# ic0002465.cif data_grzy02 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32.50 H48 B Br Co F6 Fe N14 O7.50 P' _chemical_formula_weight 1105.32 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1044(2) _cell_length_b 14.7918(2) _cell_length_c 17.7688(2) _cell_angle_alpha 84.5085(2) _cell_angle_beta 76.4880(2) _cell_angle_gamma 81.7951(2) _cell_volume 2298.04(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method ? _exptl_crystal_F_000 1126 _exptl_absorpt_coefficient_mu 1.666 _exptl_absorpt_correction_type Empirica _exptl_absorpt_correction_T_min 0.331 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14636 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.1271 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.94 _reflns_number_total 9613 _reflns_number_observed 5812 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9609 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1131 _refine_ls_R_factor_obs 0.0719 _refine_ls_wR_factor_all 0.2025 _refine_ls_wR_factor_obs 0.1782 _refine_ls_goodness_of_fit_all 0.928 _refine_ls_goodness_of_fit_obs 1.089 _refine_ls_restrained_S_all 0.949 _refine_ls_restrained_S_obs 1.089 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Br Br 0.31737(7) 0.41075(5) 0.41095(4) 0.0369(2) Uani 1 d . . Co Co 0.47442(8) 0.27209(5) 0.36497(4) 0.0197(2) Uani 1 d . . Fe Fe 1.18950(8) -0.23633(5) 0.18542(4) 0.0161(2) Uani 1 d . . P1 P 0.5000 1.0000 0.0000 0.0548(8) Uani 1 d S . P2 P 1.0000 -0.5000 0.0000 0.0651(10) Uani 1 d S . F1 F 0.5721(10) 1.0349(8) 0.0609(5) 0.162(4) Uani 1 d . . F2 F 0.5494(7) 0.8998(5) 0.0320(5) 0.133(3) Uani 1 d . . F3 F 0.3388(6) 1.0023(5) 0.0595(4) 0.116(3) Uani 1 d . . F4 F 1.0629(8) -0.5363(5) 0.0764(4) 0.120(3) Uani 1 d . . F5 F 0.9833(7) -0.3980(4) 0.0254(4) 0.107(2) Uani 1 d . . F6 F 1.1724(6) -0.4916(5) -0.0469(4) 0.108(2) Uani 1 d . . O1 O 0.5685(4) 0.3638(3) 0.2138(2) 0.0266(9) Uani 1 d . . H1A H 0.6310(4) 0.3740(3) 0.2384(2) 0.040 Uiso 1 calc R . O2 O 0.2123(5) 0.1742(3) 0.4219(2) 0.0370(11) Uani 1 d . . O3 O 0.7283(5) 0.3794(3) 0.3100(2) 0.0336(10) Uani 1 d . . O4 O 0.3803(4) 0.1824(3) 0.5172(2) 0.0311(10) Uani 1 d . . H4A H 0.3166(4) 0.1729(3) 0.4932(2) 0.047 Uiso 1 calc R . O5 O 0.9250(4) -0.1042(3) 0.1696(2) 0.0224(9) Uani 1 d . . O6 O 1.0959(4) -0.0526(3) 0.2421(2) 0.0225(9) Uani 1 d . . O7 O 0.9238(4) -0.1677(3) 0.3039(2) 