# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Lee, Hon Man' _publ_contact_author_email leehm@cc.ncue.edu.tw _publ_section_title ; Controlled assemblies of an unprecedented 2D + 3D interpenetrated array of (4,4) and pcu topologies ; loop_ _publ_author_name H.-J.Lee P.-Y.Cheng C.-Y.Chen J.-S.Shen D.Nandi H.M.Lee # Attachment '- dia.hcl366.cif' data_dia_hcl366 _database_code_depnum_ccdc_archive 'CCDC 800198' #TrackingRef '- dia.hcl366.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C20 H14 N4' _chemical_formula_sum 'C20 H14 N4' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 310.35 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.6711(11) _cell_length_b 8.1633(16) _cell_length_c 8.5872(17) _cell_angle_alpha 93.010(4) _cell_angle_beta 103.997(4) _cell_angle_gamma 93.971(4) _cell_volume 383.83(13) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1563 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28.5 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 162 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9693 _exptl_absorpt_correction_T_max 0.9944 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4614 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.66 _reflns_number_total 1968 _reflns_number_gt 1556 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0656P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1968 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_restrained_S_all 1.277 _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 0.54646(19) 0.24441(14) 0.62325(14) 0.0245(3) Uani 1 1 d . . . H1 H 0.6353 0.3189 0.5728 0.029 Uiso 1 1 calc R . . C2 C 0.4484(2) 0.04308(15) 0.75016(15) 0.0281(3) Uani 1 1 d . . . H2 H 0.4584 -0.0536 0.8075 0.034 Uiso 1 1 calc R . . C3 C 0.2451(2) 0.12657(14) 0.70895(14) 0.0262(3) Uani 1 1 d . . . H3 H 0.0915 0.1008 0.7317 0.031 Uiso 1 1 calc R . . C4 C 0.15501(18) 0.38057(13) 0.56208(13) 0.0199(2) Uani 1 1 d . . . C5 C 0.11219(18) 0.50628(13) 0.66789(13) 0.0203(2) Uani 1 1 d . . . C6 C 0.2223(2) 0.51731(15) 0.83680(14) 0.0261(3) Uani 1 1 d . . . H6 H 0.3300 0.4381 0.8809 0.031 Uiso 1 1 calc R . . C7 C 0.1743(2) 0.64018(16) 0.93490(15) 0.0303(3) Uani 1 1 d . . . H7 H 0.2485 0.6457 1.0470 0.036 Uiso 1 1 calc R . . C8 C 0.0149(2) 0.76020(15) 0.87177(15) 0.0297(3) Uani 1 1 d . . . H8 H -0.0174 0.8446 0.9423 0.036 Uiso 1 1 calc R . . C9 C -0.0923(2) 0.75600(14) 0.71181(14) 0.0252(3) Uani 1 1 d . . . H9 H -0.1971 0.8381 0.6714 0.030 Uiso 1 1 calc R . . C10 C -0.04830(17) 0.62874(13) 0.60375(13) 0.0200(2) Uani 1 1 d . . . N1 N 0.63781(17) 0.11753(12) 0.69755(12) 0.0267(3) Uani 1 1 d . . . N2 N 0.30964(15) 0.25633(11) 0.62725(11) 0.0211(2) 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 0.0169(5) 0.0239(6) 0.0342(6) 0.0058(5) 0.0077(4) 0.0046(4) C2 0.0269(6) 0.0234(6) 0.0371(6) 0.0103(5) 0.0100(5) 0.0092(5) C3 0.0220(5) 0.0220(6) 0.0383(6) 0.0100(5) 0.0122(5) 0.0056(4) C4 0.0152(5) 0.0157(5) 0.0302(6) 0.0060(4) 0.0064(4) 0.0040(4) C5 0.0154(5) 0.0180(5) 0.0281(6) 0.0042(4) 0.0059(4) 0.0023(4) C6 0.0223(5) 0.0256(6) 0.0298(6) 0.0049(5) 0.0036(4) 0.0050(4) C7 0.0305(6) 0.0325(7) 0.0267(6) 0.0008(5) 0.0047(5) 0.0032(5) C8 0.0312(6) 0.0253(6) 0.0332(6) -0.0034(5) 0.0101(5) 0.0040(5) C9 0.0237(5) 0.0184(5) 0.0350(6) 0.0015(5) 0.0094(5) 0.0049(4) C10 0.0157(5) 0.0161(5) 0.0293(6) 0.0036(4) 0.0071(4) 0.0020(4) N1 0.0198(4) 0.0256(5) 0.0360(6) 0.0061(4) 0.0068(4) 0.0084(4) N2 0.0169(4) 0.0188(5) 0.0292(5) 0.0055(4) 0.0066(4) 0.0056(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 N1 1.3160(14) . ? C1 N2 1.3618(13) . ? C1 H1 0.9500 . ? C2 C3 1.3625(15) . ? C2 N1 1.3785(15) . ? C2 H2 0.9500 . ? C3 N2 1.3773(14) . ? C3 H3 0.9500 . ? C4 C10 1.4019(16) 2_566 ? C4 C5 1.4075(15) . ? C4 N2 1.4340(12) . ? C5 C6 1.4291(16) . ? C5 C10 1.4396(13) . ? C6 C7 1.3600(17) . ? C6 H6 0.9500 . ? C7 C8 1.4189(16) . ? C7 H7 0.9500 . ? C8 C9 1.3585(17) . ? C8 H8 0.9500 . ? C9 C10 1.4316(15) . ? C9 H9 0.9500 . ? C10 C4 1.4019(16) 2_566 ? 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 N2 112.05(10) . . ? N1 C1 H1 124.0 . . ? N2 C1 H1 124.0 . . ? C3 C2 N1 111.01(10) . . ? C3 C2 H2 124.5 . . ? N1 C2 H2 124.5 . . ? C2 C3 N2 105.31(10) . . ? C2 C3 H3 127.3 . . ? N2 C3 H3 127.3 . . ? C10 C4 C5 122.27(9) 2_566 . ? C10 C4 N2 119.11(9) 2_566 . ? C5 C4 N2 118.61(9) . . ? C4 C5 C6 122.52(9) . . ? C4 C5 C10 118.85(10) . . ? C6 C5 C10 118.64(9) . . ? C7 C6 C5 120.56(10) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 120.77(11) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 120.88(10) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.44(10) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C4 C10 C9 122.42(9) 2_566 . ? C4 C10 C5 118.88(9) 2_566 . ? C9 C10 C5 118.70(10) . . ? C1 N1 C2 104.70(9) . . ? C1 N2 C3 106.93(9) . . ? C1 N2 C4 127.32(9) . . ? C3 N2 C4 125.75(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.66 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.278 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.048 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 # Attachment '- 1.hcl494.cif' data_1_hcl494 _database_code_depnum_ccdc_archive 'CCDC 800199' #TrackingRef '- 1.hcl494.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C40 H28 Co N10 O6, 2(C H2 Cl2)' _chemical_formula_sum 'C42 H32 Cl4 Co N10 O6' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 973.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.587(2) _cell_length_b 10.268(3) _cell_length_c 11.825(3) _cell_angle_alpha 93.996(6) _cell_angle_beta 98.019(6) _cell_angle_gamma 92.232(6) _cell_volume 1028.