# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Biao Wu' _publ_contact_author_email WUBIAO@LZB.AC.CN _publ_section_title ; 1D-1D Two-Fold Parallel Interpenetrated Coordination Polymers with a Bis(pyridylurea) Ligand ; loop_ _publ_author_name 'Biao Wu' 'Yongjing Hao' 'Shaoguang Li' 'Yanyan Liu' 'Xiao-Juan Yang' # Attachment '1D_interpenetration.cif' data_CdL2Cl2 _database_code_depnum_ccdc_archive 'CCDC 739485' #TrackingRef '1D_interpenetration.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 Cd Cl2 N12 O12' _chemical_formula_weight 956.14 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 14.1957(10) _cell_length_b 15.7796(11) _cell_length_c 18.5297(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4150.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8115 _exptl_absorpt_correction_T_max 0.8115 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13087 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1894 _reflns_number_gt 1744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _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 ? _computing_publication_material ? _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 on the water oxygens for compounds 1 and 3 were located from the difference Fourier map and then refined considering their chemical environments with restraints [O?H = 0.85(2) ?], with U(H) fixed at 0.08 ?2 ; _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^)+(0.0640P)^2^+29.6075P] 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 1894 _refine_ls_number_parameters 147 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.065 _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 Cd Cd 0.0000 0.0000 1.0000 0.0158(2) Uani 1 4 d S . . Cl Cl 0.5000 0.14512(16) 0.7500 0.0540(5) Uani 1 2 d S . . O1 O -0.0795(3) 0.1288(3) 1.0000 0.077(2) Uani 1 2 d SD . . H1A H -0.0587 0.1464 1.0355 0.080 Uiso 1 1 d RD . . O2 O 0.1670(2) 0.1787(3) 0.65294(18) 0.0722(15) Uani 1 1 d . . . O3 O 0.0495(4) 0.2746(4) 0.5587(3) 0.0339(13) Uani 0.50 1 d PD . . H301 H -0.0011 0.2869 0.5788 0.080 Uiso 0.50 1 d PRD . . H302 H 0.0959 0.2658 0.5862 0.080 Uiso 0.50 1 d PRD . . O4 O 0.0916(7) 0.4385(6) 0.5000 0.104(2) Uani 1 2 d SD . . H401 H 0.061(4) 0.461(4) 0.538(3) 0.080 Uiso 1 1 d D . . O5 O 0.0000 0.5000 0.6290(3) 0.0688(18) Uani 1 2 d SD . . H501 H 0.006(5) 0.546(3) 0.652(4) 0.080 Uiso 1 1 d D . . N1 N 0.0990(2) 0.0439(2) 0.90583(17) 0.0303(8) Uani 1 1 d . . . N2 N 0.2721(2) 0.1356(3) 0.7396(2) 0.0552(14) Uani 1 1 d . . . H2A H 0.3312 0.1324 0.7493 0.066 Uiso 1 1 calc R . . N3 N 0.3244(2) 0.1916(3) 0.6340(2) 0.0441(10) Uani 1 1 d . . . H3 H 0.3795 0.1779 0.6494 0.053 Uiso 1 1 calc R . . C1 C 0.0632(3) 0.0905(3) 0.8518(2) 0.0317(9) Uani 1 1 d . . . H1 H -0.0010 0.1022 0.8528 0.038 Uiso 1 1 calc R . . C2 C 0.1151(3) 0.1223(3) 0.7947(2) 0.0378(11) Uani 1 1 d . . . H2 H 0.0862 0.1541 0.7586 