0.0212(8) Uani 1 d . . N1 N 0.4645(5) 0.3145(3) 0.2601(3) 0.0227(11) Uani 1 d . . N2 N 0.2952(5) 0.2213(4) 0.3605(3) 0.0262(11) Uani 1 d . . N3 N 0.6503(5) 0.3267(3) 0.3694(2) 0.0221(10) Uani 1 d . . N4 N 0.4817(5) 0.2342(3) 0.4710(3) 0.0228(10) Uani 1 d . . N5 N 0.6081(5) 0.1559(3) 0.3290(2) 0.0169(9) Uani 1 d . . N6 N 1.2812(5) -0.2593(3) 0.0757(2) 0.0222(10) Uani 1 d . . N7 N 1.0436(5) -0.1667(3) 0.1332(3) 0.0200(10) Uani 1 d . . N8 N 1.3976(5) -0.2597(3) 0.2011(3) 0.0217(10) Uani 1 d . . N9 N 1.2156(5) -0.1219(3) 0.2205(2) 0.0186(10) Uani 1 d . . N10 N 1.1810(5) -0.3675(3) 0.1999(3) 0.0222(10) Uani 1 d . . N11 N 1.0176(5) -0.2447(3) 0.2735(2) 0.0174(10) Uani 1 d . . N12 N 1.3045(5) -0.4357(3) 0.1671(3) 0.0285(12) Uani 1 d . . N13 N 1.4028(5) -0.3316(4) 0.0519(3) 0.0296(12) Uani 1 d . . N14 N 1.5041(5) -0.3377(3) 0.1712(3) 0.0252(11) Uani 1 d . . B B 0.9436(7) -0.0852(4) 0.2495(3) 0.0188(13) Uani 1 d . . C1 C 0.3544(6) 0.2900(4) 0.2344(3) 0.0275(14) Uani 1 d . . C2 C 0.3293(7) 0.3123(5) 0.1532(3) 0.036(2) Uani 1 d . . H2B H 0.4264(7) 0.2996(5) 0.1158(3) 0.043 Uiso 1 calc R . H2C H 0.2939(7) 0.3777(5) 0.1468(3) 0.043 Uiso 1 calc R . C3 C 0.2141(10) 0.2576(7) 0.1356(5) 0.062(2) Uani 1 d . . H3B H 0.1828(10) 0.2849(7) 0.0885(5) 0.075 Uiso 1 calc R . H3C H 0.2623(10) 0.1950(7) 0.1256(5) 0.075 Uiso 1 calc R . C4 C 0.0796(9) 0.2543(7) 0.1987(5) 0.069(3) Uani 1 d . . H4B H 0.0072(9) 0.2217(7) 0.1822(5) 0.083 Uiso 1 calc R . H4C H 0.0312(9) 0.3171(7) 0.2077(5) 0.083 Uiso 1 calc R . C5 C 0.1106(7) 0.2068(5) 0.2776(4) 0.037(2) Uani 1 d . . H5A H 0.0229(7) 0.2233(5) 0.3199(4) 0.045 Uiso 1 calc R . H5B H 0.1240(7) 0.1402(5) 0.2749(4) 0.045 Uiso 1 calc R . C6 C 0.2511(6) 0.2362(4) 0.2939(3) 0.0288(14) Uani 1 d . . C7 C 0.6918(7) 0.3159(4) 0.4366(3) 0.0259(13) Uani 1 d . . C8 C 0.8175(8) 0.3590(5) 0.4547(4) 0.040(2) Uani 1 d . . H8A H 0.7884(8) 0.4254(5) 0.4552(4) 0.048 Uiso 1 calc R . H8B H 0.9091(8) 0.3476(5) 0.4134(4) 0.048 Uiso 1 calc R . C9 C 0.8551(9) 0.3235(7) 0.5322(4) 0.061(2) Uani 1 d . . H9A H 0.9239(9) 0.2661(7) 0.5251(4) 0.073 Uiso 1 calc R . H9B H 0.9091(9) 0.3680(7) 0.5490(4) 0.073 Uiso 1 calc R . C10 C 0.7184(11) 0.3071(8) 0.5944(5) 0.079(3) Uani 1 d . . H10A H 0.6536(11) 0.3656(8) 0.6041(5) 0.095 Uiso 1 calc R . H10B H 0.7517(11) 0.2851(8) 0.6423(5) 0.095 Uiso 1 calc R . C11 C 0.6213(7) 0.2371(5) 