# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_FeCu _database_code_depnum_ccdc_archive 'CCDC 892825' #TrackingRef 'web_deposit_cif_file_0_JorgePasan_1342702197.Fe_Cu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 Cu Fe2 N12 O5' _chemical_formula_weight 841.90 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' Fe Fe 0.3463 0.8444 '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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Imma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z' '-x, y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z' 'x, -y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y, z+1/2' _cell_length_a 26.182(2) _cell_length_b 12.7579(8) _cell_length_c 14.2467(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4758.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10134 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.1285 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2892 _reflns_number_gt 1379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics CRYSTALMAKER _computing_publication_material 'PARST97 (Nardelli, 1997)' _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^)+(0.1546P)^2^+1.7411P] 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 2892 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1827 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2801 _refine_ls_wR_factor_gt 0.2288 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 C1 C 0.4144(3) 0.1506(5) 0.4378(5) 0.0457(16) Uani 1 1 d . . . C2 C 0.3446(4) 0.2500 0.5466(8) 0.049(2) Uani 1 2 d S . . C3 C 0.3835(4) 0.2500 0.2818(9) 0.057(3) Uani 1 2 d S . . C4 C 0.3094(3) 0.0448(5) 0.3853(5) 0.0486(17) Uani 1 1 d . . . H4 H 0.3415 0.0141 0.3895 0.058 Uiso 1 1 calc R . . C5 C 0.2682(3) -0.0181(5) 0.3757(5) 0.060(2) Uani 1 1 d . . . H5 H 0.2729 -0.0903 0.3728 0.072 Uiso 1 1 calc R . . C6 C 0.2192(3) 0.0218(6) 0.3701(5) 0.063(2) Uani 1 1 d . . . C7 C 0.2152(3) 0.1314(5) 0.3736(5) 0.0551(18) Uani 1 1 d . . . H7 H 0.1834 0.1634 0.3703 0.066 Uiso 1 1 calc R . . C8 C 0.2589(3) 0.1914(5) 0.3822(4) 0.0446(16) Uani 1 1 d . . . C9 C 0.1731(3) -0.0449(7) 0.3615(6) 0.087(3) Uani 1 1 d . . . H9A H 0.1824 -0.1119 0.3361 0.131 Uiso 1 1 calc R . . H9B H 0.1489 -0.0116 0.3206 0.131 Uiso 1 1 calc R . . H9C H 0.1580 -0.0544 0.4224 0.131 Uiso 1 1 calc R . . Fe1 Fe 0.36185(5) 0.2500 0.41241(9) 0.0399(5) Uani 1 2 d S . . N1 N 0.4459(2) 0.0941(4) 0.4550(5) 0.0600(16) Uani 1 1 d . . . N2 N 0.3343(4) 0.2500 0.6232(7) 0.078(3) Uani 1 2 d S . . N3 N 0.3980(4) 0.2500 0.2055(8) 0.098(4) Uani 1 2 d S . . N4 N 0.30605(19) 0.1493(4) 0.3891(3) 0.0413(13) Uani 1 1 d . . . Cu1 Cu 0.5000 0.0000 0.5000 