# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1483 data_z9802 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H8 Co N2 O4' _chemical_formula_weight 303.13 _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' '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'I m m 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, z' '-x, y, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 10.9768(3) _cell_length_b 11.4017(3) _cell_length_c 5.4032(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 676.23(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2321 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 33.10 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method ? _exptl_crystal_F_000 306 _exptl_absorpt_coefficient_mu 1.278 _exptl_absorpt_correction_type 'empirical using SADABS(Siemens, 1996)' _exptl_absorpt_correction_T_min 0.670 _exptl_absorpt_correction_T_max 0.893 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2230 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 628 _reflns_number_observed 605 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXTL (Sheldrick, 1996)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1996)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1996)' _computing_publication_material ; SHELXTL (Sheldrick, 1996) PARST (Nardelli, 1995) ; _refine_special_details ; Refinement on F^2^ for ALL reflections. 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 observed R-factor 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^)+(0.0399P)^2^+0.3475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _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 0.08(6) _refine_ls_number_reflns 628 _refine_ls_number_parameters 55 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_obs 0.0257 _refine_ls_wR_factor_all 0.0671 _refine_ls_wR_factor_obs 0.0666 _refine_ls_goodness_of_fit_all 1.119 _refine_ls_goodness_of_fit_obs 1.132 _refine_ls_restrained_S_all 1.118 _refine_ls_restrained_S_obs 1.131 _refine_ls_shift/esd_max 0.000 _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 Co1 Co 0.5000 0.0000 0.4590(6) 0.0186(2) Uani 1 d S . O1 O 0.6219(6) 0.0000 0.7572(4) 0.0256(15) Uani 1 d S . O2 O 0.3755(6) 0.0000 0.1702(5) 0.0252(15) Uani 1 d S . N1 N 0.5000 0.1888(2) 0.4590(6) 0.0293(5) Uani 1 d S . C1 C 0.5720(2) 0.0000 0.9740(23) 0.0187(8) Uani 1 d S . C2 C 0.3983(2) 0.2501(2) 0.4590(6) 0.0655(12) Uani 1 d . . C3 C 0.3942(2) 0.3711(2) 0.4590(6) 0.0712(13) Uani 1 d . . C4 C 0.5000 0.4347(2) 0.4590(6) 0.0365(8) Uani 1 d S . H2 H 0.3222(28) 0.2041(28) 0.4590(6) 0.070(10) Uiso 1 d . . H3 H 0.3216(35) 0.4031(30) 0.4590(6) 0.092(13) Uiso 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 Co1 0.0228(3) 0.0142(2) 0.0189(3) 0.000 0.000 0.000 O1 0.020(3) 0.040(3) 0.017(3) 0.000 -0.010(3) 0.000 O2 0.023(3) 0.028(3) 0.025(3) 0.000 0.016(3) 0.000 N1 0.0285(11) 0.0150(9) 0.044(2) -0.002(6) 0.000 0.000 C1 0.0223(13) 0.0152(10) 0.018(2) 0.000 0.017(3) 