 0.042 Uiso 1 1 calc R . . C6D C 1.1465(3) 0.13218(16) 0.41222(14) 0.0268(6) Uani 1 1 d . . . H6D H 1.0692 0.1230 0.4363 0.032 Uiso 1 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 Mn1 0.01554(18) 0.0152(2) 0.01167(18) -0.00048(13) 0.00116(14) -0.00216(13) Fe1 0.01740(18) 0.0178(2) 0.01196(18) -0.00301(13) 0.00145(13) -0.00209(13) Cl1 0.0306(3) 0.0276(3) 0.0170(3) -0.0007(2) 0.0056(3) 0.0106(3) Cl2 0.0506(4) 0.0203(4) 0.0420(4) 0.0103(3) -0.0020(3) -0.0098(3) P1 0.0158(3) 0.0168(3) 0.0111(3) -0.0031(2) 0.0005(2) 0.0009(2) P2 0.0159(3) 0.0146(3) 0.0140(3) -0.0006(2) -0.0013(2) -0.0021(2) O1 0.0211(9) 0.0220(9) 0.0117(8) -0.0027(6) 0.0001(7) 0.0010(7) O2 0.0194(9) 0.0238(10) 0.0197(9) 0.0026(7) -0.0023(7) -0.0066(7) C1 0.0180(11) 0.0195(13) 0.0148(12) -0.0062(9) 0.0014(9) -0.0012(9) C2 0.0239(13) 0.0284(14) 0.0121(12) -0.0062(10) 0.0013(10) -0.0029(10) C3 0.0291(14) 0.0351(16) 0.0161(13) -0.0088(11) 0.0075(11) -0.0111(11) C4 0.0184(12) 0.0319(15) 0.0290(15) -0.0162(12) 0.0065(11) -0.0027(10) C5 0.0192(12) 0.0186(13) 0.0233(13) -0.0099(10) 0.0019(10) 0.0019(9) C6 0.0200(11) 0.0140(11) 0.0114(11) -0.0026(9) -0.0021(9) -0.0029(9) C7 0.0244(13) 0.0205(13) 0.0182(13) -0.0030(10) 0.0009(10) -0.0065(10) C8 0.0393(15) 0.0145(13) 0.0168(12) 0.0017(9) 0.0017(11) -0.0060(11) C9 0.0332(14) 0.0157(12) 0.0161(12) -0.0020(9) -0.0018(11) 0.0034(10) C10 0.0228(12) 0.0150(12) 0.0140(12) -0.0037(9) 0.0002(10) 0.0025(9) C1A 0.0125(10) 0.0154(12) 0.0159(12) -0.0016(9) -0.0018(9) 0.0022(8) C2A 0.0183(11) 0.0179(12) 0.0157(12) 0.0001(9) 0.0025(9) 0.0053(9) C3A 0.0167(11) 0.0159(12) 0.0229(13) 0.0035(9) 0.0015(10) 0.0018(9) C4A 0.0179(11) 0.0153(12) 0.0237(13) -0.0038(10) -0.0038(10) 0.0018(9) C5A 0.0230(12) 0.0203(13) 0.0161(12) -0.0047(9) 0.0035(10) 0.0014(10) C6A 0.0155(11) 0.0203(13) 0.0188(12) -0.0025(9) 0.0042(9) 0.0002(9) C1B 0.0178(11) 0.0136(12) 0.0161(12) -0.0013(9) 0.0004(9) -0.0005(9) C2B 0.0218(12) 0.0218(14) 0.0181(13) -0.0037(10) 0.0014(10) 0.0027(10) C3B 0.0251(13) 0.0235(14) 0.0178(13) 0.0015(10) -0.0009(10) -0.0005(10) C4B 0.0222(12) 0.0175(13) 0.0284(14) 0.0019(10) -0.0009(11) 0.0034(10) C5B 0.0239(13) 0.0214(14) 0.0237(14) -0.0038(10) 0.0044(11) 0.0052(10) C6B 0.0224(12) 0.0194(13) 0.0157(12) -0.0018(9) 0.0035(10) -0.0004(9) C1C 0.0166(11) 0.0145(12) 0.0128(11) 0.0015(9) 0.0009(9) -0.0043(9) C2C 0.0186(12) 0.0160(12) 0.0167(12) 0.0011(9) 0.0010(9) 0.0002(9) C3C 0.0196(12) 0.0200(13) 0.0208(13) 0.0029(10) -0.0029(10) -0.0040(10) C4C 0.0271(13) 0.0217(14) 0.0168(12) -0.0022(10) -0.0001(10) -0.0082(10) C5C 0.0248(13) 0.0184(13) 0.0170(12) -0.0018(9) 0.0067(10) -0.0011(10) C6C 0.0161(11) 0.0185(13) 0.0176(12) 0.0013(9) 0.0022(9) -0.0018(9) C1D 0.0250(13) 0.0162(13) 0.0166(12) -0.0051(9) -0.0047(10) 0.0032(9) C2D 0.0232(13) 0.0249(14) 0.0312(15) -0.0054(11) -0.0014(11) 0.0011(11) C3D 0.0271(15) 0.0396(18) 0.0376(18) -0.0136(13) -0.0020(13) 0.0080(12) C4D 0.0409(17) 0.0319(17) 0.0334(16) -0.0147(13) -0.0115(14) 0.0161(13) C5D 0.059(2) 0.0185(15) 0.0242(15) -0.0048(11) -0.0106(14) 0.0076(13) C6D 0.0396(16) 0.0188(14) 0.0205(14) -0.0022(10) -0.0041(12) 0.0029(11) _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 Mn1 O2 2.0172(18) . ? Mn1 O1 2.0324(19) . ? Mn1 Cl2 2.3052(11) . ? Mn1 Cl1 2.3341(9) . ? Fe1 C1 2.031(2) . ? Fe1 C6 2.036(2) . ? Fe1 C5 2.041(3) . ? Fe1 C7 2.043(3) . ? Fe1 C10 2.046(2) . ? Fe1 C2 2.047(3) . ? Fe1 C9 2.050(3) . ? Fe1 C8 2.053(3) . ? Fe1 C4 2.056(3) . ? Fe1 C3 2.057(3) . ? P1 O1 1.4982(18) . ? P1 C1 1.776(2) . ? P1 C1A 1.794(2) . ? P1 C1B 1.797(2) . ? P2 O2 1.4994(18) . ? P2 C6 1.785(2) . ? P2 C1D 1.796(2) . ? P2 C1C 1.799(2) . ? C1 C5 1.430(3) . ? C1 C2 1.430(4) . ? C2 C3 1.417(4) . ? C3 C4 1.419(4) . ? C4 C5 1.410(4) . ? C6 C7 1.435(3) . ? C6 C10 1.436(3) . ? C7 C8 1.418(4) . ? C8 C9 1.407(4) . ? C9 C10 1.415(3) . ? C1A C6A 1.388(3) . ? C1A C2A 1.397(3) . ? C2A C3A 1.382(3) . ? C3A C4A 1.389(3) . ? C4A C5A 1.381(3) . ? C5A C6A 1.393(3) . ? C1B C2B 1.392(3) . ? C1B C6B 1.396(3) . ? C2B C3B 1.382(4) . ? C3B C4B 1.387(4) . ? C4B C5B 1.385(4) . ? C5B C6B 1.389(4) . ? C1C C2C 1.382(3) . ? C1C C6C 1.396(3) . ? C2C C3C 1.393(3) . ? C3C C4C 1.379(4) . ? C4C C5C 1.386(4) . ? C5C C6C 1.388(3) . ? C1D C2D 1.390(4) . ? C1D C6D 1.397(4) . ? C2D C3D 1.382(4) . ? C3D C4D 1.375(4) . ? C4D C5D 1.381(4) . ? C5D C6D 1.392(4) . ? 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 O2 Mn1 O1 104.60(7) . . ? O2 Mn1 Cl2 105.82(6) . . ? O1 Mn1 Cl2 111.70(5) . . ? O2 Mn1 Cl1 103.77(6) . . ? O1 Mn1 Cl1 102.13(5) . . ? Cl2 Mn1 Cl1 126.74(4) . . ? C1 Fe1 C6 126.73(10) . . ? C1 Fe1 C5 41.10(10) . . ? C6 Fe1 C5 109.19(10) . . ? C1 Fe1 C7 163.39(10) . . ? C6 Fe1 C7 41.19(9) . . ? C5 Fe1 C7 125.06(10) . . ? C1 Fe1 C10 109.67(10) . . ? C6 Fe1 C10 41.20(9) . . ? C5 Fe1 C10 124.08(10) . . ? C7 Fe1 C10 68.77(10) . . ? C1 Fe1 C2 41.05(10) . . ? C6 Fe1 C2 163.64(10) . . ? C5 Fe1 C2 68.69(11) . . ? C7 Fe1 C2 153.49(10) . . ? C10 Fe1 C2 125.53(10) . . ? C1 Fe1 C9 122.15(10) . . ? C6 Fe1 C9 68.70(10) . . ? C5 Fe1 C9 158.85(10) . . ? C7 Fe1 C9 68.14(11) . . ? C10 Fe1 C9 40.43(9) . . ? C2 Fe1 C9 107.09(10) . . ? C1 Fe1 C8 155.57(10) . . ? C6 Fe1 C8 68.68(9) . . ? C5 Fe1 C8 160.41(11) . . ? C7 Fe1 C8 40.51(10) . . ? C10 Fe1 C8 68.02(10) . . ? C2 Fe1 C8 118.99(10) . . ? C9 Fe1 C8 40.13(11) . . ? C1 Fe1 C4 68.38(10) . . ? C6 Fe1 C4 121.58(11) . . ? C5 Fe1 C4 40.26(10) . . ? C7 Fe1 C4 106.67(11) . . ? C10 Fe1 C4 158.51(11) . . ? C2 Fe1 C4 68.03(11) . . ? C9 Fe1 C4 159.18(11) . . ? C8 Fe1 C4 122.99(11) . . ? C1 Fe1 C3 68.55(10) . . ? C6 Fe1 C3 155.26(10) . . ? C5 Fe1 C3 68.18(11) . . ? C7 Fe1 C3 118.68(10) . . ? C10 Fe1 C3 160.58(11) . . ? C2 Fe1 C3 40.40(10) . . ? C9 Fe1 C3 122.88(11) . . ? C8 Fe1 C3 105.18(11) . . ? C4 Fe1 C3 40.38(12) . . ? O1 P1 C1 113.77(11) . . ? O1 P1 C1A 109.72(10) . . ? C1 P1 C1A 107.74(11) . . ? O1 P1 C1B 112.39(10) . . ? C1 P1 C1B 106.77(12) . . ? C1A P1 C1B 106.04(11) . . ? O2 P2 C6 109.40(11) . . ? O2 P2 C1D 110.63(11) . . ? C6 P2 C1D 112.42(12) . . ? O2 P2 C1C 108.64(10) . . ? C6 P2 C1C 107.76(11) . . ? C1D P2 C1C 107.86(11) . . ? P1 O1 Mn1 171.50(11) . . ? P2 O2 Mn1 152.46(11) . . ? C5 C1 C2 107.5(2) . . ? C5 C1 P1 124.2(2) . . ? C2 C1 P1 128.22(19) . . ? C5 C1 Fe1 69.84(14) . . ? C2 C1 Fe1 70.06(14) . . ? P1 C1 Fe1 124.42(12) . . ? C3 C2 C1 107.9(2) . . ? C3 C2 Fe1 70.20(14) . . ? C1 C2 Fe1 68.89(14) . . ? C2 C3 C4 108.0(2) . . ? C2 C3 Fe1 69.40(14) . . ? C4 C3 Fe1 69.74(15) . . ? C5 C4 C3 108.6(2) . . ? C5 C4 Fe1 69.33(14) . . ? C3 C4 Fe1 69.88(15) . . ? C4 C5 C1 107.9(2) . . ? C4 C5 Fe1 70.41(15) . . ? C1 C5 Fe1 69.07(14) . . ? C7 C6 C10 107.1(2) . . ? C7 C6 P2 130.52(19) . . ? C10 C6 P2 122.26(18) . . ? C7 C6 Fe1 69.70(14) . . ? C10 C6 Fe1 69.79(13) . . ? P2 C6 Fe1 128.51(13) . . ? C8 C7 C6 107.9(2) . . ? C8 C7 Fe1 70.09(15) . . ? C6 C7 Fe1 69.11(14) . . ? C9 C8 C7 108.5(2) . . ? C9 C8 Fe1 69.83(14) . . ? C7 C8 Fe1 69.40(14) . . ? C8 C9 C10 108.6(2) . . ? C8 C9 Fe1 70.04(15) . . ? C10 C9 Fe1 69.65(14) . . ? C9 C10 C6 107.9(2) . . ? C9 C10 Fe1 69.93(14) . . ? C6 C10 Fe1 69.01(13) . . ? C6A C1A C2A 120.1(2) . . ? C6A C1A P1 120.88(18) . . ? C2A C1A P1 118.64(18) . . ? C3A C2A C1A 119.4(2) . . ? C2A C3A C4A 120.4(2) . . ? C5A C4A C3A 120.3(2) . . ? C4A C5A C6A 119.8(2) . . ? C1A C6A C5A 120.0(2) . . ? C2B C1B C6B 120.1(2) . . ? C2B C1B P1 120.13(18) . . ? C6B C1B P1 119.80(19) . . ? C3B C2B C1B 120.5(2) . . ? C2B C3B C4B 119.5(2) . . ? C5B C4B C3B 120.3(2) . . ? C4B C5B C6B 120.7(2) . . ? C5B C6B C1B 118.9(2) . . ? C2C C1C C6C 120.2(2) . . ? C2C C1C P2 123.00(18) . . ? C6C C1C P2 116.70(18) . . ? C1C C2C C3C 119.6(2) . . ? C4C C3C C2C 120.2(2) . . ? C3C C4C C5C 120.6(2) . . ? C4C C5C C6C 119.5(2) . . ? C5C C6C C1C 120.0(2) . . ? C2D C1D C6D 119.8(2) . . ? C2D C1D P2 123.6(2) . . ? C6D C1D P2 116.5(2) . . ? C3D C2D C1D 119.9(3) . . ? C4D C3D C2D 120.4(3) . . ? C3D C4D C5D 120.4(3) . . ? C4D C5D C6D 119.9(3) . . ? C5D C6D C1D 119.