0.5759(3) 0.036(2) Uani 1 d . . H11A H 0.6750(7) 0.1750(5) 0.5796(3) 0.043 Uiso 1 calc R . H11B H 0.5239(7) 0.2395(5) 0.6139(3) 0.043 Uiso 1 calc R . C12 C 0.5928(6) 0.2585(4) 0.4953(3) 0.0239(13) Uani 1 d . . C13 C 0.6073(7) 0.0763(4) 0.3734(3) 0.0303(14) Uani 1 d . . H13A H 0.5371(7) 0.0739(4) 0.4215(3) 0.036 Uiso 1 calc R . C14 C 0.7069(7) -0.0028(4) 0.3508(3) 0.0299(14) Uani 1 d . . H14A H 0.7020(7) -0.0568(4) 0.3833(3) 0.036 Uiso 1 calc R . C15 C 0.8145(6) -0.0012(4) 0.2793(3) 0.0194(12) Uani 1 d . . C16 C 0.8091(7) 0.0815(5) 0.2350(3) 0.038(2) Uani 1 d . . H16A H 0.8767(7) 0.0863(5) 0.1864(3) 0.046 Uiso 1 calc R . C17 C 0.7063(8) 0.1577(5) 0.2606(4) 0.039(2) Uani 1 d . . H17A H 0.7065(8) 0.2120(5) 0.2285(4) 0.046 Uiso 1 calc R . C18 C 1.1980(6) -0.2296(4) 0.0250(3) 0.0240(12) Uani 1 d . . C19 C 1.0612(6) -0.1694(4) 0.0569(3) 0.0223(12) Uani 1 d . . C20 C 1.2351(8) -0.2524(5) -0.0590(3) 0.043(2) Uani 1 d . . H20A H 1.3299(8) -0.2931(5) -0.0699(3) 0.065 Uiso 1 calc R . H20B H 1.2455(8) -0.1965(5) -0.0921(3) 0.065 Uiso 1 calc R . H20C H 1.1538(8) -0.2820(5) -0.0690(3) 0.065 Uiso 1 calc R . C21 C 0.9528(7) -0.1168(5) 0.0110(3) 0.037(2) Uani 1 d . . H21A H 0.8708(7) -0.0818(5) 0.0457(3) 0.055 Uiso 1 calc R . H21B H 0.9111(7) -0.1593(5) -0.0141(3) 0.055 Uiso 1 calc R . H21C H 1.0070(7) -0.0755(5) -0.0280(3) 0.055 Uiso 1 calc R . C22 C 1.4592(6) -0.1889(4) 0.2153(3) 0.0226(12) Uani 1 d . . C23 C 1.3470(6) -0.1090(4) 0.2333(3) 0.0235(13) Uani 1 d . . C24 C 1.6265(6) -0.1882(5) 0.2117(4) 0.039(2) Uani 1 d . . H24A H 1.6812(6) -0.2479(5) 0.1988(4) 0.059 Uiso 1 calc R . H24B H 1.6397(6) -0.1738(5) 0.2616(4) 0.059 Uiso 1 calc R . H24C H 1.6660(6) -0.1423(5) 0.1723(4) 0.059 Uiso 1 calc R . C25 C 1.3773(8) -0.0220(5) 0.2626(4) 0.041(2) Uani 1 d . . H25A H 1.2853(8) 0.0212(5) 0.2702(4) 0.062 Uiso 1 calc R . H25B H 1.4576(8) 0.0045(5) 0.2248(4) 0.062 Uiso 1 calc R . H25C H 1.4085(8) -0.0363(5) 0.3114(4) 0.062 Uiso 1 calc R . C26 C 1.0718(6) -0.4002(4) 0.2565(3) 0.0230(12) Uani 1 d . . C27 C 0.9698(6) -0.3254(4) 0.2966(3) 0.0206(12) Uani 1 d . . C28 C 1.0531(7) -0.4982(4) 0.2771(4) 0.039(2) Uani 1 d . . H28A H 1.1327(7) -0.5359(4) 0.2434(4) 0.058 Uiso 1 calc R . H28B H 0.9545(7) -0.5095(4) 0.2708(4) 0.058 Uiso 1 calc R . H28C H 1.0600(7) -0.5132(4) 0.3306(4) 0.058 Uiso 1 calc R . C29 C 0.8244(6) -0.3397(4) 0.3572(3) 