0.000 C2 0.0287(11) 0.0191(10) 0.149(4) -0.008(7) -0.019(6) -0.0022(9) C3 0.0256(11) 0.0194(11) 0.169(4) 0.009(8) -0.001(7) 0.0027(8) C4 0.0269(13) 0.0151(12) 0.068(2) 0.006(8) 0.000 0.000 _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 Co1 O2 2.074(7) . ? Co1 O2 2.074(7) 2_655 ? Co1 O1 2.094(5) . ? Co1 O1 2.094(5) 2_655 ? Co1 N1 2.153(2) 2_655 ? Co1 N1 2.153(2) . ? O1 C1 1.293(12) . ? O2 C1 1.206(13) 2_654 ? N1 C2 1.317(3) 4_655 ? N1 C2 1.317(3) . ? C1 O2 1.206(13) 2_656 ? C1 C1 1.582(5) 2_655 ? C2 C3 1.381(3) . ? C3 C4 1.369(3) . ? C4 C3 1.369(3) 4_655 ? C4 C4 1.489(5) 2_665 ? 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 Co1 O2 82.4(3) . 2_655 ? O2 Co1 O1 178.5(3) . . ? O2 Co1 O1 99.09(8) 2_655 . ? O2 Co1 O1 99.09(8) . 2_655 ? O2 Co1 O1 178.5(3) 2_655 2_655 ? O1 Co1 O1 79.4(3) . 2_655 ? O2 Co1 N1 90.0 . 2_655 ? O2 Co1 N1 90.0 2_655 2_655 ? O1 Co1 N1 90.0 . 2_655 ? O1 Co1 N1 90.0 2_655 2_655 ? O2 Co1 N1 90.0 . . ? O2 Co1 N1 90.0 2_655 . ? O1 Co1 N1 90.0 . . ? O1 Co1 N1 90.0 2_655 . ? N1 Co1 N1 180.0(3) 2_655 . ? C1 O1 Co1 115.3(5) . . ? C1 O2 Co1 110.3(5) 2_654 . ? C2 N1 C2 115.9(2) 4_655 . ? C2 N1 Co1 122.04(12) 4_655 . ? C2 N1 Co1 122.04(12) . . ? O2 C1 O1 126.5(2) 2_656 . ? O2 C1 C1 118.5(5) 2_656 2_655 ? O1 C1 C1 115.0(4) . 2_655 ? N1 C2 C3 123.9(2) . . ? C4 C3 C2 120.1(2) . . ? C3 C4 C3 116.1(3) . 4_655 ? C3 C4 C4 121.97(13) . 2_665 ? C3 C4 C4 121.97(13) 4_655 2_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C1 0.000(12) . . . . ? O2 Co1 O1 C1 180.000(2) 2_655 . . . ? O1 Co1 O1 C1 0.000(2) 2_655 . . . ? N1 Co1 O1 C1 -90.000(2) 2_655 . . . ? N1 Co1 O1 C1 90.000(2) . . . . ? O2 Co1 O2 C1 0.0 2_655 . . 2_654 ? O1 Co1 O2 C1 180.000(10) . . . 2_654 ? O1 Co1 O2 C1 180.0 2_655 . . 2_654 ? N1 Co1 O2 C1 -90.0 2_655 . . 2_654 ? N1 Co1 O2 C1 90.0 . . . 2_654 ? O2 Co1 N1 C2 -131.2(2) . . . 4_655 ? O2 Co1 N1 C2 -48.8(2) 2_655 . . 4_655 ? O1 Co1 N1 C2 50.3(2) . . . 4_655 ? O1 Co1 N1 C2 129.7(2) 2_655 . . 4_655 ? N1 Co1 N1 C2 90.0(1000) 2_655 . . 4_655 ? O2 Co1 N1 C2 48.8(2) . . . . ? O2 Co1 N1 C2 131.2(2) 2_655 . . . ? O1 Co1 N1 C2 -129.7(2) . . . . ? O1 Co1 N1 C2 -50.3(2) 2_655 . . . ? N1 Co1 N1 C2 -90.0(1000) 2_655 . . . ? Co1 O1 C1 O2 180.000(1) . . . 2_656 ? Co1 O1 C1 C1 0.0 . . . 2_655 ? C2 N1 C2 C3 0.0 4_655 . . . ? Co1 N1 C2 C3 180.0 . . . . ? N1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C3 0.0 . . . 4_655 ? C2 C3 C4 C4 180.0 . . . 2_665 ? _refine_diff_density_max 0.302 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.061 # END OF CIF data_z9801 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H32 Fe3 N8 O12' _chemical_formula_weight 1056.35 _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' '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' '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 16.2475(2) _cell_length_b 15.9840(2) _cell_length_c 16.38560(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.2776(3) _cell_angle_gamma 90.00 _cell_volume 