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.571 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.093 data_Cpd9 _database_code_depnum_ccdc_archive 'CCDC 823896' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Cl2 Co Fe O2 P2' _chemical_formula_weight 716.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6658(6) _cell_length_b 14.1127(7) _cell_length_c 19.1893(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.5930(10) _cell_angle_gamma 90.00 _cell_volume 3156.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6297 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.35 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 1.286 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5124 _exptl_absorpt_correction_T_max 0.8404 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21869 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7227 _reflns_number_gt 6209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0470P)^2^+2.1542P] 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 7227 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.42033(3) 0.86846(3) 0.389542(17) 0.02372(10) Uani 1 1 d . . . Co1 Co 0.58710(3) 0.70899(2) 0.210803(16) 0.02398(10) Uani 1 1 d . . . P1 P 0.64108(5) 0.71792(4) 0.38109(3) 0.02106(14) Uani 1 1 d . . . P2 P 0.41552(5) 0.90486(5) 0.20961(3) 0.02394(14) Uani 1 1 d . . . Cl1 Cl 0.73778(8) 0.67650(6) 0.14680(5) 0.0536(2) Uani 1 1 d . . . Cl2 Cl 0.46372(6) 0.58649(5) 0.20925(4) 0.03767(17) Uani 1 1 d . . . O1 O 0.65272(15) 0.73825(13) 0.30505(8) 0.0266(4) Uani 1 1 d . . . O2 O 0.49914(15) 0.82765(13) 0.19286(9) 0.0308(4) Uani 1 1 d . . . C1 C 0.5019(2) 0.74405(17) 0.41011(12) 0.0239(5) Uani 1 1 d . . . C2 C 0.4698(2) 0.78834(19) 0.47363(13) 0.0306(6) Uani 1 1 d . . . H2 H 0.5230 0.8083 0.5126 0.037 Uiso 1 1 calc R . . C3 C 0.3501(3) 0.7986(2) 0.47089(16) 0.0400(7) Uani 1 1 d . . . H3 H 0.3046 0.8282 0.5074 0.048 Uiso 1 1 calc R . . C4 C 0.3052(2) 0.7612(2) 0.40651(16) 0.0374(6) Uani 1 1 d . . . H4 H 0.2233 0.7603 0.3905 0.045 Uiso 1 1 calc R . . C5 C 0.3982(2) 0.72713(18) 0.36889(13) 0.0268(5) Uani 1 1 d . . . H5 H 0.3927 0.6976 0.3221 0.032 Uiso 1 1 calc R . . C6 C 0.4232(2) 0.94173(18) 0.29845(13) 0.0253(5) Uani 1 1 d . . . C7 C 0.3306(2) 0.97401(19) 0.33912(14) 0.0327(6) Uani 1 1 d . . . H7 H 0.2480 0.9728 0.3248 0.039 Uiso 1 1 calc R . . C8 C 0.3790(3) 1.0079(2) 0.40342(15) 0.0408(7) Uani 1 1 d . . . H8 H 0.3354 1.0336 0.4423 0.049 Uiso 1 1 calc R . . C9 C 0.4995(3) 0.99810(19) 0.40338(14) 0.0379(7) Uani 1 1 d . . . H9 H 0.5546 1.0154 0.4420 0.045 Uiso 1 1 calc R . . C10 C 0.5273(2) 0.95725(18) 0.33896(13) 0.0291(5) Uani 1 1 d . . . H10 H 0.6055 0.9416 0.3246 0.035 Uiso 1 1 calc R . . C11 C 0.7427(2) 0.78898(17) 0.43122(13) 0.0261(5) Uani 1 1 d . . . C12 C 0.7974(3) 0.8616(2) 0.39749(16) 0.0406(7) Uani 1 1 d . . . H12 H 0.7818 0.8722 0.3496 0.049 Uiso 1 1 calc R . . C13 C 0.8750(4) 0.9185(3) 0.4344(2) 0.0669(12) Uani 1 1 d . . . H13 H 0.9111 0.9689 0.4120 0.080 Uiso 1 1 calc R . . C14 C 0.8993(4) 0.9009(3) 0.50440(19) 0.0671(12) Uani 1 1 d . . . H14 H 0.9523 0.9396 0.5294 0.080 Uiso 1 1 calc R . . C15 C 0.8474(3) 0.8284(3) 0.53770(16) 0.0473(8) Uani 1 1 d . . . H15 H 0.8656 0.8168 0.5852 0.057 Uiso 1 1 calc R . . C16 C 0.7682(2) 0.7719(2) 0.50173(14) 0.0328(6) Uani 1 1 d . . . H16 H 0.7318 0.7222 0.5247 0.039 Uiso 1 1 calc R . . C17 C 0.6684(2) 0.59547(17) 0.40052(13) 0.0245(5) Uani 1 1 d . . . C18 C 0.7236(2) 0.54082(19) 0.35194(15) 0.0314(6) Uani 1 1 d . . . H18 H 0.7453 0.5679 0.3098 0.038 Uiso 1 1 calc R . . C19 C 0.7463(2) 0.4461(2) 0.36601(18) 0.0410(7) Uani 1 1 d . . . H19 H 0.7834 0.4087 0.3333 0.049 Uiso 1 1 calc R . . C20 C 0.7147(2) 0.4066(2) 0.42803(18) 0.0415(7) Uani 1 1 d . . . H20 H 0.7309 0.3425 0.4375 0.050 Uiso 1 1 calc R . . C21 C 0.6594(3) 0.4603(2) 0.47640(16) 0.0389(7) Uani 1 1 d . . . H21 H 0.6382 0.4327 0.5185 0.047 Uiso 1 1 calc R . . C22 C 0.6351(2) 0.55501(19) 0.46298(14) 0.0319(6) Uani 1 1 d . . . H22 H 0.5966 0.5916 0.4955 0.038 Uiso 1 1 calc R . . C23 C 0.4436(2) 1.0115(2) 0.16169(14) 0.0293(6) Uani 1 1 d . . . C24 C 0.4905(3) 1.0910(2) 0.19403(16) 0.0402(7) Uani 1 1 d . . . H24 H 0.5069 1.0904 0.2424 0.048 Uiso 1 1 calc R . . C25 C 0.5136(3) 1.1718(2) 0.15574(19) 0.0490(8) Uani 1 1 d . . . H25 H 0.5451 1.2257 0.1781 0.059 Uiso 1 1 calc R . . C26 C 0.4900(3) 1.1723(3) 0.08493(18) 0.0476(8) Uani 1 1 d . . . H26 H 0.5057 1.2268 0.0588 0.057 Uiso 1 1 calc R . . C27 C 0.4438(3) 1.0943(3) 0.05207(17) 0.0527(9) Uani 1 1 d . . . H27 H 0.4281 1.0954 0.0036 0.063 Uiso 1 1 calc R . . C28 C 0.4200(3) 1.0133(3) 0.08993(16) 0.0451(8) Uani 1 1 d . . . H28 H 0.3881 0.9599 0.0672 0.054 Uiso 1 1 calc R . . C29 C 0.2700(2) 0.87014(19) 0.18891(13) 0.0273(5) Uani 1 1 d . . . C30 C 0.2417(2) 0.7748(2) 0.18967(14) 0.0331(6) Uani 1 1 d . . . H30 H 0.2986 0.7291 0.1999 0.040 Uiso 1 1 calc R . . C31 C 0.1289(3) 0.7469(2) 0.17534(16) 0.0402(7) Uani 1 1 d . . . H31 H 0.1098 0.6822 0.1749 0.048 Uiso 1 1 calc R . . C32 C 0.0447(2) 0.8139(2) 0.16175(16) 0.0405(7) Uani 1 1 d . . . H32 H -0.0315 0.7947 0.1523 0.049 Uiso 1 1 calc R . . C33 C 0.0722(2) 0.9091(2) 0.16193(16) 0.0408(7) Uani 1 1 d . . . H33 H 0.0144 0.9546 0.1531 0.049 Uiso 1 1 calc R . . C34 C 0.1845(2) 0.9378(2) 0.17511(15) 0.0342(6) Uani 1 1 d . . . H34 H 0.2032 1.0025 0.1748 0.041 Uiso 1 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 Fe1 0.02661(19) 0.02294(19) 0.02172(18) 0.00061(14) 0.00247(14) 0.00470(14) Co1 0.02611(18) 0.02484(18) 0.02099(17) -0.00134(13) 0.00107(13) 0.00130(13) P1 0.0216(3) 0.0199(3) 0.0213(3) -0.0017(2) -0.0029(2) 0.0002(2) P2 0.0225(3) 0.0265(3) 0.0226(3) 0.0012(2) -0.0013(2) 0.0033(2) Cl1 0.0606(5) 0.0480(5) 0.0553(5) -0.0024(4) 0.0353(4) 0.0056(4) Cl2 0.0383(4) 0.0300(4) 0.0439(4) 0.0010(3) -0.0066(3) -0.0075(3) O1 0.0277(9) 0.0299(10) 0.0220(8) -0.0025(7) -0.0016(7) -0.0009(7) O2 0.0292(9) 0.0320(10) 0.0310(9) -0.0007(8) -0.0006(7) 0.0076(8) C1 0.0283(12) 0.0196(12) 0.0237(12) 0.0014(9) 0.0011(9) 0.0021(10) C2 0.0409(15) 0.0296(14) 0.0214(12) 0.0033(10) 0.0031(11) 0.0065(11) C3 0.0467(17) 0.0387(17) 0.0362(15) 0.0088(12) 0.0191(13) 0.0103(13) C4 0.0295(14) 0.0345(15) 0.0486(17) 0.0086(13) 0.0078(12) 0.0012(12) C5 0.0253(12) 0.0243(13) 0.0307(13) 0.0011(10) -0.0004(10) -0.0023(10) C6 0.0279(12) 0.0216(12) 0.0261(12) 0.0031(10) -0.0005(10) 0.0014(10) C7 0.0370(15) 0.0298(14) 0.0312(14) 0.0043(11) 0.0008(11) 0.0122(12) C8 0.064(2) 0.0282(15) 0.0300(14) -0.0011(11) 0.0035(13) 0.0163(14) C9 0.0562(18) 0.0240(14) 0.0325(14) -0.0016(11) -0.0097(13) -0.0021(13) C10 0.0317(13) 0.0247(13) 0.0304(13) 0.0063(10) -0.0028(11) -0.0031(10) C11 0.0256(12) 0.0245(13) 0.0275(12) -0.0054(10) -0.0061(10) -0.0006(10) C12 0.0428(17) 0.0392(17) 0.0385(16) 0.0080(13) -0.0123(13) -0.0128(13) C13 0.080(3) 0.056(2) 0.062(2) 0.0135(18) -0.021(2) -0.046(2) C14 0.074(3) 0.068(3) 0.057(2) -0.0074(19) -0.0183(19) -0.045(2) C15 0.0540(19) 0.058(2) 0.0292(15) -0.0075(14) -0.0101(13) -0.0178(16) C16 0.0339(14) 0.0345(15) 0.0297(13) -0.0027(11) -0.0032(11) -0.0071(12) C17 0.0193(11) 0.0202(12) 0.0335(13) -0.0014(10) -0.0038(10) 0.0001(9) C18 0.0273(13) 0.0290(14) 0.0379(14) -0.0015(11) 0.0008(11) 0.0006(11) C19 0.0291(14) 0.0320(15) 0.062(2) -0.0083(14) 0.0024(13) 0.0062(12) C20 0.0326(15) 0.0239(14) 0.067(2) 0.0063(14) -0.0074(14) 0.0034(11) C21 0.0391(15) 0.0322(15) 0.0446(17) 0.0106(13) -0.0063(13) -0.0033(12) C22 0.0318(14) 0.0307(14) 0.0329(14) 0.0028(11) -0.0023(11) 0.0016(11) C23 0.0226(12) 0.0346(15) 0.0311(13) 0.0060(11) 0.0043(10) 0.0060(10) C24 0.0510(18) 0.0334(16) 0.0365(15) 0.0034(12) 0.0060(13) 0.0013(13) C25 0.056(2) 0.0340(17) 0.058(2) 0.0078(15) 0.0123(16) 0.0010(15) C26 0.0315(15) 