0.045 Uiso 1 1 calc R . . C3 C 0.2113(3) 0.1059(4) 0.7923(2) 0.0452(13) Uani 1 1 d . . . C4 C 0.2494(3) 0.0578(4) 0.8483(2) 0.0494(14) Uani 1 1 d . . . H4 H 0.3135 0.0460 0.8491 0.059 Uiso 1 1 calc R . . C5 C 0.1917(3) 0.0277(3) 0.9024(2) 0.0403(11) Uani 1 1 d . . . H5 H 0.2185 -0.0056 0.9384 0.048 Uiso 1 1 calc R . . C6 C 0.2488(3) 0.1699(4) 0.6734(2) 0.0522(15) Uani 1 1 d . . . C7 C 0.3163(3) 0.2372(3) 0.56619(19) 0.0290(9) Uani 1 1 d . . . H7A H 0.3675 0.2777 0.5631 0.035 Uiso 1 1 calc R . . H7B H 0.2578 0.2690 0.5665 0.035 Uiso 1 1 calc R . . C8 C 0.3183(4) 0.1822(3) 0.5000 0.0295(12) Uani 1 2 d S . . H8A H 0.2642 0.1446 0.5000 0.035 Uiso 1 2 calc SR . . H8B H 0.3749 0.1478 0.5000 0.035 Uiso 1 2 calc SR . . 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 Cd 0.0148(3) 0.0199(3) 0.0129(3) 0.000 0.000 -0.00194(18) Cl 0.0181(7) 0.1051(16) 0.0387(9) 0.000 -0.0041(6) 0.000 O1 0.033(3) 0.032(3) 0.167(7) 0.000 0.000 0.010(2) O2 0.0196(15) 0.158(4) 0.0391(19) 0.060(2) -0.0045(14) -0.003(2) O3 0.033(3) 0.036(3) 0.033(3) -0.003(2) -0.010(2) 0.003(2) O4 0.123(7) 0.088(6) 0.101(7) 0.000 0.000 0.013(5) O5 0.056(3) 0.113(6) 0.038(3) 0.000 0.000 -0.015(4) N1 0.0203(15) 0.047(2) 0.0232(16) 0.0120(15) -0.0032(13) -0.0098(15) N2 0.0139(17) 0.115(4) 0.037(2) 0.049(2) -0.0063(14) -0.012(2) N3 0.0200(17) 0.076(3) 0.036(2) 0.035(2) 0.0000(15) -0.0029(17) C1 0.0171(17) 0.050(3) 0.028(2) 0.0124(19) -0.0042(16) -0.0081(17) C2 0.0203(19) 0.064(3) 0.029(2) 0.024(2) -0.0069(16) -0.0088(19) C3 0.020(2) 0.086(4) 0.029(2) 0.032(2) -0.0066(17) -0.016(2) C4 0.0172(19) 0.096(4) 0.035(2) 0.035(3) -0.0039(17) -0.007(2) C5 0.023(2) 0.069(3) 0.029(2) 0.028(2) -0.0038(17) -0.004(2) C6 0.023(2) 0.099(4) 0.035(2) 0.041(3) -0.0038(19) -0.009(2) C7 0.032(2) 0.036(2) 0.0190(19) 0.0099(16) 0.0048(15) -0.0010(17) C8 0.025(3) 0.020(3) 0.044(3) 0.000 0.000 -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 Cd O1 2.325(5) . ? Cd O1 2.325(5) 9_557 ? Cd N1 2.345(3) 2 ? Cd N1 2.345(3) 10_557 ? Cd N1 2.345(3) . ? Cd N1 2.345(3) 9_557 ? O1 H1A 0.7717 . ? O2 C6 1.231(5) . ? O3 H301 0.8318 . ? O3 H302 0.8439 . ? O4 H401 0.90(2) . ? O5 H501 0.85(2) . ? N1 C5 1.342(5) . ? N1 C1 1.343(5) . ? N2 C6 1.380(5) . ? N2 C3 1.386(5) . ? N2 H2A 0.8600 . ? N3 C6 1.342(5) . ? N3 C7 1.453(5) . ? N3 H3 0.8600 . ? C1 C2 1.383(5) . ? C1 H1 0.9300 . ? C2 C3 1.391(6) . ? C2 H2 0.9300 . ? C3 C4 1.394(6) . ? C4 C5 1.378(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.503(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C7 1.503(5) 10_556 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 O1 Cd O1 180.000(1) . 9_557 ? O1 Cd N1 88.12(12) . 2 ? O1 Cd N1 91.88(12) 9_557 2 ? O1 Cd N1 91.88(12) . 10_557 ? O1 Cd N1 88.12(12) 9_557 10_557 ? N1 Cd N1 180.000(1) 2 10_557 ? O1 Cd N1 91.88(12) . . ? O1 Cd N1 88.12(12) 9_557 . ? N1 Cd N1 83.83(15) 2 . ? N1 Cd N1 96.17(16) 10_557 . ? O1 Cd N1 88.12(12) . 