4243.49(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7444 _cell_measurement_theta_min ? _cell_measurement_theta_max 28.03 _exptl_crystal_description 'trunk' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method ? _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 1.090 _exptl_absorpt_correction_type 'empirical using SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.942 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24362 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 28.03 _reflns_number_total 9195 _reflns_number_observed 5422 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXL (Sheldrick, 1994)' _computing_structure_refinement 'SHELXL (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXL (Sheldrick, 1994)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0336P)^2^+1.9427P] 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 SHELXL _refine_ls_extinction_coef 0.00022(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9195 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_obs 0.0493 _refine_ls_wR_factor_all 0.1127 _refine_ls_wR_factor_obs 0.0887 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.023 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.001 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 Fe1 Fe 0.28486(3) 0.22416(3) 0.46061(3) 0.02282(14) Uani 1 d . . Fe2 Fe 0.24457(3) 0.55750(3) 0.50792(3) 0.02286(14) Uani 1 d . . Fe3 Fe 0.22527(3) 0.89397(3) 0.52602(3) 0.02362(14) Uani 1 d . . O1 O 0.21272(15) 0.1224(2) 0.41215(14) 0.0273(6) Uani 1 d . . O2 O 0.33464(15) 0.1246(2) 0.53328(14) 0.0287(6) Uani 1 d . . O3 O 0.22446(14) 0.32649(15) 0.40151(14) 0.0259(6) Uani 1 d . . O4 O 0.34735(14) 0.32410(15) 0.52127(14) 0.0258(6) Uani 1 d . . O5 O 0.20300(14) 0.46241(15) 0.42512(14) 0.0251(6) Uani 1 d . . O6 O 0.32938(14) 0.46098(15) 0.54305(14) 0.0261(6) Uani 1 d . . O7 O 0.15996(14) 0.65385(15) 0.47065(14) 0.0258(6) Uani 1 d . . O8 O 0.28652(14) 0.6544(2) 0.58870(13) 0.0248(6) Uani 1 d . . O9 O 0.15541(14) 0.79322(15) 0.47547(13) 0.0243(6) Uani 1 d . . O10 O 0.27681(14) 0.79383(15) 0.59709(13) 0.0251(6) Uani 1 d . . O11 O 0.18340(15) 0.99034(15) 0.44395(14) 0.0284(6) Uani 1 d . . O12 O 0.30057(15) 0.99551(15) 0.57014(14) 0.0281(6) Uani 1 d . . N1 N 0.1900(2) 0.2332(2) 0.5568(2) 0.0307(8) Uani 1 d . . N2 N -0.1079(2) 0.2140(2) 0.8517(2) 0.0338(8) Uani 1 d . . N3 N 0.3762(2) 0.1989(2) 0.3696(2) 0.0277(7) Uani 1 d . . N4 N 0.6713(2) 0.1122(2) 0.0817(2) 0.0274(7) Uani 1 d . . N5 N 0.1602(2) 0.5067(2) 0.5980(2) 0.0292(7) Uani 1 d . . N6 N -0.1333(2) 0.4311(2) 0.8896(2) 0.0281(7) Uani 1 d . . N7 N 0.3221(2) 0.8717(2) 0.4373(2) 0.0315(8) Uani 1 d . . N8 N 0.6136(2) 0.9237(2) 0.1399(2) 0.0369(8) Uani 1 d . . C1 C 0.1094(2) 0.2273(3) 0.5351(2) 0.0348(10) Uani 1 d . . H1A H 0.0927(2) 0.2250(3) 0.4796(2) 0.042 Uiso 1 calc R . C2 C 0.0498(2) 0.2244(3) 0.5901(2) 0.0355(10) Uani 1 d . . H2A H -0.0056(2) 0.2205(3) 0.5715(2) 0.043 Uiso 1 calc R . C3 C 