0.052(2) 0.060(2) 0.0265(17) 0.0104(14) 0.0055(14) C27 0.0383(17) 0.082(3) 0.0375(17) 0.0274(17) -0.0036(13) -0.0052(17) C28 0.0405(17) 0.058(2) 0.0362(16) 0.0105(14) -0.0073(13) -0.0114(15) C29 0.0236(12) 0.0344(14) 0.0237(12) 0.0005(10) -0.0011(9) 0.0015(10) C30 0.0315(14) 0.0350(15) 0.0324(14) -0.0008(11) -0.0026(11) 0.0052(11) C31 0.0442(17) 0.0330(15) 0.0436(17) -0.0014(13) 0.0016(13) -0.0084(13) C32 0.0265(14) 0.0516(19) 0.0431(16) -0.0055(14) -0.0011(12) -0.0066(13) C33 0.0269(14) 0.0444(18) 0.0503(18) -0.0036(14) -0.0062(12) 0.0089(12) C34 0.0293(13) 0.0312(15) 0.0415(15) -0.0021(12) -0.0047(11) 0.0019(11) _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 Fe1 C1 2.027(2) . ? Fe1 C6 2.032(2) . ? Fe1 C2 2.033(3) . ? Fe1 C7 2.039(3) . ? Fe1 C10 2.044(3) . ? Fe1 C8 2.047(3) . ? Fe1 C5 2.048(3) . ? Fe1 C3 2.048(3) . ? Fe1 C4 2.059(3) . ? Fe1 C9 2.061(3) . ? Co1 O1 1.9753(16) . ? Co1 O2 1.9859(18) . ? Co1 Cl1 2.2370(8) . ? Co1 Cl2 2.2489(8) . ? P1 O1 1.4992(17) . ? P1 C1 1.779(3) . ? P1 C17 1.793(2) . ? P1 C11 1.798(2) . ? P2 O2 1.5070(19) . ? P2 C6 1.781(3) . ? P2 C29 1.795(3) . ? P2 C23 1.802(3) . ? C1 C2 1.435(3) . ? C1 C5 1.436(3) . ? C2 C3 1.402(4) . ? C3 C4 1.422(4) . ? C4 C5 1.414(4) . ? C6 C10 1.429(3) . ? C6 C7 1.435(4) . ? C7 C8 1.417(4) . ? C8 C9 1.413(5) . ? C9 C10 1.415(4) . ? C11 C12 1.384(4) . ? C11 C16 1.393(4) . ? C12 C13 1.380(4) . ? C13 C14 1.383(5) . ? C14 C15 1.363(5) . ? C15 C16 1.381(4) . ? C17 C18 1.390(4) . ? C17 C22 1.399(4) . ? C18 C19 1.388(4) . ? C19 C20 1.379(4) . ? C20 C21 1.381(4) . ? C21 C22 1.388(4) . ? C23 C24 1.383(4) . ? C23 C28 1.392(4) . ? C24 C25 1.390(4) . ? C25 C26 1.374(5) . ? C26 C27 1.368(5) . ? C27 C28 1.388(5) . ? C29 C30 1.386(4) . ? C29 C34 1.397(4) . ? C30 C31 1.389(4) . ? C31 C32 1.379(4) . ? C32 C33 1.381(4) . ? C33 C34 1.384(4) . ? 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 C1 Fe1 C6 125.60(10) . . ? C1 Fe1 C2 41.38(10) . . ? C6 Fe1 C2 161.92(11) . . ? C1 Fe1 C7 162.04(10) . . ? C6 Fe1 C7 41.27(10) . . ? C2 Fe1 C7 154.73(11) . . ? C1 Fe1 C10 109.38(10) . . ? C6 Fe1 C10 41.04(10) . . ? C2 Fe1 C10 124.07(11) . . ? C7 Fe1 C10 68.79(11) . . ? C1 Fe1 C8 156.76(11) . . ? C6 Fe1 C8 68.64(11) . . ? C2 Fe1 C8 119.46(11) . . ? C7 Fe1 C8 40.57(11) . . ? C10 Fe1 C8 67.97(12) . . ? C1 Fe1 C5 41.25(9) . . ? C6 Fe1 C5 109.63(10) . . ? C2 Fe1 C5 68.94(10) . . ? C7 Fe1 C5 124.20(11) . . ? C10 Fe1 C5 125.42(11) . . ? C8 Fe1 C5 158.98(12) . . ? C1 Fe1 C3 68.61(11) . . ? C6 Fe1 C3 157.38(12) . . ? C2 Fe1 C3 40.20(12) . . ? C7 Fe1 C3 119.93(12) . . ? C10 Fe1 C3 158.52(12) . . ? C8 Fe1 C3 105.01(12) . . ? C5 Fe1 C3 68.13(11) . . ? C1 Fe1 C4 68.69(11) . . ? C6 Fe1 C4 123.10(11) . . ? C2 Fe1 C4 68.26(12) . . ? C7 Fe1 C4 106.71(12) . . ? C10 Fe1 C4 160.42(11) . . ? C8 Fe1 C4 121.80(13) . . ? C5 Fe1 C4 40.28(11) . . ? C3 Fe1 C4 40.50(13) . . ? C1 Fe1 C9 122.68(11) . . ? C6 Fe1 C9 68.56(10) . . ? C2 Fe1 C9 106.37(11) . . ? C7 Fe1 C9 68.29(12) . . ? C10 Fe1 C9 40.32(11) . . ? C8 Fe1 C9 40.23(13) . . ? C5 Fe1 C9 160.29(12) . . ? C3 Fe1 C9 121.41(12) . . ? C4 Fe1 C9 157.47(12) . . ? O1 Co1 O2 99.11(7) . . ? O1 Co1 Cl1 105.30(6) . . ? O2 Co1 Cl1 119.36(6) . . ? O1 Co1 Cl2 113.21(6) . . ? O2 Co1 Cl2 108.70(6) . . ? Cl1 Co1 Cl2 110.70(3) . . ? O1 P1 C1 112.90(11) . . ? O1 P1 C17 111.33(11) . . ? C1 P1 C17 106.92(12) . . ? O1 P1 C11 109.11(11) . . ? C1 P1 C11 107.81(12) . . ? C17 P1 C11 108.62(11) . . ? O2 P2 C6 114.24(11) . . ? O2 P2 C29 111.75(12) . . ? C6 P2 C29 107.33(12) . . ? O2 P2 C23 111.16(11) . . ? C6 P2 C23 104.01(12) . . ? C29 P2 C23 107.87(12) . . ? P1 O1 Co1 143.38(11) . . ? P2 O2 Co1 155.11(12) . . ? C2 C1 C5 107.1(2) . . ? C2 C1 P1 129.3(2) . . ? C5 C1 P1 123.49(19) . . ? C2 C1 Fe1 69.50(14) . . ? C5 C1 Fe1 70.13(14) . . ? P1 C1 Fe1 123.07(13) . . ? C3 C2 C1 108.1(2) . . ? C3 C2 Fe1 70.48(16) . . ? C1 C2 Fe1 69.11(14) . . ? C2 C3 C4 108.8(3) . . ? C2 C3 Fe1 69.32(16) . . ? C4 C3 Fe1 70.16(16) . . ? C5 C4 C3 108.0(3) . . ? C5 C4 Fe1 69.43(15) . . ? C3 C4 Fe1 69.33(17) . . ? C4 C5 C1 108.0(2) . . ? C4 C5 Fe1 70.28(16) . . ? C1 C5 Fe1 68.62(14) . . ? C10 C6 C7 107.3(2) . . ? C10 C6 P2 124.76(19) . . ? C7 C6 P2 127.36(19) . . ? C10 C6 Fe1 69.93(14) . . ? C7 C6 Fe1 69.62(14) . . ? P2 C6 Fe1 132.27(14) . . ? C8 C7 C6 107.5(2) . . ? C8 C7 Fe1 70.01(15) . . ? C6 C7 Fe1 69.11(14) . . ? C9 C8 C7 108.9(3) . . ? C9 C8 Fe1 70.43(16) . . ? C7 C8 Fe1 69.42(16) . . ? C8 C9 C10 107.9(2) . . ? C8 C9 Fe1 69.34(17) . . ? C10 C9 Fe1 69.20(15) . . ? C9 C10 C6 108.3(2) . . ? C9 C10 Fe1 70.48(16) . . ? C6 C10 Fe1 69.03(14) . . ? C12 C11 C16 120.0(2) . . ? C12 C11 P1 118.0(2) . . ? C16 C11 P1 122.0(2) . . ? C13 C12 C11 119.8(3) . . ? C12 C13 C14 119.7(3) . . ? C15 C14 C13 120.9(3) . . ? C14 C15 C16 120.0(3) . . ? C15 C16 C11 119.6(3) . . ? C18 C17 C22 120.2(2) . . ? C18 C17 P1 118.6(2) . . ? C22 C17 P1 121.2(2) . . ? C19 C18 C17 119.6(3) . . ? C20 C19 C18 120.0(3) . . ? C19 C20 C21 120.7(3) . . ? C20 C21 C22 120.1(3) . . ? C21 C22 C17 119.3(3) . . ? C24 C23 C28 119.0(3) . . ? C24 C23 P2 121.7(2) . . ? C28 C23 P2 119.2(2) . . ? C23 C24 C25 120.7(3) . . ? C26 C25 C24 119.5(3) . . ? C27 C26 C25 120.6(3) . . ? C26 C27 C28 120.4(3) . . ? C27 C28 C23 119.8(3) . . ? C30 C29 C34 119.8(2) . . ? C30 C29 P2 119.1(2) . . ? C34 C29 P2 121.0(2) . . ? C29 C30 C31 119.8(3) . . ? C32 C31 C30 120.2(3) . . ? C31 C32 C33 120.2(3) . . ? C32 C33 C34 120.1(3) . . ? C33 C34 C29 119.8(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.779 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.082 data_Cpd10 _database_code_depnum_ccdc_archive 'CCDC 823897' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Br2 Co Fe O2 P2' _chemical_formula_weight 805.10 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.1369(6) _cell_length_b 19.6944(12) _cell_length_c 16.1275(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.4830(10) _cell_angle_gamma 90.00 _cell_volume 3218.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3992 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.57 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1604 _exptl_absorpt_coefficient_mu 3.578 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2227 _exptl_absorpt_correction_T_max 0.7161 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11144 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6649 _reflns_number_gt 5923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0125P)^2^+0.9308P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(9) _refine_ls_number_reflns 6649 _refine_ls_number_parameters 425 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.4272(4) 0.3418(2) 0.3458(3) 0.0350(10) Uani 1 1 d D . . C12 C 0.2904(6) 0.3353(9) 0.3479(9) 0.053(3) Uani 0.55(2) 1 d PDU A 1 H12 H 0.2511 0.3078 0.3880 0.064 Uiso 0.55(2) 1 calc PR A 1 C13 C 0.2132(12) 0.3704(9) 0.2897(7) 0.055(3) Uani 0.55(2) 1 d PDU A 1 H13 H 0.1209 0.3657 0.2896 0.066 Uiso 0.55(2) 1 calc PR A 1 C14 C 0.2714(14) 0.4122(8) 0.2319(9) 0.052(3) Uani 0.55(2) 1 d PDU A 1 H14 H 0.2185 0.4384 0.1953 0.063 Uiso 0.55(2) 1 calc PR A 1 C15 C 0.4079(14) 0.4153(8) 0.2280(10) 0.052(3) Uani 0.55(2) 1 d PDU A 1 H15 H 0.4473 0.4414 0.1867 0.063 Uiso 0.55(2) 1 calc PR A 1 C16 C 0.4862(16) 0.3799(9) 0.2851(10) 0.049(3) Uani 0.55(2) 1 d PDU A 1 H16 H 0.5787 0.3819 0.2826 0.059 Uiso 0.55(2) 1 calc PR A 1 C12X C 0.5046(17) 0.3595(10) 0.2791(9) 0.046(4) Uani 0.45(2) 1 d PDU A 2 H12X H 0.5922 0.3439 0.2781 0.055 Uiso 0.45(2) 1 calc PR A 2 C13X C 0.4574(18) 0.3994(8) 0.2138(10) 0.049(4) Uani 0.45(2) 1 d PD A 2 H13X H 0.5131 0.4126 0.1710 0.059 Uiso 0.45(2) 1 calc PR A 2 C14X C 0.3260(19) 0.4195(9) 0.2130(10) 0.053(4) Uani 0.45(2) 1 d PDU A 2 H14X H 0.2900 0.4433 0.1672 0.064 Uiso 0.45(2) 1 calc PR A 2 C15X C 0.2478(18) 0.4044(11) 0.2801(10) 0.068(5) Uani 0.45(2) 1 d PD A 2 H15X H 0.1622 0.4226 