0.0304(14) Uani 1 d . . H29A H 0.7747(6) -0.2811(4) 0.3761(3) 0.046 Uiso 1 calc R . H29B H 0.8496(6) -0.3797(4) 0.4001(3) 0.046 Uiso 1 calc R . H29C H 0.7566(6) -0.3672(4) 0.3340(3) 0.046 Uiso 1 calc R . C30 C 1.4390(6) -0.4238(4) 0.1971(3) 0.0292(14) Uani 1 d . . H30A H 1.4101(6) -0.4278(4) 0.2539(3) 0.035 Uiso 1 calc R . H30B H 1.5184(6) -0.4749(4) 0.1814(3) 0.035 Uiso 1 calc R . C31 C 1.3429(7) -0.4199(5) 0.0810(3) 0.034(2) Uani 1 d . . H31A H 1.4190(7) -0.4700(5) 0.0594(3) 0.041 Uiso 1 calc R . H31B H 1.2513(7) -0.4223(5) 0.0616(3) 0.041 Uiso 1 calc R . C32 C 1.5355(6) -0.3239(5) 0.0840(3) 0.0296(14) Uani 1 d . . H32A H 1.5680(6) -0.2632(5) 0.0684(3) 0.036 Uiso 1 calc R . H32B H 1.6196(6) -0.3695(5) 0.0618(3) 0.036 Uiso 1 calc R . C100 C 0.9490(25) 0.0075(16) 0.4690(14) 0.023(5) Uiso 0.25 d P . C101 C 0.9191(38) 0.0975(24) 0.4559(21) 0.059(9) Uiso 0.25 d P . O100 O 0.7943(24) 0.0106(15) 0.5349(13) 0.056(6) Uiso 0.25 d P . O101 O 0.9363(27) 0.0365(18) 0.5132(16) 0.068(7) Uiso 0.25 d P . 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 Br 0.0437(4) 0.0406(4) 0.0203(3) -0.0125(3) -0.0060(3) 0.0201(3) Co 0.0198(4) 0.0304(4) 0.0056(4) -0.0047(3) -0.0010(3) 0.0070(3) Fe 0.0119(4) 0.0290(4) 0.0055(4) -0.0040(3) -0.0007(3) 0.0036(3) P1 0.041(2) 0.067(2) 0.043(2) 0.0231(15) -0.0047(13) 0.0115(14) P2 0.059(2) 0.059(2) 0.092(3) -0.005(2) -0.053(2) 0.004(2) F1 0.149(7) 0.233(11) 0.127(7) -0.043(7) -0.060(6) -0.030(7) F2 0.091(5) 0.082(5) 0.190(8) 0.065(5) -0.005(5) 0.022(4) F3 0.053(3) 0.170(7) 0.087(5) 0.052(4) 0.018(3) 0.020(4) F4 0.145(6) 0.127(6) 0.124(6) 0.037(4) -0.109(5) -0.036(5) F5 0.093(4) 0.068(4) 0.174(7) -0.036(4) -0.057(5) 0.009(3) F6 0.066(4) 0.112(5) 0.152(6) -0.032(5) -0.028(4) -0.010(4) O1 0.033(2) 0.037(2) 0.008(2) -0.002(2) -0.005(2) 0.003(2) O2 0.027(2) 0.053(3) 0.026(2) -0.001(2) 0.002(2) -0.005(2) O3 0.039(2) 0.047(3) 0.015(2) 0.008(2) -0.006(2) -0.013(2) O4 0.029(2) 0.049(3) 0.012(2) -0.002(2) 0.004(2) -0.007(2) O5 0.013(2) 0.040(2) 0.012(2) -0.009(2) -0.0039(14) 0.012(2) O6 0.017(2) 0.029(2) 0.020(2) -0.009(2) -0.006(2) 0.008(2) O7 0.021(2) 0.029(2) 0.008(2) -0.005(2) 0.0040(14) 0.008(2) N1 0.023(2) 0.034(3) 0.008(2) -0.007(2) -0.004(2) 0.009(2) N2 0.019(2) 0.039(3) 0.015(3) -0.001(2) 0.000(2) 0.008(2) N3 0.030(3) 0.028(3) 0.006(2) -0.002(2) -0.002(2) 0.003(2) N4 0.021(2) 0.033(3) 0.010(2) 