# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name C.Ziegler J.D.Harvey _publ_contact_author_name 'Prof Christopher Ziegler' _publ_contact_author_email ZIEGLER@UAKRON.EDU data_Co(NCTPP)(H2O) _database_code_depnum_ccdc_archive 'CCDC 234035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (5,10,15,20-tetraphenyl-2-aza-21-carba-porphyrinato)(water)cobalt(III) ; _chemical_name_common ;(5,10,15,20-tetraphenyl-2-aza-21-carba- porphyrinato)(water)cobalt(iii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H30 Co N4 O' _chemical_formula_weight 689.65 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' 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 Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 13.368(4) _cell_length_b 13.368(4) _cell_length_c 9.647(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1723.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 642 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 18.58 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 714 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5518 _exptl_absorpt_correction_T_max 0.9735 _exptl_absorpt_process_details ? _exptl_special_details ; 'Ratio of minimum to maximum apparent transmission: 0.566913' ; _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 5560 _diffrn_reflns_av_R_equivalents 0.1661 _diffrn_reflns_av_sigmaI/netI 0.1146 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 24.99 _reflns_number_total 815 _reflns_number_gt 462 _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. Hydrogen atoms were placed in ideal positions on pyrrole and phenyl carbons and were refined isotropically. The highest Q peaks were located near C9 and C8 and had values of 0.38 and 0.36, respectively. ; _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^)+(0.1720P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 815 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1554 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.2659 _refine_ls_wR_factor_gt 0.2302 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 0.2260(6) 1.0298(7) 0.5000 0.057(2) Uani 1 2 d S . . C2 C 0.3178(7) 0.9743(6) 0.5000 0.065(3) Uani 1 2 d S . . H2 H 0.3822 1.0007 0.5000 0.078 Uiso 1 2 calc SR . . C3 C 0.2929(6) 0.8768(7) 0.5000 0.061(2) Uani 1 2 d S . . H3 H 0.3373 0.8233 0.5000 0.074 Uiso 1 2 calc SR . . C4 C 0.1850(7) 0.8696(6) 0.5000 0.060(2) Uani 1 2 d S . . C5 C 0.1344(6) 0.7794(6) 0.5000 0.058(2) Uani 1 2 d S . . C6 C 0.1921(6) 0.6815(6) 0.5000 0.059(2) Uani 1 2 d S . . C7 C 0.2174(7) 0.6347(6) 0.6190(9) 0.094(3) Uani 1 1 d . . . H7 H 0.1984 0.6634 0.7028 0.113 Uiso 1 1 calc R . . C8 C 0.2711(7) 0.5448(6) 0.6211(10) 0.096(3) Uani 1 1 d . . . H8 H 0.2875 0.5145 0.7049 0.115 Uiso 1 1 calc R . . C9 C 0.2988(8) 0.5027(7) 0.5000 0.083(4) Uani 1 2 d S . . H9 H 0.3370 0.4445 0.5000 0.099 Uiso 1 2 calc SR . . Co1 Co 0.0000 1.0000 0.5000 0.0566(10) Uani 1 8 d S . . H1 H -0.055(3) 0.961(4) 0.785(5) 0.035(13) Uiso 1 1 d . . . N1 N 0.1454(6) 0.9655(6) 0.5000 0.068(2) Uani 1 2 d S . . O1 O 0.0000 1.0000 0.710(3) 0.110(8) Uani 0.50 4 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 0.049(5) 0.059(5) 0.064(6) 0.000 0.000 -0.005(4) C2 0.050(5) 0.048(5) 0.099(7) 0.000 0.000 0.002(4) C3 0.040(4) 0.054(5) 0.090(7) 0.000 0.000 0.007(4) C4 0.051(5) 0.050(5) 0.080(7) 0.000 0.000 0.007(4) C5 0.048(5) 0.047(5) 0.079(6) 0.000 0.000 0.005(4) C6 0.053(5) 0.043(5) 0.080(7) 0.000 0.000 0.001(4) C7 0.117(7) 0.079(5) 0.085(6) -0.003(4) 0.003(5) 0.033(5) C8 0.115(7) 0.059(4) 0.114(8) 0.018(4) 0.002(5) 0.026(4) C9 0.059(6) 0.036(5) 0.152(12) 0.000 0.000 -0.002(4) Co1 0.0441(10) 0.0441(10) 0.082(2) 0.000 0.000 0.000 N1 0.055(4) 0.057(5) 0.090(6) 0.000 0.000 0.008(4) O1 0.090(10) 0.090(10) 0.15(2) 0.000 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 1.378(11) . ? C1 C5 1.400(13) 3_665 ? C1 C2 1.434(12) . ? C2 C3 1.346(13) . ? C3 C4 1.446(12) . ? C4 C5 1.383(12) . ? C4 N1 1.386(11) . ? C5 C1 1.400(13) 11_466 ? C5 C6 1.518(12) . ? C6 C7 1.350(9) . ? C6 C7 1.350(9) 10_556 ? C7 C8 1.401(11) . ? C8 C9 1.348(10) . ? C9 C8 1.348(10) 10_556 ? Co1 N1 1.998(7) 3_665 ? Co1 N1 1.998(7) 9_576 ? Co1 N1 1.998(7) . ? Co1 N1 1.998(7) 11_466 ? Co1 O1 2.03(3) 9_576 ? Co1 O1 2.03(3) . ? 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 C5 125.7(8) . 3_665 ? N1 C1 C2 110.3(8) . . ? C5 C1 C2 124.0(8) 3_665 . ? C3 C2 C1 106.8(8) . . ? C2 C3 C4 108.1(7) . . ? C5 C4 N1 128.3(8) . . ? C5 C4 C3 123.0(8) . . ? N1 C4 C3 108.7(8) . . ? C4 C5 C1 122.2(8) . 11_466 ? C4 C5 C6 120.2(8) . . ? C1 C5 C6 117.6(8) 11_466 . ? C7 C6 C7 116.4(9) . 10_556 ? C7 C6 C5 121.8(5) . . ? C7 C6 C5 121.8(5) 10_556 . ? C6 C7 C8 122.6(8) . . ? C9 C8 C7 119.1(9) . . ? C8 C9 C8 120.1(10) 10_556 . ? N1 Co1 N1 90.000(1) 3_665 9_576 ? N1 Co1 N1 90.000(1) 3_665 . ? N1 Co1 N1 180.000(1) 9_576 . ? N1 Co1 N1 180.000(1) 3_665 11_466 ? N1 Co1 N1 90.000(1) 9_576 11_466 ? N1 Co1 N1 90.0 . 11_466 ? N1 Co1 O1 90.000(3) 3_665 9_576 ? N1 Co1 O1 90.000(5) 9_576 9_576 ? N1 Co1 O1 90.000(5) . 9_576 ? N1 Co1 O1 90.000(3) 11_466 9_576 ? N1 Co1 O1 90.000(3) 3_665 . ? N1 Co1 O1 90.000(5) 9_576 . ? N1 Co1 O1 90.000(5) . . ? N1 Co1 O1 90.000(3) 11_466 . ? O1 Co1 O1 180.000(7) 9_576 . ? C1 N1 C4 106.2(7) . . ? C1 N1 Co1 128.0(6) . . ? C4 N1 Co1 125.8(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.377 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.087 data_Co(NCTPP)(PPH3)Co(NO3)3(CH2Cl2)2 _database_code_depnum_ccdc_archive 'CCDC 234036' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2-aza-21-carba-5,10,15,20-tetraphenylporphyrinato)Cobalt(III) PPh3 ; _chemical_name_common ;(2-aza-21-carba-5,10,15,20- tetraphenylporphyrinato)Cobalt(iii) PPh3 ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H47 Cl4 Co2 N7 O9 P' _chemical_formula_weight 1348.72 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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 12.103(3) _cell_length_b 16.031(4) _cell_length_c 16.390(4) _cell_angle_alpha 91.296(4) _cell_angle_beta 102.294(4) _cell_angle_gamma 109.626(4) _cell_volume 2911.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5781 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.16 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 1.60 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1378 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.5574 _exptl_absorpt_correction_T_max 0.9353 _exptl_absorpt_process_details ? _exptl_special_details ; 'Ratio of minimum to maximum apparent transmission: 0.595961' ; _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 22525 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11319 _reflns_number_gt 9395 _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. Hydrogen atoms were placed in ideal positions on pyrrole, phenyl and solvent carbons and were refined isotropically. The highest Q peaks were located near Cl2 and Co1 and had values of 2.93 and 1.38, respectively. The solvent disorder (two dichloromethanes per unit cell) was refined as a diffuse contribution without specific atom positions using the SQUEEZE program, but the density, absorption coefficient and other parameters reflect the full formula. ; _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^)+(0.0997P)^2^+3.2192P] 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 11319 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1814 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.169 _refine_ls_shift/su_mean 0.007 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 0.2680(3) 0.7337(2) 0.1610(2) 0.0229(6) Uani 1 1 d . . . C2 C 0.1411(3) 0.6852(2) 0.1325(2) 0.0264(7) Uani 1 1 d . . . H2 H 0.0910 0.6498 0.1636 0.032 Uiso 1 1 calc R . . C3 C 0.1086(3) 0.7005(2) 0.0523(2) 0.0264(7) Uani 1 1 d . . . H3 H 0.0315 0.6776 0.0175 0.032 Uiso 1 1 calc R . . C4 C 0.2141(3) 0.7583(2) 0.0305(2) 0.0218(6) Uani 1 1 d . . . C5 C 0.2123(3) 0.8001(2) -0.0435(2) 0.0211(6) Uani 1 1 d . . . C6 C 0.3163(3) 0.85281(19) -0.0648(2) 0.0207(6) Uani 1 1 d . . . C7 C 0.3199(3) 0.8984(2) -0.1392(2) 0.0237(6) Uani 1 1 d . . . H7 H 0.2547 0.9059 -0.1759 0.028 Uiso 1 1 calc R . . C8 C 0.4351(3) 0.9280(2) -0.1458(2) 0.0238(6) Uani 1 1 d . . . H8 H 0.4645 0.9583 -0.1888 0.029 Uiso 1 1 calc R . . C9 C 0.5038(3) 0.90387(19) -0.0735(2) 0.0204(6) Uani 1 1 d . . . C10 C 0.6275(3) 0.92192(19) -0.0591(2) 0.0200(6) Uani 1 1 d . . . C11 C 0.6970(3) 0.91685(19) 0.0188(2) 0.0206(6) Uani 1 1 d . . . C12 C 0.8268(3) 0.9486(2) 0.0392(2) 0.0225(6) Uani 1 1 d . . . H12 H 0.8763 0.9673 0.0020 0.027 Uiso 1 1 calc R . . C13 C 0.8631(3) 0.9461(2) 0.1220(2) 0.0231(6) Uani 1 1 d . . . H13 H 0.9425 0.9647 0.1532 0.028 Uiso 1 1 calc R . . C14 C 0.7578(3) 0.90981(19) 0.1534(2) 0.0209(6) Uani 1 1 d . . . C15 C 0.7589(3) 0.8950(2) 0.2363(2) 0.0225(6) Uani 1 1 d . . . C16 C 0.6499(3) 0.8512(2) 0.2586(2) 0.0257(7) Uani 1 1 d . . . C17 C 0.5320(3) 0.8160(2) 0.2052(2) 0.0225(6) Uani 1 1 d . . . C18 C 0.5269(3) 0.8015(2) 0.3433(2) 0.0255(7) Uani 1 1 d . . . H18 H 0.4977 0.7874 0.3912 0.031 Uiso 1 1 calc R . . C19 C 0.4570(3) 0.7841(2) 0.2612(2) 0.0264(7) Uani 1 1 d . . . C20 C 0.3318(3) 0.7421(2) 0.2426(2) 0.0235(6) Uani 1 1 d . . . C21 C 0.0932(3) 0.7879(2) -0.1012(2) 0.0218(6) Uani 1 1 d . . . C22 C 0.0662(3) 0.7524(2) -0.1833(2) 0.0290(7) Uani 1 1 d . . . H22 H 0.1227 0.7351 -0.2030 0.035 Uiso 1 1 calc R . . C23 C -0.0438(3) 0.7419(3) -0.2372(2) 0.0359(8) Uani 1 1 d . . . H23 H -0.0609 0.7170 -0.2923 0.043 Uiso 1 1 calc R . . C24 C -0.1282(3) 0.7683(2) -0.2093(2) 0.0343(8) Uani 1 1 d . . . H24 H -0.2013 0.7624 -0.2457 0.041 Uiso 1 1 calc R . . C25 C -0.1030(3) 0.8035(2) -0.1268(2) 0.0300(7) Uani 1 1 d . . . H25 H -0.1598 0.8207 -0.1075 0.036 Uiso 1 1 calc R . . C26 C 0.0065(3) 0.8133(2) -0.0726(2) 0.0254(7) Uani 1 1 d . . . H26 H 0.0225 0.8367 -0.0172 0.030 Uiso 1 1 calc R . . C27 C 0.6876(3) 0.9565(2) -0.1279(2) 0.0215(6) Uani 1 1 d . . . C28 C 0.6638(3) 0.9032(2) -0.2021(2) 0.0265(7) Uani 1 1 d . . . H28 H 0.6111 0.8446 -0.2088 0.032 Uiso 1 1 calc R . . C29 C 0.7183(3) 0.9372(2) -0.2659(2) 0.0324(8) Uani 1 1 d . . . H29 H 0.7019 0.9013 -0.3155 0.039 Uiso 1 1 calc R . . C30 C 0.7971(3) 1.0244(2) -0.2568(2) 0.0310(7) Uani 1 1 d . . . H30 H 0.8334 1.0471 -0.3001 0.037 Uiso 1 1 calc R . . C31 C 0.8209(3) 1.0768(2) -0.1831(2) 0.0276(7) Uani 1 1 d . . . H31 H 0.8742 1.1352 -0.1764 0.033 Uiso 1 1 calc R . . C32 C 0.7669(3) 1.0437(2) -0.1193(2) 0.0240(6) Uani 1 1 d . . . H32 H 0.7835 1.0800 -0.0699 0.029 Uiso 1 1 calc R . . C33 C 0.8735(3) 0.9280(2) 0.3022(2) 0.0248(7) Uani 1 1 d . . . C34 C 0.9103(3) 0.8701(2) 0.3549(2) 0.0283(7) Uani 1 1 d . . . H34 H 0.8659 0.8094 0.3466 0.034 Uiso 1 1 calc R . . C35 C 1.0126(3) 0.9032(3) 0.4192(2) 0.0325(8) Uani 1 1 d . . . H35 H 1.0359 0.8646 0.4547 0.039 Uiso 1 1 calc R . . C36 C 1.0806(3) 0.9925(3) 0.4316(2) 0.0345(8) Uani 1 1 d . . . H36 H 1.1497 1.0139 0.4750 0.041 Uiso 1 1 calc R . . C37 C 1.0460(3) 1.0504(2) 0.3793(2) 0.0320(8) Uani 1 1 d . . . H37 H 1.0918 1.1108 0.3876 0.038 Uiso 1 1 calc R . . C38 C 0.9437(3) 1.0187(2) 0.3149(2) 0.0277(7) Uani 1 1 d . . . H38 H 0.9212 1.0579 0.2797 0.033 Uiso 1 1 calc R . . C39 C 0.2697(3) 0.7075(2) 0.3107(2) 0.0257(7) Uani 1 1 d . . . C40 C 0.3033(3) 0.6480(2) 0.3612(2) 0.0276(7) Uani 1 1 d . . . H40 H 0.3625 0.6270 0.3511 0.033 Uiso 1 1 calc R . . C41 C 0.2493(3) 0.6197(2) 0.4268(2) 0.0313(7) Uani 1 1 d . . . H41 H 0.2734 0.5805 0.4611 0.038 Uiso 1 1 calc R . . C42 C 0.1600(3) 0.6492(2) 0.4419(2) 0.0342(8) Uani 1 1 d . . . H42 H 0.1245 0.6304 0.4865 0.041 Uiso 1 1 calc R . . C43 C 0.1236(4) 0.7069(3) 0.3903(3) 0.0385(9) Uani 1 1 d . . . H43 H 0.0620 0.7258 0.3993 0.046 Uiso 1 1 calc R . . C44 C 0.1786(3) 0.7364(2) 0.3257(2) 0.0337(8) Uani 1 1 d . . . H44 H 0.1547 0.7760 0.2918 0.040 Uiso 1 1 calc R . . C45 C 0.3681(3) 0.59623(19) 0.0668(2) 0.0219(6) Uani 1 1 d . . . C46 C 0.3555(3) 0.5798(2) 0.1480(2) 0.0239(6) Uani 1 1 d . . . H46 H 0.4115 0.6173 0.1934 0.029 Uiso 1 1 calc R . . C47 C 0.2614(3) 0.5089(2) 0.1621(2) 0.0286(7) Uani 1 1 d . . . H47 H 0.2548 0.4983 0.2167 0.034 Uiso 1 1 calc R . . C48 C 0.1767(3) 0.4536(2) 0.0950(2) 0.0342(8) Uani 1 1 d . . . H48 H 0.1121 0.4064 0.1042 0.041 Uiso 1 1 calc R . . C49 C 0.1885(3) 0.4687(2) 0.0142(2) 0.0362(8) Uani 1 1 d . . . H49 H 0.1317 0.4312 -0.0309 0.043 Uiso 1 1 calc R . . C50 C 0.2841(3) 0.5391(2) -0.0008(2) 0.0293(7) Uani 1 1 d . . . H50 H 0.2921 0.5482 -0.0554 0.035 Uiso 1 1 calc R . . C51 C 0.4898(3) 0.6759(2) -0.0606(2) 0.0214(6) Uani 1 1 d . . . C52 C 0.5750(3) 0.6502(2) -0.0905(2) 0.0255(7) Uani 1 1 d . . . H52 H 0.6380 0.6410 -0.0528 0.031 Uiso 1 1 calc R . . C53 C 0.5659(3) 0.6385(2) -0.1761(2) 0.0285(7) Uani 1 1 d . . . H53 H 0.6236 0.6226 -0.1955 0.034 Uiso 1 1 calc R . . C54 C 0.4714(3) 0.6504(2) -0.2327(2) 0.0299(7) Uani 1 1 d . . . H54 H 0.4654 0.6423 -0.2901 0.036 Uiso 1 1 calc R . . C55 C 0.3857(3) 0.6743(2) -0.2041(2) 0.0284(7) Uani 1 1 d . . . H55 H 0.3216 0.6818 -0.2423 0.034 Uiso 1 1 calc R . . C56 C 0.3948(3) 0.6872(2) -0.1192(2) 0.0252(7) Uani 1 1 d . . . H56 H 0.3369 0.7037 -0.1006 0.030 Uiso 1 1 calc R . . C57 C 0.6298(3) 0.6713(2) 0.1050(2) 0.0223(6) Uani 1 1 d . . . C58 C 0.7412(3) 0.7270(2) 0.0951(2) 0.0247(7) Uani 1 1 d . . . H58 H 0.7450 0.7708 0.0585 0.030 Uiso 1 1 calc R . . C59 C 0.8466(3) 0.7175(2) 0.1394(2) 0.0301(7) Uani 1 1 d . . . H59 H 0.9208 0.7552 0.1327 0.036 Uiso 1 1 calc R . . C60 C 0.8422(3) 0.6523(2) 0.1935(2) 0.0336(8) Uani 1 1 d . . . H60 H 0.9130 0.6472 0.2247 0.040 Uiso 1 1 calc R . . C61 C 0.7321(3) 0.5949(3) 0.2010(2) 0.0342(8) Uani 1 1 d . . . H61 H 0.7289 0.5499 0.2361 0.041 Uiso 1 1 calc R . . C62 C 0.6262(3) 0.6032(2) 0.1570(2) 0.0295(7) Uani 1 1 d . . . H62 H 0.5524 0.5633 0.1620 0.035 Uiso 1 1 calc R . . C63 C 0.9448(4) 0.4448(3) 0.3464(3) 0.0561(12) Uani 1 1 d . . . H63A H 0.9139 0.3805 0.3459 0.067 Uiso 1 1 calc R . . H63B H 1.0235 0.4671 0.3850 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.84909(11) 0.48834(8) 0.38165(7) 0.0552(3) Uani 1 1 d . . . Cl2 Cl 0.96031(14) 0.47261(8) 0.24363(12) 0.0751(4) Uani 1 1 d . . . Co1 Co 0.48407(3) 0.82177(2) 0.08787(2) 0.01764(13) Uani 1 1 d . . . Co2 Co 0.35487(5) 0.39321(4) 0.46362(3) 0.03796(16) Uani 1 1 d . . . N1 N 0.3145(2) 0.77492(16) 0.09609(16) 0.0201(5) Uani 1 1 d . . . N2 N 0.4321(2) 0.86117(16) -0.02219(16) 0.0200(5) Uani 1 1 d . . . N3 N 0.6540(2) 0.89006(16) 0.08877(16) 0.0197(5) Uani 1 1 d . . . N4 N 0.6408(3) 0.8413(2) 0.3420(2) 0.0437(8) Uani 1 1 d . . . H4 H 0.7003 0.8585 0.3854 0.052 Uiso 1 1 calc R . . N5 N 0.1354(3) 0.3312(3) 0.4733(2) 0.0450(8) Uani 1 1 d . . . N6 N 0.3994(4) 0.2519(2) 0.4549(2) 0.0556(11) Uani 1 1 d . . . N7 N 0.5066(3) 0.5081(2) 0.3797(2) 0.0402(8) Uani 1 1 d . . . O1 O 0.1792(3) 0.3876(2) 0.42330(19) 0.0473(7) Uani 1 1 d . . . O2 O 0.2117(4) 0.3130(3) 0.5250(3) 0.0852(14) Uani 1 1 d . . . O3 O 0.0273(3) 0.3011(2) 0.4680(2) 0.0608(9) Uani 1 1 d . . . O4 O 0.4473(3) 0.31475(19) 0.51492(17) 0.0445(7) Uani 1 1 d . . . O5 O 0.3342(4) 0.2676(2) 0.3927(2) 0.0630(10) Uani 1 1 d . . . O6 O 0.4221(5) 0.1836(3) 0.4628(3) 0.0959(17) Uani 1 1 d . . . O7 O 0.4264(4) 0.5016(2) 0.5540(2) 0.0648(10) Uani 1 1 d . . . O8 O 0.3973(3) 0.4605(2) 0.3632(2) 0.0528(8) Uani 1 1 d . . . O9 O 0.5444(3) 0.5628(2) 0.33191(19) 0.0503(7) Uani 1 1 d . . . P1 P 0.49403(7) 0.69092(5) 0.05084(5) 0.01910(18) 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 C1 0.0217(15) 0.0164(15) 0.0345(17) 0.0049(12) 0.0113(13) 0.0089(12) C2 0.0201(15) 0.0236(16) 0.0388(19) 0.0047(13) 0.0108(13) 0.0092(13) C3 0.0187(15) 0.0235(16) 0.0353(18) 0.0020(13) 0.0059(13) 0.0057(12) C4 0.0199(15) 0.0173(15) 0.0311(16) 0.0001(12) 0.0070(12) 0.0098(12) C5 0.0179(14) 0.0175(14) 0.0302(16) -0.0011(12) 0.0062(12) 0.0091(11) C6 0.0199(14) 0.0148(14) 0.0290(16) -0.0009(11) 0.0053(12) 0.0086(11) C7 0.0213(15) 0.0202(15) 0.0310(17) 0.0015(12) 0.0027(12) 0.0110(12) C8 0.0237(15) 0.0185(15) 0.0298(17) 0.0038(12) 0.0075(13) 0.0074(12) C9 0.0187(14) 0.0153(14) 0.0290(16) 0.0025(11) 0.0072(12) 0.0072(11) C10 0.0194(14) 0.0114(13) 0.0316(16) 0.0009(11) 0.0077(12) 0.0075(11) C11 0.0187(14) 0.0129(14) 0.0329(17) 0.0022(12) 0.0078(12) 0.0081(11) C12 0.0196(15) 0.0169(15) 0.0339(17) 0.0055(12) 0.0099(12) 0.0077(12) C13 0.0186(14) 0.0165(14) 0.0338(17) 0.0033(12) 0.0046(12) 0.0067(12) C14 0.0178(14) 0.0135(14) 0.0307(16) 0.0017(11) 0.0050(12) 0.0052(11) C15 0.0201(15) 0.0187(15) 0.0289(16) 0.0018(12) 0.0040(12) 0.0080(12) C16 0.0259(16) 0.0222(16) 0.0275(16) 0.0014(12) 0.0068(13) 0.0064(13) C17 0.0213(15) 0.0209(15) 0.0264(16) 0.0037(12) 0.0057(12) 0.0087(12) C18 0.0189(15) 0.0303(17) 0.0220(15) 0.0030(12) 0.0087(12) -0.0006(13) C19 0.0263(16) 0.0226(16) 0.0301(17) 0.0028(13) 0.0061(13) 0.0085(13) C20 0.0225(15) 0.0183(15) 0.0338(17) 0.0049(12) 0.0131(13) 0.0080(12) C21 0.0183(14) 0.0154(14) 0.0310(16) 0.0018(12) 0.0034(12) 0.0065(11) C22 0.0250(16) 0.0272(17) 0.0364(19) -0.0007(14) 0.0083(14) 0.0106(13) C23 0.0315(19) 0.040(2) 0.0313(19) -0.0024(15) -0.0010(15) 0.0113(16) C24 0.0225(17) 0.0336(19) 0.043(2) 0.0064(15) 0.0000(14) 0.0096(14) C25 0.0193(15) 0.0256(17) 0.046(2) 