0.0721(2) 0.2273(2) 0.6733(2) 0.0287(9) Uani 1 d . . C4 C 0.1560(2) 0.2350(3) 0.6955(2) 0.0394(11) Uani 1 d . . H4A H 0.1746(2) 0.2382(3) 0.7505(2) 0.047 Uiso 1 calc R . C5 C 0.2112(2) 0.2379(3) 0.6364(2) 0.0415(11) Uani 1 d . . H5A H 0.2669(2) 0.2434(3) 0.6531(2) 0.050 Uiso 1 calc R . C6 C 0.0100(2) 0.2231(2) 0.7359(2) 0.0270(8) Uani 1 d . . C7 C 0.0297(2) 0.1905(2) 0.8133(2) 0.0333(9) Uani 1 d . . H7A H 0.0827(2) 0.1712(2) 0.8282(2) 0.040 Uiso 1 calc R . C8 C -0.0312(2) 0.1874(2) 0.8678(2) 0.0333(10) Uani 1 d . . H8A H -0.0173(2) 0.1650(2) 0.9194(2) 0.040 Uiso 1 calc R . C9 C -0.1259(2) 0.2453(3) 0.7771(2) 0.0349(10) Uani 1 d . . H9A H -0.1793(2) 0.2644(3) 0.7643(2) 0.042 Uiso 1 calc R . C10 C -0.0702(2) 0.2511(3) 0.7177(2) 0.0346(10) Uani 1 d . . H10A H -0.0861(2) 0.2734(3) 0.6664(2) 0.042 Uiso 1 calc R . C11 C 0.3561(2) 0.1623(2) 0.2973(2) 0.0325(9) Uani 1 d . . H11A H 0.3014(2) 0.1467(2) 0.2851(2) 0.039 Uiso 1 calc R . C12 C 0.4123(2) 0.1463(3) 0.2400(2) 0.0349(10) Uani 1 d . . H12A H 0.3948(2) 0.1220(3) 0.1901(2) 0.042 Uiso 1 calc R . C13 C 0.4948(2) 0.1669(2) 0.2570(2) 0.0274(9) Uani 1 d . . C14 C 0.5165(2) 0.2025(2) 0.3325(2) 0.0303(9) Uani 1 d . . H14A H 0.5713(2) 0.2159(2) 0.3472(2) 0.036 Uiso 1 calc R . C15 C 0.4560(2) 0.2182(2) 0.3861(2) 0.0320(9) Uani 1 d . . H15A H 0.4717(2) 0.2433(2) 0.4360(2) 0.038 Uiso 1 calc R . C16 C 0.5568(2) 0.1497(2) 0.1963(2) 0.0268(9) Uani 1 d . . C17 C 0.5363(2) 0.1560(3) 0.1132(2) 0.0325(9) Uani 1 d . . H17A H 0.4836(2) 0.1727(3) 0.0940(2) 0.039 Uiso 1 calc R . C18 C 0.5950(2) 0.1370(2) 0.0586(2) 0.0308(9) Uani 1 d . . H18A H 0.5802(2) 0.1420(2) 0.0029(2) 0.037 Uiso 1 calc R . C19 C 0.6915(2) 0.1088(3) 0.1616(2) 0.0347(10) Uani 1 d . . H19A H 0.7450(2) 0.0932(3) 0.1790(2) 0.042 Uiso 1 calc R . C20 C 0.6375(2) 0.1272(3) 0.2205(2) 0.0345(10) Uani 1 d . . H20A H 0.6550(2) 0.1244(3) 0.2758(2) 0.041 Uiso 1 calc R . C21 C 0.0854(2) 0.4768(2) 0.5765(2) 0.0327(9) Uani 1 d . . H21A H 0.0717(2) 0.4667(2) 0.5212(2) 0.039 Uiso 1 calc R . C22 C 0.0271(2) 0.4598(3) 0.6308(2) 0.0356(10) Uani 1 d . . H22A H -0.0244(2) 0.4392(3) 0.6121(2) 0.043 Uiso 1 calc R . C23 C 0.0455(2) 0.4737(2) 0.7135(2) 0.0282(9) Uani 1 d . . C24 C 0.1241(2) 0.5018(3) 0.7370(2) 0.0352(10) Uani 1 d . . H24A H 0.1402(2) 0.5099(3) 0.7921(2) 0.042 Uiso 1 calc R . C25 C 0.1785(2) 0.5179(3) 0.6785(2) 0.0370(10) Uani 1 d . . H25A H 0.2309(2) 0.5375(3) 0.6956(2) 0.044 Uiso 1 calc R . C26 C -0.0164(2) 0.4599(2) 0.7745(2) 0.0287(9) Uani 1 d . . C27 C 0.0063(2) 0.4265(2) 0.8510(2) 0.0327(9) Uani 1 d . . H27A H 0.0612(2) 0.4136(2) 0.8656(2) 0.039 Uiso 1 calc R . C28 C -0.0534(2) 0.4125(3) 0.9054(2) 0.0353(10) Uani 1 d . . H28A H -0.0370(2) 0.3889(3) 0.9559(2) 0.042 Uiso 1 calc R . C29 C -0.1540(2) 0.4655(2) 0.8165(2) 0.0312(9) Uani 1 d . . H29A H -0.2090(2) 0.4802(2) 0.8045(2) 0.037 Uiso 1 calc R . C30 C -0.0995(2) 0.4806(2) 0.7582(2) 0.0330(10) Uani 1 d . . H30A H -0.1177(2) 0.5043(2) 0.7082(2) 0.040 Uiso 1 calc