0.0611(7) Uani 1 4 d S . . O1W O 0.5000 0.0857(9) 0.6609(7) 0.131(4) Uani 1 2 d S . . O2W O 0.4314(6) 0.2500 0.7235(12) 0.097(6) Uani 0.50 2 d SP . . O3W O 0.5000 -0.073(4) 0.806(2) 0.276(19) Uani 0.50 2 d SP . . O4W O 0.4472(11) 0.295(2) 0.901(2) 0.128(13) Uani 0.25 1 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 C1 0.030(4) 0.044(3) 0.063(4) -0.002(3) -0.007(3) -0.001(3) C2 0.037(6) 0.046(5) 0.064(7) 0.000 -0.010(5) 0.000 C3 0.026(5) 0.061(6) 0.083(8) 0.000 -0.022(6) 0.000 C4 0.040(4) 0.039(3) 0.067(4) -0.002(3) -0.016(3) -0.004(3) C5 0.061(5) 0.047(4) 0.073(5) 0.005(3) -0.013(4) -0.009(4) C6 0.058(5) 0.064(5) 0.067(5) 0.017(4) -0.017(4) -0.026(4) C7 0.029(4) 0.065(4) 0.071(5) 0.005(4) -0.014(3) -0.005(3) C8 0.034(4) 0.051(3) 0.048(4) 0.000(3) -0.007(3) -0.002(3) C9 0.056(6) 0.094(6) 0.113(7) 0.016(5) -0.014(5) -0.036(5) Fe1 0.0269(7) 0.0389(7) 0.0539(9) 0.000 -0.0128(6) 0.000 N1 0.031(3) 0.049(3) 0.100(5) 0.016(3) -0.011(3) 0.003(3) N2 0.083(8) 0.091(7) 0.060(6) 0.000 -0.003(6) 0.000 N3 0.076(8) 0.161(11) 0.057(6) 0.000 -0.002(6) 0.000 N4 0.025(3) 0.045(3) 0.054(3) 0.002(2) -0.010(2) 0.000(2) Cu1 0.0207(9) 0.0459(10) 0.1167(16) 0.0325(9) 0.000 0.000 O1W 0.133(10) 0.127(8) 0.133(9) -0.019(7) 0.000 0.000 O2W 0.041(9) 0.160(16) 0.089(12) 0.000 -0.031(9) 0.000 O3W 0.34(5) 0.34(4) 0.14(3) 0.11(3) 0.000 0.000 O4W 0.077(18) 0.17(4) 0.13(2) -0.038(18) -0.016(17) 0.016(18) _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 C1 N1 1.122(8) . ? C1 Fe1 1.906(7) . ? C2 N2 1.124(13) . ? C2 Fe1 1.964(12) . ? C3 N3 1.151(14) . ? C3 Fe1 1.946(14) . ? C4 N4 1.337(7) . ? C4 C5 1.351(9) . ? C5 C6 1.382(10) . ? C6 C7 1.403(9) . ? C6 C9 1.482(10) . ? C7 C8 1.383(9) . ? C8 N4 1.349(8) . ? C8 C8 1.494(12) 12_565 ? Fe1 C1 1.906(7) 12_565 ? Fe1 N4 1.973(5) . ? Fe1 N4 1.973(5) 12_565 ? N1 Cu1 1.964(6) . ? Cu1 N1 1.964(6) 11_655 ? Cu1 N1 1.964(6) 3_556 ? Cu1 N1 1.964(6) 9_656 ? O4W O4W 1.15(5) 12_565 ? 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 N1 C1 Fe1 177.8(7) . . ? N2 C2 Fe1 179.5(10) . . ? N3 C3 Fe1 177.6(10) . . ? N4 C4 C5 123.0(7) . . ? C4 C5 C6 121.8(7) . . ? C5 C6 C7 115.7(6) . . ? C5 C6 C9 123.3(7) . . ? C7 C6 C9 120.9(7) . . ? C8 C7 C6 119.6(6) . . ? N4 C8 C7 122.9(6) . . ? N4 C8 C8 113.5(3) . 12_565 ? C7 C8 C8 123.6(4) . 12_565 ? C1 Fe1 C1 83.4(4) 12_565 . ? C1 Fe1 C3 88.3(3) 12_565 . ? C1 Fe1 C3 88.3(3) . . ? C1 Fe1 C2 89.0(3) 12_565 . ? C1 Fe1 C2 89.0(3) . . ? C3 Fe1 C2 176.4(4) . . ? C1 Fe1 N4 178.2(3) 12_565 . ? C1 Fe1 N4 97.7(2) . . ? C3 Fe1 N4 93.1(3) . . ? C2 Fe1 N4 89.6(3) . . ? C1 Fe1 N4 97.7(2) 12_565 12_565 ? C1 Fe1 N4 178.2(3) . 12_565 ? C3 Fe1 N4 93.1(3) . 12_565 ? C2 Fe1 N4 89.6(3) . 