0.0026(14) 0.0056(14) 0.0103(13) C26 0.0195(15) 0.0210(16) 0.0344(18) -0.0006(13) 0.0062(13) 0.0056(12) C27 0.0172(14) 0.0188(15) 0.0310(16) 0.0042(12) 0.0051(12) 0.0100(12) C28 0.0277(16) 0.0195(15) 0.0325(17) 0.0004(13) 0.0068(13) 0.0087(13) C29 0.0377(19) 0.0310(19) 0.0318(18) 0.0015(14) 0.0113(15) 0.0142(15) C30 0.0337(18) 0.0334(19) 0.0346(18) 0.0128(14) 0.0163(15) 0.0172(15) C31 0.0216(15) 0.0225(16) 0.0385(19) 0.0089(13) 0.0082(13) 0.0063(13) C32 0.0218(15) 0.0197(15) 0.0312(17) 0.0023(12) 0.0054(12) 0.0087(12) C33 0.0195(15) 0.0255(16) 0.0290(17) 0.0010(13) 0.0045(12) 0.0084(13) C34 0.0300(17) 0.0286(18) 0.0269(17) 0.0036(13) 0.0048(13) 0.0119(14) C35 0.0349(19) 0.042(2) 0.0268(17) 0.0027(14) 0.0065(14) 0.0221(16) C36 0.0243(17) 0.047(2) 0.0300(18) -0.0056(15) 0.0016(14) 0.0138(16) C37 0.0232(16) 0.0303(18) 0.0389(19) -0.0036(14) 0.0059(14) 0.0063(14) C38 0.0243(16) 0.0250(17) 0.0333(18) 0.0019(13) 0.0057(13) 0.0086(13) C39 0.0224(15) 0.0230(16) 0.0320(17) 0.0033(13) 0.0087(13) 0.0071(13) C40 0.0242(16) 0.0261(17) 0.0354(18) 0.0041(13) 0.0080(13) 0.0116(13) C41 0.0338(18) 0.0277(18) 0.0371(19) 0.0098(14) 0.0104(15) 0.0152(15) C42 0.038(2) 0.0337(19) 0.038(2) 0.0116(15) 0.0194(16) 0.0149(16) C43 0.045(2) 0.041(2) 0.047(2) 0.0134(17) 0.0241(18) 0.0275(18) C44 0.039(2) 0.0318(19) 0.043(2) 0.0144(15) 0.0198(16) 0.0219(16) C45 0.0192(14) 0.0140(14) 0.0341(17) 0.0022(12) 0.0084(12) 0.0067(11) C46 0.0214(15) 0.0190(15) 0.0332(17) -0.0009(12) 0.0059(13) 0.0098(12) C47 0.0314(17) 0.0221(16) 0.0369(19) 0.0057(13) 0.0156(14) 0.0104(14) C48 0.0307(18) 0.0220(17) 0.046(2) 0.0022(15) 0.0172(16) -0.0003(14) C49 0.0297(18) 0.0247(18) 0.043(2) -0.0067(15) 0.0083(15) -0.0040(14) C50 0.0281(17) 0.0212(16) 0.0363(19) 0.0010(13) 0.0107(14) 0.0039(13) C51 0.0210(14) 0.0149(14) 0.0284(16) 0.0013(11) 0.0072(12) 0.0056(11) C52 0.0223(15) 0.0199(16) 0.0372(18) 0.0023(13) 0.0082(13) 0.0102(12) C53 0.0280(17) 0.0230(17) 0.0398(19) 0.0015(14) 0.0153(14) 0.0113(13) C54 0.0385(19) 0.0209(16) 0.0316(18) 0.0009(13) 0.0120(15) 0.0096(14) C55 0.0292(17) 0.0204(16) 0.0339(18) -0.0010(13) 0.0018(14) 0.0104(13) C56 0.0238(15) 0.0182(15) 0.0347(18) -0.0008(12) 0.0057(13) 0.0097(12) C57 0.0207(15) 0.0186(15) 0.0310(16) 0.0015(12) 0.0074(12) 0.0106(12) C58 0.0227(15) 0.0166(15) 0.0372(18) 0.0017(12) 0.0092(13) 0.0086(12) C59 0.0185(15) 0.0246(17) 0.047(2) -0.0007(14) 0.0073(14) 0.0080(13) C60 0.0265(17) 0.037(2) 0.041(2) 0.0016(15) 0.0027(15) 0.0191(15) C61 0.0314(18) 0.038(2) 0.040(2) 0.0136(16) 0.0090(15) 0.0201(16) C62 0.0236(16) 0.0279(17) 0.042(2) 0.0097(14) 0.0109(14) 0.0130(13) C63 0.051(3) 0.039(2) 0.069(3) 0.009(2) -0.001(2) 0.012(2) Cl1 0.0578(7) 0.0510(6) 0.0532(6) 0.0152(5) 0.0031(5) 0.0198(5) Cl2 0.0793(9) 0.0400(6) 0.1339(13) 0.0281(7) 0.0620(9) 0.0324(6) Co1 0.0150(2) 0.0139(2) 0.0252(2) 0.00184(15) 0.00582(16) 0.00606(16) Co2 0.0428(3) 0.0400(3) 0.0371(3) 0.0071(2) 0.0087(2) 0.0224(2) N1 0.0178(12) 0.0165(12) 0.0290(14) 0.0019(10) 0.0076(10) 0.0086(10) N2 0.0169(12) 0.0137(12) 0.0300(14) 0.0003(10) 0.0054(10) 0.0065(9) N3 0.0181(12) 0.0140(12) 0.0286(14) 0.0016(10) 0.0062(10) 0.0072(10) N4 0.0343(17) 0.053(2) 0.0361(18) 0.0020(15) 0.0054(14) 0.0078(15) N5 0.046(2) 0.051(2) 0.048(2) 0.0053(16) 0.0183(16) 0.0249(17) N6 0.094(3) 0.039(2) 0.0358(19) -0.0004(15) -0.0012(19) 0.035(2) N7 0.051(2) 0.0404(19) 0.0377(18) -0.0053(15) 0.0105(15) 0.0271(17) O1 0.0471(17) 0.0492(17) 0.0520(18) 0.0105(14) 0.0118(14) 0.0245(14) O2 0.067(2) 0.100(3) 0.103(3) 0.064(3) 0.027(2) 0.040(2) O3 0.055(2) 0.070(2) 0.073(2) 0.0137(18) 0.0322(17) 0.0295(17) O4 0.0526(17) 0.0409(16) 0.0389(15) 0.0009(12) -0.0010(13) 0.0221(13) O5 0.096(3) 0.0462(18) 0.0392(17) -0.0037(13) -0.0121(17) 0.0325(18) O6 0.175(5) 0.066(3) 0.062(2) -0.0031(19) -0.005(3) 0.083(3) O7 0.104(3) 0.062(2) 0.0425(18) -0.0001(15) 0.0007(18) 0.058(2) O8 0.068(2) 0.0494(18) 0.0502(18) 0.0104(14) 0.0216(16) 0.0270(16) O9 0.0513(18) 0.0544(19) 0.0474(17) 0.0103(14) 0.0142(14) 0.0193(15) P1 0.0161(4) 0.0141(4) 0.0286(4) 0.0023(3) 0.0066(3) 0.0064(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 C1 C20 1.374(5) . ? C1 N1 1.386(4) . ? C1 C2 1.434(4) . ? C2 C3 1.342(5) . ? C3 C4 1.426(4) . ? C4 N1 1.385(4) . ? C4 C5 1.398(5) . ? C5 C6 1.381(4) . ? C5 C21 1.493(4) . ? C6 N2 1.387(4) . ? C6 C7 1.436(5) . ? C7 C8 1.342(5) . ? C8 C9 1.436(4) . ? C9 N2 1.366(4) . ? C9 C10 1.392(4) . ? C10 C11 1.392(4) . ? C10 C27 1.489(4) . ? C11 N3 1.378(4) . ? C11 C12 1.439(4) . ? C12 C13 1.340(5) . ? C13 C14 1.423(4) . ? C14 C15 1.382(5) . ? C14 N3 1.397(4) . ? C15 C16 1.401(5) . ? C15 C33 1.488(4) . ? C16 N4 1.402(5) . ? C16 C17 1.423(4) . ? C17 C19 1.412(5) . ? C17 Co1 1.900(3) . ? C18 N4 1.316(5) . ? C18 C19 1.395(5) . ? C19 C20 1.397(5) . ? C20 C39 1.490(4) . ? C21 C22 1.378(5) . ? C21 C26 1.405(4) . ? C22 C23 1.387(5) . ? C23 C24 1.383(5) . ? C24 C25 1.385(5) . ? C25 C26 1.385(5) . ? C27 C32 1.388(4) . ? C27 C28 1.390(5) . ? C28 C29 1.379(5) . ? C29 C30 1.385(5) . ? C30 C31 1.376(5) . ? C31 C32 1.374(5) . ? C33 C38 1.400(5) . ? C33 C34 1.399(5) . ? C34 C35 1.380(5) . ? C35 C36 1.375(5) . ? C36 C37 1.385(5) . ? C37 C38 1.378(5) . ? C39 C40 1.384(5) . ? C39 C44 1.395(5) . ? C40 C41 1.382(5) . ? C41 C42 1.380(5) . ? C42 C43 1.384(5) . ? C43 C44 1.379(5) . ? C45 C46 1.391(5) . ? C45 C50 1.396(5) . ? C45 P1 1.825(3) . ? C46 C47 1.377(5) . ? C47 C48 1.383(5) . ? C48 C49 1.380(5) . ? C49 C50 1.389(5) . ? C51 C52 1.402(4) . ? C51 C56 1.398(4) . ? C51 P1 1.824(3) . ? C52 C53 1.387(5) . ? C53 C54 1.381(5) . ? C54 C55 1.382(5) . ? C55 C56 1.377(5) . ? C57 C58 1.391(4) . ? C57 C62 1.395(5) . ? C57 P1 1.823(3) . ? C58 C59 1.386(5) . ? C59 C60 1.381(5) . ? C60 C61 1.373(5) . ? C61 C62 1.380(5) . ? C63 Cl1 1.724(5) . ? C63 Cl2 1.785(5) . ? Co1 N2 1.971(3) . ? Co1 N1 1.970(3) . ? Co1 N3 1.976(3) . ? Co1 P1 2.2195(9) . ? Co2 O4 2.033(3) . ? Co2 O8 2.050(3) . ? Co2 O1 2.058(3) . ? Co2 O7 2.072(3) . ? Co2 O5 2.213(3) . ? Co2 O2 2.229(4) . ? N5 O3 1.216(5) . ? N5 O2 1.231(5) . ? N5 O1 1.291(5) . ? N6 O6 1.219(5) . ? N6 O5 1.236(5) . ? N6 O4 1.280(4) . ? N7 O9 1.227(5) . ? N7 O8 1.251(5) . ? N7 O7 1.257(5) 2_666 ? O7 N7 1.257(5) 2_666 ? 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 C20 C1 N1 125.3(3) . . ? C20 C1 C2 124.1(3) . . ? N1 C1 C2 110.5(3) . . ? C3 C2 C1 107.0(3) . . ? C2 C3 C4 107.3(3) . . ? N1 C4 C5 125.2(3) . . ? N1 C4 C3 110.8(3) . . ? C5 C4 C3 123.7(3) . . ? C6 C5 C4 122.4(3) . . ? C6 C5 C21 118.9(3) . . ? C4 C5 C21 118.7(3) . . ? C5 C6 N2 124.5(3) . . ? C5 C6 C7 124.9(3) . . ? N2 C6 C7 110.2(3) . . ? C8 C7 C6 107.2(3) . . ? C7 C8 C9 106.5(3) . . ? N2 C9 C10 125.2(3) . . ? N2 C9 C8 111.4(3) . . ? C10 C9 C8 123.5(3) . . ? C11 C10 C9 122.5(3) . . ? C11 C10 C27 119.6(3) . . ? C9 C10 C27 117.6(3) . . ? N3 C11 C10 125.7(3) . . ? N3 C11 C12 110.4(3) . . ? C10 C11 C12 123.6(3) . . ? C13 C12 C11 107.2(3) . . ? C12 C13 C14 107.3(3) . . ? C15 C14 N3 125.1(3) . . ? C15 C14 C13 124.3(3) . . ? N3 C14 C13 110.6(3) . . ? C14 C15 C16 119.3(3) . . ? C14 C15 C33 120.8(3) . . ? C16 C15 C33 119.8(3) . . ? N4 C16 C15 123.2(3) . . ? N4 C16 C17 108.7(3) . . ? C15 C16 C17 128.0(3) . . ? C19 C17 C16 103.6(3) . . ? C19 C17 Co1 127.7(2) . . ? C16 C17 Co1 128.4(2) . . ? N4 C18 C19 108.9(3) . . ? C18 C19 C20 122.1(3) . . ? C18 C19 C17 109.6(3) . . ? C20 C19 C17 128.3(3) . . ? C1 C20 C19 118.7(3) . . ? C1 C20 C39 121.2(3) . . ? C19 C20 C39 120.1(3) . . ? C22 C21 C26 118.5(3) . . ? C22 C21 C5 121.0(3) . . ? C26 C21 C5 120.4(3) . . ? C21 C22 C23 121.1(3) . . ? C24 C23 C22 120.2(3) . . ? C23 C24 C25 119.5(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C21 120.3(3) . . ? C32 C27 C28 119.0(3) . . ? C32 C27 C10 120.1(3) . . ? C28 C27 C10 121.0(3) . . ? C29 C28 C27 120.0(3) . . ? C28 C29 C30 120.7(3) . . ? C31 C30 C29 119.1(3) . . ? C32 C31 C30 120.7(3) . . ? C31 C32 C27 120.5(3) . . ? C38 C33 C34 118.9(3) . . ? C38 C33 C15 120.2(3) . . ? C34 C33 C15 120.8(3) . . ? C35 C34 C33 119.8(3) . . ? C36 C35 C34 121.0(3) . . ? C35 C36 C37 119.8(3) . . ? C38 C37 C36 120.2(3) . . ? C37 C38 C33 120.4(3) . . ? C40 C39 C44 118.9(3) . . ? C40 C39 C20 120.7(3) . . ? C44 C39 C20 120.4(3) . . ? C41 C40 C39 120.3(3) . . ? C40 C41 C42 120.6(3) . . ? C43 C42 C41 119.5(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C39 120.6(3) . . ? C46 C45 C50 119.0(3) . . ? C46 C45 P1 119.6(2) . . ? C50 C45 P1 121.4(3) . . ? C47 C46 C45 121.0(3) . . ? C46 C47 C48 119.9(3) . . ? C49 C48 C47 119.7(3) . . ? C48 C49 C50 120.9(3) . . ? C49 C50 C45 119.5(3) . . ? C52 C51 C56 118.2(3) . . ? C52 C51 P1 123.0(2) . . ? C56 