9_557 ? O1 Cd N1 91.88(12) 9_557 9_557 ? N1 Cd N1 96.17(15) 2 9_557 ? N1 Cd N1 83.83(15) 10_557 9_557 ? N1 Cd N1 180.000(1) . 9_557 ? Cd O1 H1A 97.4 . . ? H301 O3 H302 116.3 . . ? C5 N1 C1 116.1(3) . . ? C5 N1 Cd 124.5(3) . . ? C1 N1 Cd 119.4(2) . . ? C6 N2 C3 127.6(4) . . ? C6 N2 H2A 116.2 . . ? C3 N2 H2A 116.2 . . ? C6 N3 C7 122.3(4) . . ? C6 N3 H3 118.8 . . ? C7 N3 H3 118.8 . . ? N1 C1 C2 124.6(4) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 118.6(4) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? N2 C3 C2 124.8(4) . . ? N2 C3 C4 117.9(4) . . ? C2 C3 C4 117.3(4) . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.5(4) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? O2 C6 N3 123.9(4) . . ? O2 C6 N2 123.0(4) . . ? N3 C6 N2 113.1(4) . . ? N3 C7 C8 114.7(4) . . ? N3 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N3 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C7 109.4(4) . 10_556 ? C7 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 10_556 . ? C7 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 10_556 . ? H8A C8 H8B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd N1 C5 139.3(4) . . . . ? O1 Cd N1 C5 -40.7(4) 9_557 . . . ? N1 Cd N1 C5 -132.8(4) 2 . . . ? N1 Cd N1 C5 47.2(4) 10_557 . . . ? N1 Cd N1 C5 40(66) 9_557 . . . ? O1 Cd N1 C1 -38.8(3) . . . . ? O1 Cd N1 C1 141.2(3) 9_557 . . . ? N1 Cd N1 C1 49.1(3) 2 . . . ? N1 Cd N1 C1 -130.9(3) 10_557 . . . ? N1 Cd N1 C1 -138(66) 9_557 . . . ? C5 N1 C1 C2 -0.5(7) . . . . ? Cd N1 C1 C2 177.8(4) . . . . ? N1 C1 C2 C3 -0.3(8) . . . . ? C6 N2 C3 C2 -15.1(10) . . . . ? C6 N2 C3 C4 166.7(6) . . . . ? C1 C2 C3 N2 -178.1(5) . . . . ? C1 C2 C3 C4 0.1(8) . . . . ? N2 C3 C4 C5 179.2(5) . . . . ? C2 C3 C4 C5 0.9(9) . . . . ? C1 N1 C5 C4 1.5(7) . . . . ? Cd N1 C5 C4 -176.6(4) . . . . ? C3 C4 C5 N1 -1.8(9) . . . . ? C7 N3 C6 O2 7.6(10) . . . . ? C7 N3 C6 N2 -173.1(5) . . . . ? C3 N2 C6 O2 0.4(11) . . . . ? C3 N2 C6 N3 -178.9(6) . . . . ? C6 N3 C7 C8 -96.7(6) . . . . ? N3 C7 C8 C7 -176.1(3) . . . 10_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O3 0.77 2.07 2.581(7) 123.5 16 O5 H501 Cl 0.85(2) 2.40(3) 3.205(5) 160(7) 14_456 O4 H401 O5 0.90(2) 1.99(2) 2.889(7) 174(7) . O3 H302 O2 0.84 2.11 2.849(6) 146.8 . N3 H3 Cl 0.86 2.58 3.373(4) 153.1 . N2 H2A Cl 0.86 2.40 3.245(3) 165.7 . C2 H2 O2 0.93 2.30 2.870(5) 118.9 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.414 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.097 ###################################### data_CdL2(NO3)2 _database_code_depnum_ccdc_archive 'CCDC 739486' #TrackingRef '1D_interpenetration.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 Cd N14 O12' _chemical_formula_weight 901.16 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 14.2829(14) _cell_length_b 15.3547(15) _cell_length_c 18.6193(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4083.