0.000(2) 0.001(2) 0.004(2) N5 0.016(2) 0.026(2) 0.008(2) -0.002(2) -0.005(2) 0.001(2) N6 0.017(2) 0.037(3) 0.010(2) -0.004(2) 0.000(2) 0.002(2) N7 0.011(2) 0.035(3) 0.012(2) -0.010(2) -0.001(2) 0.005(2) N8 0.013(2) 0.031(3) 0.017(2) -0.003(2) 0.000(2) 0.007(2) N9 0.015(2) 0.025(2) 0.013(2) -0.002(2) 0.000(2) 0.004(2) N10 0.017(2) 0.030(3) 0.016(2) -0.007(2) 0.002(2) 0.004(2) N11 0.018(2) 0.026(3) 0.006(2) -0.006(2) -0.003(2) 0.009(2) N12 0.024(3) 0.030(3) 0.025(3) -0.008(2) 0.000(2) 0.012(2) N13 0.021(2) 0.046(3) 0.017(3) -0.012(2) 0.003(2) 0.009(2) N14 0.017(2) 0.034(3) 0.021(3) -0.006(2) -0.003(2) 0.009(2) B 0.021(3) 0.027(3) 0.008(3) -0.009(2) -0.001(2) 0.001(3) C1 0.024(3) 0.038(4) 0.018(3) -0.010(3) -0.006(2) 0.012(3) C2 0.033(3) 0.059(5) 0.015(3) -0.011(3) -0.012(3) 0.015(3) C3 0.081(6) 0.083(7) 0.030(4) -0.011(4) -0.027(4) -0.002(5) C4 0.052(5) 0.105(8) 0.064(6) -0.016(5) -0.041(5) -0.004(5) C5 0.025(3) 0.054(4) 0.036(4) -0.009(3) -0.014(3) 0.000(3) C6 0.023(3) 0.039(4) 0.023(3) -0.017(3) -0.005(2) 0.011(3) C7 0.031(3) 0.038(4) 0.009(3) -0.007(2) -0.006(2) 0.001(3) C8 0.045(4) 0.062(5) 0.015(3) 0.000(3) -0.011(3) -0.012(3) C9 0.057(5) 0.101(7) 0.033(4) 0.004(4) -0.029(4) -0.016(5) C10 0.081(6) 0.142(10) 0.023(4) 0.009(5) -0.026(4) -0.028(6) C11 0.041(4) 0.058(4) 0.008(3) 0.000(3) -0.008(3) 0.002(3) C12 0.025(3) 0.038(3) 0.006(3) -0.006(2) -0.002(2) 0.004(3) C13 0.036(3) 0.036(4) 0.010(3) -0.003(2) 0.006(2) 0.009(3) C14 0.030(3) 0.034(3) 0.019(3) 0.000(3) 0.002(2) 0.005(3) C15 0.016(3) 0.029(3) 0.014(3) -0.006(2) -0.006(2) 0.003(2) C16 0.039(4) 0.046(4) 0.013(3) 0.003(3) 0.013(3) 0.016(3) C17 0.050(4) 0.035(4) 0.019(3) 0.002(3) -0.001(3) 0.021(3) C18 0.025(3) 0.034(3) 0.010(3) -0.004(2) 0.001(2) -0.002(2) C19 0.021(3) 0.038(3) 0.009(3) -0.004(2) -0.005(2) 0.000(2) C20 0.047(4) 0.069(5) 0.012(3) -0.013(3) -0.009(3) 0.010(4) C21 0.037(4) 0.056(4) 0.016(3) -0.009(3) -0.011(3) 0.008(3) C22 0.015(3) 0.033(3) 0.019(3) 0.003(2) -0.004(2) -0.001(2) C23 0.015(3) 0.038(3) 0.017(3) 0.002(2) -0.007(2) 0.000(2) C24 0.011(3) 0.058(5) 0.047(4) 0.006(3) -0.008(3) -0.004(3) C25 0.038(4) 0.039(4) 0.054(5) -0.016(3) -0.022(3) -0.005(3) C26 0.018(3) 0.030(3) 0.018(3) 0.000(2) -0.004(2) 0.004(2) C27 0.015(3) 0.033(3) 0.011(3) 0.002(2) -0.002(2) 0.001(2) C28 0.035(4) 0.032(4) 0.043(4) 0.002(3) -0.001(3) 0.001(3) C29 0.023(3) 