C51 P1 118.8(2) . . ? C53 C52 C51 120.4(3) . . ? C54 C53 C52 120.3(3) . . ? C53 C54 C55 120.0(3) . . ? C56 C55 C54 120.2(3) . . ? C55 C56 C51 121.0(3) . . ? C58 C57 C62 118.7(3) . . ? C58 C57 P1 118.8(2) . . ? C62 C57 P1 122.5(2) . . ? C57 C58 C59 120.3(3) . . ? C60 C59 C58 120.4(3) . . ? C61 C60 C59 119.4(3) . . ? C60 C61 C62 120.9(3) . . ? C61 C62 C57 120.1(3) . . ? Cl1 C63 Cl2 112.3(3) . . ? C17 Co1 N2 163.22(12) . . ? C17 Co1 N1 88.81(12) . . ? N2 Co1 N1 89.32(11) . . ? C17 Co1 N3 88.79(12) . . ? N2 Co1 N3 89.95(11) . . ? N1 Co1 N3 169.24(10) . . ? C17 Co1 P1 95.09(10) . . ? N2 Co1 P1 101.69(8) . . ? N1 Co1 P1 95.80(8) . . ? N3 Co1 P1 94.86(8) . . ? O4 Co2 O8 120.60(13) . . ? O4 Co2 O1 139.13(13) . . ? O8 Co2 O1 89.66(13) . . ? O4 Co2 O7 100.35(12) . . ? O8 Co2 O7 97.63(14) . . ? O1 Co2 O7 102.03(14) . . ? O4 Co2 O5 59.96(12) . . ? O8 Co2 O5 89.45(13) . . ? O1 Co2 O5 97.02(13) . . ? O7 Co2 O5 159.67(13) . . ? O4 Co2 O2 84.92(14) . . ? O8 Co2 O2 147.89(15) . . ? O1 Co2 O2 59.08(13) . . ? O7 Co2 O2 96.16(18) . . ? O5 Co2 O2 87.53(18) . . ? C4 N1 C1 104.1(2) . . ? C4 N1 Co1 126.0(2) . . ? C1 N1 Co1 128.4(2) . . ? C9 N2 C6 104.4(3) . . ? C9 N2 Co1 127.2(2) . . ? C6 N2 Co1 128.4(2) . . ? C11 N3 C14 104.3(2) . . ? C11 N3 Co1 125.1(2) . . ? C14 N3 Co1 129.9(2) . . ? C18 N4 C16 109.2(3) . . ? O3 N5 O2 125.0(4) . . ? O3 N5 O1 120.7(4) . . ? O2 N5 O1 114.3(4) . . ? O6 N6 O5 125.9(4) . . ? O6 N6 O4 118.7(4) . . ? O5 N6 O4 115.4(3) . . ? O9 N7 O8 119.7(3) . . ? O9 N7 O7 122.4(4) . 2_666 ? O8 N7 O7 118.0(4) . 2_666 ? N5 O1 Co2 96.3(2) . . ? N5 O2 Co2 90.0(3) . . ? N6 O4 Co2 95.6(2) . . ? N6 O5 Co2 88.5(2) . . ? N7 O7 Co2 115.5(2) 2_666 . ? N7 O8 Co2 110.6(3) . . ? C51 P1 C45 104.55(14) . . ? C51 P1 C57 105.06(15) . . ? C45 P1 C57 105.47(14) . . ? C51 P1 Co1 112.19(10) . . ? C45 P1 Co1 113.54(10) . . ? C57 P1 Co1 115.08(10) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.904 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.115 data_Co(NCTPP)(PPh3)Co(NO3)3C7H8 _database_code_depnum_ccdc_archive 'CCDC 234037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2-aza-21-carba-5,10,15,20-tetraphenylporphyrinato)Cobalt(III) PPH3 ; _chemical_name_common ;(2-aza-21-carba-5,10,15,20- tetraphenylporphyrinato)Cobalt(iii) PPH3 ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H51 Co2 N7 O9 P' _chemical_formula_weight 1271.00 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' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5294(19) _cell_length_b 15.1545(19) _cell_length_c 15.400(2) _cell_angle_alpha 70.304(2) _cell_angle_beta 63.161(2) _cell_angle_gamma 73.503(2) _cell_volume 2813.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3385 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.54 _exptl_crystal_description block _exptl_crystal_colour green-black _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1310 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7447 _exptl_absorpt_correction_T_max 0.9219 _exptl_absorpt_process_details ? _exptl_special_details ; 'Ratio of minimum to maximum apparent transmission: 0.807878' ; _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 22113 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10936 _reflns_number_gt 8118 _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. Hydrogen atoms were placed in ideal positions on pyrrole and phenyl carbons and were refined isotropically. The highest Q peaks were located near C68 and C65 and had values of 1.43 and 1.30, respectively. ; _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^)+(0.0372P)^2^+22.6151P] 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 10936 _refine_ls_number_parameters 794 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1963 _refine_ls_wR_factor_gt 0.1883 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 C1 C 0.2312(4) 0.2463(4) 0.0442(4) 0.0206(11) Uani 1 1 d . . . C2 C 0.1645(5) 0.2547(4) -0.0047(4) 0.0243(12) Uani 1 1 d . . . H2 H 0.1253 0.3105 -0.0271 0.029 Uiso 1 1 calc R . . C3 C 0.1683(5) 0.1688(4) -0.0124(4) 0.0253(12) Uani 1 1 d . . . H3 H 0.1310 0.1531 -0.0393 0.030 Uiso 1 1 calc R . . C4 C 0.2407(4) 0.1052(4) 0.0285(4) 0.0204(11) Uani 1 1 d . . . C5 C 0.2789(4) 0.0123(4) 0.0192(4) 0.0221(12) Uani 1 1 d . . . C6 C 0.3541(4) -0.0466(4) 0.0538(4) 0.0214(11) Uani 1 1 d . . . C7 C 0.4000(5) -0.1400(4) 0.0390(4) 0.0273(13) Uani 1 1 d . . . H7 H 0.3926 -0.1676 -0.0024 0.033 Uiso 1 1 calc R . . C8 C 0.4558(5) -0.1803(4) 0.0958(4) 0.0282(13) Uani 1 1 d . . . H8 H 0.4947 -0.2408 0.1008 0.034 Uiso 1 1 calc R . . C9 C 0.4437(4) -0.1113(4) 0.1481(4) 0.0218(11) Uani 1 1 d . . . C10 C 0.4812(4) -0.1299(4) 0.2209(4) 0.0219(12) Uani 1 1 d . . . C11 C 0.4809(4) -0.0598(4) 0.2613(4) 0.0203(11) Uani 1 1 d . . . C12 C 0.5246(4) -0.0766(4) 0.3335(4) 0.0253(12) Uani 1 1 d . . . H12 H 0.5534 -0.1349 0.3639 0.030 Uiso 1 1 calc R . . C13 C 0.5159(4) 0.0082(4) 0.3487(4) 0.0244(12) Uani 1 1 d . . . H13 H 0.5378 0.0190 0.3919 0.029 Uiso 1 1 calc R . . C14 C 0.4669(4) 0.0790(4) 0.2871(4) 0.0197(11) Uani 1 1 d . . . C15 C 0.4408(4) 0.1747(4) 0.2853(4) 0.0196(11) Uani 1 1 d . . . C16 C 0.3844(4) 0.2353(4) 0.2300(4) 0.0198(11) Uani 1 1 d . . . C17 C 0.3686(4) 0.3346(3) 0.2146(4) 0.0160(10) Uani 1 1 d . . . H17 H 0.3897 0.3668 0.2427 0.019 Uiso 1 1 calc R . . C18 C 0.3424(4) 0.2125(4) 0.1750(4) 0.0177(11) Uani 1 1 d . . . C19 C 0.3000(4) 0.3027(4) 0.1272(4) 0.0190(11) Uani 1 1 d . . . C20 C 0.2463(4) 0.3214(4) 0.0667(4) 0.0204(11) Uani 1 1 d . . . C21 C 0.2297(4) -0.0292(4) -0.0221(4) 0.0239(12) Uani 1 1 d . . . C22 C 0.1611(7) -0.0922(6) 0.0398(5) 0.052(2) Uani 1 1 d . . . H22 H 0.1489 -0.1123 0.1077 0.063 Uiso 1 1 calc R . . C23 C 0.1095(7) -0.1268(6) 0.0046(6) 0.057(2) Uani 1 1 d . . . H23 H 0.0630 -0.1691 0.0485 0.068 Uiso 1 1 calc R . . C24 C 0.1271(6) -0.0986(5) -0.0953(5) 0.0393(16) Uani 1 1 d . . . H24 H 0.0911 -0.1199 -0.1193 0.047 Uiso 1 1 calc R . . C25 C 0.1979(6) -0.0389(5) -0.1591(5) 0.0383(16) Uani 1 1 d . . . H25 H 0.2121 -0.0213 -0.2274 0.046 Uiso 1 1 calc R . . C26 C 0.2493(5) -0.0039(5) -0.1227(4) 0.0340(15) Uani 1 1 d . . . H26 H 0.2973 0.0369 -0.1671 0.041 Uiso 1 1 calc R . . C27 C 0.5190(4) -0.2307(4) 0.2626(4) 0.0217(12) Uani 1 1 d . . . C28 C 0.4470(5) -0.2946(4) 0.3171(4) 0.0266(13) Uani 1 1 d . . . H28 H 0.3775 -0.2738 0.3255 0.032 Uiso 1 1 calc R . . C29 C 0.4788(5) -0.3884(4) 0.3586(5) 0.0323(14) Uani 1 1 d . . . H29 H 0.4303 -0.4300 0.3953 0.039 Uiso 1 1 calc R . . C30 C 0.5814(5) -0.4201(4) 0.3459(5) 0.0307(14) Uani 1 1 d . . . H30 H 0.6023 -0.4831 0.3737 0.037 Uiso 1 1 calc R . . C31 C 0.6545(5) -0.3579(4) 0.2912(5) 0.0310(14) Uani 1 1 d . . . H31 H 0.7242 -0.3795 0.2819 0.037 Uiso 1 1 calc R . . C32 C 0.6227(4) -0.2642(4) 0.2509(4) 0.0256(12) Uani 1 1 d . . . H32 H 0.6713 -0.2227 0.2154 0.031 Uiso 1 1 calc R . . C33 C 0.4728(4) 0.2133(4) 0.3438(4) 0.0223(12) Uani 1 1 d . . . C34 C 0.3970(5) 0.2649(4) 0.4118(4) 0.0268(13) Uani 1 1 d . . . H34 H 0.3272 0.2729 0.4224 0.032 Uiso 1 1 calc R . . C35 C 0.4250(5) 0.3045(4) 0.4636(5) 0.0313(14) Uani 1 1 d . . . H35 H 0.3741 0.3398 0.5079 0.038 Uiso 1 1 calc R . . C36 C 0.5266(5) 0.2919(5) 0.4502(5) 0.0353(15) Uani 1 1 d . . . H36 H 0.5449 0.3180 0.4857 0.042 Uiso 1 1 calc R . . C37 C 0.6028(5) 0.2400(5) 0.3836(5) 0.0370(16) Uani 1 1 d . . . H37 H 0.6722 0.2312 0.3748 0.044 Uiso 1 1 calc R . . C38 C 0.5763(5) 0.2011(4) 0.3300(5) 0.0303(14) Uani 1 1 d . . . H38 H 0.6278 0.1669 0.2849 0.036 Uiso 1 1 calc R . . C39 C 0.1990(4) 0.4198(4) 0.0294(4) 0.0218(12) Uani 1 1 d . . . C40 C 0.1252(5) 0.4742(4) 0.0952(4) 0.0258(13) Uani 1 1 d . . . H40 H 0.1063 0.4497 0.1640 0.031 Uiso 1 1 calc R . . C41 C 0.0798(5) 0.5638(4) 0.0596(5) 0.0308(14) Uani 1 1 d . . . H41 H 0.0298 0.5993 0.1042 0.037 Uiso 1 1 calc R . . C42 C 0.1089(5) 0.6012(4) -0.0430(5) 0.0342(15) Uani 1 1 d . . . H42 H 0.0785 0.6619 -0.0672 0.041 Uiso 1 1 calc R . . C43 C 0.1825(5) 0.5486(4) -0.1090(5) 0.0348(15) Uani 1 1 d . . . H43 H 0.2013 0.5738 -0.1777 0.042 Uiso 1 1 calc R . . C44 C 0.2283(5) 0.4591(4) -0.0741(4) 0.0287(13) Uani 1 1 d . . . H44 H 0.2790 0.4246 -0.1193 0.034 Uiso 1 1 calc R . . C45 C 0.0839(4) 0.1226(4) 0.2892(4) 0.0211(11) Uani 1 1 d . . . C46 C 0.0679(4) 0.2213(4) 0.2621(4) 0.0229(12) Uani 1 1 d . . . H46 H 0.1190 0.2539 0.2514 0.027 Uiso 1 1 calc R . . C47 C -0.0244(4) 0.2715(4) 0.2510(4) 0.0254(12) Uani 1 1 d . . . H47 H -0.0350 0.3374 0.2330 0.031 Uiso 1 1 calc R . . C48 C -0.0990(5) 0.2232(4) 0.2666(4) 0.0298(13) Uani 1 1 d . . . H48 H -0.1600 0.2567 0.2581 0.036 Uiso 1 1 calc