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8578 _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14027 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0293 _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 -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2073 _reflns_number_gt 1774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _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 ? _computing_publication_material ? _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^)+(0.0406P)^2^+13.6222P] 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 2073 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Cd1 Cd 0.0000 0.0000 0.0000 0.03663(18) Uani 1 4 d S . . O1 O -0.0771(2) 0.1350(2) 0.0000 0.0405(8) Uani 1 2 d S . . H101 H -0.0744 0.1599 0.0473 0.049 Uiso 1 1 d R . . O2 O 0.16682(18) 0.18804(16) 0.34304(14) 0.0425(6) Uani 1 1 d . . . O3 O 0.4268(3) 0.0434(3) 0.2554(3) 0.0408(19) Uani 0.500(10) 1 d P . . O4 O 0.5000 0.0824(5) 0.2500 0.0437(16) Uani 0.50 2 d SP . . O5 O 0.5063(4) 1.0306(3) 0.4372(3) 0.0471(13) Uani 0.50 1 d P . . O6 O 0.4499(5) 0.9416(5) 0.5000 0.0433(17) Uani 0.50 2 d SP . . N1 N 0.0980(2) 0.04612(19) 0.09337(16) 0.0397(7) Uani 1 1 d . . . N2 N 0.2693(2) 0.1338(2) 0.26180(16) 0.0432(8) Uani 1 1 d . . . H2A H 0.3297 0.1274 0.2540 0.052 Uiso 1 1 calc R . . N3 N 0.3259(2) 0.18421(19) 0.36742(16) 0.0415(7) Uani 1 1 d . . . H3 H 0.3803 0.1627 0.3542 0.050 Uiso 1 1 calc R . . N4 N 0.5000 0.0000 0.2500 0.0464(15) Uani 1 4 d S . . N5 N 0.5000 1.0000 0.5000 0.0454(15) Uani 1 4 d S . . C1 C 0.0587(2) 0.0960(2) 0.14758(18) 0.0314(7) Uani 1 1 d . . . H1 H -0.0059 0.1106 0.1457 0.038 Uiso 1 1 calc R . . C2 C 0.1133(2) 0.1246(2) 0.2047(2) 0.0399(8) Uani 1 1 d . . . H2 H 0.0861 0.1580 0.2422 0.048 Uiso 1 1 calc R . . C3 C 0.2083(3) 0.1038(2) 0.2065(2) 0.0418(9) Uani 1 1 d . . . C4 C 0.2473(2) 0.0549(2) 0.15250(18) 0.0323(7) Uani 1 1 d . . . H4 H 0.3121 0.0411 0.1540 0.039 Uiso 1 1 calc R . . C5 C 0.1929(2) 0.0256(2) 0.0958(2) 0.0369(8) Uani 1 1 d . . . H5 H 0.2203 -0.0084 0.0587 0.044 Uiso 1 1 calc R . . C6 C 0.2448(3) 0.1714(2) 0.32549(19) 0.0362(8) Uani 1 1 d . . . C7 C 0.3162(3) 0.2351(2) 0.4346(2) 0.0411(8) Uani 1 1 d . . . H7A H 0.2576 0.2695 0.4329 0.049 Uiso 1 1 calc R . . H7B H 0.3693 0.2763 0.4388 0.049 Uiso 1 1 calc R . . C8 C 0.3146(3) 0.1757(3) 0.5000 0.0370(11) Uani 1 2 d S . . H8A H 0.2573 0.1394 0.5000 0.044 Uiso 1 2 calc SR . . H8B H 0.3698 0.1367 0.5000 0.044 Uiso 1 2 calc SR . . 