0.2828 0.081 Uiso 0.45(2) 1 calc PR A 2 C16X C 0.2960(17) 0.3624(11) 0.3433(12) 0.057(3) Uani 0.45(2) 1 d PDU A 2 H16X H 0.2391 0.3478 0.3848 0.069 Uiso 0.45(2) 1 calc PR A 2 Co1 Co 0.35375(5) 0.35935(3) 0.60446(4) 0.03209(14) Uani 1 1 d . A . Br1 Br 0.18197(6) 0.43674(3) 0.56998(5) 0.0651(2) Uani 1 1 d . . . Br2 Br 0.29971(7) 0.26443(3) 0.68806(5) 0.0679(2) Uani 1 1 d . . . Fe1 Fe 0.78026(6) 0.32525(3) 0.55029(4) 0.03280(15) Uani 1 1 d . A . P1 P 0.50561(11) 0.30094(6) 0.43376(7) 0.0305(2) Uani 1 1 d . A . P2 P 0.62237(11) 0.40061(6) 0.70763(7) 0.0324(2) Uani 1 1 d . A . O1 O 0.4235(3) 0.31238(19) 0.5079(2) 0.0429(8) Uani 1 1 d . . . O2 O 0.4994(3) 0.41238(18) 0.6556(2) 0.0393(7) Uani 1 1 d . . . C1 C 0.6671(4) 0.3348(3) 0.4445(3) 0.0354(10) Uani 1 1 d . . . C2 C 0.7907(4) 0.3022(3) 0.4271(3) 0.0388(11) Uani 1 1 d . A . H2 H 0.8021 0.2564 0.4031 0.047 Uiso 1 1 calc R . . C3 C 0.8922(5) 0.3478(3) 0.4505(3) 0.0506(14) Uani 1 1 d . . . H3 H 0.9879 0.3386 0.4465 0.061 Uiso 1 1 calc R A . C4 C 0.8366(5) 0.4080(3) 0.4823(3) 0.0464(13) Uani 1 1 d . A . H4 H 0.8859 0.4480 0.5036 0.056 Uiso 1 1 calc R . . C5 C 0.6952(5) 0.4005(3) 0.4776(3) 0.0376(10) Uani 1 1 d . A . H5 H 0.6296 0.4343 0.4956 0.045 Uiso 1 1 calc R . . C6 C 0.7255(4) 0.3351(2) 0.6703(3) 0.0330(10) Uani 1 1 d . . . C7 C 0.8666(5) 0.3377(3) 0.6639(3) 0.0422(11) Uani 1 1 d . A . H7 H 0.9242 0.3759 0.6813 0.051 Uiso 1 1 calc R . . C8 C 0.9088(5) 0.2756(3) 0.6301(3) 0.0501(14) Uani 1 1 d . . . H8 H 1.0011 0.2632 0.6184 0.060 Uiso 1 1 calc R A . C9 C 0.7962(5) 0.2345(3) 0.6137(3) 0.0447(12) Uani 1 1 d . A . H9 H 0.7966 0.1888 0.5883 0.054 Uiso 1 1 calc R . . C10 C 0.6825(5) 0.2708(2) 0.6377(3) 0.0360(10) Uani 1 1 d . A . H10 H 0.5901 0.2546 0.6331 0.043 Uiso 1 1 calc R . . C17 C 0.5255(4) 0.2115(2) 0.4175(3) 0.0325(9) Uani 1 1 d . . . C18 C 0.5717(5) 0.1862(3) 0.3433(3) 0.0402(11) Uani 1 1 d . A . H18 H 0.5822 0.2154 0.2978 0.048 Uiso 1 1 calc R . . C19 C 0.6024(6) 0.1173(3) 0.3365(4) 0.0529(14) Uani 1 1 d . . . H19 H 0.6325 0.0999 0.2860 0.063 Uiso 1 1 calc R A . C20 C 0.5891(6) 0.0755(3) 0.4022(4) 0.0573(16) Uani 1 1 d . A . H20 H 0.6139 0.0297 0.3980 0.069 Uiso 1 1 calc R . . C21 C 0.5390(6) 0.0998(3) 0.4758(4) 0.0547(14) Uani 1 1 d . . . H21 H 0.5263 0.0698 0.5203 0.066 Uiso 1 1 calc R A . C22 C 0.5079(6) 0.1677(3) 0.4842(3) 0.0445(12) Uani 1 1 d . A . H22 H 0.4752 0.1842 0.5343 0.053 Uiso 1 1 calc R . . C23 C 0.5861(5) 0.3812(3) 0.8139(3) 0.0395(11) Uani 1 1 d . . . C24 C 0.4875(6) 0.4176(4) 0.8509(4) 0.0630(17) Uani 1 1 d . A . H24 H 0.4377 0.4497 0.8203 0.076 Uiso 1 1 calc R . . C25 C 0.4625(7) 0.4060(5) 0.9349(5) 0.077(2) Uani 1 1 d . . . H25 H 0.3943 0.4300 0.9604 0.093 Uiso 1 1 calc R A . C26 C 0.5353(7) 0.3609(4) 0.9796(4) 0.073(2) Uani 1 1 d . A . H26 H 0.5185 0.3544 1.0361 0.088 Uiso 1 1 calc R . . C27 C 0.6347(7) 0.3240(4) 0.9426(4) 0.0677(19) Uani 1 1 d . . . H27 H 0.6841 0.2920 0.9735 0.081 Uiso 1 1 calc R A . C28 C 0.6604(6) 0.3349(3) 0.8592(3) 0.0541(14) Uani 1 1 d . A . H28 H 0.7284 0.3107 0.8338 0.065 Uiso 1 1 calc R . . C29 C 0.7212(4) 0.4759(2) 0.7103(3) 0.0325(9) Uani 1 1 d . . . C30 C 0.7123(6) 0.5209(3) 0.6442(4) 0.0492(13) Uani 1 1 d . A . H30 H 0.6513 0.5130 0.6004 0.059 Uiso 1 1 calc R . . C31 C 0.7936(6) 0.5776(3) 0.6428(4) 0.0584(15) Uani 1 1 d . . . H31 H 0.7897 0.6073 0.5972 0.070 Uiso 1 1 calc R A . C32 C 0.8790(6) 0.5899(3) 0.7075(4) 0.0572(15) Uani 1 1 d . A . H32 H 0.9325 0.6289 0.7067 0.069 Uiso 1 1 calc R . . C33 C 0.8884(5) 0.5464(3) 0.7740(4) 0.0525(14) Uani 1 1 d . . . H33 H 0.9479 0.5555 0.8182 0.063 Uiso 1 1 calc R A . C34 C 0.8090(5) 0.4887(3) 0.7754(3) 0.0448(12) Uani 1 1 d . A . H34 H 0.8152 0.4585 0.8205 0.054 Uiso 1 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 C11 0.037(2) 0.029(2) 0.038(2) -0.0014(19) -0.0082(19) -0.0008(19) C12 0.050(4) 0.058(8) 0.051(5) 0.015(5) -0.005(4) 0.028(5) C13 0.045(4) 0.063(7) 0.057(5) 0.013(5) -0.008(4) 0.023(4) C14 0.051(6) 0.053(6) 0.053(6) 0.010(5) -0.009(5) 0.012(5) C15 0.056(6) 0.045(6) 0.055(5) 0.015(5) -0.014(5) -0.005(5) C16 0.053(5) 0.039(8) 0.055(5) 0.019(5) -0.019(4) -0.014(5) C12X 0.050(6) 0.037(9) 0.049(5) 0.013(6) -0.010(5) -0.012(6) C13X 0.059(9) 0.034(8) 0.053(8) -0.006(6) -0.009(7) 0.001(7) C14X 0.059(8) 0.048(7) 0.052(7) 0.004(5) -0.017(6) 0.005(7) C15X 0.065(10) 0.063(12) 0.074(11) 0.032(10) -0.015(9) 0.006(9) C16X 0.050(5) 0.067(9) 0.054(5) 0.013(7) -0.003(5) 0.029(6) Co1 0.0291(3) 0.0309(3) 0.0363(3) -0.0004(3) 0.0012(2) -0.0008(2) Br1 0.0462(3) 0.0519(3) 0.0959(5) -0.0065(3) -0.0270(3) 0.0142(3) Br2 0.0790(4) 0.0475(3) 0.0791(4) 0.0195(3) 0.0406(3) 0.0057(3) Fe1 0.0280(3) 0.0371(4) 0.0331(3) -0.0018(3) -0.0040(2) -0.0001(3) P1 0.0275(5) 0.0348(6) 0.0291(5) -0.0005(4) -0.0011(4) -0.0041(5) P2 0.0314(5) 0.0320(6) 0.0335(6) -0.0018(5) -0.0059(4) 0.0009(5) O1 0.0354(16) 0.053(2) 0.0407(19) -0.0052(16) 0.0057(14) -0.0059(16) O2 0.0330(15) 0.0400(19) 0.0444(19) -0.0067(15) -0.0100(14) 0.0029(15) C1 0.0244(19) 0.049(3) 0.032(2) 0.0021(19) -0.0050(17) -0.0036(19) C2 0.031(2) 0.056(3) 0.029(2) -0.001(2) -0.0013(18) -0.006(2) C3 0.031(2) 0.078(4) 0.042(3) 0.002(3) 0.004(2) -0.007(3) C4 0.042(3) 0.055(3) 0.042(3) 0.004(2) -0.006(2) -0.022(3) C5 0.039(2) 0.039(3) 0.034(2) 0.0080(19) -0.0084(19) -0.008(2) C6 0.039(2) 0.033(2) 0.027(2) 0.0042(18) -0.0041(18) 0.0040(19) C7 0.040(2) 0.047(3) 0.039(3) -0.002(2) -0.012(2) 0.004(2) C8 0.042(3) 0.062(4) 0.046(3) -0.004(2) -0.008(2) 0.022(3) C9 0.048(3) 0.033(3) 0.052(3) 0.002(2) 0.001(2) 0.014(2) C10 0.041(2) 0.031(2) 0.036(2) 0.0052(18) -0.0036(19) 0.002(2) C17 0.030(2) 0.032(2) 0.035(2) 0.0034(18) -0.0044(17) -0.0044(18) C18 0.038(2) 0.044(3) 0.038(3) 0.000(2) -0.002(2) -0.005(2) C19 0.053(3) 0.055(4) 0.050(3) -0.013(3) -0.002(3) 0.006(3) C20 0.062(3) 0.033(3) 0.076(4) -0.005(3) -0.016(3) 0.004(3) C21 0.071(4) 0.041(3) 0.052(3) 0.006(2) -0.008(3) -0.010(3) C22 0.056(3) 0.040(3) 0.037(3) -0.005(2) 0.001(2) -0.011(2) C23 0.035(2) 0.048(3) 0.035(2) -0.001(2) -0.0041(19) -0.010(2) C24 0.053(3) 0.089(5) 0.048(3) -0.005(3) 0.007(3) 0.006(3) C25 0.051(3) 0.122(7) 0.061(4) -0.007(4) 0.023(3) 0.006(4) C26 0.075(4) 0.106(6) 0.040(3) 0.005(3) 0.010(3) -0.032(4) C27 0.075(4) 0.086(5) 0.042(3) 0.014(3) 0.001(3) -0.010(4) C28 0.062(3) 0.064(4) 0.037(3) 0.007(3) 0.005(3) 0.004(3) C29 0.030(2) 0.030(2) 0.037(2) -0.0021(18) -0.0045(17) -0.0005(18) C30 0.063(3) 0.032(3) 0.051(3) -0.001(2) -0.021(3) 0.003(2) C31 0.071(4) 0.041(3) 0.063(4) 0.016(3) -0.012(3) -0.006(3) C32 0.050(3) 0.033(3) 0.088(5) 0.000(3) -0.006(3) -0.010(2) C33 0.041(3) 0.052(3) 0.064(4) -0.001(3) -0.016(3) -0.011(3) C34 0.045(3) 0.045(3) 0.043(3) 0.003(2) -0.011(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C16 1.382(14) . ? C11 C16X 1.391(17) . ? C11 C12X 1.393(5) . ? C11 C12 1.394(5) . ? C11 P1 1.798(5) . ? C12 C13 1.390(5) . ? C13 C14 1.388(5) . ? C14 C15 1.388(5) . ? C15 C16 1.388(5) . ? C12X C13X 1.390(5) . ? C13X C14X 1.389(5) . ? C14X C15X 1.390(5) . ? C15X C16X 1.391(5) . ? Co1 O1 1.959(3) . ? Co1 O2 1.972(3) . ? Co1 Br1 2.3695(8) . ? Co1 Br2 2.3770(8) . ? Fe1 C7 2.024(5) . ? Fe1 C6 2.036(5) . ? Fe1 C1 2.040(4) . ? Fe1 C3 2.042(5) . ? Fe1 C2 2.043(5) . ? Fe1 C10 2.048(5) . ? Fe1 C4 2.053(5) . ? Fe1 C8 2.055(5) . ? Fe1 C9 2.063(5) . ? Fe1 C5 2.064(5) . ? P1 O1 1.491(4) . ? P1 C1 1.772(5) . ? P1 C17 1.793(5) . ? P2 O2 1.502(3) . ? P2 C6 1.775(5) . ? P2 C29 1.790(5) . ? P2 C23 1.803(5) . ? C1 C5 1.426(7) . ? C1 C2 1.442(7) . ? C2 C3 1.409(8) . ? C3 C4 1.414(9) . ? C4 C5 1.441(7) . ? C6 C10 1.434(7) . ? C6 C7 1.438(7) . ? C7 C8 1.409(8) . ? C8 C9 1.418(8) . ? C9 C10 1.419(7) . ? C17 C18 1.388(7) . ? C17 C22 1.394(7) . ? C18 C19 1.398(8) . ? C19 C20 1.351(9) . ? C20 C21 1.388(9) . ? C21 C22 1.382(8) . ? C23 C24 1.379(8) . ? C23 C28 1.380(8) . ? C24 C25 1.403(9) . ? C25 C26 1.352(11) . ? C26 C27 1.390(11) . ? C27 C28 1.393(8) . ? C29 C34 1.383(7) . ? C29 C30 1.387(7) . ? C30 C31 1.388(8) . ? C31 C32 1.361(8) . ? C32 C33 1.374(9) . ? C33 C34 1.392(8) . ? 