R . . C49 C -0.0852(5) 0.1251(4) 0.2949(4) 0.0263(13) Uani 1 1 d . . . H49 H -0.1372 0.0932 0.3066 0.032 Uiso 1 1 calc R . . C50 C 0.0060(5) 0.0747(4) 0.3058(4) 0.0249(12) Uani 1 1 d . . . H50 H 0.0156 0.0087 0.3241 0.030 Uiso 1 1 calc R . . C51 C 0.1882(4) -0.0650(4) 0.3449(4) 0.0219(12) Uani 1 1 d . . . C52 C 0.1865(4) -0.1059(4) 0.2774(4) 0.0247(12) Uani 1 1 d . . . H52 H 0.1963 -0.0703 0.2124 0.030 Uiso 1 1 calc R . . C53 C 0.1704(5) -0.1987(4) 0.3055(5) 0.0278(13) Uani 1 1 d . . . H53 H 0.1689 -0.2251 0.2598 0.033 Uiso 1 1 calc R . . C54 C 0.1567(5) -0.2516(4) 0.4007(5) 0.0308(14) Uani 1 1 d . . . H54 H 0.1466 -0.3143 0.4194 0.037 Uiso 1 1 calc R . . C55 C 0.1577(5) -0.2127(4) 0.4700(5) 0.0322(14) Uani 1 1 d . . . H55 H 0.1482 -0.2490 0.5347 0.039 Uiso 1 1 calc R . . C56 C 0.1729(4) -0.1193(4) 0.4417(4) 0.0263(12) Uani 1 1 d . . . H56 H 0.1729 -0.0926 0.4880 0.032 Uiso 1 1 calc R . . C57 C 0.1978(4) 0.0862(4) 0.4128(4) 0.0223(12) Uani 1 1 d . . . C58 C 0.2680(4) 0.0331(4) 0.4561(4) 0.0237(12) Uani 1 1 d . . . H58 H 0.3183 -0.0145 0.4281 0.028 Uiso 1 1 calc R . . C59 C 0.2638(5) 0.0504(4) 0.5417(4) 0.0254(12) Uani 1 1 d . . . H59 H 0.3113 0.0145 0.5702 0.030 Uiso 1 1 calc R . . C60 C 0.1892(5) 0.1206(4) 0.5835(4) 0.0274(13) Uani 1 1 d . . . H60 H 0.1870 0.1327 0.6398 0.033 Uiso 1 1 calc R . . C61 C 0.1182(5) 0.1728(4) 0.5424(4) 0.0279(13) Uani 1 1 d . . . H61 H 0.0673 0.2193 0.5718 0.033 Uiso 1 1 calc R . . C62 C 0.1216(5) 0.1567(4) 0.4571(4) 0.0260(13) Uani 1 1 d . . . H62 H 0.0735 0.1927 0.4294 0.031 Uiso 1 1 calc R . . C63 C 0.3479(6) 0.6283(5) 0.0564(5) 0.0430(17) Uani 1 1 d . . . C64 C 0.2545(6) 0.6251(5) 0.1401(5) 0.0383(16) Uani 1 1 d . . . H64 H 0.1919 0.6502 0.1317 0.046 Uiso 1 1 calc R . . C65 C 0.2527(6) 0.5856(4) 0.2350(5) 0.0379(16) Uani 1 1 d . . . H65 H 0.1890 0.5825 0.2899 0.045 Uiso 1 1 calc R . . C66 C 0.3442(6) 0.5504(5) 0.2496(5) 0.0404(16) Uani 1 1 d . . . H66 H 0.3427 0.5243 0.3142 0.048 Uiso 1 1 calc R . . C67 C 0.4393(6) 0.5544(5) 0.1666(6) 0.0487(19) Uani 1 1 d . . . H67 H 0.5019 0.5307 0.1753 0.058 Uiso 1 1 calc R . . C68 C 0.4398(6) 0.5936(5) 0.0714(6) 0.0442(18) Uani 1 1 d . . . H68 H 0.5033 0.5968 0.0162 0.053 Uiso 1 1 calc R . . C69 C 0.3503(7) 0.6688(6) -0.0485(6) 0.061(2) Uani 1 1 d . . . H69A H 0.4133 0.6952 -0.0918 0.091 Uiso 1 1 calc R . . H69B H 0.2910 0.7176 -0.0474 0.091 Uiso 1 1 calc R . . H69C H 0.3479 0.6193 -0.0729 0.091 Uiso 1 1 calc R . . Co1 Co 0.34757(6) 0.09049(5) 0.16210(5) 0.01745(18) Uani 1 1 d . . . Co2 Co 0.90026(6) 0.54268(6) 0.42679(6) 0.0276(2) Uani 1 1 d . . . N1 N 0.2769(4) 0.1521(3) 0.0677(3) 0.0196(9) Uani 1 1 d . . . N2 N 0.3854(3) -0.0269(3) 0.1168(3) 0.0198(9) Uani 1 1 d . . . N3 N 0.4429(3) 0.0364(3) 0.2336(3) 0.0178(9) Uani 1 1 d . . . N4 N 0.3190(4) 0.3746(4) 0.1535(4) 0.0310(12) Uani 1 1 d . . . H4 H 0.3012 0.4346 0.1332 0.037 Uiso 1 1 calc R . . N5 N 0.8051(4) 0.4501(4) 0.3936(4) 0.0351(13) Uani 1 1 d . . . N6 N 0.9241(5) 0.6907(4) 0.2897(4) 0.0408(14) Uani 1 1 d . . . N7 N 0.9101(4) 0.5932(3) 0.5826(4) 0.0261(11) Uani 1 1 d . . . O1 O 0.7703(4) 0.4777(3) 0.4747(3) 0.0360(10) Uani 1 1 d . . . O2 O 0.8903(4) 0.4747(3) 0.3279(4) 0.0403(11) Uani 1 1 d . . . O3 O 0.7576(4) 0.4023(3) 0.3831(4) 0.0484(13) Uani 1 1 d . . . O4 O 0.8344(4) 0.6794(3) 0.3536(3) 0.0367(11) Uani 1 1 d . . . O5 O 0.9981(4) 0.6259(3) 0.3039(3) 0.0437(12) Uani 1 1 d . . . O6 O 0.9409(5) 0.7607(4) 0.2194(4) 0.0685(18) Uani 1 1 d . . . O7 O 0.8412(3) 0.5918(3) 0.5543(3) 0.0334(10) Uani 1 1 d . . . O8 O 0.9948(3) 0.4234(3) 0.4762(3) 0.0332(10) Uani 1 1 d . . . O9 O 0.8854(4) 0.6110(3) 0.6616(3) 0.0394(11) Uani 1 1 d . . . P1 P 0.20583(11) 0.06021(9) 0.30179(10) 0.0183(3) 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 C1 0.023(3) 0.018(3) 0.017(3) -0.004(2) -0.008(2) 0.000(2) C2 0.033(3) 0.022(3) 0.018(3) 0.000(2) -0.015(2) -0.004(2) C3 0.030(3) 0.033(3) 0.016(3) -0.004(2) -0.012(2) -0.007(3) C4 0.024(3) 0.018(3) 0.018(3) 0.001(2) -0.009(2) -0.009(2) C5 0.029(3) 0.021(3) 0.018(3) -0.006(2) -0.007(2) -0.006(2) C6 0.027(3) 0.018(3) 0.019(3) -0.006(2) -0.007(2) -0.005(2) C7 0.038(3) 0.022(3) 0.027(3) -0.012(2) -0.015(3) -0.001(2) C8 0.031(3) 0.024(3) 0.033(3) -0.018(3) -0.012(3) 0.005(2) C9 0.022(3) 0.016(3) 0.026(3) -0.003(2) -0.011(2) -0.002(2) C10 0.019(3) 0.020(3) 0.023(3) -0.005(2) -0.006(2) -0.002(2) C11 0.016(3) 0.018(3) 0.022(3) -0.002(2) -0.006(2) -0.002(2) C12 0.026(3) 0.023(3) 0.028(3) -0.007(2) -0.014(3) 0.000(2) C13 0.025(3) 0.024(3) 0.029(3) -0.008(2) -0.017(3) 0.001(2) C14 0.022(3) 0.019(3) 0.023(3) -0.005(2) -0.012(2) -0.005(2) C15 0.021(3) 0.019(3) 0.020(3) -0.005(2) -0.008(2) -0.005(2) C16 0.025(3) 0.016(3) 0.022(3) -0.005(2) -0.012(2) -0.004(2) C17 0.024(3) 0.010(2) 0.021(3) -0.004(2) -0.014(2) -0.004(2) C18 0.024(3) 0.013(2) 0.018(3) -0.003(2) -0.010(2) -0.005(2) C19 0.026(3) 0.015(3) 0.016(3) -0.003(2) -0.007(2) -0.004(2) C20 0.024(3) 0.015(3) 0.018(3) -0.002(2) -0.006(2) -0.002(2) C21 0.028(3) 0.022(3) 0.024(3) -0.005(2) -0.011(2) -0.005(2) C22 0.077(6) 0.072(5) 0.023(3) 0.011(3) -0.025(4) -0.053(5) C23 0.080(6) 0.069(5) 0.042(4) 0.006(4) -0.030(4) -0.054(5) C24 0.060(5) 0.042(4) 0.032(4) -0.002(3) -0.027(3) -0.023(3) C25 0.056(4) 0.046(4) 0.021(3) 0.000(3) -0.020(3) -0.022(3) C26 0.046(4) 0.037(4) 0.020(3) -0.003(3) -0.009(3) -0.018(3) C27 0.030(3) 0.018(3) 0.019(3) -0.007(2) -0.011(2) 0.000(2) C28 0.033(3) 0.019(3) 0.031(3) -0.005(2) -0.017(3) -0.003(2) C29 0.046(4) 0.024(3) 0.034(3) -0.003(3) -0.022(3) -0.011(3) C30 0.047(4) 0.021(3) 0.032(3) -0.008(3) -0.025(3) 0.002(3) C31 0.035(3) 0.031(3) 0.033(3) -0.017(3) -0.019(3) 0.010(3) C32 0.025(3) 0.024(3) 0.028(3) -0.009(2) -0.011(3) 0.000(2) C33 0.029(3) 0.017(3) 0.027(3) -0.002(2) -0.017(3) -0.006(2) C34 0.029(3) 0.027(3) 0.029(3) -0.008(3) -0.013(3) -0.005(2) C35 0.040(4) 0.026(3) 0.033(3) -0.010(3) -0.019(3) -0.002(3) C36 0.053(4) 0.035(4) 0.033(3) -0.010(3) -0.024(3) -0.015(3) C37 0.024(3) 0.056(4) 0.041(4) -0.017(3) -0.015(3) -0.011(3) C38 0.030(3) 0.028(3) 0.036(3) -0.010(3) -0.013(3) -0.006(3) C39 0.032(3) 0.015(3) 0.021(3) -0.001(2) -0.015(2) -0.005(2) C40 0.039(3) 0.021(3) 0.020(3) 0.000(2) -0.018(3) -0.003(2) C41 0.039(4) 0.024(3) 0.032(3) -0.009(3) -0.019(3) 0.003(3) C42 0.049(4) 0.020(3) 0.036(4) -0.001(3) -0.028(3) 0.004(3) C43 0.052(4) 0.023(3) 0.027(3) 0.004(3) -0.021(3) -0.005(3) C44 0.042(4) 0.021(3) 0.021(3) -0.001(2) -0.013(3) -0.005(3) C45 0.021(3) 0.020(3) 0.019(3) -0.003(2) -0.007(2) -0.002(2) C46 0.026(3) 0.022(3) 0.018(3) -0.002(2) -0.008(2) -0.006(2) C47 0.028(3) 0.018(3) 0.023(3) 0.002(2) -0.010(2) -0.001(2) C48 0.029(3) 0.033(3) 0.026(3) 0.000(3) -0.015(3) -0.004(3) C49 0.028(3) 0.029(3) 0.027(3) -0.003(2) -0.015(3) -0.008(2) C50 0.034(3) 0.019(3) 0.025(3) -0.002(2) -0.015(3) -0.008(2) C51 0.026(3) 0.014(3) 0.022(3) -0.005(2) -0.007(2) 0.000(2) C52 0.030(3) 0.021(3) 0.020(3) -0.001(2) -0.008(2) -0.008(2) C53 0.036(3) 0.019(3) 0.030(3) -0.008(2) -0.014(3) -0.003(2) C54 0.038(4) 0.018(3) 0.032(3) -0.002(2) -0.011(3) -0.007(3) C55 0.045(4) 0.023(3) 0.023(3) 0.005(2) -0.014(3) -0.008(3) C56 0.027(3) 0.024(3) 0.029(3) -0.007(2) -0.012(3) -0.001(2) C57 0.026(3) 0.023(3) 0.019(3) -0.004(2) -0.009(2) -0.008(2) C58 0.024(3) 0.024(3) 0.022(3) -0.003(2) -0.010(2) -0.005(2) C59 0.028(3) 0.029(3) 0.023(3) -0.002(2) -0.015(2) -0.008(2) C60 0.044(4) 0.026(3) 0.021(3) -0.004(2) -0.017(3) -0.012(3) C61 0.037(3) 0.023(3) 0.029(3) -0.009(2) -0.016(3) -0.004(3) C62 0.035(3) 0.020(3) 0.024(3) -0.004(2) -0.016(3) 0.000(2) C63 0.057(5) 0.034(4) 0.040(4) -0.015(3) -0.011(4) -0.018(3) C64 0.045(4) 0.030(3) 0.040(4) -0.013(3) -0.011(3) -0.012(3) C65 0.051(4) 0.022(3) 0.043(4) -0.011(3) -0.015(3) -0.012(3) C66 0.052(4) 0.035(4) 0.042(4) -0.016(3) -0.017(3) -0.011(3) C67 0.045(4) 0.050(5) 0.061(5) -0.024(4) -0.017(4) -0.017(4) C68 0.038(4) 0.038(4) 0.054(5) -0.022(3) -0.001(3) -0.017(3) C69 0.074(6) 0.064(6) 0.043(5) -0.011(4) -0.018(4) -0.020(5) Co1 0.0222(4) 0.0136(4) 0.0183(4) -0.0038(3) -0.0097(3) -0.0025(3) Co2 0.0305(5) 0.0231(4) 0.0269(4) -0.0065(3) -0.0101(4) -0.0024(3) N1 0.026(2) 0.017(2) 0.017(2) -0.0035(18) -0.0086(19) -0.0056(19) N2 0.023(2) 0.016(2) 0.022(2) -0.0064(18) -0.009(2) -0.0015(18) N3 0.019(2) 0.014(2) 0.020(2) -0.0053(18) -0.0060(19) -0.0032(17) N4 0.042(3) 0.020(3) 0.035(3) -0.003(2) -0.020(3) -0.006(2) N5 0.042(3) 0.023(3) 0.047(3) -0.009(2) -0.029(3) 0.007(2) N6 0.066(4) 0.027(3) 0.028(3) -0.003(2) -0.015(3) -0.014(3) N7 0.030(3) 0.021(2) 0.026(3) -0.003(2) -0.010(2) -0.004(2) O1 0.040(3) 0.028(2) 