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 616 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 19.5 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 497 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9296 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12181 _diffrn_reflns_av_R_equivalents 0.1107 _diffrn_reflns_av_sigmaI/netI 0.2389 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.80 _reflns_number_total 5263 _reflns_number_gt 1919 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0788P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5263 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1853 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.808 _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 0.7790(5) 0.7267(4) 0.0208(4) 0.0278(12) Uani 1 1 d . . . H1 H 0.6933 0.6725 -0.0183 0.033 Uiso 1 1 calc R . . C2 C 0.9137(6) 0.8988(5) 0.1070(4) 0.0325(13) Uani 1 1 d . . . H2 H 0.9443 0.9850 0.1391 0.039 Uiso 1 1 calc R . . C3 C 1.0050(6) 0.7948(4) 0.1052(4) 0.0310(12) Uani 1 1 d . . . H3 H 1.1126 0.7964 0.1379 0.037 Uiso 1 1 calc R . . C4 C 0.6303(5) 0.9287(4) 0.0255(4) 0.0292(12) Uani 1 1 d . . . C5 C 0.4006(5) 1.0303(4) 0.0847(4) 0.0300(12) Uani 1 1 d . . . C6 C 0.3041(6) 1.0567(5) 0.1709(4) 0.0331(13) Uani 1 1 d . . . H6 H 0.2124 1.1047 0.1540 0.040 Uiso 1 1 calc R . . C7 C 0.3406(6) 1.0149(5) 0.2755(5) 0.0407(14) Uani 1 1 d . . . H7 H 0.2738 1.0330 0.3317 0.049 Uiso 1 1 calc R . . C8 C 0.4780(6) 0.9436(5) 0.3039(5) 0.0400(14) Uani 1 1 d . . . H8 H 0.5027 0.9160 0.3790 0.048 Uiso 1 1 calc R . . C9 C 0.5734(6) 0.9151(5) 0.2247(4) 0.0369(13) Uani 1 1 d . . . H9 H 0.6643 0.8671 0.2447 0.044 Uiso 1 1 calc R . . C10 C 0.5391(6) 0.9562(4) 0.1110(4) 0.0292(12) Uani 1 1 d . . . C11 C 1.2354(6) 0.5048(5) 0.2179(4) 0.0296(12) Uani 1 1 d . . . H11 H 1.1556 0.4662 0.2548 0.036 Uiso 1 1 calc R . . C12 C 1.3576(6) 0.5892(5) 0.0932(4) 0.0314(12) Uani 1 1 d . . . H12 H 1.3780 0.6228 0.0236 0.038 Uiso 1 1 calc R . . C13 C 1.4655(6) 0.5840(5) 0.1875(4) 0.0338(13) Uani 1 1 d . . . H13 H 1.5738 0.6110 0.1959 0.041 Uiso 1 1 calc R . . C14 C 1.4476(6) 0.5169(5) 0.3874(4) 0.0302(12) Uani 1 1 d . . . C15 C 1.4008(5) 0.6042(5) 0.4709(4) 0.0300(12) Uani 1 1 d . . . C16 C 1.3042(6) 0.7093(5) 0.4449(4) 0.0356(13) Uani 1 1 d . . . H16 H 1.2677 0.7230 0.3672 0.043 Uiso 1 1 calc R . . C17 C 1.2632(6) 0.7910(5) 0.5296(5) 0.0393(14) Uani 1 1 d . . . H17 H 1.1978 0.8610 0.5103 0.047 Uiso 1 1 calc R . . C18 C 1.3154(6) 0.7742(5) 0.6458(5) 0.0387(13) Uani 1 1 d . . . H18 H 1.2846 0.8324 0.7038 0.046 Uiso 1 1 calc R . . C19 C 1.4091(6) 0.6757(5) 0.6748(4) 0.0330(12) Uani 1 1 d . . . H19 H 1.4444 0.6654 0.7534 0.040 Uiso 1 1 calc R . . C20 C 1.4559(6) 0.5866(5) 0.5887(4) 0.0298(12) Uani 1 1 d . . . C21 C 0.8691(7) 0.6812(5) 0.4941(5) 0.0501(16) Uani 1 1 d . . . H21A H 0.7759 0.6467 0.5252 0.060 Uiso 1 1 calc R . . H21B H 0.9631 0.6723 0.5514 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.88953(18) 0.58833(15) 0.36632(13) 0.0560(5) Uani 1 1 d . . . Cl2 Cl 0.8479(2) 0.84527(17) 0.47200(15) 0.0784(6) Uani 1 1 d . . . Co1 Co 1.0000 0.5000 0.0000 0.0235(3) Uani 1 2 d S . . N1 N 0.7696(5) 0.8549(4) 0.0536(3) 0.0306(10) Uani 1 1 d . . . N2 N 0.9222(4) 0.6867(4) 0.0501(3) 0.0252(10) Uani 1 1 d . . . N3 N 1.2148(4) 0.5387(4) 0.1128(3) 0.0248(10) Uani 1 1 d . . . N4 N 1.3877(4) 0.5326(4) 0.2679(3) 0.0287(10) Uani 1 1 d . . . N5 N 0.8911(6) 0.2964(5) 0.1517(4) 0.0367(11) Uani 1 1 d . . . O1 O 0.8940(4) 0.4204(3) 0.1356(3) 0.0296(8) Uani 1 1 d . . . O2 O 0.9993(4) 0.2544(4) 0.2198(3) 0.0489(11) Uani 1 1 d . . . O3 O 0.7826(5) 0.2238(4) 0.1012(3) 0.0461(10) 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 0.030(3) 0.019(2) 0.034(3) -0.003(2) 0.003(2) 0.010(2) C2 0.027(3) 0.032(3) 0.035(3) -0.005(2) -0.005(2) 0.011(2) C3 0.030(3) 0.030(3) 0.032(3) -0.002(2) -0.002(2) 0.014(2) C4 0.027(3) 0.023(3) 0.037(3) -0.001(2) 0.000(2) 0.012(2) C5 0.030(3) 0.023(3) 0.034(3) -0.005(2) -0.001(2) 0.011(2) C6 0.037(3) 0.028(3) 0.036(3) -0.002(2) 0.011(3) 0.008(2) C7 0.043(3) 0.046(3) 0.036(4) -0.008(3) 0.017(3) 0.006(3) C8 0.051(4) 0.038(3) 0.031(3) -0.002(3) 0.007(3) 0.012(3) C9 0.041(3) 0.029(3) 0.042(4) 0.005(3) 0.007(3) 0.011(2) C10 0.035(3) 0.023(3) 0.028(3) -0.004(2) 0.001(2) 0.008(2) C11 0.024(3) 0.036(3) 0.028(3) -0.003(2) 0.001(2) 0.006(2) C12 0.030(3) 0.038(3) 0.023(3) 0.004(2) -0.005(2) 0.003(2) C13 0.028(3) 0.047(3) 0.027(3) 0.006(3) 0.002(3) 0.000(2) C14 0.031(3) 0.040(3) 0.020(3) 0.007(2) 0.002(2) 0.007(2) C15 0.027(3) 0.043(3) 0.019(3) 0.002(2) -0.003(2) 0.007(2) C16 0.038(3) 0.041(3) 0.028(3) 0.006(3) 0.002(3) 0.010(3) C17 0.038(3) 0.043(3) 0.039(4) 0.006(3) 0.006(3) 0.015(3) C18 0.042(3) 0.040(3) 0.034(3) -0.007(3) 0.011(3) 0.004(3) C19 0.033(3) 0.038(3) 0.027(3) -0.001(2) 0.001(2) 0.003(2) C20 0.028(3) 0.040(3) 0.020(3) 0.002(2) 0.000(2) 0.004(2) C21 0.051(4) 0.056(4) 0.045(4) -0.001(3) 0.014(3) -0.004(3) Cl1 0.0502(10) 0.0609(10) 0.0547(10) -0.0131(8) 0.0075(8) 0.0063(8) Cl2 0.0978(15) 0.0731(12) 0.0621(12) -0.0076(10) -0.0016(10) 0.0451(11) Co1 0.0271(5) 0.0249(5) 0.0177(5) -0.0018(4) -0.0024(4) 0.0156(4) N1 0.032(2) 0.025(2) 0.034(3) -0.0045(19) 0.001(2) 0.0186(19) N2 0.025(2) 0.028(2) 0.021(2) -0.0036(18) -0.0001(18) 0.0125(18) N3 0.029(2) 0.030(2) 0.015(2) -0.0004(18) -0.0003(18) 0.0134(19) N4 0.026(2) 0.038(2) 0.021(2) 0.0021(19) -0.0047(19) 0.0081(19) N5 0.043(3) 0.041(3) 0.027(3) -0.001(2) 0.009(2) 0.010(2) O1 0.039(2) 0.0222(18) 0.029(2) 0.0010(15) 0.0073(16) 0.0123(15) O2 0.041(2) 0.059(3) 0.049(3) 0.021(2) 0.002(2) 0.023(2) O3 0.059(3) 0.042(2) 0.034(2) -0.0010(19) 0.000(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.320(5) . ? C1 N1 1.355(5) . ? C1 H1 0.9500 . ? C2 C3 1.350(6) . ? C2 N1 1.354(6) . ? C2 H2 0.9500 . ? C3 N2 1.368(6) . ? C3 H3 0.9500 . ? C4 C10 1.384(6) . ? C4 C5 1.390(6) 2_675 ? C4 N1 1.452(5) . ? C5 C4 1.390(6) 2_675 ? C5 C6 1.420(6) . ? C5 C10 1.446(6) . ? C6 C7 1.338(7) . ? C6 H6 0.9500 . ? C7 C8 1.425(7) . ? C7 H7 0.9500 . ? C8 C9 1.353(7) . ? C8 H8 0.9500 . ? C9 C10 1.431(7) . ? C9 H9 0.9500 . ? C11 N3 1.305(6) . ? C11 N4 1.369(6) . ? C11 H11 0.9500 . ? C12 C13 1.352(6) . ? C12 N3 1.368(6) . ? C12 H12 0.9500 . ? C13 N4 1.360(6) . ? C13 H13 0.9500 . ? C14 C20 1.393(6) 2_866 ? C14 C15 1.399(6) . ? C14 N4 1.456(6) . ? C15 C16 1.412(6) . ? C15 C20 1.433(6) . ? C16 C17 1.355(7) . ? C16 H16 0.9500 . ? C17 C18 1.409(7) . ? C17 H17 0.9500 . ? C18 C19 1.351(6) . ? C18 H18 0.9500 . ? C19 C20 1.431(6) . ? C19 H19 0.9500 . ? C20 C14 1.393(6) 2_866 ? C21 Cl2 1.735(6) . ? C21 Cl1 1.763(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? Co1 N3 2.126(4) 2_765 ? Co1 N3 2.126(4) . ? Co1 N2 2.127(3) 2_765 ? Co1 N2 2.127(3) . ? Co1 O1 2.145(3) . ? Co1 O1 2.145(3) 2_765 ? N5 O3 1.229(5) . ? N5 O2 1.252(5) . ? N5 O1 1.301(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 111.4(4) . . ? N2 C1 H1 124.3 . . ? N1 C1 H1 124.3 . . ? C3 C2 N1 105.7(4) . . ? C3 C2 H2 127.2 . . ? N1 C2 H2 127.2 . . ? C2 C3 N2 111.2(4) . . ? C2 C3 H3 124.4 . . ? N2 C3 H3 124.4 . . ? C10 C4 C5 124.3(4) . 