12_565 ? N4 Fe1 N4 81.2(3) . 12_565 ? C1 N1 Cu1 173.5(7) . . ? C4 N4 C8 117.0(5) . . ? C4 N4 Fe1 127.4(4) . . ? C8 N4 Fe1 115.5(4) . . ? N1 Cu1 N1 180.0(2) 11_655 3_556 ? N1 Cu1 N1 87.7(3) 11_655 9_656 ? N1 Cu1 N1 92.3(3) 3_556 9_656 ? N1 Cu1 N1 92.3(3) 11_655 . ? N1 Cu1 N1 87.7(3) 3_556 . ? N1 Cu1 N1 180.0(4) 9_656 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.800 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.119 data_FeNi _database_code_depnum_ccdc_archive 'CCDC 892826' #TrackingRef 'web_deposit_cif_file_1_JorgePasan_1342702197.Fe_Ni.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H46 Fe2 N12 Ni O11' _chemical_formula_weight 945.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Imma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z' '-x, y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z' 'x, -y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y, z+1/2' _cell_length_a 26.780(3) _cell_length_b 12.585(2) _cell_length_c 14.116(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4757.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150.00(10) _cell_measurement_reflns_used 1267 _cell_measurement_theta_min 3.2978 _cell_measurement_theta_max 52.5640 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.2579 _exptl_crystal_size_mid 0.0509 _exptl_crystal_size_min 0.0295 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 5.819 _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 1.017 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.00(10) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5953 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3388 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 52.62 _reflns_number_total 1469 _reflns_number_gt 1027 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics CRYSTALMAKER _computing_publication_material 'PARST97 (Nardelli, 1997)' _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^)+(0.1408P)^2^+104.5455P] 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 1469 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1432 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.3068 _refine_ls_wR_factor_gt 0.2786 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 C1 C 0.4113(5) 0.1526(12) 0.4332(9) 0.051(4) Uani 1 1 d . . . C2 C 0.3424(6) 0.2500 0.5470(16) 0.039(5) Uani 1 2 d S . . C3 C 0.3816(7) 0.2500 0.2735(18) 0.067(6) Uani 1 2 d S . . C4 C 0.3092(5) 0.0412(11) 0.3827(9) 0.050(4) Uani 1 1 d . . . H4 H 0.3407 0.0105 0.3844 0.060 Uiso 1 1 calc R . . C5 C 0.2683(5) -0.0230(11) 0.3747(10) 0.058(4) Uani 1 1 d . . . H5 H 0.2720 -0.0965 0.3732 0.070 Uiso 1 1 calc R . . C6 C 0.2205(4) 0.0226(12) 0.3689(10) 0.053(4) Uani 