0.040(3) -0.011(2) -0.014(2) -0.006(2) O2 0.048(3) 0.039(3) 0.040(3) -0.012(2) -0.020(2) -0.007(2) O3 0.060(3) 0.029(3) 0.078(4) -0.016(2) -0.047(3) -0.002(2) O4 0.047(3) 0.026(2) 0.036(3) -0.0061(19) -0.017(2) -0.004(2) O5 0.048(3) 0.040(3) 0.030(3) -0.005(2) -0.004(2) -0.012(2) O6 0.110(5) 0.037(3) 0.035(3) 0.008(2) -0.018(3) -0.017(3) O7 0.032(2) 0.035(2) 0.037(2) -0.011(2) -0.016(2) -0.0031(19) O8 0.031(2) 0.026(2) 0.032(2) -0.0006(18) -0.009(2) -0.0046(18) O9 0.048(3) 0.041(3) 0.031(2) -0.014(2) -0.018(2) -0.001(2) P1 0.0234(7) 0.0145(7) 0.0185(7) -0.0037(5) -0.0106(6) -0.0015(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 C1 N1 1.392(7) . ? C1 C20 1.394(8) . ? C1 C2 1.429(8) . ? C2 C3 1.331(8) . ? C3 C4 1.430(8) . ? C4 C5 1.389(8) . ? C4 N1 1.391(7) . ? C5 C6 1.388(8) . ? C5 C21 1.499(8) . ? C6 N2 1.381(7) . ? C6 C7 1.430(7) . ? C7 C8 1.338(8) . ? C8 C9 1.453(8) . ? C9 C10 1.372(8) . ? C9 N2 1.387(7) . ? C10 C11 1.399(8) . ? C10 C27 1.493(7) . ? C11 N3 1.396(7) . ? C11 C12 1.434(8) . ? C12 C13 1.344(8) . ? C13 C14 1.431(7) . ? C14 C15 1.385(7) . ? C14 N3 1.400(7) . ? C15 C16 1.385(7) . ? C15 C33 1.503(7) . ? C16 C17 1.409(7) . ? C16 C18 1.411(7) . ? C17 N4 1.324(7) . ? C18 C19 1.430(7) . ? C18 Co1 1.903(5) . ? C19 C20 1.382(8) . ? C19 N4 1.412(7) . ? C20 C39 1.490(7) . ? C21 C22 1.373(9) . ? C21 C26 1.376(8) . ? C22 C23 1.383(9) . ? C23 C24 1.371(9) . ? C24 C25 1.363(9) . ? C25 C26 1.399(9) . ? C27 C32 1.393(8) . ? C27 C28 1.403(8) . ? C28 C29 1.387(8) . ? C29 C30 1.373(9) . ? C30 C31 1.397(9) . ? C31 C32 1.381(8) . ? C33 C38 1.385(8) . ? C33 C34 1.394(8) . ? C34 C35 1.384(8) . ? C35 C36 1.360(9) . ? C36 C37 1.386(9) . ? C37 C38 1.386(9) . ? C39 C40 1.391(8) . ? C39 C44 1.403(8) . ? C40 C41 1.378(8) . ? C41 C42 1.388(9) . ? C42 C43 1.375(9) . ? C43 C44 1.375(8) . ? C45 C46 1.390(8) . ? C45 C50 1.399(8) . ? C45 P1 1.818(5) . ? C46 C47 1.396(8) . ? C47 C48 1.366(8) . ? C48 C49 1.383(8) . ? C49 C50 1.381(8) . ? C51 C52 1.389(8) . ? C51 C56 1.389(8) . ? C51 P1 1.839(5) . ? C52 C53 1.379(8) . ? C53 C54 1.366(8) . ? C54 C55 1.388(9) . ? C55 C56 1.385(8) . ? C57 C58 1.385(8) . ? C57 C62 1.403(8) . ? C57 P1 1.827(5) . ? C58 C59 1.400(8) . ? C59 C60 1.378(8) . ? C60 C61 1.371(8) . ? C61 C62 1.392(8) . ? C63 C68 1.383(11) . ? C63 C64 1.385(10) . ? C63 C69 1.511(10) . ? C64 C65 1.371(10) . ? C65 C66 1.374(10) . ? C66 C67 1.396(10) . ? C67 C68 1.381(11) . ? Co1 N2 1.972(4) . ? Co1 N1 1.982(4) . ? Co1 N3 1.982(4) . ? Co1 P1 2.2249(16) . ? Co2 O5 2.043(5) . ? Co2 O7 2.061(4) . ? Co2 O8 2.084(4) . ? Co2 O1 2.094(5) . ? Co2 O2 2.178(5) . ? Co2 O4 2.180(4) . ? N5 O3 1.222(7) . ? N5 O2 1.253(7) . ? N5 O1 1.285(7) . ? N6 O6 1.221(7) . ? N6 O4 1.245(7) . ? N6 O5 1.279(7) . ? N7 O9 1.205(6) . ? N7 O7 1.267(6) . ? N7 O8 1.272(6) 2_766 ? O8 N7 1.272(6) 2_766 ? 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 C20 125.1(5) . . ? N1 C1 C2 110.3(5) . . ? C20 C1 C2 124.7(5) . . ? C3 C2 C1 108.0(5) . . ? C2 C3 C4 107.0(5) . . ? C5 C4 N1 124.6(5) . . ? C5 C4 C3 124.2(5) . . ? N1 C4 C3 110.8(5) . . ? C6 C5 C4 123.4(5) . . ? C6 C5 C21 118.2(5) . . ? C4 C5 C21 118.2(5) . . ? N2 C6 C5 124.2(5) . . ? N2 C6 C7 110.9(5) . . ? C5 C6 C7 124.5(5) . . ? C8 C7 C6 107.5(5) . . ? C7 C8 C9 106.8(5) . . ? C10 C9 N2 125.9(5) . . ? C10 C9 C8 124.1(5) . . ? N2 C9 C8 110.0(5) . . ? C9 C10 C11 123.3(5) . . ? C9 C10 C27 118.2(5) . . ? C11 C10 C27 118.5(5) . . ? C10 C11 N3 124.8(5) . . ? C10 C11 C12 124.3(5) . . ? N3 C11 C12 110.7(5) . . ? C13 C12 C11 106.9(5) . . ? C12 C13 C14 108.2(5) . . ? C15 C14 N3 124.8(5) . . ? C15 C14 C13 125.1(5) . . ? N3 C14 C13 110.0(4) . . ? C14 C15 C16 120.1(5) . . ? C14 C15 C33 120.3(5) . . ? C16 C15 C33 119.6(5) . . ? C15 C16 C17 122.0(5) . . ? C15 C16 C18 128.2(5) . . ? C17 C16 C18 109.6(5) . . ? N4 C17 C16 108.8(5) . . ? C16 C18 C19 103.9(4) . . ? C16 C18 Co1 128.0(4) . . ? C19 C18 Co1 128.0(4) . . ? C20 C19 N4 123.1(5) . . ? C20 C19 C18 128.2(5) . . ? N4 C19 C18 108.7(5) . . ? C19 C20 C1 119.4(5) . . ? C19 C20 C39 121.5(5) . . ? C1 C20 C39 119.0(5) . . ? C22 C21 C26 117.5(6) . . ? C22 C21 C5 121.0(5) . . ? C26 C21 C5 121.5(5) . . ? C21 C22 C23 122.1(6) . . ? C24 C23 C22 119.8(7) . . ? C25 C24 C23 119.3(6) . . ? C24 C25 C26 120.5(6) . . ? C21 C26 C25 120.7(6) . . ? C32 C27 C28 118.3(5) . . ? C32 C27 C10 122.9(5) . . ? C28 C27 C10 118.8(5) . . ? C29 C28 C27 120.5(6) . . ? C30 C29 C28 120.3(6) . . ? C29 C30 C31 120.2(6) . . ? C32 C31 C30 119.6(6) . . ? C31 C32 C27 121.2(6) . . ? C38 C33 C34 119.0(5) . . ? C38 C33 C15 121.8(5) . . ? C34 C33 C15 119.3(5) . . ? C35 C34 C33 120.4(6) . . ? C36 C35 C34 120.4(6) . . ? C35 C36 C37 120.0(6) . . ? C36 C37 C38 120.4(6) . . ? C33 C38 C37 119.9(6) . . ? C40 C39 C44 118.6(5) . . ? C40 C39 C20 121.5(5) . . ? C44 C39 C20 119.9(5) . . ? C41 C40 C39 120.7(5) . . ? C40 C41 C42 119.9(6) . . ? C43 C42 C41 120.0(5) . . ? C44 C43 C42 120.5(6) . . ? C43 C44 C39 120.3(6) . . ? C46 C45 C50 119.1(5) . . ? C46 C45 P1 118.7(4) . . ? C50 C45 P1 122.2(4) . . ? C45 C46 C47 120.2(5) . . ? C48 C47 C46 119.7(5) . . ? C47 C48 C49 120.9(6) . . ? C50 C49 C48 120.0(6) . . ? C49 C50 C45 120.1(5) . . ? C52 C51 C56 118.7(5) . . ? C52 C51 P1 117.8(4) . . ? C56 C51 P1 123.5(4) . . ? C53 C52 C51 121.0(5) . . ? C54 C53 C52 119.7(6) . . ? C53 C54 C55 120.7(5) . . ? C56 C55 C54 119.4(5) . . ? C55 C56 C51 120.6(5) . . ? C58 C57 C62 118.8(5) . . ? C58 C57 P1 118.8(4) . . ? C62 C57 P1 122.3(4) . . ? C57 C58 C59 120.5(5) . . ? C60 C59 C58 119.9(5) . . ? C61 C60 C59 120.2(5) . . ? C60 C61 C62 120.6(6) . . ? C61 C62 C57 120.0(5) . . ? C68 C63 C64 118.1(7) . . ? C68 C63 C69 120.4(7) . . ? C64 C63 C69 121.5(7) . . ? C65 C64 C63 121.3(7) . . ? C64 C65 C66 120.5(7) . . ? C65 C66 C67 119.3(7) . . ? C68 C67 C66 119.5(7) . . ? C67 C68 C63 121.3(7) . . ? C18 Co1 N2 165.0(2) . . ? C18 Co1 N1 89.0(2) . . ? N2 Co1 N1 89.02(18) . . ? C18 Co1 N3 89.0(2) . . ? N2 Co1 N3 90.09(18) . . ? N1 Co1 N3 168.86(18) . . ? C18 Co1 P1 93.87(16) . . ? N2 Co1 P1 101.12(14) . . ? N1 Co1 P1 97.77(14) . . ? N3 Co1 P1 93.30(13) . . ? O5 Co2 O7 113.06(19) . . ? O5 Co2 O8 106.58(19) . . ? O7 Co2 O8 95.12(17) . . ? O5 Co2 O1 141.9(2) . . ? O7 Co2 O1 93.32(17) . . ? O8 Co2 O1 97.37(17) . . ? O5 Co2 O2 89.16(19) . . ? O7 Co2 O2 153.47(18) . . ? O8 Co2 O2 91.92(18) . . ? O1 Co2 O2 60.37(18) . . ? O5 Co2 O4 60.78(19) . . ? O7 Co2 O4 88.46(17) . . ? O8 Co2 O4 167.14(18) . . ? O1 Co2 O4 94.74(18) . . ? O2 Co2 O4 90.31(17) . . ? C4 N1 C1 103.8(4) . . ? C4 N1 Co1 125.6(3) . . ? C1 N1 Co1 129.1(4) . . ? C6 N2 C9 104.5(4) . . ? C6 N2 Co1 128.5(4) . . ? C9 N2 Co1 126.9(4) . . ? C11 N3 C14 104.2(4) . . ? C11 N3 Co1 125.6(4) . . ? C14 N3 Co1 128.7(3) . . ? C17 N4 C19 109.0(5) . . ? O3 N5 O2 123.0(6) . . ? O3 N5 O1 121.3(6) . . ? O2 N5 O1 115.7(5) . . ? O6 N6 O4 122.2(7) . . ? O6 N6 O5 121.8(7) . . ? O4 N6 O5 116.0(5) . . ? O9 N7 O7 120.7(5) . . ? O9 N7 O8 122.0(5) . 2_766 ? O7 N7 O8 117.3(5) . 2_766 ? N5 O1 Co2 93.4(4) . . ? N5 O2 Co2 90.5(4) . . ? N6 O4 Co2 88.9(4) . . ? N6 O5 Co2 94.2(4) . . ? N7 O7 Co2 114.0(3) . . ? N7 O8 Co2 118.3(3) 2_766 . ? C45 P1 C57 104.3(3) . . ? C45 P1 C51 103.1(3) . . ? C57 P1 C51 103.5(3) . . ? C45 P1 Co1 114.09(18) . . ? C57 P1 Co1 116.93(19) . . ? C51 P1 Co1 113.40(18) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.433 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.111 #loop_ #_platon_squeeze_void_nr #_platon_squeeze_void_average_x #_platon_squeeze_void_average_y #_platon_squeeze_void_average_z #_platon_squeeze_void_volume #_platon_squeeze_void_count_electrons #1 0.500 1.000 0.500 288.9 65.5 #_platon_squeeze_details data_Co(NCTPP)(py)2 _database_code_depnum_ccdc_archive 'CCDC 234038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (5,10,15,20-tetraphenyl-2-aza-21-carba-porphyrinato)(bispyridine)cobalt(III) ; _chemical_name_common ;(5,10,15,20-tetraphenyl-2-aza-21-carba- porphyrinato)(bispyridine)cobalt(iii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H38 Co N6' _chemical_formula_weight 908.93 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' Co Co 0.3494 0.9721 '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 10.664(3) _cell_length_b 14.584(4) _cell_length_c 16.371(5) _cell_angle_alpha 112.333(4) _cell_angle_beta 96.324(5) _cell_angle_gamma 91.474(5) _cell_volume 2334.