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 C16 C11 C16X 104.6(9) . . ? C16 C11 C12X 18.9(11) . . ? C16X C11 C12X 117.5(11) . . ? C16 C11 C12 121.1(8) . . ? C16X C11 C12 22.5(9) . . ? C12X C11 C12 128.5(10) . . ? C16 C11 P1 127.7(7) . . ? C16X C11 P1 123.8(8) . . ? C12X C11 P1 118.4(8) . . ? C12 C11 P1 111.1(6) . . ? C13 C12 C11 118.8(9) . . ? C14 C13 C12 120.4(11) . . ? C15 C14 C13 119.8(11) . . ? C16 C15 C14 120.2(13) . . ? C11 C16 C15 119.4(13) . . ? C13X C12X C11 122.5(14) . . ? C14X C13X C12X 118.6(15) . . ? C13X C14X C15X 119.9(14) . . ? C14X C15X C16X 120.0(15) . . ? C11 C16X C15X 120.8(15) . . ? O1 Co1 O2 107.51(14) . . ? O1 Co1 Br1 113.27(11) . . ? O2 Co1 Br1 107.17(10) . . ? O1 Co1 Br2 99.95(12) . . ? O2 Co1 Br2 111.13(11) . . ? Br1 Co1 Br2 117.40(3) . . ? C7 Fe1 C6 41.48(19) . . ? C7 Fe1 C1 165.1(2) . . ? C6 Fe1 C1 128.65(18) . . ? C7 Fe1 C3 116.8(2) . . ? C6 Fe1 C3 154.0(2) . . ? C1 Fe1 C3 68.5(2) . . ? C7 Fe1 C2 151.0(2) . . ? C6 Fe1 C2 165.34(19) . . ? C1 Fe1 C2 41.36(19) . . ? C3 Fe1 C2 40.4(2) . . ? C7 Fe1 C10 69.2(2) . . ? C6 Fe1 C10 41.11(19) . . ? C1 Fe1 C10 110.64(19) . . ? C3 Fe1 C10 161.0(2) . . ? C2 Fe1 C10 126.3(2) . . ? C7 Fe1 C4 105.5(2) . . ? C6 Fe1 C4 121.2(2) . . ? C1 Fe1 C4 68.8(2) . . ? C3 Fe1 C4 40.4(3) . . ? C2 Fe1 C4 68.6(2) . . ? C10 Fe1 C4 158.4(2) . . ? C7 Fe1 C8 40.4(2) . . ? C6 Fe1 C8 68.56(19) . . ? C1 Fe1 C8 154.4(2) . . ? C3 Fe1 C8 103.9(2) . . ? C2 Fe1 C8 117.1(2) . . ? C10 Fe1 C8 68.3(2) . . ? C4 Fe1 C8 122.1(2) . . ? C7 Fe1 C9 68.2(2) . . ? C6 Fe1 C9 68.4(2) . . ? C1 Fe1 C9 122.0(2) . . ? C3 Fe1 C9 122.8(2) . . ? C2 Fe1 C9 106.5(2) . . ? C10 Fe1 C9 40.4(2) . . ? C4 Fe1 C9 158.9(2) . . ? C8 Fe1 C9 40.3(2) . . ? C7 Fe1 C5 126.3(2) . . ? C6 Fe1 C5 110.5(2) . . ? C1 Fe1 C5 40.7(2) . . ? C3 Fe1 C5 68.2(2) . . ? C2 Fe1 C5 68.8(2) . . ? C10 Fe1 C5 124.4(2) . . ? C4 Fe1 C5 41.0(2) . . ? C8 Fe1 C5 161.1(2) . . ? C9 Fe1 C5 158.4(2) . . ? O1 P1 C1 113.5(2) . . ? O1 P1 C17 109.5(2) . . ? C1 P1 C17 106.1(2) . . ? O1 P1 C11 108.7(2) . . ? C1 P1 C11 107.3(2) . . ? C17 P1 C11 111.9(2) . . ? O2 P2 C6 114.2(2) . . ? O2 P2 C29 109.9(2) . . ? C6 P2 C29 106.0(2) . . ? O2 P2 C23 112.2(2) . . ? C6 P2 C23 107.8(2) . . ? C29 P2 C23 106.3(2) . . ? P1 O1 Co1 158.3(2) . . ? P2 O2 Co1 138.9(2) . . ? C5 C1 C2 108.1(4) . . ? C5 C1 P1 123.6(4) . . ? C2 C1 P1 128.2(4) . . ? C5 C1 Fe1 70.6(2) . . ? C2 C1 Fe1 69.4(2) . . ? P1 C1 Fe1 123.1(3) . . ? C3 C2 C1 107.3(5) . . ? C3 C2 Fe1 69.8(3) . . ? C1 C2 Fe1 69.2(3) . . ? C2 C3 C4 109.6(5) . . ? C2 C3 Fe1 69.8(3) . . ? C4 C3 Fe1 70.2(3) . . ? C3 C4 C5 107.5(5) . . ? C3 C4 Fe1 69.4(3) . . ? C5 C4 Fe1 69.9(3) . . ? C1 C5 C4 107.5(5) . . ? C1 C5 Fe1 68.8(3) . . ? C4 C5 Fe1 69.1(3) . . ? C10 C6 C7 107.3(4) . . ? C10 C6 P2 126.1(4) . . ? C7 C6 P2 126.5(4) . . ? C10 C6 Fe1 69.9(3) . . ? C7 C6 Fe1 68.8(3) . . ? P2 C6 Fe1 124.7(2) . . ? C8 C7 C6 108.1(5) . . ? C8 C7 Fe1 71.0(3) . . ? C6 C7 Fe1 69.7(3) . . ? C7 C8 C9 108.4(4) . . ? C7 C8 Fe1 68.6(3) . . ? C9 C8 Fe1 70.2(3) . . ? C8 C9 C10 108.5(5) . . ? C8 C9 Fe1 69.6(3) . . ? C10 C9 Fe1 69.2(3) . . ? C9 C10 C6 107.7(4) . . ? C9 C10 Fe1 70.4(3) . . ? C6 C10 Fe1 69.0(3) . . ? C18 C17 C22 119.8(5) . . ? C18 C17 P1 121.3(4) . . ? C22 C17 P1 118.5(4) . . ? C17 C18 C19 119.8(5) . . ? C20 C19 C18 120.1(5) . . ? C19 C20 C21 120.6(6) . . ? C22 C21 C20 120.3(5) . . ? C21 C22 C17 119.3(5) . . ? C24 C23 C28 120.4(5) . . ? C24 C23 P2 118.0(4) . . ? C28 C23 P2 121.4(4) . . ? C23 C24 C25 119.0(7) . . ? C26 C25 C24 120.8(7) . . ? C25 C26 C27 120.4(6) . . ? C26 C27 C28 119.3(7) . . ? C23 C28 C27 120.0(6) . . ? C34 C29 C30 119.7(5) . . ? C34 C29 P2 121.2(4) . . ? C30 C29 P2 119.1(4) . . ? C29 C30 C31 120.0(5) . . ? C32 C31 C30 119.8(6) . . ? C31 C32 C33 121.1(6) . . ? C32 C33 C34 119.6(5) . . ? C29 C34 C33 119.8(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.809 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.083 data_Cpd11 _database_code_depnum_ccdc_archive 'CCDC 823898' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Co Fe I2 O2 P2' _chemical_formula_weight 899.08 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.3600(7) _cell_length_b 20.4629(13) _cell_length_c 16.0513(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.800(2) _cell_angle_gamma 90.00 _cell_volume 3398.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5160 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.95 _exptl_crystal_description PLATE _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 2.854 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2792 _exptl_absorpt_correction_T_max 0.7257 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11844 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6255 _reflns_number_gt 5824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0572P)^2^+0.9318P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 6255 _refine_ls_number_parameters 425 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.4210(6) 0.3399(3) 0.3427(4) 0.0407(13) Uani 1 1 d D . . C12 C 0.2873(7) 0.3310(7) 0.3397(7) 0.048(3) Uani 0.63(3) 1 d PDU A 1 H12 H 0.2506 0.3036 0.3792 0.057 Uiso 0.63(3) 1 calc PR A 1 C13 C 0.2070(14) 0.3616(7) 0.2797(8) 0.058(3) Uani 0.63(3) 1 d PDU A 1 H13 H 0.1170 0.3555 0.2776 0.069 Uiso 0.63(3) 1 calc PR A 1 C14 C 0.2661(17) 0.4017(6) 0.2230(9) 0.061(3) Uani 0.63(3) 1 d PDU A 1 H14 H 0.2146 0.4235 0.1820 0.073 Uiso 0.63(3) 1 calc PR A 1 C15 C 0.3993(18) 0.4107(8) 0.2253(9) 0.064(3) Uani 0.63(3) 1 d PDU A 1 H15 H 0.4373 0.4378 0.1861 0.076 Uiso 0.63(3) 1 calc PR A 1 C16 C 0.4753(18) 0.3788(7) 0.2864(7) 0.064(4) Uani 0.63(3) 1 d PDU A 1 H16 H 0.5654 0.3845 0.2884 0.077 Uiso 0.63(3) 1 calc PR A 1 C12X C 0.499(2) 0.3609(10) 0.2796(10) 0.058(4) Uani 0.37(3) 1 d PDU A 2 H12X H 0.5870 0.3503 0.2835 0.070 Uiso 0.37(3) 1 calc PR A 2 C13X C 0.452(2) 0.3967(10) 0.2110(16) 0.053(6) Uani 0.37(3) 1 d PD A 2 H13X H 0.5055 0.4105 0.1689 0.063 Uiso 0.37(3) 1 calc PR A 2 C14X C 0.320(2) 0.4110(10) 0.2081(14) 0.057(6) Uani 0.37(3) 1 d PDU A 2 H14X H 0.2847 0.4352 0.1627 0.068 Uiso 0.37(3) 1 calc PR A 2 C15X C 0.240(2) 0.3910(16) 0.2699(15) 0.090(11) Uani 0.37(3) 1 d PD A 2 H15X H 0.1514 0.4016 0.2663 0.107 Uiso 0.37(3) 1 calc PR A 2 C16X C 0.291(3) 0.3551(13) 0.3372(15) 0.058(4) Uani 0.37(3) 1 d PDU A 2 H16X H 0.2373 0.3412 0.3792 0.070 Uiso 0.37(3) 1 calc PR A 2 Co1 Co 0.36132(7) 0.35984(4) 0.60441(5) 0.03221(16) Uani 1 1 d . A . I1 I 0.17761(6) 0.44031(2) 0.56806(4) 0.06151(15) Uani 1 1 d . . . I2 I 0.30946(6) 0.26049(2) 0.69507(4) 0.05967(15) Uani 1 1 d . . . Fe1 Fe 0.77615(8) 0.32970(4) 0.54804(5) 0.03358(18) Uani 1 1 d . A . P1 P 0.50074(14) 0.30278(7) 0.43295(9) 0.0326(3) Uani 1 1 d . A . P2 P 0.62720(14) 0.40099(7) 0.70705(9) 0.0334(3) Uani 1 1 d . A . O1 O 0.4222(4) 0.3149(2) 0.5074(3) 0.0431(10) Uani 1 1 d . . . O2 O 0.5045(4) 0.4107(2) 0.6539(3) 0.0397(9) Uani 1 1 d . . . C1 C 0.6584(6) 0.3365(3) 0.4427(4) 0.0408(13) Uani 1 1 d . . . C2 C 0.7780(6) 0.3064(4) 0.4249(4) 0.0434(14) Uani 1 1 d . A . H2 H 0.7892 0.2621 0.4014 0.052 Uiso 1 1 calc R . . C3 C 0.8784(6) 0.3516(4) 0.4465(4) 0.0512(17) Uani 1 1 d . . . H3 H 0.9719 0.3437 0.4414 0.061 Uiso 1 1 calc R A . C4 C 0.8226(8) 0.4101(4) 0.4780(4) 0.0540(18) Uani 1 1 d . A . H4 H 0.8697 0.4495 0.4982 0.065 Uiso 1 1 calc R . . C5 C 0.6863(6) 0.4003(3) 0.4756(4) 0.0431(14) Uani 1 1 d . A . H5 H 0.6217 0.4320 0.4945 0.052 Uiso 1 1 calc R . . C6 C 0.7305(5) 0.3384(3) 0.6692(3) 0.0354(12) Uani 1 1 d . . . C7 C 0.8666(6) 0.3432(3) 0.6618(4) 0.0435(14) Uani 1 1 d . A . H7 H 0.9218 0.3808 0.6790 0.052 Uiso 1 1 calc R . . C8 C 0.9090(6) 0.2834(4) 0.6269(4) 0.0522(17) Uani 1 1 d . . . H8 H 0.9991 