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 Cd1 0.0368(3) 0.0382(3) 0.0349(3) 0.000 0.000 -0.0001(2) O1 0.0333(18) 0.049(2) 0.039(2) 0.000 0.000 0.0130(15) O2 0.0449(15) 0.0446(14) 0.0380(14) -0.0103(12) -0.0091(11) -0.0071(12) O3 0.041(3) 0.043(3) 0.039(3) -0.008(2) -0.008(2) 0.011(2) O4 0.038(4) 0.045(4) 0.048(4) 0.000 0.001(4) 0.000 O5 0.047(3) 0.048(3) 0.046(3) -0.007(2) -0.002(3) -0.011(3) O6 0.040(4) 0.038(4) 0.052(5) 0.000 0.000 -0.007(4) N1 0.0387(15) 0.0422(16) 0.0382(17) -0.0064(13) 0.0060(13) -0.0075(13) N2 0.0409(17) 0.0488(17) 0.0399(19) 0.0015(14) -0.0096(13) -0.0121(14) N3 0.0466(17) 0.0413(16) 0.0367(17) 0.0021(13) -0.0132(14) -0.0169(14) N4 0.041(4) 0.048(4) 0.050(4) 0.000 0.000 0.000 N5 0.043(3) 0.051(4) 0.042(4) 0.000 0.000 -0.017(3) C1 0.0267(15) 0.0322(16) 0.0354(19) 0.0026(14) -0.0040(14) -0.0120(13) C2 0.0378(19) 0.0444(19) 0.037(2) -0.0087(16) 0.0038(16) -0.0127(16) C3 0.0415(19) 0.044(2) 0.040(2) 0.0035(17) -0.0033(17) -0.0163(16) C4 0.0301(15) 0.0306(15) 0.0362(18) 0.0047(14) -0.0029(15) -0.0099(13) C5 0.0379(18) 0.0374(18) 0.0354(19) -0.0077(15) 0.0010(15) -0.0131(14) C6 0.0433(19) 0.0286(16) 0.0366(19) 0.0047(14) -0.0182(17) -0.0130(15) C7 0.0444(19) 0.0374(18) 0.041(2) -0.0032(16) -0.0181(17) -0.0132(16) C8 0.031(2) 0.035(2) 0.045(3) 0.000 0.000 -0.011(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 Cd1 N1 2.342(3) 9 ? Cd1 N1 2.342(3) . ? Cd1 N1 2.342(3) 2 ? Cd1 N1 2.342(3) 10 ? Cd1 O1 2.348(3) . ? Cd1 O1 2.348(3) 9 ? O1 H101 0.9601 . ? O2 C6 1.189(4) . ? O3 O4 1.209(6) . ? O3 N4 1.244(5) . ? O3 O3 1.348(10) 8_445 ? O4 O3 1.209(6) 7_545 ? O4 N4 1.265(7) . ? O5 O5 0.956(9) 2_675 ? O5 N5 1.263(5) . ? O5 O6 1.393(6) 9_676 ? O6 N5 1.148(7) . ? O6 O5 1.393(6) 9_676 ? O6 O5 1.393(6) 2_675 ? N1 C1 1.386(4) . ? N1 C5 1.392(5) . ? N2 C6 1.365(5) . ? N2 C3 1.425(5) . ? N2 H2A 0.8800 . ? N3 C6 1.410(4) . ? N3 C7 1.482(5) . ? N3 H3 0.8800 . ? N4 O3 1.244(5) 8_445 ? N4 O3 1.244(5) 7_545 ? N4 O3 1.244(5) 2_655 ? N4 O4 1.265(7) 2_655 ? N5 O6 1.148(7) 9_676 ? N5 O5 1.263(5) 10_556 ? N5 O5 1.263(5) 2_675 ? N5 O5 1.263(5) 9_676 ? C1 C2 1.391(5) . ? C1 H1 0.9500 . ? C2 C3 1.394(5) . ? C2 H2 0.9500 . ? C3 C4 1.374(5) . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 C8 1.522(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C7 1.522(5) 10_556 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? 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 Cd1 N1 180.0(2) 9 . ? N1 Cd1 N1 95.86(14) 9 2 ? N1 Cd1 N1 84.14(14) . 2 ? N1 Cd1 N1 84.14(14) 9 10 ? N1 Cd1 N1 95.86(14) . 10 ? N1 Cd1 N1 180.0(2) 2 10 ? N1 Cd1 O1 89.23(9) 9 . ? N1 Cd1 O1 90.77(9) . . ? N1 Cd1 O1 89.23(9) 2 . ? N1 Cd1 O1 90.77(9) 10 . ? N1 Cd1 O1 90.77(9) 9 9 ? N1 Cd1 O1 89.23(9) . 9 ? N1 Cd1 O1 90.77(9) 2 9 ? N1 Cd1 O1 89.23(9) 10 9 ? O1 Cd1 O1 180.00(15) . 9 ? Cd1 O1 H101 109.4 . . ? O4 O3 N4 62.1(4) . . ? O4 O3 O3 118.5(4) . 8_445 ? N4 O3 O3 57.2(2) . 8_445 ? O3 O4 O3 120.6(7) 7_545 . ? O3 O4 N4 60.3(4) 7_545 . ? O3 O4 N4 60.3(4) . . ? O5 O5 N5 67.7(2) 2_675 . ? O5 O5 O6 112.7(5) 2_675 9_676 ? N5 O5 O6 50.9(3) . 9_676 ? N5 O6 O5 58.7(3) . 9_676 ? N5 O6 O5 58.7(3) . 