R . C31 C 0.3022(2) 0.8574(2) 0.3579(2) 0.0341(10) Uani 1 d . . H31A H 0.2483(2) 0.8411(2) 0.3424(2) 0.041 Uiso 1 calc R . C32 C 0.3563(2) 0.8654(3) 0.2976(2) 0.0339(10) Uani 1 d . . H32A H 0.3391(2) 0.8547(3) 0.2432(2) 0.041 Uiso 1 calc R . C33 C 0.4372(2) 0.8897(2) 0.3195(2) 0.0290(9) Uani 1 d . . C34 C 0.4589(2) 0.9026(3) 0.4018(2) 0.0365(10) Uani 1 d . . H34A H 0.5126(2) 0.9180(3) 0.4192(2) 0.044 Uiso 1 calc R . C36 C 0.4980(2) 0.9021(2) 0.2565(2) 0.0286(9) Uani 1 d . . C35 C 0.4007(2) 0.8925(3) 0.4580(2) 0.0396(11) Uani 1 d . . H35A H 0.4168(2) 0.9007(3) 0.5130(2) 0.048 Uiso 1 calc R . C37 C 0.5813(2) 0.8861(3) 0.2753(2) 0.0355(10) Uani 1 d . . H37A H 0.6004(2) 0.8684(3) 0.3274(2) 0.043 Uiso 1 calc R . C38 C 0.6350(2) 0.8972(3) 0.2148(2) 0.0398(11) Uani 1 d . . H38A H 0.6905(2) 0.8852(3) 0.2277(2) 0.048 Uiso 1 calc R . C39 C 0.5339(3) 0.9400(3) 0.1231(2) 0.0366(10) Uani 1 d . . H39A H 0.5173(3) 0.9594(3) 0.0709(2) 0.044 Uiso 1 calc R . C40 C 0.4740(2) 0.9300(2) 0.1783(2) 0.0334(9) Uani 1 d . . H40A H 0.4189(2) 0.9418(2) 0.1631(2) 0.040 Uiso 1 calc R . C41 C 0.2403(2) 0.3944(2) 0.4382(2) 0.0201(8) Uani 1 d . . C42 C 0.3123(2) 0.3934(2) 0.5063(2) 0.0211(8) Uani 1 d . . C43 C 0.1836(2) 0.7231(2) 0.4991(2) 0.0209(8) Uani 1 d . . C44 C 0.2543(2) 0.7234(2) 0.5677(2) 0.0193(7) Uani 1 d . . C45 C 0.2232(2) 1.0566(2) 0.4544(2) 0.0238(8) Uani 1 d . . C46 C 0.2924(2) 0.0589(2) 0.5257(2) 0.0227(8) Uani 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 Fe1 0.0259(3) 0.0176(3) 0.0256(3) -0.0009(2) 0.0060(2) -0.0002(2) Fe2 0.0267(3) 0.0178(3) 0.0248(3) 0.0000(2) 0.0069(2) 0.0002(2) Fe3 0.0273(3) 0.0187(3) 0.0257(3) 0.0004(2) 0.0073(2) 0.0001(2) O1 0.0320(15) 0.0216(14) 0.0278(14) 0.0031(11) -0.0008(12) 0.0001(11) O2 0.0300(15) 0.0227(15) 0.0326(14) 0.0006(12) -0.0031(12) -0.0057(12) O3 0.0304(14) 0.0217(15) 0.0251(13) -0.0032(11) -0.0009(11) -0.0010(11) O4 0.0239(14) 0.0232(15) 0.0297(14) 0.0010(11) -0.0019(11) 0.0035(11) O5 0.0286(14) 0.0204(14) 0.0260(13) -0.0006(11) 0.0006(11) 0.0040(11) O6 0.0282(14) 0.0221(14) 0.0274(14) -0.0054(11) -0.0020(11) -0.0001(11) O7 0.0267(14) 0.0201(14) 0.0302(14) -0.0039(11) -0.0014(11) 0.0000(11) O8 0.0254(14) 0.0242(15) 0.0249(13) 0.0027(11) 0.0018(11) 0.0049(11) O9 0.0253(14) 0.0199(15) 0.0271(13) 0.0019(11) -0.0011(11) 0.0020(11) O10 0.0252(14) 0.025(2) 0.0245(13) -0.0014(11) -0.0005(11) -0.0012(11) O11 0.0322(15) 0.0227(15) 0.0293(14) 0.0011(11) -0.0043(12) -0.0062(12) O12 0.0360(15) 0.0222(15) 0.0254(14) 0.0043(11) -0.0021(12) -0.0032(11) N1 0.024(2) 0.038(2) 0.030(2) -0.0007(15) 0.0052(15) -0.0021(15) N2 0.031(2) 0.038(2) 0.034(2) -0.005(2) 0.009(2) -0.005(2) N3 0.029(2) 0.028(2) 0.028(2) 0.0017(14) 0.0085(14) 0.0044(14) N4 0.028(2) 0.029(2) 0.026(2) -0.0029(14) 0.0084(14) 0.0028(14) N5 0.028(2) 0.030(2) 0.030(2) 0.0034(14) 0.0072(14) -0.0016(14) N6 0.031(2) 0.031(2) 0.023(2) 0.0006(14) 0.0069(14) -0.0041(14) N7 0.030(2) 0.032(2) 0.033(2) 0.0010(15) 0.006(2) 