0.2727 0.6141 0.063 Uiso 1 1 calc R A . C9 C 0.8024(7) 0.2432(3) 0.6126(4) 0.0476(15) Uani 1 1 d . A . H9 H 0.8040 0.1991 0.5873 0.057 Uiso 1 1 calc R . . C10 C 0.6895(6) 0.2764(3) 0.6383(3) 0.0356(11) Uani 1 1 d . A . H10 H 0.6000 0.2593 0.6355 0.043 Uiso 1 1 calc R . . C17 C 0.5204(5) 0.2162(3) 0.4189(4) 0.0367(12) Uani 1 1 d . . . C18 C 0.5621(6) 0.1917(3) 0.3444(4) 0.0421(13) Uani 1 1 d . A . H18 H 0.5700 0.2195 0.2984 0.051 Uiso 1 1 calc R . . C19 C 0.5919(7) 0.1261(3) 0.3380(4) 0.0496(16) Uani 1 1 d . . . H19 H 0.6199 0.1092 0.2875 0.060 Uiso 1 1 calc R A . C20 C 0.5806(8) 0.0855(4) 0.4061(5) 0.0578(18) Uani 1 1 d . A . H20 H 0.6038 0.0412 0.4025 0.069 Uiso 1 1 calc R . . C21 C 0.5355(8) 0.1096(4) 0.4792(5) 0.0595(19) Uani 1 1 d . . . H21 H 0.5251 0.0813 0.5244 0.071 Uiso 1 1 calc R A . C22 C 0.5055(7) 0.1747(3) 0.4867(4) 0.0476(15) Uani 1 1 d . A . H22 H 0.4752 0.1910 0.5369 0.057 Uiso 1 1 calc R . . C23 C 0.5928(6) 0.3813(4) 0.8131(4) 0.0443(14) Uani 1 1 d . . . C24 C 0.4912(8) 0.4132(6) 0.8479(5) 0.074(3) Uani 1 1 d . A . H24 H 0.4402 0.4434 0.8169 0.089 Uiso 1 1 calc R . . C25 C 0.4662(10) 0.3988(7) 0.9319(7) 0.093(3) Uani 1 1 d . . . H25 H 0.3973 0.4199 0.9568 0.111 Uiso 1 1 calc R A . C26 C 0.5389(10) 0.3554(6) 0.9773(6) 0.084(3) Uani 1 1 d . A . H26 H 0.5196 0.3464 1.0328 0.101 Uiso 1 1 calc R . . C27 C 0.6418(10) 0.3243(5) 0.9419(5) 0.075(3) Uani 1 1 d . . . H27 H 0.6932 0.2944 0.9732 0.090 Uiso 1 1 calc R A . C28 C 0.6677(8) 0.3380(4) 0.8603(4) 0.0543(17) Uani 1 1 d . A . H28 H 0.7380 0.3174 0.8363 0.065 Uiso 1 1 calc R . . C29 C 0.7216(5) 0.4744(3) 0.7097(4) 0.0376(12) Uani 1 1 d . . . C30 C 0.7059(7) 0.5186(3) 0.6436(5) 0.0518(16) Uani 1 1 d . A . H30 H 0.6418 0.5118 0.6010 0.062 Uiso 1 1 calc R . . C31 C 0.7856(10) 0.5720(4) 0.6419(6) 0.071(2) Uani 1 1 d . . . H31 H 0.7765 0.6018 0.5974 0.085 Uiso 1 1 calc R A . C32 C 0.8799(8) 0.5827(4) 0.7053(6) 0.066(2) Uani 1 1 d . A . H32 H 0.9335 0.6197 0.7035 0.079 Uiso 1 1 calc R . . C33 C 0.8944(7) 0.5402(4) 0.7690(5) 0.0570(18) Uani 1 1 d . . . H33 H 0.9580 0.5477 0.8117 0.068 Uiso 1 1 calc R A . C34 C 0.8155(6) 0.4852(4) 0.7721(4) 0.0484(15) Uani 1 1 d . A . H34 H 0.8262 0.4556 0.8166 0.058 Uiso 1 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 C11 0.039(3) 0.045(3) 0.037(3) -0.004(2) -0.012(2) 0.005(3) C12 0.048(5) 0.041(7) 0.053(5) 0.001(5) -0.009(4) 0.016(5) C13 0.053(5) 0.057(6) 0.062(5) 0.009(5) -0.009(4) 0.020(4) C14 0.065(7) 0.059(6) 0.057(6) 0.010(5) -0.015(6) 0.004(5) C15 0.072(7) 0.060(7) 0.056(6) 0.021(5) -0.020(5) -0.006(6) C16 0.069(7) 0.061(7) 0.060(6) 0.030(5) -0.021(5) -0.022(6) C12X 0.068(8) 0.050(8) 0.055(7) 0.021(6) -0.021(6) -0.019(7) C13X 0.050(12) 0.032(10) 0.076(15) 0.006(9) -0.003(11) 0.007(9) C14X 0.060(10) 0.059(9) 0.051(9) 0.013(7) -0.009(8) -0.001(8) C15X 0.046(14) 0.13(3) 0.09(2) 0.05(2) -0.027(15) 0.003(16) C16X 0.055(6) 0.057(9) 0.062(7) 0.007(8) -0.007(6) 0.030(7) Co1 0.0280(3) 0.0331(4) 0.0354(4) 0.0013(3) 0.0002(3) 0.0000(3) I1 0.0418(2) 0.0482(3) 0.0922(4) -0.0025(2) -0.0200(2) 0.0109(2) I2 0.0701(3) 0.0481(2) 0.0635(3) 0.0185(2) 0.0304(2) 0.0042(2) Fe1 0.0270(4) 0.0435(5) 0.0299(4) -0.0027(3) -0.0016(3) -0.0006(3) P1 0.0299(6) 0.0408(7) 0.0268(6) 0.0010(5) -0.0021(5) -0.0036(6) P2 0.0297(6) 0.0365(7) 0.0333(7) -0.0046(5) -0.0042(5) 0.0007(5) O1 0.038(2) 0.052(3) 0.040(2) -0.0077(19) 0.0080(18) -0.0061(18) O2 0.0320(19) 0.036(2) 0.051(2) -0.0076(17) -0.0088(17) 0.0033(17) C1 0.033(3) 0.058(4) 0.031(3) -0.004(2) -0.002(2) -0.004(3) C2 0.035(3) 0.067(4) 0.028(3) -0.006(3) 0.001(2) -0.004(3) C3 0.036(3) 0.080(5) 0.039(3) 0.003(3) 0.005(3) -0.012(3) C4 0.057(4) 0.068(5) 0.037(3) 0.006(3) -0.001(3) -0.024(4) C5 0.044(3) 0.050(4) 0.034(3) 0.010(3) -0.007(2) -0.008(3) C6 0.034(3) 0.041(3) 0.031(3) 0.002(2) -0.006(2) 0.003(2) C7 0.036(3) 0.061(4) 0.033(3) -0.009(3) -0.014(2) 0.005(3) C8 0.034(3) 0.080(5) 0.042(3) 0.006(3) -0.004(3) 0.019(3) C9 0.055(4) 0.040(3) 0.047(4) 0.004(3) 0.005(3) 0.016(3) C10 0.042(3) 0.034(3) 0.031(3) 0.001(2) -0.001(2) 0.001(2) C17 0.029(3) 0.044(3) 0.036(3) -0.001(2) -0.004(2) -0.004(2) C18 0.039(3) 0.051(4) 0.036(3) -0.001(2) -0.003(2) -0.004(3) C19 0.054(4) 0.049(4) 0.045(4) -0.012(3) -0.005(3) 0.003(3) C20 0.067(5) 0.037(4) 0.069(5) -0.007(3) -0.012(4) 0.002(3) C21 0.077(5) 0.041(4) 0.059(5) 0.007(3) -0.012(4) -0.006(3) C22 0.053(4) 0.048(4) 0.042(3) 0.005(3) -0.002(3) -0.009(3) C23 0.032(3) 0.064(4) 0.036(3) -0.004(3) -0.003(2) -0.005(3) C24 0.054(4) 0.118(8) 0.052(4) -0.008(5) 0.015(4) 0.016(5) C25 0.068(6) 0.144(11) 0.069(6) -0.013(6) 0.031(5) 0.002(6) C26 0.076(6) 0.134(9) 0.044(4) -0.004(5) 0.017(4) -0.039(6) C27 0.085(6) 0.094(7) 0.045(4) 0.012(4) 0.004(4) -0.008(5) C28 0.058(4) 0.068(5) 0.037(3) 0.007(3) 0.005(3) 0.001(3) C29 0.031(3) 0.039(3) 0.043(3) -0.008(2) -0.003(2) 0.001(2) C30 0.052(4) 0.040(3) 0.062(4) 0.003(3) -0.017(3) -0.004(3) C31 0.083(6) 0.046(4) 0.081(6) 0.019(4) -0.020(5) -0.009(4) C32 0.047(4) 0.039(4) 0.111(7) 0.006(4) -0.013(4) -0.008(3) C33 0.042(4) 0.050(4) 0.077(5) -0.011(4) -0.016(3) 0.000(3) C34 0.044(3) 0.054(4) 0.046(3) -0.001(3) -0.007(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C16 1.349(16) . ? C11 C16X 1.38(3) . ? C11 C12X 1.392(5) . ? C11 C12 1.395(5) . ? C11 P1 1.800(6) . ? C12 C13 1.390(5) . ? C13 C14 1.389(5) . ? C14 C15 1.390(5) . ? C15 C16 1.389(5) . ? C12X C13X 1.391(5) . ? C13X C14X 1.389(5) . ? C14X C15X 1.389(5) . ? C15X C16X 1.390(5) . ? Co1 O1 1.940(4) . ? Co1 O2 1.950(4) . ? Co1 I1 2.5624(8) . ? Co1 I2 2.5722(8) . ? Fe1 C7 2.030(6) . ? Fe1 C6 2.031(6) . ? Fe1 C2 2.035(6) . ? Fe1 C3 2.036(6) . ? Fe1 C1 2.040(6) . ? Fe1 C5 2.049(6) . ? Fe1 C8 2.055(6) . ? Fe1 C10 2.055(6) . ? Fe1 C4 2.063(7) . ? Fe1 C9 2.063(7) . ? P1 O1 1.498(4) . ? P1 C1 1.773(6) . ? P1 C17 1.798(7) . ? P2 O2 1.509(4) . ? P2 C29 1.792(6) . ? P2 C6 1.794(6) . ? P2 C23 1.801(7) . ? C1 C2 1.425(9) . ? C1 C5 1.433(10) . ? C2 C3 1.422(9) . ? C3 C4 1.431(12) . ? C4 C5 1.425(10) . ? C6 C10 1.420(8) . ? C6 C7 1.424(8) . ? C7 C8 1.424(10) . ? C8 C9 1.388(11) . ? C9 C10 1.432(9) . ? C17 C18 1.385(8) . ? C17 C22 1.396(9) . ? C18 C19 1.381(10) . ? C19 C20 1.384(11) . ? C20 C21 1.374(12) . ? C21 C22 1.374(10) . ? C23 C28 1.379(10) . ? C23 C24 1.380(10) . ? C24 C25 1.417(13) . ? C25 C26 1.354(17) . ? C26 C27 1.386(15) . ? C27 C28 1.380(10) . ? C29 C34 1.379(9) . ? C29 C30 1.397(10) . ? C30 C31 1.372(11) . ? C31 C32 1.392(13) . ? C32 C33 1.346(12) . ? C33 C34 1.393(10) . ? 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 C16 C11 C16X 105.2(12) . . ? C16 C11 C12X 19.0(10) . . ? C16X C11 C12X 118.7(16) . . ? C16 C11 C12 120.0(9) . . ? C16X C11 C12 20.6(10) . . ? C12X C11 C12 128.5(13) . . ? C16 C11 P1 126.8(8) . . ? C16X C11 P1 123.7(12) . . ? C12X C11 P1 117.2(11) . . ? C12 C11 P1 112.9(6) . . ? C13 C12 C11 121.6(11) . . ? C14 C13 C12 116.8(12) . . ? C13 C14 C15 122.0(13) . . ? C16 C15 C14 118.9(13) . . ? C11 C16 C15 120.6(13) . . ? C13X C12X C11 123(2) . . ? C14X C13X C12X 116(2) . . ? C15X C14X C13X 122(2) . . ? C14X C15X C16X 119(2) . . ? C11 C16X C15X 120(2) . . ? O1 Co1 O2 108.04(18) . . ? O1 Co1 I1 112.86(14) . . ? O2 Co1 I1 106.94(12) . . ? O1 Co1 I2 99.48(14) . . ? O2 Co1 I2 111.57(13) . . ? I1 Co1 I2 117.61(3) . . ? C7 Fe1 C6 41.0(2) . . ? C7 Fe1 C2 151.7(3) . . ? C6 Fe1 C2 164.7(2) . . ? C7 Fe1 C3 117.0(3) . . ? C6 Fe1 C3 154.3(3) . . ? C2 Fe1 C3 40.9(3) . . ? C7 Fe1 C1 165.2(3) . . ? C6 Fe1 C1 129.0(2) . . ? C2 Fe1 C1 40.9(2) . . ? C3 Fe1 C1 68.6(3) . . ? C7 Fe1 C5 126.2(3) . . ? C6 Fe1 C5 111.1(3) . . ? C2 Fe1 C5 68.9(3) . . ? C3 Fe1 C5 68.3(3) . . ? C1 Fe1 C5 41.0(3) . . ? C7 Fe1 C8 40.8(3) . . ? C6 Fe1 C8 68.3(2) . . ? C2 Fe1 C8 116.9(3) . . ? C3 Fe1 C8 103.6(3) . . ? C1 Fe1 C8 153.8(3) . . ? C5 Fe1 C8 161.1(3) . . ? C7 Fe1 C10 68.7(3) . . ? C6 Fe1 C10 40.7(2) . . ? C2 Fe1 C10 