1 1 d . . . C7 C 0.2170(4) 0.1305(12) 0.3742(9) 0.049(4) Uani 1 1 d . . . H7 H 0.1857 0.1626 0.3727 0.059 Uiso 1 1 calc R . . C8 C 0.2587(4) 0.1918(10) 0.3817(8) 0.042(3) Uani 1 1 d . . . C9 C 0.1745(5) -0.0487(12) 0.3626(12) 0.079(5) Uani 1 1 d . . . H9A H 0.1848 -0.1217 0.3596 0.118 Uiso 1 1 calc R . . H9B H 0.1558 -0.0311 0.3068 0.118 Uiso 1 1 calc R . . H9C H 0.1540 -0.0380 0.4176 0.118 Uiso 1 1 calc R . . Fe1 Fe 0.36016(9) 0.2500 0.40876(19) 0.0421(10) Uani 1 2 d S . . N1 N 0.4449(4) 0.0956(10) 0.4499(8) 0.053(3) Uani 1 1 d . . . N2 N 0.3343(6) 0.2500 0.6220(12) 0.078(7) Uani 1 2 d S . . N3 N 0.3952(6) 0.2500 0.1986(13) 0.082(7) Uani 1 2 d S . . N4 N 0.3051(3) 0.1478(9) 0.3881(6) 0.042(3) Uani 1 1 d . . . Ni1 Ni 0.5000 0.0000 0.5000 0.0440(13) Uani 1 4 d S . . O1W O 0.5000 0.0845(11) 0.6282(8) 0.056(4) Uani 1 2 d S . . O2W O 0.4368(6) 0.2500 0.6896(12) 0.098(5) Uani 1 2 d S . . O3W O 0.4512(7) 0.2944(18) 0.8839(14) 0.094(10) Uani 0.50 1 d P . . O4W O 0.4034(7) 0.3270(18) 0.0188(13) 0.083(7) Uani 0.50 1 d P . . O5W O 0.4640(10) 0.510(2) 0.9272(18) 0.111(9) Uani 0.50 1 d P . . O6W O 0.5000 0.574(3) 0.774(2) 0.17(2) Uani 0.50 2 d SP . . 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 C1 0.035(8) 0.068(10) 0.049(8) -0.004(8) -0.010(6) -0.009(8) C2 0.022(9) 0.027(10) 0.069(14) 0.000 -0.012(9) 0.000 C3 0.035(11) 0.089(17) 0.079(17) 0.000 -0.005(12) 0.000 C4 0.039(7) 0.051(9) 0.060(9) -0.009(8) -0.011(6) -0.009(7) C5 0.067(9) 0.039(9) 0.069(10) 0.001(8) -0.029(8) 0.000(7) C6 0.037(7) 0.056(10) 0.064(9) 0.010(9) -0.011(7) -0.009(7) C7 0.023(7) 0.072(11) 0.053(8) 0.008(8) -0.004(6) 0.000(7) C8 0.019(6) 0.068(8) 0.038(7) 0.009(6) -0.003(5) -0.002(6) C9 0.054(9) 0.070(11) 0.113(13) 0.001(11) -0.031(9) -0.021(8) Fe1 0.0231(15) 0.062(2) 0.0416(17) 0.000 -0.0027(12) 0.000 N1 0.038(6) 0.071(8) 0.052(7) -0.004(7) -0.009(5) -0.006(6) N2 0.053(11) 0.15(2) 0.027(9) 0.000 0.001(8) 0.000 N3 0.042(10) 0.16(2) 0.043(11) 0.000 0.003(9) 0.000 N4 0.034(6) 0.057(8) 0.037(6) -0.002(6) -0.006(5) -0.009(5) Ni1 0.022(2) 0.064(3) 0.046(3) 0.006(2) 0.000 0.000 O1W 0.046(7) 0.074(9) 0.048(7) 0.002(8) 0.000 0.000 O2W 0.076(10) 0.133(15) 0.084(12) 0.000 -0.011(9) 0.000 O3W 0.067(12) 0.15(3) 0.066(12) 0.023(13) -0.010(9) -0.043(13) O4W 0.070(12) 0.114(17) 0.065(13) 0.015(13) 0.009(10) 0.055(13) O5W 0.103(17) 0.11(2) 0.116(19) 0.002(18) -0.015(15) -0.035(17) O6W 0.37(7) 0.12(3) 0.026(17) -0.04(2) 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 C1 N1 1.175(16) . ? C1 Fe1 1.870(16) . ? C2 N2 1.08(2) . ? C2 Fe1 2.01(2) . ? C3 N3 1.12(2) . ? C3 Fe1 1.99(3) . ? C4 N4 1.348(16) . ? C4 C5 1.366(18) . ? C5 C6 1.404(18) . ? C6 C7 1.363(18) . ? C6 C9 1.526(18) . ? C7 C8 1.362(17) . ? C8 N4 1.364(14) . ? C8 C8 1.46(3) 12_565 ? Fe1 C1 1.870(16) 12_565 ? Fe1 N4 1.978(10) . ? Fe1 N4 1.978(10) 12_565 ? N1 Ni1 2.031(12) . ? Ni1 N1 2.031(12) 11_655 ? Ni1 N1 2.031(12) 3_556 ? Ni1 N1 2.031(12) 9_656 ? Ni1 O1W 2.099(12) . ? Ni1 O1W 2.099(12) 9_656 ? O3W O3W 1.12(5) 12_565 ? 