2_675 ? C10 C4 N1 117.7(4) . . ? C5 C4 N1 118.0(4) 2_675 . ? C4 C5 C6 123.7(4) 2_675 . ? C4 C5 C10 117.3(4) 2_675 . ? C6 C5 C10 119.1(5) . . ? C7 C6 C5 120.8(5) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 121.1(5) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 120.5(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.8(5) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C4 C10 C9 123.8(4) . . ? C4 C10 C5 118.5(4) . . ? C9 C10 C5 117.7(4) . . ? N3 C11 N4 110.7(4) . . ? N3 C11 H11 124.7 . . ? N4 C11 H11 124.7 . . ? C13 C12 N3 110.0(5) . . ? C13 C12 H12 125.0 . . ? N3 C12 H12 125.0 . . ? C12 C13 N4 106.2(5) . . ? C12 C13 H13 126.9 . . ? N4 C13 H13 126.9 . . ? C20 C14 C15 124.2(4) 2_866 . ? C20 C14 N4 117.9(4) 2_866 . ? C15 C14 N4 117.9(4) . . ? C14 C15 C16 123.3(4) . . ? C14 C15 C20 118.0(4) . . ? C16 C15 C20 118.6(4) . . ? C17 C16 C15 120.6(5) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 121.4(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 120.1(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.7(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C14 C20 C19 123.7(5) 2_866 . ? C14 C20 C15 117.8(4) 2_866 . ? C19 C20 C15 118.5(4) . . ? Cl2 C21 Cl1 111.8(3) . . ? Cl2 C21 H21A 109.3 . . ? Cl1 C21 H21A 109.3 . . ? Cl2 C21 H21B 109.3 . . ? Cl1 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? N3 Co1 N3 180.0 2_765 . ? N3 Co1 N2 90.38(13) 2_765 2_765 ? N3 Co1 N2 89.62(13) . 2_765 ? N3 Co1 N2 89.62(13) 2_765 . ? N3 Co1 N2 90.38(13) . . ? N2 Co1 N2 180.0 2_765 . ? N3 Co1 O1 89.94(14) 2_765 . ? N3 Co1 O1 90.06(14) . . ? N2 Co1 O1 91.04(13) 2_765 . ? N2 Co1 O1 88.97(13) . . ? N3 Co1 O1 90.06(14) 2_765 2_765 ? N3 Co1 O1 89.94(14) . 2_765 ? N2 Co1 O1 88.96(13) 2_765 2_765 ? N2 Co1 O1 91.04(13) . 2_765 ? O1 Co1 O1 180.0 . 2_765 ? C2 N1 C1 107.4(4) . . ? C2 N1 C4 128.5(4) . . ? C1 N1 C4 124.0(4) . . ? C1 N2 C3 104.4(4) . . ? C1 N2 Co1 124.9(3) . . ? C3 N2 Co1 130.4(3) . . ? C11 N3 C12 106.1(4) . . ? C11 N3 Co1 123.1(3) . . ? C12 N3 Co1 130.6(3) . . ? C13 N4 C11 107.0(4) . . ? C13 N4 C14 127.9(4) . . ? C11 N4 C14 125.0(4) . . ? O3 N5 O2 121.7(5) . . ? O3 N5 O1 119.6(4) . . ? O2 N5 O1 118.6(5) . . ? N5 O1 Co1 122.7(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.80 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.610 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.104 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 # Attachment '- 2.jen291a.cif' data_2_jen291a _database_code_depnum_ccdc_archive 'CCDC 800200' #TrackingRef '- 2.jen291a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C50 H35 Co N11 O3, N O3, H2 O' _chemical_formula_sum 'C50 H37 Co N12 O7' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 150(2) _chemical_formula_weight 976.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1791(5) _cell_length_b 13.7563(6) _cell_length_c 16.5846(8) _cell_angle_alpha 66.855(2) _cell_angle_beta 87.383(3) _cell_angle_gamma 86.095(3) _cell_volume 2129.97(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3531 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 23.4 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8822 _exptl_absorpt_correction_T_max 0.9495 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32065 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.72 _reflns_number_total 10957 _reflns_number_gt 6482 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0678P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10957 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.9717(3) 1.2626(2) 0.0499(2) 0.0228(7) Uani 1 1 d . . . H1 H 1.0631 1.2549 0.0379 0.027 Uiso 1 1 calc R . . C2 C 0.7790(3) 1.3297(2) 0.0646(2) 0.0220(7) Uani 1 1 d . . . H2 H 0.7094 1.3793 0.0647 0.026 Uiso 1 1 calc R . . C3 C 0.7658(3) 1.2243(2) 0.0875(2) 0.0216(7) Uani 1 1 d . . . H3 H 0.6874 1.1873 0.1063 0.026 Uiso 1 1 calc R . . C4 C 0.9271(3) 1.0705(2) 0.1099(2) 0.0195(6) Uani 1 1 d . . . C5 C 0.8658(3) 1.0074(2) 0.0755(2) 0.0196(6) Uani 1 1 d . . . C6 C 0.7817(3) 1.0509(2) 0.0017(2) 0.0248(7) Uani 1 1 d . . . H6 H 0.7702 1.1256 -0.0280 0.030 Uiso 1 1 calc R . . C7 C 0.7178(3) 0.9869(2) -0.0267(2) 0.0311(8) Uani 1 1 d . . . H7 H 0.6636 1.0173 -0.0766 0.037 Uiso 1 1 calc R . . C8 C 0.7316(3) 0.8751(2) 0.0176(2) 0.0292(8) Uani 1 1 d . . . H8 H 0.6835 0.8315 -0.0013 0.035 Uiso 1 1 calc R . . C9 C 0.8129(3) 0.8299(2) 0.0870(2) 0.0237(7) Uani 1 1 d . . . H9 H 0.8214 0.7550 0.1157 0.028 Uiso 1 1 calc R . . C10 C 0.8858(3) 0.8941(2) 0.11698(19) 0.0183(6) Uani 1 1 d . . . C11 C 0.9728(3) 0.8530(2) 0.18600(19) 0.0184(6) Uani 1 1 d . . . C12 C 1.0435(3) 0.9157(2) 0.21480(19) 0.0198(6) Uani 1 1 d . . . C13 C 1.1394(3) 0.8719(2) 0.2823(2) 0.0240(7) Uani 1 1 d . . . H13 H 1.1605 0.7978 0.3054 0.029 Uiso 1 1 calc R . . C14 C 1.2007(3) 0.9336(3) 0.3140(2) 0.0285(8) Uani 1 1 d . . . H14 H 1.2655 0.9032 0.3576 0.034 Uiso 1 1 calc R . . C15 C 1.1676(3) 1.0432(3) 0.2817(2) 0.0292(8) Uani 1 1 d . . . H15 H 1.2068 1.0853 0.3067 0.035 Uiso 1 1 calc R . . C16 C 1.0809(3) 1.0901(2) 0.2157(2) 0.0238(7) Uani 1 1 d . . . H16 H 1.0620 1.1644 0.1945 0.029 Uiso 1 1 calc R . . C17 C 1.0174(3) 1.0281(2) 0.1775(2) 0.0188(6) Uani 1 1 d . . . C18 C 0.9484(3) 0.6909(2) 0.31915(19) 0.0168(6) Uani 1 1 d . . . H18 H 0.8864 0.7220 0.3478 0.020 Uiso 1 1 calc R . . C19 C 1.0781(3) 0.6690(2) 0.2176(2) 0.0227(7) Uani 1 1 d . . . H19 H 1.1247 0.6804 0.1639 0.027 Uiso 1 1 calc R . . C20 C 1.0850(3) 0.5809(2) 0.29241(19) 0.0202(7) Uani 1 1 d . . . H20 H 1.1372 0.5182 0.2995 0.024 Uiso 1 1 calc R . . C21 C 0.7549(3) 0.4657(2) 0.41282(19) 0.0157(6) Uani 1 1 d . . . H21 H 0.8008 0.4938 0.3581 0.019 Uiso 1 1 calc R . . C22 C 0.7045(3) 0.4134(2) 0.55022(19) 0.0165(6) Uani 1 1 d . . . H22 H 0.7103 0.3982 0.6110 0.020 Uiso 1 1 calc R . . C23 C 0.6004(3) 0.3930(2) 0.51233(19) 0.0179(6) Uani 1 1 d . . . H23 H 0.5215 0.3618 0.5405 0.021 Uiso 1 1 calc R . . C24 C 0.5575(3) 0.4192(2) 0.35604(19) 0.0169(6) Uani 1 1 d . . . C25 C 0.5326(3) 0.3186(2) 0.36042(19) 0.0169(6) Uani 1 1 d . . . C26 C 0.5731(3) 0.2238(2) 0.4311(2) 0.0202(6) Uani 1 1 d . . . H26 H 0.6171 0.2277 0.4790 0.024 Uiso 1 1 calc R . . C27 C 0.5500(3) 0.1270(2) 0.4314(2) 0.0251(7) Uani 1 1 d . . . H27 H 0.5785 0.0644 0.4791 0.030 Uiso 1 1 calc R . . C28 C 0.4834(3) 0.1193(2) 0.3609(2) 0.0231(7) Uani 1 1 d . . . H28 H 0.4694 0.0516 0.3613 0.028 Uiso 1 1 calc R . . C29 C 0.4399(3) 0.2074(2) 0.2932(2) 0.0214(7) Uani 1 1 d . . . H29 H 0.3937 0.2008 0.2473 0.026 Uiso 1 1 calc R . . C30 C 0.4627(3) 0.3103(2) 0.28986(19) 0.0170(6) Uani 1 1 d . . . C31 C 0.4219(3) 0.4031(2) 0.21983(19) 0.0172(6) Uani 1 1 d . . . C32 C 0.4497(3) 0.5037(2) 0.21481(19) 0.0181(6) Uani 1 1 d . . . C33 C 0.4159(3) 0.5979(2) 0.1397(2) 0.0221(7) Uani 1 1 d . . . H33 H 0.3720 0.5931 0.0921 0.026 Uiso 1 1 calc R . . C34 C 0.4467(3) 0.6943(2) 0.1364(2) 0.0262(7) Uani 1 1 d . . . H34 H 0.4254 0.7562 0.0859 0.031 Uiso 1 1 calc