125.9(3) . . ? C3 Fe1 C10 160.6(3) . . ? C1 Fe1 C10 110.9(2) . . ? C5 Fe1 C10 124.9(2) . . ? C8 Fe1 C10 67.9(3) . . ? C7 Fe1 C4 105.8(3) . . ? C6 Fe1 C4 121.5(3) . . ? C2 Fe1 C4 69.1(3) . . ? C3 Fe1 C4 40.9(3) . . ? C1 Fe1 C4 68.9(3) . . ? C5 Fe1 C4 40.5(3) . . ? C8 Fe1 C4 122.4(3) . . ? C10 Fe1 C4 158.3(3) . . ? C7 Fe1 C9 67.7(3) . . ? C6 Fe1 C9 68.0(3) . . ? C2 Fe1 C9 106.2(3) . . ? C3 Fe1 C9 122.0(3) . . ? C1 Fe1 C9 122.2(3) . . ? C5 Fe1 C9 159.3(3) . . ? C8 Fe1 C9 39.4(3) . . ? C10 Fe1 C9 40.7(2) . . ? C4 Fe1 C9 158.4(3) . . ? O1 P1 C1 113.5(3) . . ? O1 P1 C17 109.4(3) . . ? C1 P1 C17 106.6(3) . . ? O1 P1 C11 109.0(3) . . ? C1 P1 C11 107.0(3) . . ? C17 P1 C11 111.4(3) . . ? O2 P2 C29 110.3(3) . . ? O2 P2 C6 113.7(2) . . ? C29 P2 C6 105.8(3) . . ? O2 P2 C23 111.3(3) . . ? C29 P2 C23 107.3(3) . . ? C6 P2 C23 108.0(3) . . ? P1 O1 Co1 158.2(3) . . ? P2 O2 Co1 139.7(3) . . ? C2 C1 C5 107.8(6) . . ? C2 C1 P1 128.3(5) . . ? C5 C1 P1 123.7(5) . . ? C2 C1 Fe1 69.3(3) . . ? C5 C1 Fe1 69.8(3) . . ? P1 C1 Fe1 123.9(3) . . ? C3 C2 C1 107.6(6) . . ? C3 C2 Fe1 69.6(4) . . ? C1 C2 Fe1 69.7(3) . . ? C2 C3 C4 109.1(6) . . ? C2 C3 Fe1 69.5(3) . . ? C4 C3 Fe1 70.6(4) . . ? C5 C4 C3 106.8(6) . . ? C5 C4 Fe1 69.2(4) . . ? C3 C4 Fe1 68.6(4) . . ? C4 C5 C1 108.6(6) . . ? C4 C5 Fe1 70.2(4) . . ? C1 C5 Fe1 69.2(4) . . ? C10 C6 C7 108.3(5) . . ? C10 C6 P2 125.6(4) . . ? C7 C6 P2 126.0(5) . . ? C10 C6 Fe1 70.6(3) . . ? C7 C6 Fe1 69.4(3) . . ? P2 C6 Fe1 123.9(3) . . ? C6 C7 C8 107.4(6) . . ? C6 C7 Fe1 69.5(3) . . ? C8 C7 Fe1 70.5(3) . . ? C9 C8 C7 108.5(6) . . ? C9 C8 Fe1 70.6(4) . . ? C7 C8 Fe1 68.7(3) . . ? C8 C9 C10 109.0(6) . . ? C8 C9 Fe1 70.0(4) . . ? C10 C9 Fe1 69.4(3) . . ? C6 C10 C9 106.8(5) . . ? C6 C10 Fe1 68.8(3) . . ? C9 C10 Fe1 69.9(4) . . ? C18 C17 C22 120.2(6) . . ? C18 C17 P1 120.5(5) . . ? C22 C17 P1 119.0(5) . . ? C19 C18 C17 119.8(6) . . ? C18 C19 C20 119.8(6) . . ? C21 C20 C19 120.2(7) . . ? C22 C21 C20 120.7(7) . . ? C21 C22 C17 119.2(7) . . ? C28 C23 C24 120.1(7) . . ? C28 C23 P2 122.0(5) . . ? C24 C23 P2 117.8(6) . . ? C23 C24 C25 117.7(9) . . ? C26 C25 C24 121.8(9) . . ? C25 C26 C27 119.9(8) . . ? C28 C27 C26 119.0(9) . . ? C23 C28 C27 121.5(8) . . ? C34 C29 C30 119.9(6) . . ? C34 C29 P2 121.1(5) . . ? C30 C29 P2 118.7(5) . . ? C31 C30 C29 118.9(7) . . ? C30 C31 C32 120.8(8) . . ? C33 C32 C31 120.1(7) . . ? C32 C33 C34 120.3(7) . . ? C29 C34 C33 119.9(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.374 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.103 data_Cpd12 _database_code_depnum_ccdc_archive 'CCDC 823899' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28.50 Cl2 Fe O2.25 P2 Zn' _chemical_formula_weight 727.13 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' O O 0.0106 0.0060 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 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 11.3093(4) _cell_length_b 18.4373(7) _cell_length_c 31.0211(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6468.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2264 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 19.53 _exptl_crystal_description Rod _exptl_crystal_colour Orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2964 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6169 _exptl_absorpt_correction_T_max 0.8657 _exptl_absorpt_process_details 'SADABS, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43884 _diffrn_reflns_av_R_equivalents 0.1108 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7423 _reflns_number_gt 5215 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0595P)^2^+14.3187P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7423 _refine_ls_number_parameters 394 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.01558(5) 0.35971(3) 0.120589(18) 0.02690(16) Uani 1 1 d . . . Fe1 Fe 0.73156(7) 0.17913(4) 0.11191(2) 0.02764(19) Uani 1 1 d . . . Cl1 Cl 1.05495(14) 0.45561(7) 0.16098(5) 0.0445(4) Uani 1 1 d . . . Cl2 Cl 1.14029(17) 0.32562(10) 0.07005(6) 0.0680(5) Uani 1 1 d . . . P1 P 0.93051(11) 0.22644(7) 0.19013(4) 0.0246(3) Uani 1 1 d . . . P2 P 0.77690(11) 0.34126(7) 0.06042(4) 0.0259(3) Uani 1 1 d . . . O1 O 0.9916(3) 0.27612(19) 0.15923(11) 0.0346(8) Uani 1 1 d . . . O2 O 0.8567(3) 0.37123(18) 0.09431(11) 0.0332(8) Uani 1 1 d . . . C1 C 0.7894(4) 0.1955(3) 0.17305(15) 0.0284(11) Uani 1 1 d . . . C2 C 0.7507(5) 0.1221(3) 0.16780(15) 0.0349(13) Uani 1 1 d . . . H2 H 0.7996 0.0780 0.1718 0.042 Uiso 1 1 calc R . . C3 C 0.6301(5) 0.1237(3) 0.15573(18) 0.0456(15) Uani 1 1 d . . . H3 H 0.5805 0.0808 0.1493 0.055 Uiso 1 1 calc R . . C4 C 0.5930(5) 0.1958(3) 0.15356(17) 0.0412(14) Uani 1 1 d . . . H4 H 0.5129 0.2126 0.1454 0.049 Uiso 1 1 calc R . . C5 C 0.6908(5) 0.2414(3) 0.16423(16) 0.0337(12) Uani 1 1 d . . . H5 H 0.6903 0.2951 0.1653 0.040 Uiso 1 1 calc R . . C6 C 0.7677(5) 0.2451(3) 0.06107(14) 0.0278(11) Uani 1 1 d . . . C7 C 0.6663(5) 0.1999(3) 0.05216(15) 0.0389(13) Uani 1 1 d . . . H7 H 0.5855 0.2171 0.0454 0.047 Uiso 1 1 calc R . . C8 C 0.7028(6) 0.1271(3) 0.05465(18) 0.0489(17) Uani 1 1 d . . . H8 H 0.6518 0.0841 0.0503 0.059 Uiso 1 1 calc R . . C9 C 0.8255(6) 0.1259(3) 0.06481(17) 0.0453(15) Uani 1 1 d . . . H9 H 0.8739 0.0817 0.0691 0.054 Uiso 1 1 calc R . . C10 C 0.8658(5) 0.1977(3) 0.06896(15) 0.0313(12) Uani 1 1 d . . . H10 H 0.9473 0.2129 0.0763 0.038 Uiso 1 1 calc R . . C1A C 0.9058(4) 0.2699(2) 0.24087(15) 0.0259(10) Uani 1 1 d . . . C2A C 0.8114(5) 0.2503(3) 0.26792(16) 0.0349(12) Uani 1 1 d . . . H2A H 0.7590 0.2134 0.2594 0.042 Uiso 1 1 calc R . . C3A C 0.7949(5) 0.2849(3) 0.30704(19) 0.0452(15) Uani 1 1 d . . . H3A H 0.7320 0.2713 0.3252 0.054 Uiso 1 1 calc R . . C4A C 0.8707(6) 0.3392(3) 0.3192(2) 0.0478(15) Uani 1 1 d . . . H4A H 0.8588 0.3632 0.3456 0.057 Uiso 1 1 calc R . . C5A C 0.9641(5) 0.3589(3) 0.29324(19) 0.0419(14) Uani 1 1 d . . . H5A H 1.0158 0.3960 0.3020 0.050 Uiso 1 1 calc R . . C6A C 0.9821(5) 0.3243(3) 0.25423(17) 0.0330(12) Uani 1 1 d . . . H6A H 1.0462 0.3377 0.2367 0.040 Uiso 1 1 calc R . . C1B C 1.0215(4) 0.1483(3) 0.19909(15) 0.0275(11) Uani 1 1 d . . . C2B C 1.1101(5) 0.1322(3) 0.16948(17) 0.0362(13) Uani 1 1 d . . . H2B H 1.1187 0.1606 0.1445 0.043 Uiso 1 1 calc R . . C3B C 1.1857(5) 0.0746(3) 0.17677(19) 0.0451(15) Uani 1 1 d . . . H3B H 1.2471 0.0650 0.1572 0.054 Uiso 1 1 calc R . . C4B C 1.1719(5) 0.0313(3) 0.2123(2) 0.0473(15) Uani 1 1 d . . . H4B H 1.2228 -0.0083 0.2166 0.057 Uiso 1 1 calc R . . C5B C 1.0840(6) 0.0458(3) 0.24142(18) 0.0452(15) Uani 1 1 d . . . H5B H 1.0744 0.0160 0.2657 0.054 Uiso 1 1 calc R . . C6B C 1.0092(5) 0.1045(3) 0.23501(17) 0.0370(13) Uani 1 1 d . . . H6B H 0.9498 0.1147 0.2553 0.044 Uiso 1 1 calc R . . C1C C 0.6331(5) 0.3808(3) 0.06759(16) 0.0319(12) Uani 1 1 d . . . C2C C 0.5423(5) 0.3702(4) 0.0378(2) 0.0511(16) Uani 1 1 d . . . H2C H 0.5540 0.3405 0.0135 0.061 Uiso 1 1 calc R . . C3C C 0.4341(6) 0.4041(5) 0.0445(2) 0.069(2) Uani 1 1 d . . . H3C H 0.3711 0.3955 0.0255 0.082 Uiso 1 1 calc R . . C4C C 0.4186(5) 0.4501(4) 0.0788(2) 0.059(2) Uani 1 1 d . . . H4C H 0.3457 0.4737 0.0827 0.071 Uiso 1 1 calc R . . C5C C 0.5084(6) 0.4617(3) 0.1074(2) 0.0477(16) Uani 1 1 d . . . H5C H 0.4971 0.4933 0.1308 0.057 Uiso 1 1 calc R . . C6C C 0.6154(5) 0.4272(3) 0.10211(17) 0.0351(12) Uani 1 1 d . . . H6C H 0.6767 0.4352 0.1220 0.042 Uiso 1 1 calc R . . C1D C 0.8215(4) 0.3655(3) 0.00685(16) 0.0296(11) Uani 1 1 d . . . C2D C 0.8147(5) 0.3174(3) -0.02683(17) 0.0408(13) Uani 1 1 d . . . H2D H 0.7917 0.2691 -0.0220 0.049 Uiso 1 1 calc R . . C3D C 0.8425(6) 0.3410(4) -0.0684(2) 0.0595(19) Uani 1 1 d . . . H3D H 0.8363 0.3086 -0.0917 0.071 Uiso 1 1 calc R . . C4D C 0.8781(5) 0.4100(5) -0.0755(2) 0.065(2) Uani 1 1 d . . . H4D H 0.8989 0.4246 -0.1035 0.078 Uiso 1 1 calc R . . C5D C 0.8843(6) 0.4586(4) -0.0423(3) 0.065(2) Uani 1 1 d . . . H5D H 0.9070 0.5068 -0.0475 0.078 Uiso 1 1 calc R . . C6D C 0.8566(6) 0.4359(3) -0.0010(2) 0.0507(16) Uani 1 1 d . . . H6D H 0.8618 0.4689 0.0220 0.061 Uiso 1 1 calc R . . O1W O 0.7685(13) 0.4232(8) 0.1946(4) 0.035(3) Uani 0.25 1 d PD . . H2W H 0.73(2) 0.460(9) 0.201(7) 0.080 Uiso 0.25 1 d PD . . H1W H 0.79(2) 0.401(12) 0.217(4) 0.080 Uiso 0.25 1 d PD . . 