0.0024(15) N8 0.041(2) 0.039(2) 0.033(2) -0.003(2) 0.015(2) -0.007(2) C1 0.032(2) 0.048(3) 0.024(2) -0.005(2) 0.001(2) 0.001(2) C2 0.025(2) 0.054(3) 0.028(2) -0.003(2) 0.007(2) 0.003(2) C3 0.022(2) 0.036(2) 0.028(2) -0.002(2) 0.003(2) 0.002(2) C4 0.031(2) 0.064(3) 0.024(2) -0.003(2) 0.006(2) -0.001(2) C5 0.026(2) 0.068(3) 0.031(2) -0.002(2) 0.000(2) -0.004(2) C6 0.023(2) 0.033(2) 0.026(2) -0.003(2) 0.005(2) -0.004(2) C7 0.029(2) 0.038(2) 0.033(2) 0.001(2) 0.006(2) 0.003(2) C8 0.034(2) 0.039(3) 0.028(2) 0.003(2) 0.007(2) -0.001(2) C9 0.025(2) 0.045(3) 0.035(2) -0.004(2) 0.005(2) 0.004(2) C10 0.031(2) 0.048(3) 0.026(2) -0.001(2) 0.003(2) -0.001(2) C11 0.029(2) 0.037(2) 0.033(2) -0.005(2) 0.008(2) -0.004(2) C12 0.034(2) 0.042(3) 0.029(2) -0.008(2) 0.005(2) 0.002(2) C13 0.026(2) 0.032(2) 0.025(2) -0.001(2) 0.007(2) 0.004(2) C14 0.026(2) 0.036(2) 0.030(2) -0.008(2) 0.005(2) 0.001(2) C15 0.031(2) 0.039(3) 0.026(2) -0.006(2) 0.004(2) 0.005(2) C16 0.027(2) 0.024(2) 0.030(2) -0.004(2) 0.007(2) 0.003(2) C17 0.023(2) 0.045(3) 0.030(2) -0.001(2) 0.003(2) 0.002(2) C18 0.030(2) 0.039(2) 0.024(2) 0.001(2) 0.007(2) 0.001(2) C19 0.026(2) 0.047(3) 0.031(2) -0.008(2) 0.005(2) 0.006(2) C20 0.030(2) 0.050(3) 0.024(2) -0.006(2) 0.003(2) 0.005(2) C21 0.035(2) 0.042(3) 0.021(2) -0.002(2) 0.006(2) -0.008(2) C22 0.029(2) 0.049(3) 0.029(2) 0.002(2) 0.004(2) -0.006(2) C23 0.028(2) 0.032(2) 0.025(2) 0.006(2) 0.006(2) -0.001(2) C24 0.030(2) 0.055(3) 0.021(2) 0.005(2) 0.003(2) -0.011(2) C25 0.027(2) 0.053(3) 0.032(2) 0.006(2) 0.002(2) -0.013(2) C26 0.027(2) 0.034(2) 0.026(2) 0.000(2) 0.008(2) -0.006(2) C27 0.022(2) 0.042(3) 0.034(2) 0.006(2) 0.003(2) -0.003(2) C28 0.035(2) 0.048(3) 0.023(2) 0.009(2) 0.004(2) -0.004(2) C29 0.023(2) 0.041(3) 0.030(2) 0.006(2) 0.003(2) -0.001(2) C30 0.030(2) 0.045(3) 0.024(2) 0.010(2) 0.003(2) -0.002(2) C31 0.027(2) 0.041(3) 0.035(2) -0.004(2) 0.004(2) -0.003(2) C32 0.033(2) 0.043(3) 0.026(2) -0.004(2) 0.004(2) -0.003(2) C33 0.025(2) 0.038(3) 0.025(2) -0.002(2) 0.004(2) 0.003(2) C34 0.022(2) 0.056(3) 0.031(2) -0.004(2) 0.002(2) 0.000(2) C36 0.029(2) 0.032(2) 0.025(2) -0.001(2) 0.008(2) 0.000(2) C35 0.038(3) 0.058(3) 0.023(2) -0.003(2) 0.005(2) 0.004(2) C37 0.031(2) 0.051(3) 0.024(2) -0.002(2) 0.003(2) 0.001(2) C38 0.030(2) 0.055(3) 0.036(2) -0.004(2) 0.010(2) -0.001(2) C39 0.047(3) 0.037(3) 0.026(2) 0.000(2) 0.005(2) -0.005(2) C40 0.031(2) 0.038(3) 0.031(2) 0.002(2) 0.001(2) 0.001(2) C41 0.020(2) 0.026(2) 0.015(2) 0.000(2) 0.0056(15) -0.001(2) C42 0.021(2) 0.021(2) 0.022(2) 0.001(2) 0.008(2) -0.001(2) C43 0.020(2) 0.023(2) 0.020(2) -0.001(2) 0.0074(15) -0.001(2) C44 0.023(2) 0.019(2) 0.017(2) -0.002(2) 0.0067(15) -0.002(2) C45 0.030(2) 0.020(2) 0.022(2) -0.001(2) 0.005(2) 0.001(2) C46 0.024(2) 0.022(2) 0.023(2) -0.002(2) 0.004(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O4 2.102(2) . ? Fe1 O3 2.106(2) . ? Fe1 O2 2.112(3) . ? Fe1 O1 2.124(3) . ? Fe1 N3 2.217(3) . ? Fe1 N1 2.290(3) . ? Fe2 O5 