0.041(4) 0.020(3) 0.002(3) 0.005(2) 0.000(3) C30 0.026(3) 0.036(4) 0.020(3) -0.005(3) -0.001(2) 0.011(3) C31 0.033(3) 0.045(4) 0.020(3) -0.021(3) -0.003(3) 0.014(3) C32 0.017(3) 0.043(4) 0.023(3) -0.008(3) 0.005(2) 0.008(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 Br Co 2.4200(9) . ? Co N2 1.912(5) . ? Co N3 1.913(5) . ? Co N1 1.926(4) . ? Co N4 1.926(4) . ? Co N5 2.023(4) . ? Fe N7 1.921(4) . ? Fe N9 1.922(5) . ? Fe N10 1.944(5) . ? Fe N11 1.946(4) . ? Fe N8 1.957(4) . ? Fe N6 1.975(4) . ? P1 F1 1.550(7) 2_675 ? P1 F1 1.550(7) . ? P1 F2 1.579(6) . ? P1 F2 1.579(6) 2_675 ? P1 F3 1.593(5) 2_675 ? P1 F3 1.593(5) . ? P2 F5 1.592(6) 2_745 ? P2 F5 1.592(6) . ? P2 F4 1.611(5) . ? P2 F4 1.611(5) 2_745 ? P2 F6 1.612(6) . ? P2 F6 1.612(6) 2_745 ? O1 N1 1.351(6) . ? O2 N2 1.365(6) . ? O3 N3 1.370(6) . ? O4 N4 1.357(6) . ? O5 N7 1.392(5) . ? O5 B 1.526(7) . ? O6 N9 1.395(5) . ? O6 B 1.506(7) . ? O7 N11 1.394(5) . ? O7 B 1.487(8) . ? N1 C1 1.302(7) . ? N2 C6 1.326(7) . ? N3 C7 1.324(7) . ? N4 C12 1.295(7) . ? N5 C17 1.330(7) . ? N5 C13 1.354(7) . ? N6 C18 1.314(7) . ? N6 N13 1.441(6) . ? N7 C19 1.332(7) . ? N8 C22 1.325(7) . ? N8 N14 1.453(6) . ? N9 C23 1.312(6) . ? N10 C26 1.345(7) . ? N10 N12 1.450(6) . ? N11 C27 1.324(7) . ? N12 C30 1.483(7) . ? N12 C31 1.491(8) . ? N13 C32 1.474(7) . ? N13 C31 1.488(9) . ? N14 C30 1.471(8) . ? N14 C32 1.506(7) . ? B C15 1.621(8) . ? C1 C6 1.492(9) . ? C1 C2 1.512(8) . ? C2 C3 1.516(10) . ? C3 C4 1.456(12) . ? C4 C5 1.575(11) . ? C5 C6 1.505(8) . ? C7 C12 1.493(8) . ? C7 C8 1.497(8) . ? C8 C9 1.523(9) . ? C9 C10 1.491(11) . ? C10 C11 1.558(11) . ? C11 C12 1.511(7) . ? C13 C14 1.403(8) . ? C14 C15 1.413(7) . ? C15 C16 1.390(8) . ? C16 C17 1.397(8) . ? C18 C19 1.455(7) . ? C18 C20 1.511(7) . ? C19 C21 1.509(8) . ? C22 C23 1.455(8) . ? C22 C24 1.512(7) . ? C23 C25 1.516(8) . ? C26 C27 1.463(8) . ? C26 C28 1.485(9) . ? C27 C29 1.525(7) . ? C100 O101 0.91(3) . ? C100 O101 1.24(3) 2_756 ? C100 C101 1.33(4) . ? C100 C100 1.58(5) 2_756 ? C100 O100 1.61(3) . ? C101 O101 1.32(4) . ? O100 O101 1.36(3) . ? O101 C100 1.24(3) 2_756 ? O101 O101 1.49(5) 2_756 ? 