R . . C35 C 0.5097(3) 0.7035(2) 0.2069(2) 0.0259(7) Uani 1 1 d . . . H35 H 0.5280 0.7716 0.2040 0.031 Uiso 1 1 calc R . . C36 C 0.5446(3) 0.6167(2) 0.2787(2) 0.0216(7) Uani 1 1 d . . . H36 H 0.5869 0.6247 0.3255 0.026 Uiso 1 1 calc R . . C37 C 0.5182(3) 0.5131(2) 0.28494(19) 0.0161(6) Uani 1 1 d . . . C38 C 0.2184(3) 0.4246(2) 0.1368(2) 0.0213(7) Uani 1 1 d . . . H38 H 0.1613 0.4437 0.1758 0.026 Uiso 1 1 calc R . . C39 C 0.3953(3) 0.3748(2) 0.0801(2) 0.0237(7) Uani 1 1 d . . . H39 H 0.4832 0.3531 0.0704 0.028 Uiso 1 1 calc R . . C40 C 0.2922(3) 0.3906(2) 0.0271(2) 0.0220(7) Uani 1 1 d . . . H40 H 0.2958 0.3810 -0.0267 0.026 Uiso 1 1 calc R . . C41 C 1.0045(3) 0.2781(2) 0.49471(19) 0.0154(6) Uani 1 1 d . . . H41 H 0.9159 0.2712 0.5159 0.019 Uiso 1 1 calc R . . C42 C 1.1936(3) 0.3402(2) 0.4477(2) 0.0191(6) Uani 1 1 d . . . H42 H 1.2635 0.3870 0.4297 0.023 Uiso 1 1 calc R . . C43 C 1.1997(3) 0.2412(2) 0.4478(2) 0.0208(7) Uani 1 1 d . . . H43 H 1.2726 0.2066 0.4303 0.025 Uiso 1 1 calc R . . C44 C 1.0379(3) 0.0990(2) 0.48963(19) 0.0173(6) Uani 1 1 d . . . C45 C 0.9494(3) 0.0926(2) 0.43012(19) 0.0170(6) Uani 1 1 d . . . C46 C 0.8988(3) 0.1827(2) 0.3586(2) 0.0220(7) Uani 1 1 d . . . H46 H 0.9234 0.2512 0.3512 0.026 Uiso 1 1 calc R . . C47 C 0.8161(3) 0.1728(2) 0.3011(2) 0.0239(7) Uani 1 1 d . . . H47 H 0.7824 0.2341 0.2542 0.029 Uiso 1 1 calc R . . C48 C 0.7794(3) 0.0710(2) 0.3103(2) 0.0236(7) Uani 1 1 d . . . H48 H 0.7223 0.0648 0.2690 0.028 Uiso 1 1 calc R . . C49 C 0.8254(3) -0.0176(2) 0.3777(2) 0.0208(7) Uani 1 1 d . . . H49 H 0.8001 -0.0851 0.3830 0.025 Uiso 1 1 calc R . . C50 C 0.9110(3) -0.0103(2) 0.44041(19) 0.0179(6) Uani 1 1 d . . . Co1 Co 1.0000 0.5000 0.5000 0.01226(13) Uani 1 2 d S . . Co2 Co 0.0000 0.5000 0.0000 0.01610(14) Uani 1 2 d S . . N1 N 0.9083(2) 1.35403(18) 0.04112(16) 0.0207(6) Uani 1 1 d . . . N2 N 0.8894(2) 1.18231(18) 0.07796(17) 0.0213(6) Uani 1 1 d . . . N3 N 0.9885(2) 0.73925(17) 0.23521(16) 0.0185(5) Uani 1 1 d . . . N4 N 1.0054(2) 0.59513(17) 0.35723(15) 0.0156(5) Uani 1 1 d . . . N5 N 0.8011(2) 0.45919(16) 0.48808(15) 0.0138(5) Uani 1 1 d . . . N6 N 0.6332(2) 0.42709(17) 0.42412(15) 0.0163(5) Uani 1 1 d . . . N7 N 0.3482(2) 0.39621(18) 0.15077(16) 0.0195(5) Uani 1 1 d . . . N8 N 0.1813(2) 0.42260(18) 0.06244(16) 0.0194(5) Uani 1 1 d . . . N9 N 1.0719(2) 0.36305(16) 0.47730(15) 0.0151(5) Uani 1 1 d . . . N10 N 1.0792(2) 0.20178(17) 0.47821(16) 0.0172(5) Uani 1 1 d . . . N11 N -0.1170(3) 0.4928(2) 0.17779(19) 0.0330(7) Uani 1 1 d . . . N12 N 0.6064(3) 0.8363(2) 0.3289(2) 0.0293(6) Uani 1 1 d . . . O1 O -0.0667(2) 0.54699(16) 0.10267(14) 0.0291(5) Uani 1 1 d . . . O2 O -0.2121(3) 0.5359(3) 0.2015(2) 0.1174(17) Uani 1 1 d . . . O3 O -0.0649(3) 0.4131(2) 0.2269(2) 0.0630(9) Uani 1 1 d . . . O4 O 0.6751(3) 0.8776(2) 0.26033(17) 0.0471(7) Uani 1 1 d . . . O5 O 0.6485(2) 0.75259(19) 0.38743(17) 0.0401(6) Uani 1 1 d . . . O6 O 0.4998(3) 0.8789(2) 0.3380(2) 0.0602(8) Uani 1 1 d . . . O7 O 0.5153(3) 0.0613(2) 0.15124(19) 0.0596(8) Uani 1 1 d . . . H7A H 0.5211 0.0173 0.1814 0.085 Uiso 1 1 d . . . H7B H 0.4194 0.0650 0.1700 0.050 Uiso 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 0.0221(16) 0.0161(15) 0.0272(18) -0.0053(14) 0.0016(14) -0.0023(12) C2 0.0196(16) 0.0183(15) 0.0242(18) -0.0042(13) -0.0032(13) 0.0008(12) C3 0.0154(15) 0.0197(16) 0.0248(18) -0.0032(13) -0.0035(13) 0.0000(11) C4 0.0207(15) 0.0113(14) 0.0217(17) -0.0012(13) -0.0003(13) -0.0015(11) C5 0.0202(15) 0.0169(15) 0.0174(16) -0.0020(13) -0.0002(13) -0.0005(12) C6 0.0310(18) 0.0175(16) 0.0206(17) -0.0016(13) -0.0048(14) 0.0002(13) C7 0.0355(19) 0.0296(19) 0.0261(19) -0.0090(16) -0.0131(16) 0.0082(15) C8 0.0331(19) 0.0264(18) 0.031(2) -0.0129(16) -0.0063(16) -0.0037(14) C9 0.0289(17) 0.0177(15) 0.0229(18) -0.0063(14) -0.0005(14) -0.0012(13) C10 0.0217(15) 0.0147(14) 0.0157(16) -0.0034(12) 0.0025(13) -0.0006(11) C11 0.0214(16) 0.0119(14) 0.0176(16) -0.0019(12) 0.0028(13) 0.0006(11) C12 0.0200(15) 0.0167(15) 0.0181(16) -0.0019(13) 0.0021(13) -0.0019(12) C13 0.0212(16) 0.0195(16) 0.0265(18) -0.0039(14) -0.0021(14) 0.0004(12) C14 0.0179(16) 0.0358(19) 0.030(2) -0.0101(16) -0.0037(14) -0.0035(13) C15 0.0228(17) 0.0326(19) 0.034(2) -0.0131(16) -0.0039(15) -0.0075(14) C16 0.0203(16) 0.0165(15) 0.0312(19) -0.0051(14) 0.0015(14) -0.0060(12) C17 0.0156(15) 0.0161(15) 0.0223(17) -0.0049(13) 0.0021(13) -0.0026(11) C18 0.0186(15) 0.0141(14) 0.0170(16) -0.0052(12) -0.0015(13) -0.0006(11) C19 0.0263(17) 0.0226(16) 0.0187(17) -0.0083(14) 0.0041(14) 0.0007(13) C20 0.0269(17) 0.0170(15) 0.0180(16) -0.0089(13) -0.0026(13) 0.0049(12) C21 0.0133(14) 0.0156(14) 0.0178(16) -0.0057(12) -0.0031(12) -0.0015(11) C22 0.0193(15) 0.0165(14) 0.0124(15) -0.0039(12) -0.0008(12) -0.0017(11) C23 0.0145(14) 0.0206(15) 0.0168(16) -0.0054(13) 0.0027(12) -0.0041(11) C24 0.0138(14) 0.0204(15) 0.0173(16) -0.0075(13) -0.0017(12) -0.0050(11) C25 0.0145(14) 0.0194(15) 0.0180(16) -0.0083(13) -0.0014(12) -0.0017(11) C26 0.0215(16) 0.0209(16) 0.0174(16) -0.0058(13) -0.0042(13) -0.0037(12) C27 0.0262(17) 0.0202(16) 0.0253(18) -0.0047(14) -0.0034(14) -0.0016(13) C28 0.0236(16) 0.0174(15) 0.0299(19) -0.0104(14) -0.0003(14) -0.0056(12) C29 0.0228(16) 0.0219(16) 0.0225(18) -0.0110(14) -0.0027(14) -0.0043(12) C30 0.0147(14) 0.0213(15) 0.0178(16) -0.0103(13) -0.0010(12) -0.0039(11) C31 0.0122(14) 0.0244(16) 0.0175(16) -0.0101(13) -0.0031(12) -0.0045(11) C32 0.0148(14) 0.0207(15) 0.0195(16) -0.0086(13) -0.0030(13) 0.0002(11) C33 0.0211(16) 0.0269(17) 0.0188(17) -0.0092(14) -0.0090(13) 0.0013(13) C34 0.0262(17) 0.0202(16) 0.0272(19) -0.0032(14) -0.0097(15) 0.0014(13) C35 0.0279(17) 0.0194(16) 0.032(2) -0.0105(15) -0.0058(15) -0.0011(13) C36 0.0231(16) 0.0196(16) 0.0230(18) -0.0088(14) -0.0030(14) -0.0026(12) C37 0.0147(14) 0.0175(15) 0.0159(16) -0.0060(13) -0.0007(12) -0.0025(11) C38 0.0181(15) 0.0234(16) 0.0252(18) -0.0126(14) -0.0042(13) 0.0020(12) C39 0.0187(16) 0.0315(18) 0.0258(18) -0.0168(15) -0.0034(14) 0.0023(13) C40 0.0249(17) 0.0241(16) 0.0206(17) -0.0125(14) -0.0068(14) 0.0023(12) C41 0.0170(14) 0.0140(14) 0.0171(16) -0.0078(12) -0.0001(12) -0.0016(11) C42 0.0172(15) 0.0145(14) 0.0261(18) -0.0082(13) 0.0013(13) -0.0027(11) C43 0.0178(15) 0.0159(15) 0.0306(18) -0.0117(14) 0.0054(14) -0.0024(11) C44 0.0181(15) 0.0114(14) 0.0252(17) -0.0099(13) -0.0002(13) -0.0018(11) C45 0.0191(15) 0.0117(14) 0.0207(16) -0.0066(12) 0.0001(13) -0.0010(11) C46 0.0281(17) 0.0109(14) 0.0253(18) -0.0055(13) -0.0008(14) -0.0004(12) C47 0.0279(17) 0.0169(15) 