2.114(2) . ? Fe2 O8 2.117(2) . ? Fe2 O6 2.119(2) . ? Fe2 O7 2.123(2) . ? Fe2 N5 2.240(3) . ? Fe2 N4 2.256(3) 2_655 ? Fe3 O9 2.104(2) . ? Fe3 O10 2.115(2) . ? Fe3 O11 2.123(2) . ? Fe3 O12 2.126(2) . ? Fe3 N6 2.193(3) 2_556 ? Fe3 N7 2.249(3) . ? O1 C45 1.264(4) 1_545 ? O2 C46 1.256(4) . ? O3 C41 1.259(4) . ? O4 C42 1.261(4) . ? O5 C41 1.254(4) . ? O6 C42 1.258(4) . ? O7 C43 1.250(4) . ? O8 C44 1.257(4) . ? O9 C43 1.260(4) . ? O10 C44 1.267(4) . ? O11 C45 1.246(4) . ? O12 C46 1.249(4) 1_565 ? N1 C5 1.326(5) . ? N1 C1 1.335(5) . ? N2 C8 1.324(5) . ? N2 C9 1.333(5) . ? N3 C11 1.339(4) . ? N3 C15 1.342(5) . ? N4 C19 1.326(4) . ? N4 C18 1.329(5) . ? N4 Fe2 2.256(3) 2_645 ? N5 C21 1.328(5) . ? N5 C25 1.343(5) . ? N6 C29 1.338(4) . ? N6 C28 1.337(5) . ? N6 Fe3 2.193(3) 2_546 ? N7 C31 1.337(4) . ? N7 C35 1.338(5) . ? N8 C38 1.320(5) . ? N8 C39 1.329(5) . ? C1 C2 1.372(5) . ? C2 C3 1.386(5) . ? C3 C4 1.389(5) . ? C3 C6 1.492(4) . ? C4 C5 1.369(5) . ? C6 C7 1.386(5) . ? C6 C10 1.389(5) . ? C7 C8 1.384(5) . ? C9 C10 1.382(5) . ? C11 C12 1.382(5) . ? C12 C13 1.389(5) . ? C13 C14 1.383(5) . ? C13 C16 1.493(4) . ? C14 C15 1.389(5) . ? C16 C17 1.380(5) . ? C16 C20 1.389(5) . ? C17 C18 1.390(5) . ? C19 C20 1.383(5) . ? C21 C22 1.376(5) . ? C22 C23 1.383(5) . ? C23 C24 1.382(5) . ? C23 C26 1.486(4) . ? C24 C25 1.376(5) . ? C26 C27 1.387(5) . ? C26 C30 1.396(5) . ? C27 C28 1.383(5) . ? C29 C30 1.373(5) . ? C31 C32 1.376(5) . ? C32 C33 1.392(5) . ? C33 C34 1.385(5) . ? C33 C36 1.495(4) . ? C34 C35 1.377(5) . ? C36 C37 1.389(5) . ? C36 C40 1.386(5) . ? C37 C38 1.381(5) . ? C39 C40 1.386(5) . ? C41 C42 1.556(5) . ? C43 C44 1.547(5) . ? C45 O1 1.264(4) 1_565 ? C45 C46 1.559(5) 1_565 ? C46 O12 1.249(4) 1_545 ? C46 C45 1.559(5) 1_545 ? 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 Fe1 O3 79.58(9) . . ? O4 Fe1 O2 98.91(9) . . ? O3 Fe1 O2 171.99(9) . . ? O4 Fe1 O1 172.84(9) . . ? O3 Fe1 O1 101.40(9) . . ? O2 Fe1 O1 79.12(9) . . ? O4 Fe1 N3 97.61(10) . . ? O3 Fe1 N3 98.29(10) . . ? O2 Fe1 N3 89.71(10) . . ? O1 Fe1 N3 89.28(10) . . ? O4 Fe1 N1 87.29(10) . . ? O3 Fe1 N1 87.31(10) . . ? O2 Fe1 N1 84.75(10) . . ? O1 Fe1 N1 85.68(10) . . ? N3 Fe1 N1 173.13(12) . . ? O5 Fe2 O8 178.78(9) . . ? O5 Fe2 O6 79.69(9) . . ? O8 Fe2 O6 100.98(9) . . ? O5 Fe2 O7 99.66(9) . . ? O8 Fe2 O7 79.65(9) . . ? O6 Fe2 O7 179.05(9) . . ? O5 Fe2 N5 88.87(10) . . ? O8 Fe2 N5 92.15(10) . . ? O6 Fe2 N5 88.56(10) . . ? O7 Fe2 N5 92.13(10) . . ? O5 Fe2 N4 92.34(10) . 2_655 ? O8 Fe2 N4 86.62(10) . 2_655 ? O6 Fe2 N4 92.63(10) . 2_655 ? O7 Fe2 N4 86.69(10) . 2_655 ? N5 Fe2 N4 178.43(11) . 2_655 ? O9 Fe3 O10 79.47(9) . . ? O9 Fe3 O11 99.67(9) . . ? O10 Fe3 O11 173.10(9) . . ? O9 Fe3 O12 176.17(9) . . ? O10 Fe3 O12 101.32(10) . . ? O11 Fe3 O12 79.09(9) . . ? O9 Fe3 N6 94.71(10) . 2_556 ? O10 Fe3 N6 96.77(10) . 2_556 ? O11 Fe3 N6 90.12(10) . 2_556 ? O12 Fe3 N6 88.93(10) . 