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 N1 C1 Fe1 176.6(12) . . ? N2 C2 Fe1 177.8(16) . . ? N3 C3 Fe1 177.8(19) . . ? N4 C4 C5 122.0(12) . . ? C4 C5 C6 119.6(12) . . ? C7 C6 C5 117.9(11) . . ? C7 C6 C9 122.2(12) . . ? C5 C6 C9 119.9(12) . . ? C6 C7 C8 120.8(12) . . ? C7 C8 N4 121.5(12) . . ? C7 C8 C8 124.5(8) . 12_565 ? N4 C8 C8 114.0(7) . 12_565 ? C1 Fe1 C1 82.0(8) 12_565 . ? C1 Fe1 N4 177.7(5) 12_565 . ? C1 Fe1 N4 98.4(5) . . ? C1 Fe1 N4 98.4(5) 12_565 12_565 ? C1 Fe1 N4 177.7(5) . 12_565 ? N4 Fe1 N4 81.1(6) . 12_565 ? C1 Fe1 C3 88.0(6) 12_565 . ? C1 Fe1 C3 88.0(6) . . ? N4 Fe1 C3 94.2(5) . . ? N4 Fe1 C3 94.2(5) 12_565 . ? C1 Fe1 C2 89.7(5) 12_565 . ? C1 Fe1 C2 89.7(5) . . ? N4 Fe1 C2 88.1(4) . . ? N4 Fe1 C2 88.1(4) 12_565 . ? C3 Fe1 C2 176.9(7) . . ? C1 N1 Ni1 171.2(11) . . ? C4 N4 C8 118.3(10) . . ? C4 N4 Fe1 126.6(8) . . ? C8 N4 Fe1 115.1(9) . . ? N1 Ni1 N1 180.0(7) 11_655 3_556 ? N1 Ni1 N1 93.2(6) 11_655 . ? N1 Ni1 N1 86.8(6) 3_556 . ? N1 Ni1 N1 86.8(6) 11_655 9_656 ? N1 Ni1 N1 93.2(6) 3_556 9_656 ? N1 Ni1 N1 180.0(6) . 9_656 ? N1 Ni1 O1W 90.0(4) 11_655 . ? N1 Ni1 O1W 90.0(4) 3_556 . ? N1 Ni1 O1W 90.0(4) . . ? N1 Ni1 O1W 90.0(4) 9_656 . ? N1 Ni1 O1W 90.0(4) 11_655 9_656 ? N1 Ni1 O1W 90.0(4) 3_556 9_656 ? N1 Ni1 O1W 90.0(4) . 9_656 ? N1 Ni1 O1W 90.0(4) 9_656 9_656 ? O1W Ni1 O1W 180.000(1) . 9_656 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 52.62 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.081 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.140 data_Fe-Co _database_code_depnum_ccdc_archive 'CCDC 892827' #TrackingRef '12708_web_deposit_cif_file_2_JorgePasan_1342702197.Fe_Co.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H35 Co Fe2 N12 O5.50' _chemical_formula_weight 846.53 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' Fe Fe 0.3463 0.8444 '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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Imma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z' '-x, y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z' 'x, -y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y, z+1/2' _cell_length_a 27.235(2) _cell_length_b 12.4825(8) _cell_length_c 14.2559(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4846.