0.0257(18) -0.0071(14) -0.0050(14) 0.0017(12) C48 0.0264(17) 0.0231(16) 0.0238(18) -0.0113(14) -0.0055(14) -0.0011(13) C49 0.0203(15) 0.0174(15) 0.0278(18) -0.0115(14) -0.0028(14) -0.0032(12) C50 0.0199(15) 0.0147(14) 0.0206(17) -0.0088(13) -0.0007(13) 0.0006(11) Co1 0.0149(3) 0.0083(3) 0.0140(3) -0.0046(2) -0.0036(2) -0.0003(2) Co2 0.0177(3) 0.0144(3) 0.0160(3) -0.0055(2) -0.0047(2) 0.0001(2) N1 0.0190(13) 0.0178(13) 0.0219(14) -0.0038(11) -0.0044(11) -0.0001(10) N2 0.0209(13) 0.0129(12) 0.0272(15) -0.0048(11) -0.0013(11) -0.0007(10) N3 0.0234(13) 0.0106(12) 0.0175(14) -0.0016(10) -0.0013(11) 0.0018(10) N4 0.0170(12) 0.0132(12) 0.0176(13) -0.0066(10) -0.0044(10) -0.0016(9) N5 0.0152(12) 0.0125(12) 0.0148(13) -0.0059(10) -0.0031(10) -0.0021(9) N6 0.0165(12) 0.0173(12) 0.0150(13) -0.0055(10) -0.0043(10) -0.0023(9) N7 0.0164(12) 0.0225(13) 0.0212(14) -0.0100(11) -0.0066(11) 0.0015(10) N8 0.0213(13) 0.0190(13) 0.0198(14) -0.0095(11) -0.0031(11) -0.0005(10) N9 0.0170(12) 0.0110(11) 0.0177(13) -0.0059(10) -0.0038(10) -0.0004(9) N10 0.0217(13) 0.0115(12) 0.0198(14) -0.0076(10) -0.0024(11) -0.0006(9) N11 0.0230(16) 0.048(2) 0.0235(17) -0.0097(15) -0.0025(13) 0.0022(13) N12 0.0234(15) 0.0365(17) 0.0374(18) -0.0231(15) -0.0016(14) -0.0087(13) O1 0.0380(14) 0.0306(13) 0.0218(13) -0.0133(11) 0.0013(11) -0.0036(10) O2 0.062(2) 0.175(4) 0.051(2) 0.012(2) 0.0227(18) 0.058(2) O3 0.0581(19) 0.0356(16) 0.062(2) 0.0154(14) 0.0067(16) 0.0030(14) O4 0.0537(17) 0.0555(18) 0.0364(16) -0.0201(14) 0.0158(14) -0.0299(14) O5 0.0396(15) 0.0332(14) 0.0442(16) -0.0103(13) -0.0096(13) -0.0048(11) O6 0.0338(16) 0.067(2) 0.083(2) -0.0350(18) -0.0005(15) 0.0130(14) O7 0.0564(19) 0.0593(19) 0.059(2) -0.0157(16) -0.0115(16) -0.0175(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.332(3) . ? C1 N2 1.351(4) . ? C1 H1 0.9500 . ? C2 C3 1.361(4) . ? C2 N1 1.380(4) . ? C2 H2 0.9500 . ? C3 N2 1.377(3) . ? C3 H3 0.9500 . ? C4 C17 1.397(4) . ? C4 C5 1.401(4) . ? C4 N2 1.447(3) . ? C5 C6 1.428(4) . ? C5 C10 1.439(4) . ? C6 C7 1.361(4) . ? C6 H6 0.9500 . ? C7 C8 1.420(4) . ? C7 H7 0.9500 . ? C8 C9 1.360(4) . ? C8 H8 0.9500 . ? C9 C10 1.430(4) . ? C9 H9 0.9500 . ? C10 C11 1.389(4) . ? C11 C12 1.390(4) . ? C11 N3 1.454(3) . ? C12 C17 1.432(4) . ? C12 C13 1.435(4) . ? C13 C14 1.355(4) . ? C13 H13 0.9500 . ? C14 C15 1.409(4) . ? C14 H14 0.9500 . ? C15 C16 1.359(4) . ? C15 H15 0.9500 . ? C16 C17 1.443(4) . ? C16 H16 0.9500 . ? C18 N4 1.321(3) . ? C18 N3 1.343(4) . ? C18 H18 0.9500 . ? C19 C20 1.352(4) . ? C19 N3 1.389(3) . ? C19 H19 0.9500 . ? C20 N4 1.384(4) . ? C20 H20 0.9500 . ? C21 N5 1.322(3) . ? C21 N6 1.357(3) . ? C21 H21 0.9500 . ? C22 C23 1.355(4) . ? C22 N5 1.381(4) . ? C22 H22 0.9500 . ? C23 N6 1.382(4) . ? C23 H23 0.9500 . ? C24 C25 1.397(4) . ? C24 C37 1.412(4) . ? C24 N6 1.438(3) . ? C25 C26 1.420(4) . ? C25 C30 1.442(4) . ? C26 C27 1.366(4) . ? C26 H26 0.9500 . ? C27 C28 1.420(4) . ? C27 H27 0.9500 . ? C28 C29 1.352(4) . ? C28 H28 0.9500 . ? C29 C30 1.429(4) . ? C29 H29 0.9500 . ? C30 C31 1.399(4) . ? C31 C32 1.401(4) . ? C31 N7 1.434(3) . ? C32 C37 1.435(4) . ? C32 C33 1.436(4) . ? C33 C34 1.363(4) . ? C33 H33 0.9500 . ? C34 C35 1.412(4) . ? C34 H34 0.9500 . ? C35 C36 1.353(4) . ? C35 H35 0.9500 . ? C36 C37 1.432(4) . ? C36 H36 0.9500 . ? C38 N8 1.318(4) . ? C38 N7 1.356(3) . ? C38 H38 0.9500 . ? C39 C40 1.351(4) . ? C39 N7 1.376(4) . ? C39 H39 0.9500 . ? C40 N8 1.373(4) . ? C40 H40 0.9500 . ? C41 N9 1.322(3) . ? C41 N10 1.361(3) . ? C41 H41 0.9500 . ? C42 C43 1.358(4) . ? C42 N9 1.373(3) . ? C42 H42 0.9500 . ? C43 N10 1.369(4) . ? C43 H43 0.9500 . ? C44 C45 1.398(4) . ? C44 C50 1.400(4) 2_756 ? C44 N10 1.441(3) . ? C45 C46 1.422(4) . ? C45 C50 1.437(4) . ? C46 C47 1.353(4) . ? C46 H46 0.9500 . ? C47 C48 1.421(4) . ? C47 H47 0.9500 . ? C48 C49 1.362(4) . ? C48 H48 0.9500 . ? C49 C50 1.423(4) . ? C49 H49 0.9500 . ? C50 C44 1.400(4) 2_756 ? Co1 N9 2.138(2) . ? Co1 N9 2.138(2) 2_766 ? Co1 N5 2.176(2) 2_766 ? Co1 N5 2.176(2) . ? Co1 N4 2.210(2) . ? Co1 N4 2.210(2) 2_766 ? Co2 O1 2.116(2) 2_565 ? Co2 O1 2.116(2) . ? Co2 N1 2.119(2) 2_675 ? Co2 N1 2.119(2) 1_445 ? Co2 N8 2.157(2) . ? Co2 N8 2.157(2) 2_565 ? N1 Co2 2.119(2) 1_665 ? N11 O3 1.186(3) . ? N11 O2 1.230(4) . ? N11 O1 1.278(3) . ? N12 O6 1.230(3) . ? N12 O5 1.242(3) . ? N12 O4 1.256(3) . ? O7 H7A 0.6164 . ? O7 H7B 1.0154 . ? 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 N2 111.3(3) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? C3 C2 N1 110.1(3) . . ? C3 C2 H2 124.9 . . ? N1 C2 H2 124.9 . . ? C2 C3 N2 106.0(3) . . ? C2 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? C17 C4 C5 122.3(3) . . ? C17 C4 N2 118.8(2) . . ? C5 C4 N2 118.8(2) . . ? C4 C5 C6 122.6(3) . . ? C4 C5 C10 119.0(3) . . ? C6 C5 C10 118.4(3) . . ? C7 C6 C5 120.9(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.6(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 123.5(3) . . ? C11 C10 C5 117.8(3) . . ? C9 C10 C5 118.7(3) . . ? C10 C11 C12 123.3(3) . . ? C10 C11 N3 120.2(2) . . ? C12 C11 N3 116.4(2) . . ? C11 C12 C17 118.9(3) . . ? C11 C12 C13 122.5(3) . . ? C17 C12 C13 118.6(3) . . ? C14 C13 C12 121.6(3) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 121.7(3) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C4 C17 C12 118.3(3) . . ? C4 C17 C16 124.0(3) . . ? C12 C17 C16 117.6(3) . . ? N4 C18 N3 112.1(2) . . ? N4 C18 H18 123.9 . . ? N3 C18 H18 123.9 . . ? C20 C19 N3 105.8(3) . . ? C20 C19 H19 127.1 . . ? N3 C19 H19 127.1 . . ? C19 C20 N4 110.3(2) . . ? C19 C20 H20 124.9 . . ? N4 C20 H20 124.9 . . ? N5 C21 N6 111.0(3) . . ? N5 C21 H21 124.5 . . ? N6 C21 H21 124.5 . . ? C23 C22 N5 110.5(3) . . ? C23 C22 H22 124.8 . . ? N5 C22 H22 124.8 . . ? C22 C23 N6 105.5(3) . . ? C22 C23 H23 127.2 . . ? N6 C23 H23 127.2 . . ? C25 C24 C37 122.7(2) . . ? C25 C24 N6 118.5(2) . . ? C37 C24 N6 118.6(2) . . ? C24 C25 C26 123.0(3) . . ? C24 C25 C30 118.7(3) . . ? C26 C25 C30 118.3(2) . . ? C27 C26 C25 121.0(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.4(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 120.7(3) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.8(3) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 122.3(2) . . ? C31 C30 C25 118.9(2) . . ? C29 C30 C25 118.7(3) . . ? C30 C31 C32 122.2(2) . . ? C30 C31 N7 119.5(2) . . ? C32 C31 N7 118.3(2) . . ? C31 C32 C37 119.5(3) . . ? C31 C32 C33 121.7(3) . . ? C37 C32 C33 118.8(2) . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.9(3) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 121.1(3) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 120.6(3) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C24 C37 C36 123.5(3) . . ? C24 C37 C32 118.1(2) . . ? C36 C37 C32 118.5(3) . . ? N8 C38 N7 111.6(3) . . ? N8 C38 H38 124.2 . . ? N7 C38 H38 124.2 . . ? C40 C39 N7 106.5(3) . . ? C40 C39 H39 126.7 . . ? N7 C39 H39 126.7 . . ? C39 C40 N8 110.0(3) . . ? C39 C40 H40 125.0 . . ? N8 C40 H40 125.0 . . ? N9 C41 N10 110.8(2) . . ? N9 C41 H41 124.6 . . ? N10 C41 H41 124.6 . . ? C43 C42 N9 110.4(3) . . ? C43 C42 H42 124.8 . . ? N9 C42 H42 124.8 . . ? C42 C43 N10 105.8(2) . . ? C42 C43 H43 127.1 . . ? N10 C43 H43 127.1 . . ? C45 C44 C50 123.2(2) . 2_756 ? C45 C44 N10 118.4(2) . . ? C50 C44 N10 118.3(2) 2_756 . ? C44 C45 C46 123.0(2) . . ? C44 C45 C50 118.3(2) . . ? C46 C45 C50 118.6(2) . . ? C47 C46 C45 121.2(3) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 120.3(3) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C49 C48 C47 120.6(3) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 120.8(3) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C44 C50 C49 123.0(2) 2_756 . ? C44 C50 C45 118.5(2) 2_756 . ? C49 C50 C45 118.5(2) . . ? N9 Co1 N9 179.999(1) . 2_766 ? N9 Co1 N5 91.71(8) . 2_766 ? N9 Co1 N5 88.29(8) 2_766 2_766 ? N9 Co1 N5 88.29(8) . . ? N9 Co1 N5 91.71(8) 2_766 . ? N5 Co1 N5 179.999(1) 2_766 . ? N9 Co1 N4 89.95(8) . . ? N9 Co1 N4 90.05(8) 2_766 . ? N5 Co1 N4 90.95(8) 2_766 . ? N5 Co1 N4 89.05(8) . . ? N9 Co1 N4 90.05(8) . 2_766 ? N9 Co1 N4 89.95(8) 2_766 2_766 ? N5 Co1 N4 89.05(8) 2_766 2_766 ? N5 Co1 N4 90.95(8) . 2_766 ? N4 Co1 N4 179.998(1) . 2_766 ? O1 Co2 O1 180.0 2_565 . ? O1 Co2 N1 99.19(9) 2_565 2_675 ? O1 Co2 N1 80.81(9) . 2_675 ? O1 Co2 N1 80.81(9) 2_565 1_445 ? O1 Co2 N1 99.19(9) . 1_445 ? N1 Co2 N1 180.00(14) 2_675 1_445 ? O1 Co2 N8 85.16(8) 2_565 . ? O1 Co2 N8 94.84(8) . . ? N1 Co2 N8 88.08(9) 2_675 . ? N1 Co2 N8 91.92(9) 1_445 . ? O1 Co2 N8 94.84(8) 2_565 2_565 ? O1 Co2 N8 85.16(8) . 2_565 ? N1 Co2 N8 91.92(9) 2_675 2_565 ? N1 Co2 N8 88.08(9) 1_445 2_565 ? N8 Co2 N8 180.00(6) . 2_565 ? C1 N1 C2 105.2(2) . . ? C1 N1 Co2 123.9(2) . 1_665 ? C2 N1 Co2 130.85(18) . 1_665 ? C1 N2 C3 107.4(2) . . ? C1 N2 C4 126.4(2) . . ? C3 N2 C4 125.1(2) . . ? C18 N3 C19 106.8(2) . . ? C18 N3 C11 123.3(2) . . ? C19 N3 C11 127.0(2) . . ? C18 N4 C20 104.9(2) . . ? C18 N4 Co1 124.43(19) . . ? C20 N4 Co1 129.45(17) . . ? C21 N5 C22 105.5(2) . . ? C21 N5 Co1 122.42(19) . . ? C22 N5 Co1 131.74(18) . . ? C21 N6 C23 107.5(2) . . ? C21 N6 C24 125.1(2) . . ? C23 N6 C24 127.3(2) . . ? C38 N7 C39 106.4(2) . . ? C38 N7 C31 125.0(2) . . ? C39 N7 C31 128.0(2) . . ? C38 N8 C40 105.6(2) . . ? C38 N8 Co2 122.74(19) . . ? C40 N8 Co2 129.34(19) . . ? C41 N9 C42 105.5(2) . . ? C41 N9 Co1 124.52(19) . . ? C42 N9 Co1 129.86(18) . . ? C41 N10 C43 107.5(2) . . ? C41 N10 C44 126.1(2) . . ? C43 N10 C44 126.4(2) . . ? O3 N11 O2 121.3(3) . . ? O3 N11 O1 122.1(3) . . ? O2 N11 O1 115.8(3) . . ? O6 N12 O5 120.7(3) . . ? O6 N12 O4 120.3(3) . . ? O5 N12 O4 119.1(3) . . ? N11 O1 Co2 130.02(19) . . ? H7A O7 H7B 87.9 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.251 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.083 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 # Attachment '- 3.hcl611.cif' data_3_hcl611 _database_code_depnum_ccdc_archive 'CCDC 800201' #TrackingRef '- 3.hcl611.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C48 H32 Co N8 O4, C28 H22 Co N4 O6, 2(H O0.50)' _chemical_formula_sum 'C76 H56 Co2 N12 O11' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 150(2) _chemical_formula_weight 1431.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2647(13) _cell_length_b 13.3120(17) _cell_length_c 13.6154(17) _cell_angle_alpha 61.920(4) _cell_angle_beta 71.986(4) _cell_angle_gamma 75.482(4) _cell_volume 1699.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1348 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 20.4 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8726 _exptl_absorpt_correction_T_max 0.9461 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19933 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.1530 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.68 _reflns_number_total 8673 _reflns_number_gt 4326 _reflns_threshold_expression I>2\s _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'DIAMOND (Brandenburg, 2006)' _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^)+(0.0531P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8673 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1443 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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 0.5122(3) 0.5319(3) 0.2050(2) 0.0259(8) Uani 1 1 d . . . H1 H 0.5853 0.4770 0.2121 0.031 Uiso 1 1 calc R . . C2 C 0.3549(3) 0.6506(3) 0.1412(3) 0.0293(8) Uani 1 1 d . . . H2 H 0.2967 0.6952 0.0939 0.035 Uiso 1 1 calc R . . C3 C 0.3510(4) 0.6513(3) 0.2418(3) 0.0400(10) Uani 1 1 d . . . H3 H 0.2905 0.6952 0.2773 0.048 Uiso 1 1 calc R . . C4 C 0.4777(4) 0.5370(3) 0.3929(3) 0.0333(9) Uani 1 1 d . . . C5 C 0.5835(4) 0.5677(3) 0.3991(3) 0.0339(9) Uani 1 1 d . . . C6 C 0.6685(4) 0.6373(3) 0.3022(3) 0.0447(11) Uani 1 1 d . . . H6 H 0.6549 0.6637 0.2280 0.054 Uiso 1 1 calc R . . C7 C 0.7679(5) 0.6664(4) 0.3141(3) 0.0558(12) Uani 1 1 d . . . H7 H 0.8243 0.7115 0.2479 0.067 Uiso 1 1 calc R . . C8 C 0.7901(4) 0.6306(4) 0.4246(3) 0.0537(12) Uani 1 1 d . . . H8 H 0.8598 0.6529 0.4315 0.064 Uiso 1 1 calc R . . C9 C 0.7112(4) 0.5648(3) 0.5193(3) 0.0418(10) Uani 1 1 d . . . H9 H 0.7260 0.5417 0.5924 0.050 Uiso 1 1 calc R . . C10 C 0.6064(4) 0.5294(3) 0.5109(3) 0.0363(9) Uani 1 1 d . . . C11 C 0.5045(3) 0.2614(2) 0.2112(2) 0.0204(7) Uani 1 1 d . . . H11 H 0.5925 0.2419 0.1886 0.024 Uiso 1 1 calc R . . C12 C 0.3138(3) 0.3468(3) 0.2115(3) 0.0254(8) Uani 1 1 d . . . H12 H 0.2434 0.4003 0.1872 0.030 Uiso 1 1 calc R . . C13 C 0.3096(3) 0.2556(3) 0.3143(3) 0.0296(8) Uani 1 1 d . . . H13 H 0.2373 0.2333 0.3745 0.035 Uiso 1 1 calc R . . C14 C 0.4696(3) 0.0991(3) 0.4072(2) 0.0226(7) Uani 1 1 d . . . C15 C 0.4425(3) -0.0053(3) 0.4231(2) 0.0230(7) Uani 1 1 d . . . C16 C 0.3864(3) -0.0159(3) 0.3478(3) 0.0326(8) Uani 1 1 d . . . H16 H 0.3671 0.0505 0.2826 0.039 Uiso 1 1 calc R . . C17 C 0.3606(4) -0.1181(3) 0.3677(3) 0.0401(10) Uani 1 1 d . . . H17 H 0.3232 -0.1231 0.3167 0.048 Uiso 1 1 calc R . . C18 C 0.3888(3) -0.2177(3) 0.4639(3) 0.0385(9) Uani 1 1 d . . . H18 H 0.3672 -0.2887 0.4783 0.046 Uiso 1 1 calc R . . C19 C 0.4463(3) -0.2146(3) 0.5364(3) 