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 Zn1 0.0257(3) 0.0232(3) 0.0318(3) 0.0016(2) 0.0026(2) -0.0010(2) Fe1 0.0346(4) 0.0237(4) 0.0246(4) -0.0007(3) 0.0002(3) -0.0088(3) Cl1 0.0585(10) 0.0273(7) 0.0478(8) -0.0025(6) -0.0123(7) -0.0090(6) Cl2 0.0655(12) 0.0620(11) 0.0765(12) -0.0061(9) 0.0428(10) 0.0039(9) P1 0.0266(7) 0.0223(6) 0.0250(6) 0.0029(5) 0.0004(5) -0.0043(5) P2 0.0266(7) 0.0241(6) 0.0269(6) 0.0003(5) -0.0039(5) -0.0014(5) O1 0.038(2) 0.031(2) 0.035(2) 0.0100(15) -0.0025(16) -0.0107(16) O2 0.032(2) 0.0294(19) 0.038(2) -0.0082(15) -0.0120(16) 0.0039(15) C1 0.032(3) 0.030(3) 0.023(2) 0.002(2) 0.006(2) -0.006(2) C2 0.046(3) 0.032(3) 0.027(3) 0.010(2) -0.003(2) -0.012(2) C3 0.051(4) 0.050(4) 0.036(3) 0.006(3) 0.000(3) -0.030(3) C4 0.028(3) 0.061(4) 0.034(3) -0.004(3) -0.001(2) -0.004(3) C5 0.032(3) 0.038(3) 0.031(3) -0.004(2) 0.002(2) -0.003(2) C6 0.035(3) 0.027(3) 0.021(2) -0.0016(19) -0.004(2) -0.003(2) C7 0.049(4) 0.046(3) 0.022(3) 0.001(2) -0.010(2) -0.015(3) C8 0.078(5) 0.035(3) 0.034(3) -0.014(2) 0.008(3) -0.023(3) C9 0.076(5) 0.027(3) 0.033(3) -0.006(2) 0.014(3) 0.000(3) C10 0.041(3) 0.023(3) 0.029(3) -0.001(2) 0.006(2) 0.001(2) C1A 0.029(3) 0.021(2) 0.028(3) -0.0022(19) -0.004(2) 0.003(2) C2A 0.034(3) 0.037(3) 0.034(3) -0.007(2) 0.002(2) -0.007(2) C3A 0.037(3) 0.055(4) 0.043(3) -0.009(3) 0.010(3) -0.001(3) C4A 0.052(4) 0.045(4) 0.047(4) -0.018(3) -0.001(3) 0.012(3) C5A 0.045(4) 0.026(3) 0.054(4) -0.013(3) -0.012(3) -0.005(3) C6A 0.032(3) 0.032(3) 0.036(3) 0.000(2) -0.001(2) -0.005(2) C1B 0.027(3) 0.030(3) 0.025(2) -0.002(2) -0.003(2) -0.003(2) C2B 0.034(3) 0.042(3) 0.033(3) 0.003(2) 0.007(2) -0.005(3) C3B 0.034(3) 0.054(4) 0.048(4) -0.006(3) 0.014(3) 0.008(3) C4B 0.044(4) 0.037(3) 0.061(4) -0.009(3) -0.008(3) 0.008(3) C5B 0.063(4) 0.035(3) 0.037(3) 0.007(2) -0.001(3) 0.010(3) C6B 0.044(3) 0.036(3) 0.031(3) 0.004(2) 0.007(2) 0.005(3) C1C 0.028(3) 0.038(3) 0.030(3) 0.005(2) 0.000(2) 0.002(2) C2C 0.031(3) 0.077(5) 0.045(4) -0.001(3) -0.005(3) 0.007(3) C3C 0.038(4) 0.113(7) 0.055(4) 0.010(4) -0.012(3) 0.008(4) C4C 0.027(3) 0.084(5) 0.066(5) 0.028(4) 0.009(3) 0.022(3) C5C 0.051(4) 0.041(3) 0.051(4) 0.010(3) 0.018(3) 0.015(3) C6C 0.036(3) 0.029(3) 0.040(3) 0.007(2) -0.001(2) 0.001(2) C1D 0.024(3) 0.029(3) 0.036(3) 0.008(2) -0.002(2) -0.002(2) C2D 0.045(3) 0.045(3) 0.033(3) 0.004(2) 0.006(2) -0.009(3) C3D 0.053(4) 0.091(6) 0.034(3) 0.009(3) 0.005(3) -0.008(4) C4D 0.027(3) 0.109(7) 0.058(4) 0.040(5) -0.001(3) -0.007(4) C5D 0.053(4) 0.056(4) 0.087(6) 0.041(4) 0.004(4) -0.009(4) C6D 0.060(4) 0.031(3) 0.062(4) 0.010(3) 0.001(3) -0.004(3) O1W 0.034(8) 0.029(8) 0.043(9) 0.000(6) -0.013(7) 0.007(6) _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 Zn1 O1 1.971(3) . ? Zn1 O2 1.985(3) . ? Zn1 Cl2 2.2005(16) . ? Zn1 Cl1 2.2122(14) . ? Fe1 C1 2.029(5) . ? Fe1 C7 2.031(5) . ? Fe1 C6 2.033(5) . ? Fe1 C2 2.039(5) . ? Fe1 C5 2.041(5) . ? Fe1 C8 2.045(5) . ? Fe1 C10 2.049(5) . ? Fe1 C3 2.051(5) . ? Fe1 C4 2.054(6) . ? Fe1 C9 2.056(6) . ? P1 O1 1.495(3) . ? P1 C1 1.776(5) . ? P1 C1A 1.788(5) . ? P1 C1B 1.792(5) . ? P2 O2 1.491(3) . ? P2 C6 1.776(5) . ? P2 C1D 1.793(5) . ? P2 C1C 1.796(5) . ? C1 C5 1.426(7) . ? C1 C2 1.433(7) . ? C2 C3 1.415(8) . ? C3 C4 1.396(9) . ? C4 C5 1.428(7) . ? C6 C10 1.433(7) . ? C6 C7 1.444(7) . ? C7 C8 1.406(8) . ? C8 C9 1.423(9) . ? C9 C10 1.407(7) . ? C1A C6A 1.386(7) . ? C1A C2A 1.406(7) . ? C2A C3A 1.384(7) . ? C3A C4A 1.371(8) . ? C4A C5A 1.377(9) . ? C5A C6A 1.383(7) . ? C1B C6B 1.383(7) . ? C1B C2B 1.392(7) . ? C2B C3B 1.382(8) . ? C3B C4B 1.368(8) . ? C4B C5B 1.370(8) . ? C5B C6B 1.389(7) . ? C1C C6C 1.385(7) . ? C1C C2C 1.396(7) . ? C2C C3C 1.389(9) . ? C3C C4C 1.371(10) . ? C4C C5C 1.365(9) . ? C5C C6C 1.377(8) . ? C1D C2D 1.373(7) . ? C1D C6D 1.379(7) . ? C2D C3D 1.397(8) . ? C3D C4D 1.352(10) . ? C4D C5D 1.367(11) . ? C5D C6D 1.382(9) . ? O1W H1W 0.85(2) . ? 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 O1 Zn1 O2 102.07(15) . . ? O1 Zn1 Cl2 107.33(12) . . ? O2 Zn1 Cl2 108.56(12) . . ? O1 Zn1 Cl1 107.94(11) . . ? O2 Zn1 Cl1 109.23(11) . . ? Cl2 Zn1 Cl1 120.19(7) . . ? C1 Fe1 C7 160.4(2) . . ? C1 Fe1 C6 124.83(19) . . ? C7 Fe1 C6 41.6(2) . . ? C1 Fe1 C2 41.25(19) . . ? C7 Fe1 C2 155.7(2) . . ? C6 Fe1 C2 161.2(2) . . ? C1 Fe1 C5 41.0(2) . . ? C7 Fe1 C5 122.5(2) . . ? C6 Fe1 C5 109.0(2) . . ? C2 Fe1 C5 68.8(2) . . ? C1 Fe1 C8 159.0(2) . . ? C7 Fe1 C8 40.3(2) . . ? C6 Fe1 C8 68.8(2) . . ? C2 Fe1 C8 120.9(2) . . ? C5 Fe1 C8 156.8(3) . . ? C1 Fe1 C10 110.1(2) . . ? C7 Fe1 C10 69.2(2) . . ? C6 Fe1 C10 41.1(2) . . ? C2 Fe1 C10 124.1(2) . . ? C5 Fe1 C10 126.2(2) . . ? C8 Fe1 C10 68.4(2) . . ? C1 Fe1 C3 68.6(2) . . ? C7 Fe1 C3 119.7(2) . . ? C6 Fe1 C3 157.6(2) . . ? C2 Fe1 C3 40.5(2) . . ? C5 Fe1 C3 68.1(2) . . ? C8 Fe1 C3 104.7(2) . . ? C10 Fe1 C3 158.2(2) . . ? C1 Fe1 C4 68.6(2) . . ? C7 Fe1 C4 105.6(2) . . ? C6 Fe1 C4 123.5(2) . . ? C2 Fe1 C4 67.9(2) . . ? C5 Fe1 C4 40.8(2) . . ? C8 Fe1 C4 119.7(2) . . ? C10 Fe1 C4 161.7(2) . . ? C3 Fe1 C4 39.8(2) . . ? C1 Fe1 C9 124.7(2) . . ? C7 Fe1 C9 68.2(2) . . ? C6 Fe1 C9 68.3(2) . . ? C2 Fe1 C9 107.6(2) . . ? C5 Fe1 C9 161.9(2) . . ? C8 Fe1 C9 40.6(3) . . ? C10 Fe1 C9 40.1(2) . . ? C3 Fe1 C9 121.5(2) . . ? C4 Fe1 C9 155.9(2) . . ? O1 P1 C1 114.9(2) . . ? O1 P1 C1A 111.2(2) . . ? C1 P1 C1A 105.4(2) . . ? O1 P1 C1B 109.1(2) . . ? C1 P1 C1B 107.7(2) . . ? C1A P1 C1B 108.3(2) . . ? O2 P2 C6 113.4(2) . . ? O2 P2 C1D 113.0(2) . . ? C6 P2 C1D 106.0(2) . . ? O2 P2 C1C 108.0(2) . . ? C6 P2 C1C 110.6(2) . . ? C1D P2 C1C 105.6(2) . . ? P1 O1 Zn1 158.8(3) . . ? P2 O2 Zn1 142.9(2) . . ? C5 C1 C2 107.5(5) . . ? C5 C1 P1 124.7(4) . . ? C2 C1 P1 127.7(4) . . ? C5 C1 Fe1 69.9(3) . . ? C2 C1 Fe1 69.8(3) . . ? P1 C1 Fe1 128.1(3) . . ? C3 C2 C1 107.7(5) . . ? C3 C2 Fe1 70.2(3) . . ? C1 C2 Fe1 69.0(3) . . ? C4 C3 C2 108.9(5) . . ? C4 C3 Fe1 70.2(3) . . ? C2 C3 Fe1 69.3(3) . . ? C3 C4 C5 108.5(5) . . ? C3 C4 Fe1 70.0(3) . . ? C5 C4 Fe1 69.1(3) . . ? C1 C5 C4 107.5(5) . . ? C1 C5 Fe1 69.0(3) . . ? C4 C5 Fe1 70.1(3) . . ? C10 C6 C7 107.2(5) . . ? C10 C6 P2 124.4(4) . . ? C7 C6 P2 128.3(4) . . ? C10 C6 Fe1 70.0(3) . . ? C7 C6 Fe1 69.1(3) . . ? P2 C6 Fe1 128.1(3) . . ? C8 C7 C6 107.9(5) . . ? C8 C7 Fe1 70.3(3) . . ? C6 C7 Fe1 69.3(3) . . ? C7 C8 C9 108.3(5) . . ? C7 C8 Fe1 69.3(3) . . ? C9 C8 Fe1 70.1(3) . . ? C10 C9 C8 108.7(5) . . ? C10 C9 Fe1 69.7(3) . . ? C8 C9 Fe1 69.3(3) . . ? C9 C10 C6 107.9(5) . . ? C9 C10 Fe1 70.2(3) . . ? C6 C10 Fe1 68.9(3) . . ? C6A C1A C2A 118.7(4) . . ? C6A C1A P1 119.4(4) . . ? C2A C1A P1 121.9(4) . . ? C3A C2A C1A 120.5(5) . . ? C4A C3A C2A 119.6(5) . . ? C3A C4A C5A 120.7(5) . . ? C4A C5A C6A 120.2(5) . . ? C5A C6A C1A 120.3(5) . . ? C6B C1B C2B 118.6(5) . . ? C6B C1B P1 122.5(4) . . ? C2B C1B P1 118.9(4) . . ? C3B C2B C1B 120.1(5) . . ? C4B C3B C2B 120.6(5) . . ? C3B C4B C5B 120.0(6) . . ? C4B C5B C6B 120.0(5) . . ? C1B C6B C5B 120.6(5) . . ? C6C C1C C2C 119.5(5) . . ? C6C C1C P2 118.5(4) . . ? C2C C1C P2 121.8(4) . . ? C3C C2C C1C 119.0(6) . . ? C4C C3C C2C 120.5(6) . . ? C5C C4C C3C 120.3(6) . . ? C4C C5C C6C 120.3(6) . . ? C5C C6C C1C 120.3(5) . . ? C2D C1D C6D 119.3(5) . . ? C2D C1D P2 121.9(4) . . ? C6D C1D P2 118.7(4) . . ? C1D C2D C3D 119.3(6) . . ? C4D C3D C2D 120.7(7) . . ? C3D C4D C5D 120.6(6) . . ? C4D C5D C6D 119.2(6) . . ? C1D C6D C5D 121.0(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.550 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.112