2_675 ? O5 O6 O5 114.1(7) 9_676 2_675 ? C1 N1 C5 119.8(3) . . ? C1 N1 Cd1 117.7(2) . . ? C5 N1 Cd1 122.5(2) . . ? C6 N2 C3 127.4(3) . . ? C6 N2 H2A 116.3 . . ? C3 N2 H2A 116.3 . . ? C6 N3 C7 117.7(3) . . ? C6 N3 H3 121.1 . . ? C7 N3 H3 121.1 . . ? O3 N4 O3 170.6(5) 8_445 7_545 ? O3 N4 O3 115.2(5) 8_445 2_655 ? O3 N4 O3 65.6(5) 7_545 2_655 ? O3 N4 O3 65.6(5) 8_445 . ? O3 N4 O3 115.2(5) 7_545 . ? O3 N4 O3 170.6(5) 2_655 . ? O3 N4 O4 57.6(2) 8_445 2_655 ? O3 N4 O4 122.4(2) 7_545 2_655 ? O3 N4 O4 57.6(2) 2_655 2_655 ? O3 N4 O4 122.4(2) . 2_655 ? O3 N4 O4 122.4(2) 8_445 . ? O3 N4 O4 57.6(2) 7_545 . ? O3 N4 O4 122.4(2) 2_655 . ? O3 N4 O4 57.6(2) . . ? O4 N4 O4 180.0 2_655 . ? O6 N5 O6 180.000(2) 9_676 . ? O6 N5 O5 70.4(2) 9_676 10_556 ? O6 N5 O5 109.6(2) . 10_556 ? O6 N5 O5 109.6(2) 9_676 2_675 ? O6 N5 O5 70.4(2) . 2_675 ? O5 N5 O5 180.000(2) 10_556 2_675 ? O6 N5 O5 70.4(2) 9_676 . ? O6 N5 O5 109.6(2) . . ? O5 N5 O5 135.5(4) 10_556 . ? O5 N5 O5 44.5(4) 2_675 . ? O6 N5 O5 109.6(2) 9_676 9_676 ? O6 N5 O5 70.4(2) . 9_676 ? O5 N5 O5 44.5(4) 10_556 9_676 ? O5 N5 O5 135.5(4) 2_675 9_676 ? O5 N5 O5 180.000(2) . 9_676 ? N1 C1 C2 120.3(3) . . ? N1 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? C1 C2 C3 119.5(3) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 N2 117.2(3) . . ? C2 C3 N2 122.6(4) . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 N1 119.8(3) . . ? C4 C5 H5 120.1 . . ? N1 C5 H5 120.1 . . ? O2 C6 N2 124.7(3) . . ? O2 C6 N3 126.0(3) . . ? N2 C6 N3 109.3(3) . . ? N3 C7 C8 111.1(3) . . ? N3 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N3 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C7 106.2(4) 10_556 . ? C7 C8 H8A 110.5 10_556 . ? C7 C8 H8A 110.5 . . ? C7 C8 H8B 110.5 10_556 . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 O3 O4 O3 0.0 . . . 7_545 ? O3 O3 O4 O3 -9.8(5) 8_445 . . 7_545 ? O3 O3 O4 N4 -9.8(5) 8_445 . . . ? N1 Cd1 N1 C1 164.5(2) 9 . . . ? N1 Cd1 N1 C1 -49.8(2) 2 . . . ? N1 Cd1 N1 C1 130.2(2) 10 . . . ? O1 Cd1 N1 C1 39.4(2) . . . . ? O1 Cd1 N1 C1 -140.6(2) 9 . . . ? N1 Cd1 N1 C5 -15.3(3) 9 . . . ? N1 Cd1 N1 C5 130.5(3) 2 . . . ? N1 Cd1 N1 C5 -49.5(3) 10 . . . ? O1 Cd1 N1 C5 -140.4(3) . . . . ? O1 Cd1 N1 C5 39.6(3) 9 . . . ? O4 O3 N4 O3 -169.7(5) . . . 8_445 ? O4 O3 N4 O3 0.0 . . . 7_545 ? O3 O3 N4 O3 169.7(5) 8_445 . . 7_545 ? O4 O3 N4 O3 92.98(15) . . . 2_655 ? O3 O3 N4 O3 -97.3(4) 8_445 . . 2_655 ? O4 O3 N4 O4 180.0 . . . 2_655 ? O3 O3 N4 O4 -10.3(5) 8_445 . . 2_655 ? O3 O3 N4 O4 169.7(5) 8_445 . . . ? O3 O4 N4 O3 -168.9(6) 7_545 . . 8_445 ? O3 O4 N4 O3 11.1(6) . . . 8_445 ? O3 O4 N4 O3 180.0 . . . 7_545 ? O3 O4 N4 O3 11.1(6) 7_545 . . 2_655 ? O3 O4 N4 O3 -168.9(6) . . . 2_655 ? O3 O4 N4 O3 180.0 7_545 . . . ? O3 O4 N4 O4 -174(100) 7_545 . . 2_655 ? O3 O4 N4 O4 6(100) . . . 2_655 ? O5 O6 N5 O6 -100.8(3) 9_676 . . 9_676 ? O5 O6 N5 O6 100.8(3) 2_675 . . 9_676 ? O5 O6 N5 O5 -21.6(6) 9_676 . . 10_556 ? O5 O6 N5 O5 180.000(2) 2_675 . . 