0.0292(8) Uani 1 1 d . . . H19 H 0.4675 -0.2835 0.5988 0.035 Uiso 1 1 calc R . . C20 C 0.4750(3) -0.1087(3) 0.5195(3) 0.0230(7) Uani 1 1 d . . . C21 C 0.7831(3) 0.3909(3) 0.0411(2) 0.0210(7) Uani 1 1 d . . . C22 C 0.8960(3) 0.4471(3) 0.0205(2) 0.0185(7) Uani 1 1 d . . . C23 C 0.8818(3) 0.5627(3) -0.0025(2) 0.0227(7) Uani 1 1 d . . . H23 H 0.8009 0.6062 -0.0041 0.027 Uiso 1 1 calc R . . C24 C 1.0155(3) 0.3852(3) 0.0230(3) 0.0235(7) Uani 1 1 d . . . H24 H 1.0267 0.3063 0.0389 0.028 Uiso 1 1 calc R . . C25 C 0.9905(3) -0.0060(3) 0.2283(3) 0.0366(9) Uani 1 1 d . . . H25 H 1.0768 0.0050 0.2024 0.044 Uiso 1 1 calc R . . C26 C 0.8068(3) -0.0306(3) 0.2365(3) 0.0333(9) Uani 1 1 d . . . H26 H 0.7382 -0.0404 0.2165 0.040 Uiso 1 1 calc R . . C27 C 0.8018(3) -0.0289(3) 0.3365(3) 0.0354(9) Uani 1 1 d . . . H27 H 0.7306 -0.0370 0.3983 0.043 Uiso 1 1 calc R . . C28 C 0.9616(3) -0.0060(3) 0.4167(3) 0.0310(8) Uani 1 1 d . . . C29 C 0.9524(3) 0.1019(3) 0.4129(3) 0.0326(9) Uani 1 1 d . . . C30 C 0.9068(4) 0.2066(3) 0.3271(3) 0.0392(9) Uani 1 1 d . . . H30 H 0.8806 0.2042 0.2683 0.047 Uiso 1 1 calc R . . C31 C 0.9005(4) 0.3092(4) 0.3283(3) 0.0451(10) Uani 1 1 d . . . H31 H 0.8725 0.3780 0.2692 0.054 Uiso 1 1 calc R . . C32 C 0.9353(4) 0.3145(3) 0.4173(3) 0.0427(10) Uani 1 1 d . . . H32 H 0.9284 0.3867 0.4181 0.051 Uiso 1 1 calc R . . C33 C 0.9784(3) 0.2179(3) 0.5010(3) 0.0388(9) Uani 1 1 d . . . H33 H 1.0002 0.2233 0.5603 0.047 Uiso 1 1 calc R . . C34 C 0.9913(3) 0.1083(3) 0.5015(3) 0.0325(8) Uani 1 1 d . . . C35 C 0.7612(3) -0.0727(3) 0.0096(3) 0.0264(8) Uani 1 1 d . . . C36 C 0.6261(3) -0.0359(3) 0.0050(3) 0.0256(8) Uani 1 1 d . . . C37 C 0.5583(3) -0.1047(3) -0.0030(3) 0.0310(8) Uani 1 1 d . . . H37 H 0.5973 -0.1762 -0.0045 0.037 Uiso 1 1 calc R . . C38 C 0.5677(3) 0.0674(3) 0.0090(3) 0.0311(9) Uani 1 1 d . . . H38 H 0.6141 0.1135 0.0158 0.037 Uiso 1 1 calc R . . Co1 Co 0.5000 0.5000 0.0000 0.01561(15) Uani 1 2 d S . . Co2 Co 1.0000 0.0000 0.0000 0.02450(17) Uani 1 2 d S . . N1 N 0.4559(2) 0.5755(2) 0.1187(2) 0.0232(6) Uani 1 1 d . . . N2 N 0.4517(3) 0.5760(2) 0.2821(2) 0.0320(7) Uani 1 1 d . . . N3 N 0.4360(2) 0.3508(2) 0.14687(19) 0.0187(6) Uani 1 1 d . . . N4 N 0.4308(2) 0.2014(2) 0.3146(2) 0.0234(6) Uani 1 1 d . . . N5 N 0.9258(2) -0.0163(2) 0.1683(2) 0.0280(7) Uani 1 1 d . . . N6 N 0.9196(3) -0.0129(2) 0.3306(2) 0.0308(7) Uani 1 1 d . . . O1 O 0.68075(19) 0.45712(18) 0.02854(17) 0.0241(5) Uani 1 1 d . . . O2 O 0.79648(19) 0.28522(18) 0.06982(18) 0.0280(5) Uani 1 1 d . . . O3 O 0.8227(2) 0.0057(2) -0.01114(18) 0.0289(6) Uani 1 1 d . . . O4 O 0.8053(2) -0.1757(2) 0.0333(2) 0.0390(6) Uani 1 1 d . . . O5 O 1.0301(2) -0.18428(19) 0.06113(18) 0.0314(6) Uani 1 1 d . . . H9A H 1.0729 -0.2009 0.0118 0.047 Uiso 1 1 d R . . H10 H 0.9671 -0.2070 0.0614 0.047 Uiso 1 1 d R . . O6 O 1.0601(5) 0.7085(5) 0.2870(4) 0.0484(15) Uani 0.50 1 d P . . H6B H 1.0670 0.6597 0.2860 0.051 Uiso 0.50 1 d P . . H6A H 1.0728 0.7575 0.2243 0.046 Uiso 0.50 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 0.034(2) 0.0256(18) 0.0211(17) -0.0112(15) -0.0091(15) -0.0030(15) C2 0.040(2) 0.0232(18) 0.0255(18) -0.0112(15) -0.0116(16) 0.0013(16) C3 0.057(3) 0.032(2) 0.035(2) -0.0206(18) -0.0170(19) 0.0107(19) C4 0.059(3) 0.0265(19) 0.0208(18) -0.0110(16) -0.0174(17) -0.0030(18) C5 0.054(2) 0.0279(19) 0.0241(18) -0.0135(16) -0.0143(17) -0.0008(17) C6 0.076(3) 0.039(2) 0.0205(19) -0.0076(18) -0.0151(19) -0.014(2) C7 0.083(3) 0.054(3) 0.033(2) -0.010(2) -0.017(2) -0.025(3) C8 0.072(3) 0.059(3) 0.042(2) -0.019(2) -0.019(2) -0.025(2) C9 0.062(3) 0.040(2) 0.029(2) -0.0127(18) -0.0180(19) -0.009(2) C10 0.060(3) 0.029(2) 0.0264(19) -0.0122(17) -0.0186(18) -0.0049(18) C11 0.0206(17) 0.0205(16) 0.0156(15) -0.0054(14) -0.0006(13) -0.0045(13) C12 0.0211(18) 0.0262(18) 0.0237(17) -0.0048(15) -0.0074(14) -0.0035(14) C13 0.0171(17) 0.0317(19) 0.0269(18) -0.0049(16) 0.0007(14) -0.0043(15) C14 0.0206(17) 0.0199(17) 0.0171(16) -0.0018(14) -0.0022(13) -0.0007(13) C15 0.0195(17) 0.0247(18) 0.0189(16) -0.0074(14) -0.0020(13) 0.0001(14) C16 0.044(2) 0.028(2) 0.0249(18) -0.0079(16) -0.0143(16) -0.0020(17) C17 0.049(3) 0.039(2) 0.043(2) -0.0206(19) -0.0199(19) -0.0031(19) C18 0.042(2) 0.029(2) 0.048(2) -0.0179(19) -0.0126(19) -0.0055(17) C19 0.033(2) 0.0217(18) 0.0278(18) -0.0073(15) -0.0069(15) -0.0016(15) C20 0.0188(17) 0.0218(17) 0.0211(16) -0.0065(14) -0.0010(13) -0.0005(13) C21 0.0201(17) 0.0276(19) 0.0143(15) -0.0074(14) -0.0047(13) -0.0034(14) C22 0.0149(16) 0.0241(17) 0.0172(15) -0.0078(14) -0.0063(12) -0.0024(13) C23 0.0155(17) 0.0271(18) 0.0270(17) -0.0121(15) -0.0078(13) -0.0001(14) C24 0.0188(17) 0.0226(17) 0.0294(18) -0.0112(15) -0.0061(14) -0.0022(14) C25 0.027(2) 0.068(3) 0.0231(18) -0.0258(19) -0.0008(15) -0.0131(19) C26 0.025(2) 0.051(2) 0.0270(18) -0.0185(18) -0.0044(15) -0.0093(17) C27 0.0210(19) 0.058(3) 0.0272(19) -0.0205(18) 0.0024(15) -0.0092(17) C28 0.028(2) 0.054(2) 0.0197(17) -0.0233(18) 0.0015(14) -0.0124(18) C29 0.034(2) 0.049(2) 0.0196(17) -0.0188(17) 0.0010(15) -0.0123(18) C30 0.045(2) 0.051(3) 0.0242(19) -0.0170(18) -0.0074(17) -0.009(2) C31 0.054(3) 0.045(2) 0.033(2) -0.013(2) -0.0111(19) -0.007(2) C32 0.047(3) 0.043(2) 0.043(2) -0.025(2) -0.0055(19) -0.0072(19) C33 0.039(2) 0.055(3) 0.034(2) -0.028(2) -0.0004(17) -0.017(2) C34 0.028(2) 0.049(2) 0.0247(18) -0.0195(18) 0.0022(15) -0.0136(17) C35 0.0206(18) 0.038(2) 0.0219(17) -0.0126(16) -0.0073(14) -0.0038(16) C36 0.0207(18) 0.0290(19) 0.0260(18) -0.0094(16) -0.0069(14) -0.0040(15) C37 0.0238(19) 0.0271(19) 0.048(2) -0.0193(18) -0.0140(16) 0.0010(15) C38 0.0180(18) 0.032(2) 0.048(2) -0.0157(18) -0.0133(16) -0.0074(15) Co1 0.0144(3) 0.0178(3) 0.0142(3) -0.0045(3) -0.0057(2) -0.0029(2) Co2 0.0166(3) 0.0400(4) 0.0225(3) -0.0173(3) -0.0043(3) -0.0048(3) N1 0.0320(16) 0.0204(14) 0.0179(13) -0.0058(12) -0.0078(12) -0.0066(12) N2 0.053(2) 0.0287(16) 0.0196(14) -0.0120(13) -0.0155(14) -0.0005(14) N3 0.0184(14) 0.0215(14) 0.0157(13) -0.0061(11) -0.0055(11) -0.0032(11) N4 0.0211(15) 0.0205(14) 0.0181(13) 0.0005(12) -0.0038(11) -0.0043(11) N5 0.0226(16) 0.0443(18) 0.0213(14) -0.0173(14) -0.0010(12) -0.0093(13) N6 0.0308(17) 0.0479(19) 0.0216(14) -0.0201(14) -0.0023(12) -0.0113(14) O1 0.0164(12) 0.0284(13) 0.0235(12) -0.0052(10) -0.0092(9) -0.0024(10) O2 0.0205(12) 0.0246(13) 0.0385(13) -0.0129(11) -0.0038(10) -0.0070(10) O3 0.0183(13) 0.0397(14) 0.0350(13) -0.0181(12) -0.0084(10) -0.0063(11) O4 0.0217(13) 0.0370(15) 0.0613(17) -0.0229(14) -0.0136(12) 0.0007(11) O5 0.0208(12) 