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1703 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details ? _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 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14347 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 6.43 _diffrn_reflns_theta_max 23.50 _reflns_number_total 1886 _reflns_number_gt 1414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics CRYSTALMAKER _computing_publication_material 'PARST97 (Nardelli, 1997)' _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^)+(0.1064P)^2^+23.6600P] 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 1886 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.2142 _refine_ls_wR_factor_gt 0.1921 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 C1 C 0.4123(2) 0.1486(5) 0.4264(5) 0.0604(17) Uani 1 1 d . . . C2 C 0.3476(3) 0.2500 0.5391(8) 0.057(2) Uani 1 2 d S . . C3 C 0.3792(3) 0.2500 0.2721(8) 0.063(2) Uani 1 2 d S . . C4 C 0.3099(2) 0.0406(6) 0.3834(5) 0.0623(17) Uani 1 1 d . . . H4 H 0.3408 0.0093 0.3870 0.075 Uiso 1 1 calc R . . C5 C 0.2699(3) -0.0248(6) 0.3754(5) 0.0690(19) Uani 1 1 d . . . H5 H 0.2742 -0.0987 0.3729 0.083 Uiso 1 1 calc R . . C6 C 0.2235(3) 0.0175(6) 0.3711(5) 0.0700(19) Uani 1 1 d . . . C7 C 0.2196(2) 0.1290(6) 0.3747(5) 0.0617(17) Uani 1 1 d . . . H7 H 0.1889 0.1614 0.3731 0.074 Uiso 1 1 calc R . . C8 C 0.26146(19) 0.1911(5) 0.3805(4) 0.0512(14) Uani 1 1 d . . . C9 C 0.1778(3) -0.0510(8) 0.3664(7) 0.099(3) Uani 1 1 d . . . H9A H 0.1779 -0.0915 0.3091 0.148 Uiso 1 1 calc R . . H9B H 0.1493 -0.0058 0.3681 0.148 Uiso 1 1 calc R . . H9C H 0.1772 -0.0991 0.4189 0.148 Uiso 1 1 calc R . . Fe1 Fe 0.36122(4) 0.2500 0.40493(9) 0.0502(5) Uani 1 2 d S . . N1 N 0.44437(19) 0.0927(5) 0.4422(5) 0.0715(16) Uani 1 1 d . . . N2 N 0.3396(4) 0.2500 0.6172(7) 0.083(3) Uani 1 2 d S . . N3 N 0.3895(3) 0.2500 0.1980(7) 0.096(3) Uani 1 2 d S . . N4 N 0.30681(16) 0.1472(4) 0.3863(3) 0.0508(12) Uani 1 1 d . . . Co1 Co 0.5000 0.0000 0.5000 0.0502(6) Uani 1 4 d S . . O1W O 0.5000 0.0983(7) 0.6230(6) 0.102(3) Uani 1 2 d S . . O2W O 0.4338(5) 0.2500 0.7010(11) 0.269(11) Uani 1 2 d S . . O3W O 0.4516(9) 0.2500 0.8833(19) 0.20(3) Uani 0.25 2 d SP . . O4W O 0.416(2) 0.366(10) 0.025(3) 0.63(11) Uani 0.25 1 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 C1 0.040(3) 0.068(4) 0.074(4) 0.003(3) -0.009(3) -0.001(3) C2 0.044(5) 0.060(6) 0.067(6) 0.000 -0.007(4) 0.000 C3 0.044(5) 0.082(7) 0.063(6) 0.000 -0.014(5) 0.000 C4 0.049(4) 0.064(4) 0.074(4) 0.001(3) -0.014(3) 0.004(3) C5 0.065(4) 0.060(4) 0.082(5) 0.005(3) -0.017(4) -0.008(3) C6 0.061(4) 0.075(5) 0.074(5) 0.014(4) -0.017(4) -0.018(4) C7 0.039(3) 0.081(5) 0.065(4) 0.010(3) -0.009(3) -0.001(3) C8 