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8387 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.26 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7457 _exptl_absorpt_correction_T_max 0.9603 _exptl_absorpt_process_details ? _exptl_special_details ; 'Ratio of minimum to maximum apparent transmission: 0.776617' ; _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 18117 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9037 _reflns_number_gt 7396 _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. Hydrogen atoms were placed in ideal positions on pyrrole, phenyl, and pyridine carbons and were refined isotropically. The highest Q peaks were located near Co2 and Co1 and had values of 0.83 and 0.73, respectively. The solvent disorder (two pyrdines per unit cell) was refined as a diffuse contribution without specific atom positions using the SQUEEZE program, but the density, absorption coefficient and other parameters reflect the full formula. ; _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^)+(0.1450P)^2^+5.4283P] 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 9037 _refine_ls_number_parameters 553 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2295 _refine_ls_wR_factor_gt 0.2210 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _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 0.7681(3) 0.5935(3) 0.0704(2) 0.0274(7) Uani 1 1 d . . . C2 C 0.8693(3) 0.6101(3) 0.1448(3) 0.0327(8) Uani 1 1 d . . . H2 H 0.9491 0.6425 0.1541 0.039 Uiso 1 1 calc R . . C3 C 0.8204(3) 0.5677(3) 0.1970(2) 0.0273(7) Uani 1 1 d . . . H3 H 0.8619 0.5657 0.2492 0.033 Uiso 1 1 calc R . . C4 C 0.6942(3) 0.5267(3) 0.1575(2) 0.0286(7) Uani 1 1 d . . . C5 C 0.6186(3) 0.4798(3) 0.1961(2) 0.0309(8) Uani 1 1 d . . . C6 C 0.4962(3) 0.4389(3) 0.1568(2) 0.0305(7) Uani 1 1 d . . . C7 C 0.4183(4) 0.3874(3) 0.1941(3) 0.0364(8) Uani 1 1 d . . . H7 H 0.4391 0.3776 0.2468 0.044 Uiso 1 1 calc R . . C8 C 0.3090(4) 0.3557(3) 0.1385(3) 0.0348(8) Uani 1 1 d . . . H8 H 0.2413 0.3185 0.1449 0.042 Uiso 1 1 calc R . . C9 C 0.3162(3) 0.3900(3) 0.0675(2) 0.0300(7) Uani 1 1 d . . . C10 C 0.2200(3) 0.3725(3) -0.0015(2) 0.0300(7) Uani 1 1 d . . . C11 C 0.6674(3) 0.4722(3) 0.2819(3) 0.0347(8) Uani 1 1 d . . . C12 C 0.6593(4) 0.5488(3) 0.3622(3) 0.0430(9) Uani 1 1 d . . . H12 H 0.6258 0.6072 0.3626 0.052 Uiso 1 1 calc R . . C13 C 0.7003(4) 0.5408(4) 0.4426(3) 0.0482(11) Uani 1 1 d . . . H13 H 0.6922 0.5928 0.4961 0.058 Uiso 1 1 calc R . . C14 C 0.7525(4) 0.4562(4) 0.4429(3) 0.0476(11) Uani 1 1 d . . . H14 H 0.7827 0.4515 0.4966 0.057 Uiso 1 1 calc R . . C15 C 0.7603(4) 0.3780(4) 0.3635(4) 0.0516(12) Uani 1 1 d . . . H15 H 0.7935 0.3198 0.3639 0.062 Uiso 1 1 calc R . . C16 C 0.7190(4) 0.3854(3) 0.2829(3) 0.0405(9) Uani 1 1 d . . . H16 H 0.7256 0.3326 0.2297 0.049 Uiso 1 1 calc R . . C17 C 0.1008(4) 0.3148(3) -0.0022(2) 0.0351(8) Uani 1 1 d . . . C18 C 0.0062(4) 0.3635(4) 0.0467(3) 0.0477(11) Uani 1 1 d . . . H18 H 0.0151 0.4321 0.0771 0.057 Uiso 1 1 calc R . . C19 C -0.1004(5) 0.3103(5) 0.0500(4) 0.0681(16) Uani 1 1 d . . . H19 H -0.1631 0.3432 0.0828 0.082 Uiso 1 1 calc R . . C20 C -0.1142(5) 0.2104(6) 0.0058(5) 0.078(2) Uani 1 1 d . . . H20 H -0.1861 0.1750 0.0090 0.093 Uiso 1 1 calc R . . C21 C -0.0236(6) 0.1608(5) -0.0436(4) 0.0733(18) Uani 1 1 d . . . H21 H -0.0348 0.0923 -0.0745 0.088 Uiso 1 1 calc R . . C22 C 0.0863(5) 0.2132(4) -0.0476(3) 0.0528(12) Uani 1 1 d . . . H22 H 0.1485 0.1798 -0.0805 0.063 Uiso 1 1 calc R . . C23 C 0.4946(4) 0.7157(3) 0.0820(3) 0.0365(8) Uani 1 1 d . . . H23 H 0.5703 0.7151 0.0586 0.044 Uiso 1 1 calc R . . C24 C 0.4497(4) 0.8066(3) 0.1297(3) 0.0412(9) Uani 1 1 d . . . H24 H 0.4948 0.8653 0.1375 0.049 Uiso 1 1 calc R . . C25 C 0.3398(4) 0.8096(3) 0.1651(3) 0.0412(9) Uani 1 1 d . . . H25 H 0.3089 0.8700 0.1976 0.049 Uiso 1 1 calc R . . C26 C 0.2748(4) 0.7205(3) 0.1515(3) 0.0452(10) Uani 1 1 d . . . H26 H 0.1995 0.7202 0.1752 0.054 Uiso 1 1 calc R . . C27 C 0.3232(4) 0.6317(3) 0.1022(3) 0.0359(8) Uani 1 1 d . . . H27 H 0.2781 0.5723 0.0924 0.043 Uiso 1 1 calc R . . C28 C 0.2725(3) -0.0032(3) 0.3700(2) 0.0289(7) Uani 1 1 d . . . C29 C 0.3051(3) 0.0890(3) 0.3686(2) 0.0308(8) Uani 1 1 d . . . C30 C 0.4155(3) 0.1450(3) 0.4165(2) 0.0292(7) Uani 1 1 d . . . C31 C 0.4527(4) 0.2412(3) 0.4162(3) 0.0348(8) Uani 1 1 d . . . H31 H 0.4102 0.2731 0.3831 0.042 Uiso 1 1 calc R . . C32 C 0.5604(4) 0.2757(3) 0.4731(3) 0.0341(8) Uani 1 1 d . . . H32 H 0.6055 0.3362 0.4866 0.041 Uiso 1 1 calc R . . C33 C 0.5933(3) 0.2026(3) 0.5092(2) 0.0297(7) Uani 1 1 d . . . C34 C 0.6999(3) 0.2135(3) 0.5696(2) 0.0307(8) Uani 1 1 d . . . C35 C 0.7301(3) 0.1407(3) 0.6032(2) 0.0305(7) Uani 1 1 d . . . C36 C 0.8451(3) 0.1458(3) 0.6606(2) 0.0315(8) Uani 1 1 d . . . H36 H 0.9080 0.1977 0.6825 0.038 Uiso 1 1 calc R . . C37 C 0.8448(3) 0.0620(3) 0.6769(2) 0.0312(8) Uani 1 1 d . . . H37 H 0.9076 0.0448 0.7115 0.037 Uiso 1 1 calc R . . C38 C 0.2169(4) 0.1320(3) 0.3175(3) 0.0382(9) Uani 1 1 d . . . C39 C 0.2068(5) 0.1007(3) 0.2259(3) 0.0528(12) Uani 1 1 d . . . H39 H 0.2549 0.0505 0.1935 0.063 Uiso 1 1 calc R . . C40 C 0.1232(6) 0.1454(5) 0.1822(4) 0.0751(19) Uani 1 1 d . . . H40 H 0.1143 0.1244 0.1205 0.090 Uiso 1 1 calc R . . C41 C 0.0535(6) 0.2221(5) 0.2326(6) 0.087(2) Uani 1 1 d . . . H41 H -0.0021 0.2515 0.2037 0.105 Uiso 1 1 calc R . . C42 C 0.0649(6) 0.2545(5) 0.3227(5) 0.0768(18) Uani 1 1 d . . . H42 H 0.0192 0.3065 0.3553 0.092 Uiso 1 1 calc R . . C43 C 0.1452(5) 0.2093(4) 0.3653(4) 0.0573(13) Uani 1 1 d . . . H43 H 0.1521 0.2304 0.4270 0.069 Uiso 1 1 calc R . . C44 C 0.7898(3) 0.3032(3) 0.5958(3) 0.0328(8) Uani 1 1 d . . . C45 C 0.8993(4) 0.2969(3) 0.5555(3) 0.0389(9) Uani 1 1 d . . . H45 H 0.9157 0.2368 0.5120 0.047 Uiso 1 1 calc R . . C46 C 0.9837(4) 0.3789(3) 0.5793(3) 0.0452(10) Uani 1 1 d . . . H46 H 1.0565 0.3736 0.5519 0.054 Uiso 1 1 calc R . . C47 C 0.9611(4) 0.4682(3) 0.6433(3) 0.0432(10) Uani 1 1 d . . . H47 H 1.0179 0.5234 0.6588 0.052 Uiso 1 1 calc R . . C48 C 0.8539(5) 0.4753(3) 0.6842(3) 0.0496(11) Uani 1 1 d . . . H48 H 0.8389 0.5355 0.7280 0.059 Uiso 1 1 calc R . . C49 C 0.7673(4) 0.3932(3) 0.6607(3) 0.0430(10) Uani 1 1 d . . . H49 H 0.6947 0.3989 0.6884 0.052 Uiso 1 1 calc R . . C50 C 0.5834(4) -0.1622(3) 0.3513(3) 0.0338(8) Uani 1 1 d . . . H50 H 0.5092 -0.1958 0.3532 0.041 Uiso 1 1 calc R . . C51 C 0.6652(4) -0.2131(3) 0.2926(3) 0.0410(9) Uani 1 1 d . . . H51 H 0.6466 -0.2800 0.2566 0.049 Uiso 1 1 calc R . . C52 C 0.7756(4) -0.1635(3) 0.2879(3) 0.0462(10) Uani 1 1 d . . . H52 H 0.8328 -0.1964 0.2496 0.055 Uiso 1 1 calc R . . C53 C 0.7977(5) -0.0646(4) 0.3415(3) 0.0527(12) Uani 1 1 d . . . H53 H 0.8701 -0.0291 0.3393 0.063 Uiso 1 1 calc R . . C54 C 0.7118(4) -0.0177(3) 0.3988(3) 0.0413(9) Uani 1 1 d . . . H54 H 0.7273 0.0497 0.4339 0.050 Uiso 1 1 calc R . . Co1 Co 0.5000 0.5000 0.0000 0.0257(2) Uani 1 2 d S . . Co2 Co 0.5000 0.0000 0.5000 0.02471(19) Uani 1 2 d S . . N1 N 0.6622(3) 0.5427(2) 0.0796(2) 0.0300(6) Uani 1 1 d . . . N2 N 0.4334(3) 0.4406(2) 0.0794(2) 0.0292(6) Uani 1 1 d . . . N3 N 0.4325(3) 0.6283(2) 0.06811(19) 0.0288(6) Uani 1 1 d . . . N4 N 0.3418(3) -0.0522(2) 0.4153(2) 0.0297(6) Uani 1 1 d . . . N5 N 0.5041(3) 0.1215(2) 0.4733(2) 0.0288(6) Uani 1 1 d . . . N6 N 0.6069(3) -0.0661(2) 0.40556(19) 0.0277(6) 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 C1 0.0303(17) 0.0252(17) 0.0279(17) 0.0112(14) 0.0048(14) 0.0046(13) C2 0.0288(18) 0.0327(19) 0.041(2) 0.0185(16) 0.0072(15) 0.0047(14) C3 0.0258(17) 0.0313(18) 0.0279(17) 0.0166(14) -0.0018(13) 0.0008(13) C4 0.0289(18) 0.0260(17) 0.0309(18) 0.0120(14) -0.0004(14) 0.0025(13) C5 0.0332(19) 0.0289(18) 0.0350(19) 0.0166(15) 0.0065(15) 0.0051(14) C6 0.0338(19) 0.0288(18) 0.0344(18) 0.0181(15) 0.0042(15) 0.0048(14) C7 0.037(2) 0.040(2) 0.039(2) 0.0233(17) 0.0042(16) 0.0000(16) C8 0.035(2) 0.038(2) 0.037(2) 0.0215(17) 0.0048(16) -0.0030(15) C9 0.0348(19) 0.0269(18) 0.0330(18) 0.0157(15) 0.0083(15) 0.0045(14) C10 0.0324(18) 0.0277(18) 0.0340(18) 0.0145(15) 0.0110(15) 0.0070(14) C11 0.0303(19) 0.040(2) 0.041(2) 0.0243(17) 0.0029(15) -0.0024(15) C12 0.051(2) 0.041(2) 0.040(2) 0.0198(18) 0.0003(18) -0.0004(18) C13 0.055(3) 0.051(3) 0.040(2) 0.023(2) -0.0035(19) -0.013(2) C14 0.036(2) 0.070(3) 0.049(3) 0.042(2) -0.0085(18) -0.016(2) C15 0.039(2) 0.068(3) 0.071(3) 0.053(3) 0.005(2) 0.005(2) C16 0.038(2) 0.046(2) 0.051(2) 0.032(2) 0.0087(18) 0.0082(17) C17 0.035(2) 0.044(2) 0.0314(18) 0.0229(17) -0.0043(15) -0.0055(16) C18 0.034(2) 0.067(3) 0.053(3) 0.035(2) 0.0074(19) 0.007(2) C19 0.037(3) 0.109(5) 0.086(4) 0.069(4) 0.007(2) -0.003(3) C20 0.038(3) 0.124(6) 0.099(5) 0.084(5) -0.021(3) -0.028(3) C21 0.081(4) 0.064(3) 0.075(4) 0.041(3) -0.031(3) -0.037(3) C22 0.065(3) 0.046(3) 0.049(3) 0.023(2) -0.003(2) -0.014(2) C23 0.039(2) 0.0300(19) 0.042(2) 0.0151(17) 0.0093(17) 