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 N2 Co N3 178.2(2) . . ? N2 Co N1 81.8(2) . . ? N3 Co N1 97.6(2) . . ? N2 Co N4 98.8(2) . . ? N3 Co N4 81.8(2) . . ? N1 Co N4 177.9(2) . . ? N2 Co N5 91.4(2) . . ? N3 Co N5 90.3(2) . . ? N1 Co N5 91.7(2) . . ? N4 Co N5 90.4(2) . . ? N2 Co Br 89.45(14) . . ? N3 Co Br 88.85(14) . . ? N1 Co Br 89.66(14) . . ? N4 Co Br 88.31(14) . . ? N5 Co Br 178.50(12) . . ? N7 Fe N9 86.4(2) . . ? N7 Fe N10 116.1(2) . . ? N9 Fe N10 152.0(2) . . ? N7 Fe N11 85.2(2) . . ? N9 Fe N11 88.2(2) . . ? N10 Fe N11 78.0(2) . . ? N7 Fe N8 149.1(2) . . ? N9 Fe N8 77.7(2) . . ? N10 Fe N8 88.2(2) . . ? N11 Fe N8 120.0(2) . . ? N7 Fe N6 77.9(2) . . ? N9 Fe N6 117.0(2) . . ? N10 Fe N6 85.5(2) . . ? N11 Fe N6 148.1(2) . . ? N8 Fe N6 86.0(2) . . ? F1 P1 F1 179.999(2) 2_675 . ? F1 P1 F2 92.7(5) 2_675 . ? F1 P1 F2 87.3(5) . . ? F1 P1 F2 87.3(5) 2_675 2_675 ? F1 P1 F2 92.7(5) . 2_675 ? F2 P1 F2 179.998(2) . 2_675 ? F1 P1 F3 91.4(4) 2_675 2_675 ? F1 P1 F3 88.6(4) . 2_675 ? F2 P1 F3 89.4(3) . 2_675 ? F2 P1 F3 90.6(3) 2_675 2_675 ? F1 P1 F3 88.6(4) 2_675 . ? F1 P1 F3 91.4(4) . . ? F2 P1 F3 90.6(3) . . ? F2 P1 F3 89.4(3) 2_675 . ? F3 P1 F3 180.0 2_675 . ? F5 P2 F5 180.0 2_745 . ? F5 P2 F4 90.8(4) 2_745 . ? F5 P2 F4 89.2(3) . . ? F5 P2 F4 89.3(4) 2_745 2_745 ? F5 P2 F4 90.8(4) . 2_745 ? F4 P2 F4 179.999(2) . 2_745 ? F5 P2 F6 89.8(3) 2_745 . ? F5 P2 F6 90.2(3) . . ? F4 P2 F6 89.2(4) . . ? F4 P2 F6 90.8(4) 2_745 . ? F5 P2 F6 90.2(3) 2_745 2_745 ? F5 P2 F6 89.8(3) . 2_745 ? F4 P2 F6 90.8(4) . 2_745 ? F4 P2 F6 89.2(4) 2_745 2_745 ? F6 P2 F6 180.0 . 2_745 ? N7 O5 B 111.6(4) . . ? N9 O6 B 111.7(4) . . ? N11 O7 B 111.7(4) . . ? C1 N1 O1 120.9(5) . . ? C1 N1 Co 116.3(4) . . ? O1 N1 Co 122.7(3) . . ? C6 N2 O2 120.4(5) . . ? C6 N2 Co 116.2(4) . . ? O2 N2 Co 123.4(3) . . ? C7 N3 O3 119.0(5) . . ? C7 N3 Co 116.3(4) . . ? O3 N3 Co 124.6(3) . . ? C12 N4 O4 121.4(5) . . ? C12 N4 Co 116.0(4) . . ? O4 N4 Co 122.6(3) . . ? C17 N5 C13 117.9(5) . . ? C17 N5 Co 119.5(4) . . ? C13 N5 Co 122.6(4) . . ? C18 N6 N13 115.8(4) . . ? C18 N6 Fe 117.1(4) . . ? N13 N6 Fe 123.2(3) . . ? C19 N7 O5 116.0(4) . . ? C19 N7 Fe 120.3(4) . . ? O5 N7 Fe 123.3(3) . . ? C22 N8 N14 115.8(4) . . ? C22 N8 Fe 117.4(4) . . ? N14 N8 Fe 122.8(3) . . ? C23 N9 O6 115.8(4) . . ? C23 N9 Fe 120.5(4) . . ? O6 N9 Fe 123.3(3) . . ? C26 N10 N12 115.0(5) . . ? C26 N10 Fe 119.2(4) . . ? N12 N10 Fe 124.1(4) . . ? C27 N11 O7 117.2(4) . . ? C27 N11 Fe 119.1(3) . . ? O7 N11 Fe 122.5(3) . . ? N10 N12 C30 107.7(4) . . ? N10 N12 C31 109.6(4) . . ? C30 N12 C31 108.6(5) . . ? N6 N13 C32 