10_556 ? O5 O6 N5 O5 158.4(6) 9_676 . . 2_675 ? O5 O6 N5 O5 180.000(2) 9_676 . . . ? O5 O6 N5 O5 21.6(6) 2_675 . . . ? O5 O6 N5 O5 -158.4(6) 2_675 . . 9_676 ? O5 O5 N5 O6 150.4(8) 2_675 . . 9_676 ? O5 O5 N5 O6 -29.6(8) 2_675 . . . ? O6 O5 N5 O6 180.000(2) 9_676 . . . ? O5 O5 N5 O5 180.000(5) 2_675 . . 10_556 ? O6 O5 N5 O5 29.6(8) 9_676 . . 10_556 ? O6 O5 N5 O5 -150.4(8) 9_676 . . 2_675 ? O5 O5 N5 O5 -80(100) 2_675 . . 9_676 ? O6 O5 N5 O5 129.7(10) 9_676 . . 9_676 ? C5 N1 C1 C2 -0.8(5) . . . . ? Cd1 N1 C1 C2 179.5(2) . . . . ? N1 C1 C2 C3 0.9(5) . . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? C1 C2 C3 N2 177.4(3) . . . . ? C6 N2 C3 C4 -169.3(3) . . . . ? C6 N2 C3 C2 12.8(6) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? N2 C3 C4 C5 -178.1(3) . . . . ? C3 C4 C5 N1 0.3(5) . . . . ? C1 N1 C5 C4 0.2(5) . . . . ? Cd1 N1 C5 C4 179.9(2) . . . . ? C3 N2 C6 O2 -3.2(6) . . . . ? C3 N2 C6 N3 174.7(3) . . . . ? C7 N3 C6 O2 -10.2(5) . . . . ? C7 N3 C6 N2 171.9(3) . . . . ? C6 N3 C7 C8 102.5(4) . . . . ? N3 C7 C8 C7 173.5(2) . . . 10_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O3 0.88 1.89 2.646(6) 142.4 . N2 H2A O4 0.88 2.53 3.395(4) 167.9 . C2 H2 O2 0.95 2.25 2.858(4) 121.0 . C4 H4 O3 0.95 2.50 3.206(6) 131.1 . C7 H7A O2 0.99 2.46 2.826(4) 101.3 . O1 H101 O2 0.96 2.47 3.293(3) 143.7 7_445 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.423 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.072 #################### data_CoL2Cl2 _database_code_depnum_ccdc_archive 'CCDC 739487' #TrackingRef '1D_interpenetration.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 Cl2 Co N12 O12' _chemical_formula_weight 902.67 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 14.128(8) _cell_length_b 16.005(10) _cell_length_c 18.140(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4102(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8260 _exptl_absorpt_correction_T_max 0.8453 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12853 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.73 _reflns_number_total 1830 _reflns_number_gt 1388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _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 ? _computing_publication_material ? _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 on the water oxygens for compounds 1 and 3 were located from the difference Fourier map and then refined considering their chemical environments with restraints [O?H = 0.85(2) ?], with U(H) fixed at 0.08 ?2 ; _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^)+(0.0919P)^2^+17.4993P] 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 1830 _refine_ls_number_parameters 147 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1941 _refine_ls_wR_factor_gt 0.1779 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.0000 0.0000 1.0000 0.0273(4) Uani 1 4 d S . . Cl Cl 