0.033(3) 0.070(3) 0.050(3) 0.005(3) -0.007(2) -0.002(3) C9 0.068(5) 0.112(7) 0.117(7) 0.024(6) -0.020(5) -0.037(5) Fe1 0.0312(7) 0.0610(9) 0.0583(8) 0.000 -0.0107(5) 0.000 N1 0.037(3) 0.078(4) 0.100(5) 0.012(3) -0.010(3) 0.006(3) N2 0.095(7) 0.094(7) 0.060(6) 0.000 -0.005(5) 0.000 N3 0.059(6) 0.163(10) 0.066(6) 0.000 0.003(5) 0.000 N4 0.039(3) 0.060(3) 0.054(3) -0.001(2) -0.011(2) 0.002(2) Co1 0.0252(8) 0.0539(10) 0.0716(12) 0.0017(8) 0.000 0.000 O1W 0.062(4) 0.128(7) 0.116(6) -0.058(5) 0.000 0.000 O2W 0.127(11) 0.53(4) 0.152(13) 0.000 -0.045(9) 0.000 O3W 0.023(15) 0.56(11) 0.028(15) 0.000 -0.008(11) 0.000 O4W 0.38(7) 1.3(3) 0.17(4) 0.35(9) 0.20(4) 0.63(13) _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 C1 N1 1.139(8) . ? C1 Fe1 1.907(7) . ? C2 N2 1.134(12) . ? C2 Fe1 1.948(11) . ? C3 N3 1.092(12) . ? C3 Fe1 1.956(11) . ? C4 N4 1.333(8) . ? C4 C5 1.365(9) . ? C5 C6 1.373(10) . ? C6 C7 1.397(10) . ? C6 C9 1.510(10) . ? C7 C8 1.381(8) . ? C8 N4 1.354(7) . ? C8 C8 1.470(13) 12_565 ? Fe1 C1 1.907(7) 12_565 ? Fe1 N4 1.978(5) . ? Fe1 N4 1.978(5) 12_565 ? N1 Co1 2.077(6) . ? Co1 N1 2.077(6) 3_556 ? Co1 N1 2.077(6) 9_656 ? Co1 N1 2.077(6) 11_655 ? Co1 O1W 2.140(7) . ? Co1 O1W 2.140(7) 9_656 ? 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 N1 C1 Fe1 175.8(6) . . ? N2 C2 Fe1 179.9(9) . . ? N3 C3 Fe1 179.7(9) . . ? N4 C4 C5 123.4(6) . . ? C4 C5 C6 120.5(7) . . ? C5 C6 C7 116.8(6) . . ? C5 C6 C9 122.9(7) . . ? C7 C6 C9 120.2(7) . . ? C8 C7 C6 120.0(6) . . ? N4 C8 C7 121.9(6) . . ? N4 C8 C8 113.9(3) . 12_565 ? C7 C8 C8 124.1(4) . 12_565 ? C1 Fe1 C1 83.2(4) 12_565 . ? C1 Fe1 C2 89.0(3) 12_565 . ? C1 Fe1 C2 89.0(3) . . ? C1 Fe1 C3 88.4(3) 12_565 . ? C1 Fe1 C3 88.4(3) . . ? C2 Fe1 C3 176.5(4) . . ? C1 Fe1 N4 178.0(2) 12_565 . ? C1 Fe1 N4 97.9(2) . . ? C2 Fe1 N4 89.3(2) . . ? C3 Fe1 N4 93.3(2) . . ? C1 Fe1 N4 97.9(2) 12_565 12_565 ? C1 Fe1 N4 178.0(2) . 12_565 ? C2 Fe1 N4 89.3(2) . 12_565 ? C3 Fe1 N4 93.3(2) . 12_565 ? N4 Fe1 N4 80.9(3) . 12_565 ? C1 N1 Co1 168.0(6) . . ? C4 N4 C8 117.3(5) . . ? C4 N4 Fe1 127.2(4) . . ? C8 N4 Fe1 115.4(4) . . ? N1 Co1 N1 93.7(3) 3_556 9_656 ? N1 Co1 N1 86.3(3) 3_556 . ? N1 Co1 N1 180.0(2) 9_656 . ? N1 Co1 N1 180.0(4) 3_556 11_655 ? N1 Co1 N1 86.3(3) 9_656 11_655 ? N1 Co1 N1 93.7(3) . 11_655 ? N1 Co1 O1W 89.7(3) 3_556 . ? N1 Co1 O1W 89.7(3) 9_656 . ? N1 Co1 O1W 90.3(3) . . ? N1 Co1 O1W 90.3(3) 11_655 . ? N1 Co1 O1W 90.3(3) 3_556 9_656 ? N1 Co1 O1W 90.3(3) 9_656 9_656 ? N1 Co1 O1W 89.7(3) . 9_656 ? N1 Co1 O1W 89.7(3) 11_655 9_656 ? O1W Co1 O1W 180.000(1) . 9_656 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.776 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.087