0.0423(14) 0.0344(13) -0.0190(12) -0.0063(10) -0.0038(11) O6 0.043(3) 0.066(4) 0.029(3) -0.017(3) -0.012(2) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.325(4) . ? C1 N2 1.358(4) . ? C1 H1 0.9500 . ? C2 C3 1.360(4) . ? C2 N1 1.375(4) . ? C2 H2 0.9500 . ? C3 N2 1.375(4) . ? C3 H3 0.9500 . ? C4 C5 1.390(5) . ? C4 C10 1.399(5) 2_666 ? C4 N2 1.446(4) . ? C5 C6 1.425(5) . ? C5 C10 1.447(4) . ? C6 C7 1.349(5) . ? C6 H6 0.9500 . ? C7 C8 1.432(5) . ? C7 H7 0.9500 . ? C8 C9 1.355(5) . ? C8 H8 0.9500 . ? C9 C10 1.428(5) . ? C9 H9 0.9500 . ? C10 C4 1.399(5) 2_666 ? C11 N3 1.325(4) . ? C11 N4 1.364(4) . ? C11 H11 0.9500 . ? C12 C13 1.350(4) . ? C12 N3 1.384(4) . ? C12 H12 0.9500 . ? C13 N4 1.375(4) . ? C13 H13 0.9500 . ? C14 C20 1.395(4) 2_656 ? C14 C15 1.400(4) . ? C14 N4 1.435(4) . ? C15 C16 1.433(4) . ? C15 C20 1.447(4) . ? C16 C17 1.346(5) . ? C16 H16 0.9500 . ? C17 C18 1.409(5) . ? C17 H17 0.9500 . ? C18 C19 1.358(5) . ? C18 H18 0.9500 . ? C19 C20 1.422(4) . ? C19 H19 0.9500 . ? C20 C14 1.395(4) 2_656 ? C21 O2 1.251(4) . ? C21 O1 1.267(3) . ? C21 C22 1.522(4) . ? C22 C24 1.392(4) . ? C22 C23 1.395(4) . ? C23 C24 1.385(4) 2_765 ? C23 H23 0.9500 . ? C24 C23 1.385(4) 2_765 ? C24 H24 0.9500 . ? C25 N5 1.318(4) . ? C25 N6 1.347(4) . ? C25 H25 0.9500 . ? C26 C27 1.356(4) . ? C26 N5 1.374(4) . ? C26 H26 0.9500 . ? C27 N6 1.369(4) . ? C27 H27 0.9500 . ? C28 C29 1.392(5) . ? C28 C34 1.398(5) 2_756 ? C28 N6 1.439(4) . ? C29 C30 1.432(5) . ? C29 C34 1.448(4) . ? C30 C31 1.358(5) . ? C30 H30 0.9500 . ? C31 C32 1.420(5) . ? C31 H31 0.9500 . ? C32 C33 1.355(5) . ? C32 H32 0.9500 . ? C33 C34 1.427(5) . ? C33 H33 0.9500 . ? C34 C28 1.398(5) 2_756 ? C35 O4 1.254(4) . ? C35 O3 1.269(4) . ? C35 C36 1.489(4) . ? C36 C38 1.385(5) . ? C36 C37 1.389(4) . ? C37 C38 1.395(4) 2_655 ? C37 H37 0.9500 . ? C38 C37 1.395(4) 2_655 ? C38 H38 0.9500 . ? Co1 O1 2.078(2) . ? Co1 O1 2.078(2) 2_665 ? Co1 N3 2.133(2) 2_665 ? Co1 N3 2.133(2) . ? Co1 N1 2.156(3) . ? Co1 N1 2.156(3) 2_665 ? Co2 O3 2.030(2) 2_755 ? Co2 O3 2.030(2) . ? Co2 N5 2.106(3) 2_755 ? Co2 N5 2.106(3) . ? Co2 O5 2.159(2) 2_755 ? Co2 O5 2.159(2) . ? O5 H9A 0.7870 . ? O5 H10 0.8360 . ? O6 H6B 0.6398 . ? O6 H6A 0.7884 . ? 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 N2 111.2(3) . . ? N1 C1 H1 124.4 . . ? N2 C1 H1 124.4 . . ? C3 C2 N1 109.5(3) . . ? C3 C2 H2 125.2 . . ? N1 C2 H2 125.2 . . ? C2 C3 N2 106.6(3) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? C5 C4 C10 123.2(3) . 2_666 ? C5 C4 N2 119.0(3) . . ? C10 C4 N2 117.8(3) 2_666 . ? C4 C5 C6 123.9(3) . . ? C4 C5 C10 118.0(3) . . ? C6 C5 C10 118.1(4) . . ? C7 C6 C5 121.1(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 121.2(4) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 121.1(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C4 C10 C9 122.5(3) 2_666 . ? C4 C10 C5 118.8(3) 2_666 . ? C9 C10 C5 118.7(3) . . ? N3 C11 N4 110.4(3) . . ? N3 C11 H11 124.8 . . ? N4 C11 H11 124.8 . . ? C13 C12 N3 109.8(3) . . ? C13 C12 H12 125.1 . . ? N3 C12 H12 125.1 . . ? C12 C13 N4 106.4(3) . . ? C12 C13 H13 126.8 . . ? N4 C13 H13 126.8 . . ? C20 C14 C15 123.2(3) 2_656 . ? C20 C14 N4 119.1(3) 2_656 . ? C15 C14 N4 117.6(3) . . ? C14 C15 C16 123.5(3) . . ? C14 C15 C20 118.5(3) . . ? C16 C15 C20 118.0(3) . . ? C17 C16 C15 121.3(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 121.5(3) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C14 C20 C19 123.2(3) 2_656 . ? C14 C20 C15 118.3(3) 2_656 . ? C19 C20 C15 118.5(3) . . ? O2 C21 O1 125.2(3) . . ? O2 C21 C22 119.1(3) . . ? O1 C21 C22 115.7(3) . . ? C24 C22 C23 118.5(3) . . ? C24 C22 C21 121.1(3) . . ? C23 C22 C21 120.4(3) . . ? C24 C23 C22 120.7(3) 2_765 . ? C24 C23 H23 119.7 2_765 . ? C22 C23 H23 119.7 . . ? C23 C24 C22 120.8(3) 2_765 . ? C23 C24 H24 119.6 2_765 . ? C22 C24 H24 119.6 . . ? N5 C25 N6 112.0(3) . . ? N5 C25 H25 124.0 . . ? N6 C25 H25 124.0 . . ? C27 C26 N5 110.0(3) . . ? C27 C26 H26 125.0 . . ? N5 C26 H26 125.0 . . ? C26 C27 N6 106.3(3) . . ? C26 C27 H27 126.9 . . ? N6 C27 H27 126.9 . . ? C29 C28 C34 124.4(3) . 2_756 ? C29 C28 N6 117.9(3) . . ? C34 C28 N6 117.7(3) 2_756 . ? C28 C29 C30 124.1(3) . . ? C28 C29 C34 117.7(3) . . ? C30 C29 C34 118.2(3) . . ? C31 C30 C29 121.1(3) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 120.4(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 120.9(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 121.0(3) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C28 C34 C33 123.8(3) 2_756 . ? C28 C34 C29 117.8(3) 2_756 . ? C33 C34 C29 118.4(3) . . ? O4 C35 O3 125.3(3) . . ? O4 C35 C36 119.1(3) . . ? O3 C35 C36 115.5(3) . . ? C38 C36 C37 119.9(3) . . ? C38 C36 C35 119.8(3) . . ? C37 C36 C35 120.3(3) . . ? C36 C37 C38 119.2(3) . 2_655 ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 2_655 . ? C36 C38 C37 120.9(3) . 2_655 ? C36 C38 H38 119.5 . . ? C37 C38 H38 119.5 2_655 . ? O1 Co1 O1 180.0 . 2_665 ? O1 Co1 N3 87.47(8) . 2_665 ? O1 Co1 N3 92.53(8) 2_665 2_665 ? O1 Co1 N3 92.53(8) . . ? O1 Co1 N3 87.47(8) 2_665 . ? N3 Co1 N3 180.000(1) 2_665 . ? O1 Co1 N1 85.73(9) . . ? O1 Co1 N1 94.27(9) 2_665 . ? N3 Co1 N1 95.31(9) 2_665 . ? N3 Co1 N1 84.69(9) . . ? O1 Co1 N1 94.27(9) . 2_665 ? O1 Co1 N1 85.73(9) 2_665 2_665 ? N3 Co1 N1 84.69(9) 2_665 2_665 ? N3 Co1 N1 95.31(9) . 2_665 ? N1 Co1 N1 180.00(10) . 2_665 ? O3 Co2 O3 180.0 2_755 . ? O3 Co2 N5 88.42(9) 2_755 2_755 ? O3 Co2 N5 91.58(9) . 2_755 ? O3 Co2 N5 91.58(9) 2_755 . ? O3 Co2 N5 88.42(9) . . ? N5 Co2 N5 180.0 2_755 . ? O3 Co2 O5 91.05(9) 2_755 2_755 ? O3 Co2 O5 88.96(9) . 2_755 ? N5 Co2 O5 90.69(10) 2_755 2_755 ? N5 Co2 O5 89.31(10) . 2_755 ? O3 Co2 O5 88.95(9) 2_755 . ? O3 Co2 O5 91.05(9) . . ? N5 Co2 O5 89.31(10) 2_755 . ? N5 Co2 O5 90.69(10) . . ? O5 Co2 O5 180.0 2_755 . ? C1 N1 C2 105.9(3) . . ? C1 N1 Co1 121.3(2) . . ? C2 N1 Co1 131.0(2) . . ? C1 N2 C3 106.8(3) . . ? C1 N2 C4 125.8(3) . . ? C3 N2 C4 126.8(3) . . ? C11 N3 C12 106.0(2) . . ? C11 N3 Co1 127.8(2) . . ? C12 N3 Co1 123.55(19) . . ? C11 N4 C13 107.4(2) . . ? C11 N4 C14 127.3(3) . . ? C13 N4 C14 125.3(2) . . ? C25 N5 C26 105.0(3) . . ? C25 N5 Co2 123.5(2) . . ? C26 N5 Co2 131.3(2) . . ? C25 N6 C27 106.7(3) . . ? C25 N6 C28 126.1(3) . . ? C27 N6 C28 127.2(3) . . ? C21 O1 Co1 152.7(2) . . ? C35 O3 Co2 131.7(2) . . ? Co2 O5 H9A 109.8 . . ? Co2 O5 H10 109.7 . . ? H9A O5 H10 92.8 . . ? H6B O6 H6A 110.4 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.479 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.081 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0