2_556 ? O9 Fe3 N7 90.41(10) . . ? O10 Fe3 N7 88.19(10) . . ? O11 Fe3 N7 84.97(10) . . ? O12 Fe3 N7 85.87(11) . . ? N6 Fe3 N7 173.44(12) 2_556 . ? C45 O1 Fe1 112.6(2) 1_545 . ? C46 O2 Fe1 113.0(2) . . ? C41 O3 Fe1 112.3(2) . . ? C42 O4 Fe1 112.4(2) . . ? C41 O5 Fe2 112.7(2) . . ? C42 O6 Fe2 112.3(2) . . ? C43 O7 Fe2 111.2(2) . . ? C44 O8 Fe2 111.3(2) . . ? C43 O9 Fe3 112.8(2) . . ? C44 O10 Fe3 111.8(2) . . ? C45 O11 Fe3 113.0(2) . . ? C46 O12 Fe3 112.8(2) 1_565 . ? C5 N1 C1 116.3(3) . . ? C5 N1 Fe1 122.9(3) . . ? C1 N1 Fe1 120.7(2) . . ? C8 N2 C9 116.3(3) . . ? C11 N3 C15 116.5(3) . . ? C11 N3 Fe1 122.9(2) . . ? C15 N3 Fe1 120.6(2) . . ? C19 N4 C18 116.7(3) . . ? C19 N4 Fe2 120.7(2) . 2_645 ? C18 N4 Fe2 121.8(2) . 2_645 ? C21 N5 C25 116.1(3) . . ? C21 N5 Fe2 123.2(2) . . ? C25 N5 Fe2 119.8(2) . . ? C29 N6 C28 116.1(3) . . ? C29 N6 Fe3 122.5(2) . 2_546 ? C28 N6 Fe3 121.0(2) . 2_546 ? C31 N7 C35 116.5(3) . . ? C31 N7 Fe3 121.7(3) . . ? C35 N7 Fe3 119.8(2) . . ? C38 N8 C39 116.2(3) . . ? N1 C1 C2 123.7(3) . . ? C1 C2 C3 120.0(4) . . ? C2 C3 C4 116.1(3) . . ? C2 C3 C6 122.2(3) . . ? C4 C3 C6 121.6(3) . . ? C5 C4 C3 119.9(4) . . ? N1 C5 C4 124.0(4) . . ? C7 C6 C10 117.8(3) . . ? C7 C6 C3 121.5(3) . . ? C10 C6 C3 120.6(3) . . ? C8 C7 C6 118.5(4) . . ? N2 C8 C7 124.5(4) . . ? N2 C9 C10 124.2(4) . . ? C9 C10 C6 118.7(4) . . ? N3 C11 C12 123.6(4) . . ? C11 C12 C13 119.8(4) . . ? C14 C13 C12 117.1(3) . . ? C14 C13 C16 122.1(3) . . ? C12 C13 C16 120.8(3) . . ? C13 C14 C15 119.7(3) . . ? N3 C15 C14 123.4(3) . . ? C17 C16 C20 117.1(3) . . ? C17 C16 C13 121.2(3) . . ? C20 C16 C13 121.7(3) . . ? C16 C17 C18 119.5(3) . . ? N4 C18 C17 123.5(3) . . ? N4 C19 C20 123.9(4) . . ? C19 C20 C16 119.3(4) . . ? N5 C21 C22 124.0(3) . . ? C21 C22 C23 119.5(4) . . ? C24 C23 C22 117.0(3) . . ? C24 C23 C26 121.2(3) . . ? C22 C23 C26 121.8(3) . . ? C25 C24 C23 119.7(3) . . ? N5 C25 C24 123.5(4) . . ? C27 C26 C30 116.9(3) . . ? C27 C26 C23 121.2(3) . . ? C30 C26 C23 121.9(3) . . ? C28 C27 C26 119.5(3) . . ? N6 C28 C27 123.8(4) . . ? N6 C29 C30 124.2(3) . . ? C29 C30 C26 119.4(3) . . ? N7 C31 C32 124.2(4) . . ? C31 C32 C33 118.8(4) . . ? C34 C33 C32 117.4(3) . . ? C34 C33 C36 121.2(3) . . ? C32 C33 C36 121.3(3) . . ? C35 C34 C33 119.7(4) . . ? C37 C36 C40 117.9(3) . . ? C37 C36 C33 120.4(3) . . ? C40 C36 C33 121.7(3) . . ? N7 C35 C34 123.4(4) . . ? C38 C37 C36 118.3(4) . . ? N8 C38 C37 124.9(4) . . ? N8 C39 C40 124.2(4) . . ? C39 C40 C36 118.5(4) . . ? O5 C41 O3 125.9(3) . . ? O5 C41 C42 117.4(3) . . ? O3 C41 C42 116.7(3) . . ? O6 C42 O4 125.5(3) . . ? O6 C42 C41 117.5(3) . . ? O4 C42 C41 117.0(3) . . ? O7 C43 O9 125.4(3) . . ? O7 C43 C44 117.6(3) . . ? O9 C43 C44 117.0(3) . . ? O8 C44 O10 124.9(3) . . ? O8 C44 C43 117.9(3) . . ? O10 C44 C43 117.1(3) . . ? O11 C45 O1 125.7(3) . 1_565 ? O11 C45 C46 117.5(3) . 1_565 ? O1 C45 C46 116.8(3) 1_565 1_565 ? O12 C46 O2 125.9(3) 1_545 . ? O12 C46 C45 117.2(3) 1_545 1_545 ? O2 C46 C45 116.9(3) . 1_545 ? _refine_diff_density_max 0.357 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.081