111.3(4) . . ? N6 N13 C31 107.3(4) . . ? C32 N13 C31 109.6(5) . . ? N8 N14 C30 110.9(4) . . ? N8 N14 C32 106.5(4) . . ? C30 N14 C32 110.2(4) . . ? O7 B O6 112.1(4) . . ? O7 B O5 110.7(4) . . ? O6 B O5 109.6(4) . . ? O7 B C15 110.8(4) . . ? O6 B C15 107.1(4) . . ? O5 B C15 106.4(4) . . ? N1 C1 C6 113.1(5) . . ? N1 C1 C2 125.1(6) . . ? C6 C1 C2 121.8(5) . . ? C1 C2 C3 112.4(6) . . ? C4 C3 C2 112.7(6) . . ? C3 C4 C5 115.1(6) . . ? C6 C5 C4 110.4(6) . . ? N2 C6 C1 112.6(5) . . ? N2 C6 C5 125.9(6) . . ? C1 C6 C5 121.5(5) . . ? N3 C7 C12 112.1(5) . . ? N3 C7 C8 125.1(5) . . ? C12 C7 C8 122.7(5) . . ? C7 C8 C9 113.5(6) . . ? C10 C9 C8 113.5(6) . . ? C9 C10 C11 114.6(7) . . ? C12 C11 C10 110.3(6) . . ? N4 C12 C7 113.7(5) . . ? N4 C12 C11 125.4(5) . . ? C7 C12 C11 120.8(5) . . ? N5 C13 C14 122.8(5) . . ? C13 C14 C15 120.0(6) . . ? C16 C15 C14 115.2(5) . . ? C16 C15 B 120.0(5) . . ? C14 C15 B 124.7(5) . . ? C15 C16 C17 122.1(5) . . ? N5 C17 C16 122.1(6) . . ? N6 C18 C19 113.4(5) . . ? N6 C18 C20 125.7(5) . . ? C19 C18 C20 120.9(5) . . ? N7 C19 C18 110.5(5) . . ? N7 C19 C21 124.0(5) . . ? C18 C19 C21 125.5(5) . . ? N8 C22 C23 112.2(5) . . ? N8 C22 C24 125.1(5) . . ? C23 C22 C24 122.6(5) . . ? N9 C23 C22 110.9(5) . . ? N9 C23 C25 124.2(5) . . ? C22 C23 C25 124.8(5) . . ? N10 C26 C27 110.9(5) . . ? N10 C26 C28 125.9(5) . . ? C27 C26 C28 123.2(5) . . ? N11 C27 C26 112.2(5) . . ? N11 C27 C29 124.4(5) . . ? C26 C27 C29 123.4(5) . . ? N14 C30 N12 115.6(5) . . ? N13 C31 N12 114.8(5) . . ? N13 C32 N14 113.4(4) . . ? O101 C100 O101 86.4(30) . 2_756 ? O101 C100 C101 69.2(27) . . ? O101 C100 C101 128.4(27) 2_756 . ? O101 C100 C100 51.5(22) . 2_756 ? O101 C100 C100 34.9(15) 2_756 2_756 ? C101 C100 C100 106.5(27) . 2_756 ? O101 C100 O100 57.8(22) . . ? O101 C100 O100 116.4(23) 2_756 . ? C101 C100 O100 88.6(21) . . ? C100 C100 O100 92.4(21) 2_756 . ? O101 C101 C100 40.0(16) . . ? O101 O100 C100 34.3(12) . . ? C100 O101 C100 93.6(30) . 2_756 ? C100 O101 C101 70.8(28) . . ? C100 O101 C101 132.1(28) 2_756 . ? C100 O101 O100 87.9(27) . . ? C100 O101 O100 124.5(24) 2_756 . ? C101 O101 O100 100.6(24) . . ? C100 O101 O101 56.2(23) . 2_756 ? C100 O101 O101 37.4(15) 2_756 2_756 ? C101 O101 O101 110.9(31) . 2_756 ? O100 O101 O101 116.7(29) . 2_756 ? _refine_diff_density_max 1.432 _refine_diff_density_min -1.170 _refine_diff_density_rms 0.165 #===END