0.0048(15) C24 0.047(2) 0.0279(19) 0.049(2) 0.0147(17) 0.0087(18) 0.0053(16) C25 0.046(2) 0.030(2) 0.044(2) 0.0089(17) 0.0103(18) 0.0104(17) C26 0.043(2) 0.039(2) 0.052(3) 0.0110(19) 0.0200(19) 0.0092(18) C27 0.037(2) 0.0292(19) 0.042(2) 0.0122(16) 0.0122(16) 0.0039(15) C28 0.0291(17) 0.0282(18) 0.0310(18) 0.0119(14) 0.0075(14) 0.0056(14) C29 0.0321(18) 0.0295(18) 0.0340(18) 0.0146(15) 0.0072(15) 0.0074(14) C30 0.0326(18) 0.0274(18) 0.0308(18) 0.0145(14) 0.0054(14) 0.0029(14) C31 0.041(2) 0.0307(19) 0.039(2) 0.0212(16) 0.0013(16) 0.0014(15) C32 0.038(2) 0.0286(19) 0.041(2) 0.0205(16) 0.0031(16) -0.0031(15) C33 0.0308(18) 0.0288(18) 0.0348(18) 0.0173(15) 0.0077(14) 0.0012(14) C34 0.0299(18) 0.0274(18) 0.0385(19) 0.0163(15) 0.0068(15) 0.0013(14) C35 0.0272(17) 0.0321(19) 0.0347(19) 0.0157(15) 0.0037(14) -0.0005(14) C36 0.0244(17) 0.0322(19) 0.0365(19) 0.0129(15) 0.0009(14) -0.0041(14) C37 0.0253(17) 0.037(2) 0.0350(19) 0.0183(16) 0.0018(14) 0.0067(14) C38 0.033(2) 0.034(2) 0.052(2) 0.0251(18) -0.0062(17) -0.0036(15) C39 0.068(3) 0.039(2) 0.052(3) 0.026(2) -0.016(2) -0.009(2) C40 0.088(4) 0.067(4) 0.076(4) 0.049(3) -0.039(3) -0.034(3) C41 0.062(4) 0.076(4) 0.143(7) 0.078(5) -0.034(4) -0.011(3) C42 0.055(3) 0.074(4) 0.121(6) 0.062(4) -0.003(3) 0.015(3) C43 0.048(3) 0.056(3) 0.080(4) 0.039(3) 0.006(2) 0.016(2) C44 0.0319(19) 0.034(2) 0.038(2) 0.0215(16) -0.0011(15) -0.0029(15) C45 0.035(2) 0.039(2) 0.048(2) 0.0226(18) 0.0074(17) 0.0010(16) C46 0.032(2) 0.052(3) 0.064(3) 0.037(2) 0.0045(19) -0.0047(18) C47 0.043(2) 0.046(2) 0.047(2) 0.031(2) -0.0146(18) -0.0164(18) C48 0.066(3) 0.034(2) 0.046(2) 0.0143(19) 0.003(2) -0.009(2) C49 0.049(2) 0.038(2) 0.046(2) 0.0189(19) 0.0116(19) -0.0031(18) C50 0.0327(19) 0.035(2) 0.037(2) 0.0171(16) 0.0044(15) 0.0035(15) C51 0.046(2) 0.038(2) 0.038(2) 0.0114(17) 0.0112(17) 0.0084(17) C52 0.044(2) 0.047(2) 0.044(2) 0.0105(19) 0.0196(19) 0.0105(19) C53 0.045(2) 0.050(3) 0.058(3) 0.012(2) 0.022(2) -0.002(2) C54 0.039(2) 0.039(2) 0.045(2) 0.0128(18) 0.0147(18) -0.0003(17) Co1 0.0298(4) 0.0223(3) 0.0285(4) 0.0126(3) 0.0069(3) 0.0048(2) Co2 0.0250(3) 0.0239(3) 0.0288(4) 0.0130(3) 0.0071(3) 0.0034(2) N1 0.0302(16) 0.0287(15) 0.0328(16) 0.0139(13) 0.0030(12) 0.0031(12) N2 0.0315(15) 0.0266(15) 0.0329(16) 0.0148(13) 0.0054(12) 0.0041(12) N3 0.0329(16) 0.0278(15) 0.0289(15) 0.0142(12) 0.0049(12) 0.0054(12) N4 0.0271(15) 0.0298(15) 0.0345(16) 0.0146(13) 0.0050(12) 0.0018(12) N5 0.0304(15) 0.0256(15) 0.0329(15) 0.0137(12) 0.0058(12) 0.0019(12) N6 0.0274(15) 0.0280(15) 0.0311(15) 0.0140(12) 0.0069(12) 0.0051(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 C1 N1 1.389(5) . ? C1 C10 1.409(5) 2_665 ? C1 C2 1.476(5) . ? C2 C3 1.367(5) . ? C3 C4 1.435(5) . ? C4 C5 1.389(5) . ? C4 N1 1.390(5) . ? C5 C6 1.399(5) . ? C5 C11 1.489(5) . ? C6 N2 1.377(5) . ? C6 C7 1.434(5) . ? C7 C8 1.349(6) . ? C8 C9 1.437(5) . ? C9 C10 1.381(5) . ? C9 N2 1.391(5) . ? C10 C1 1.409(5) 2_665 ? C10 C17 1.503(5) . ? C11 C12 1.377(6) . ? C11 C16 1.398(6) . ? C12 C13 1.389(6) . ? C13 C14 1.368(7) . ? C14 C15 1.378(7) . ? C15 C16 1.389(6) . ? C17 C22 1.377(6) . ? C17 C18 1.395(6) . ? C18 C19 1.377(7) . ? C19 C20 1.354(10) . ? C20 C21 1.369(10) . ? C21 C22 1.404(7) . ? C23 N3 1.348(5) . ? C23 C24 1.387(6) . ? C24 C25 1.357(6) . ? C25 C26 1.385(6) . ? C26 C27 1.389(6) . ? C27 N3 1.340(5) . ? C28 N4 1.383(5) . ? C28 C29 1.389(5) . ? C28 C37 1.456(5) 2_656 ? C29 C30 1.389(5) . ? C29 C38 1.494(5) . ? C30 N5 1.393(5) . ? C30 C31 1.450(5) . ? C31 C32 1.349(6) . ? C32 C33 1.436(5) . ? C33 C34 1.386(5) . ? C33 N5 1.392(5) . ? C34 C35 1.400(5) . ? C34 C44 1.494(5) . ? C35 N4 1.395(5) 2_656 ? C35 C36 1.442(5) . ? C36 C37 1.347(5) . ? C37 C28 1.456(5) 2_656 ? C38 C39 1.382(6) . ? C38 C43 1.405(7) . ? C39 C40 1.407(7) . ? C40 C41 1.400(11) . ? C41 C42 1.357(10) . ? C42 C43 1.379(7) . ? C44 C49 1.385(6) . ? C44 C45 1.392(5) . ? C45 C46 1.381(6) . ? C46 C47 1.373(7) . ? C47 C48 1.373(7) . ? C48 C49 1.397(6) . ? C50 N6 1.342(5) . ? C50 C51 1.383(5) . ? C51 C52 1.390(6) . ? C52 C53 1.371(6) . ? C53 C54 1.387(6) . ? C54 N6 1.344(5) . ? Co1 N1 1.977(3) 2_665 ? Co1 N1 1.977(3) . ? Co1 N3 1.981(3) . ? Co1 N3 1.981(3) 2_665 ? Co1 N2 1.992(3) . ? Co1 N2 1.992(3) 2_665 ? Co2 N5 1.980(3) 2_656 ? Co2 N5 1.980(3) . ? Co2 N6 1.983(3) 2_656 ? Co2 N6 1.983(3) . ? Co2 N4 1.992(3) 2_656 ? Co2 N4 1.992(3) . ? N4 C35 1.395(5) 2_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 C10 126.1(3) . 2_665 ? N1 C1 C2 110.7(3) . . ? C10 C1 C2 123.2(3) 2_665 . ? C3 C2 C1 105.0(3) . . ? C2 C3 C4 108.5(3) . . ? C5 C4 N1 127.2(3) . . ? C5 C4 C3 122.2(3) . . ? N1 C4 C3 110.6(3) . . ? C4 C5 C6 122.0(3) . . ? C4 C5 C11 119.9(3) . . ? C6 C5 C11 118.1(3) . . ? N2 C6 C5 126.8(3) . . ? N2 C6 C7 110.4(3) . . ? C5 C6 C7 122.8(3) . . ? C8 C7 C6 107.1(3) . . ? C7 C8 C9 107.4(3) . . ? C10 C9 N2 126.7(3) . . ? C10 C9 C8 123.7(3) . . ? N2 C9 C8 109.6(3) . . ? C9 C10 C1 121.8(3) . 2_665 ? C9 C10 C17 118.1(3) . . ? C1 C10 C17 120.1(3) 2_665 . ? C12 C11 C16 118.3(4) . . ? C12 C11 C5 121.1(4) . . ? C16 C11 C5 120.6(4) . . ? C11 C12 C13 121.4(4) . . ? C14 C13 C12 119.9(5) . . ? C13 C14 C15 119.9(4) . . ? C14 C15 C16 120.5(4) . . ? C15 C16 C11 120.0(4) . . ? C22 C17 C18 119.4(4) . . ? C22 C17 C10 120.5(4) . . ? C18 C17 C10 120.0(4) . . ? C19 C18 C17 120.2(5) . . ? C20 C19 C18 120.2(6) . . ? C19 C20 C21 120.8(5) . . ? C20 C21 C22 120.0(6) . . ? C17 C22 C21 119.3(5) . . ? N3 C23 C24 122.5(4) . . ? C25 C24 C23 120.0(4) . . ? C24 C25 C26 118.3(4) . . ? C27 C26 C25 119.3(4) . . ? N3 C27 C26 122.6(4) . . ? N4 C28 C29 126.8(3) . . ? N4 C28 C37 110.0(3) . 2_656 ? C29 C28 C37 123.2(3) . 2_656 ? C30 C29 C28 121.9(3) . . ? C30 C29 C38 118.4(3) . . ? C28 C29 C38 119.6(3) . . ? C29 C30 N5 126.9(3) . . ? C29 C30 C31 123.4(3) . . ? N5 C30 C31 109.6(3) . . ? C32 C31 C30 107.1(3) . . ? C31 C32 C33 107.9(3) . . ? C34 C33 N5 126.8(3) . . ? C34 C33 C32 123.4(3) . . ? N5 C33 C32 109.8(3) . . ? C33 C34 C35 122.2(3) . . ? C33 C34 C44 119.0(3) . . ? C35 C34 C44 118.7(3) . . ? N4 C35 C34 126.2(3) 2_656 . ? N4 C35 C36 110.1(3) 2_656 . ? C34 C35 C36 123.7(3) . . ? C37 C36 C35 107.5(3) . . ? C36 C37 C28 107.1(3) . 2_656 ? C39 C38 C43 119.3(4) . . ? C39 C38 C29 122.4(4) . . ? C43 C38 C29 118.2(4) . . ? C38 C39 C40 119.4(5) . . ? C41 C40 C39 119.2(6) . . ? C42 C41 C40 121.7(5) . . ? C41 C42 C43 119.0(6) . . ? C42 C43 C38 121.3(6) . . ? C49 C44 C45 118.9(4) . . ? C49 C44 C34 121.3(3) . . ? C45 C44 C34 119.8(4) . . ? C46 C45 C44 120.6(4) . . ? C47 C46 C45 120.6(4) . . ? C48 C47 C46 119.4(4) . . ? C47 C48 C49 120.8(4) . . ? C44 C49 C48 119.8(4) . . ? N6 C50 C51 122.6(4) . . ? C50 C51 C52 119.4(4) . . ? C53 C52 C51 118.0(4) . . ? C52 C53 C54 119.8(4) . . ? N6 C54 C53 122.4(4) . . ? N1 Co1 N1 180.0 2_665 . ? N1 Co1 N3 90.01(12) 2_665 . ? N1 Co1 N3 89.99(12) . . ? N1 Co1 N3 89.99(12) 2_665 2_665 ? N1 Co1 N3 90.01(12) . 2_665 ? N3 Co1 N3 180.00(18) . 2_665 ? N1 Co1 N2 89.29(13) 2_665 . ? N1 Co1 N2 90.71(13) . . ? N3 Co1 N2 90.15(12) . . ? N3 Co1 N2 89.85(12) 2_665 . ? N1 Co1 N2 90.71(13) 2_665 2_665 ? N1 Co1 N2 89.29(13) . 2_665 ? N3 Co1 N2 89.85(12) . 2_665 ? N3 Co1 N2 90.15(12) 2_665 2_665 ? N2 Co1 N2 180.00(13) . 2_665 ? N5 Co2 N5 180.000(1) 2_656 . ? N5 Co2 N6 91.34(12) 2_656 2_656 ? N5 Co2 N6 88.66(12) . 2_656 ? N5 Co2 N6 88.66(12) 2_656 . ? N5 Co2 N6 91.34(12) . . ? N6 Co2 N6 180.00(14) 2_656 . ? N5 Co2 N4 90.08(13) 2_656 2_656 ? N5 Co2 N4 89.92(13) . 2_656 ? N6 Co2 N4 91.93(12) 2_656 2_656 ? N6 Co2 N4 88.07(12) . 2_656 ? N5 Co2 N4 89.92(13) 2_656 . ? N5 Co2 N4 90.08(13) . . ? N6 Co2 N4 88.07(12) 2_656 . ? N6 Co2 N4 91.93(12) . . ? N4 Co2 N4 180.0 2_656 . ? C1 N1 C4 105.2(3) . . ? C1 N1 Co1 128.3(2) . . ? C4 N1 Co1 126.5(2) . . ? C6 N2 C9 105.4(3) . . ? C6 N2 Co1 126.8(2) . . ? C9 N2 Co1 127.8(2) . . ? C27 N3 C23 117.4(3) . . ? C27 N3 Co1 121.3(3) . . ? C23 N3 Co1 121.3(3) . . ? C28 N4 C35 105.3(3) . 2_656 ? C28 N4 Co2 127.0(2) . . ? C35 N4 Co2 127.3(2) 2_656 . ? C33 N5 C30 105.5(3) . . ? C33 N5 Co2 127.5(2) . . ? C30 N5 Co2 126.9(2) . . ? C50 N6 C54 117.7(3) . . ? C50 N6 Co2 121.6(2) . . ? C54 N6 Co2 120.4(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 4.768 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.109 #loop_ #_platon_squeeze_void_nr #_platon_squeeze_void_average_x #_platon_squeeze_void_average_y #_platon_squeeze_void_average_z #_platon_squeeze_void_volume #_platon_squeeze_void_count_electrons #1 0.000 0.000 0.500 40.9 0.8 #2 0.500 0.000 1.000 358.8 74.7 #3 0.423 0.470 0.405 9.5 -0.2 #4 0.577 0.530 0.595 9.5 -0.3 #_platon_squeeze_details