0.5000 0.1435(2) 0.7500 0.0894(9) Uani 1 2 d S . . O1 O -0.0754(3) 0.1156(3) 1.0000 0.0597(15) Uani 1 2 d SD . . H1A H -0.0679 0.1365 1.0409 0.080 Uiso 1 1 d RD . . O2 O 0.1652(3) 0.1730(4) 0.6522(3) 0.0975(19) Uani 1 1 d . . . O3 O 0.0518(7) 0.2656(6) 0.5565(5) 0.087(3) Uani 0.50 1 d PD . . H301 H 0.0012 0.2778 0.5766 0.080 Uiso 0.50 1 d PRD . . H302 H 0.0982 0.2567 0.5839 0.080 Uiso 0.50 1 d PRD . . O4 O 0.0880(14) 0.4286(10) 0.5000 0.195(6) Uani 1 2 d SD . . H401 H 0.070(4) 0.445(4) 0.545(2) 0.080 Uiso 1 1 d D . . O5 O 0.0000 0.5000 0.6273(5) 0.124(3) Uani 1 2 d SD . . H501 H 0.004(6) 0.545(3) 0.654(4) 0.080 Uiso 1 1 d D . . N1 N 0.0931(2) 0.0426(3) 0.9110(2) 0.0397(10) Uani 1 1 d . . . N2 N 0.2698(3) 0.1326(4) 0.7420(3) 0.0698(16) Uani 1 1 d . . . H2A H 0.3292 0.1286 0.7518 0.084 Uiso 1 1 calc R . . N3 N 0.3222(3) 0.1920(3) 0.6360(3) 0.0637(14) Uani 1 1 d . . . H3 H 0.3777 0.1808 0.6527 0.076 Uiso 1 1 calc R . . C1 C 0.0588(3) 0.0902(3) 0.8556(3) 0.0434(12) Uani 1 1 d . . . H1 H -0.0054 0.1030 0.8563 0.052 Uiso 1 1 calc R . . C2 C 0.1116(3) 0.1208(3) 0.7988(3) 0.0489(14) Uani 1 1 d . . . H2 H 0.0835 0.1533 0.7624 0.059 Uiso 1 1 calc R . . C3 C 0.2078(3) 0.1029(4) 0.7958(3) 0.0558(15) Uani 1 1 d . . . C4 C 0.2442(4) 0.0545(4) 0.8517(3) 0.0666(18) Uani 1 1 d . . . H4 H 0.3085 0.0420 0.8526 0.080 Uiso 1 1 calc R . . C5 C 0.1861(3) 0.0248(4) 0.9061(3) 0.0574(16) Uani 1 1 d . . . H5 H 0.2124 -0.0098 0.9419 0.069 Uiso 1 1 calc R . . C6 C 0.2466(4) 0.1675(4) 0.6752(3) 0.0667(18) Uani 1 1 d . . . C7 C 0.3143(4) 0.2365(3) 0.5667(3) 0.0541(14) Uani 1 1 d . . . H7A H 0.3648 0.2775 0.5641 0.065 Uiso 1 1 calc R . . H7B H 0.2547 0.2665 0.5662 0.065 Uiso 1 1 calc R . . C8 C 0.3191(5) 0.1829(5) 0.5000 0.0502(18) Uani 1 2 d S . . H8A H 0.2667 0.1437 0.5000 0.060 Uiso 1 2 calc SR . . H8B H 0.3777 0.1513 0.5000 0.060 Uiso 1 2 calc SR . . 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 Co 0.0219(6) 0.0361(6) 0.0240(6) 0.000 0.000 -0.0021(5) Cl 0.0420(11) 0.145(2) 0.0809(17) 0.000 -0.0081(12) 0.000 O1 0.042(3) 0.049(3) 0.088(4) 0.000 0.000 0.007(2) O2 0.041(2) 0.183(5) 0.068(3) 0.073(3) 0.000(2) -0.002(3) O3 0.082(6) 0.101(7) 0.078(7) -0.009(6) -0.004(5) 0.016(5) O4 0.271(16) 0.209(13) 0.105(9) 0.000 0.000 0.045(12) O5 0.140(8) 0.157(9) 0.076(6) 0.000 0.000 0.001(8) N1 0.0264(18) 0.058(2) 0.034(2) 0.011(2) 0.0008(17) -0.0054(18) N2 0.030(2) 0.129(4) 0.050(3) 0.044(3) 0.002(2) -0.011(3) N3 0.045(3) 0.098(4) 0.049(3) 0.027(3) 0.005(2) -0.012(2) C1 0.027(2) 0.063(3) 0.040(3) 0.013(2) -0.001(2) -0.006(2) C2 0.031(3) 0.074(4) 0.042(3) 0.022(3) -0.010(2) -0.007(2) C3 0.034(3) 0.090(4) 0.043(3) 0.026(3) -0.001(2) -0.011(3) C4 0.027(2) 0.118(5) 0.055(4) 0.036(4) 0.001(3) 0.001(3) C5 0.033(3) 0.091(4) 0.049(3) 0.034(3) -0.002(2) 0.002(3) C6 0.043(3) 0.107(5) 0.050(3) 0.035(3) 0.002(3) -0.014(3) C7 0.066(3) 0.060(3) 0.036(3) 0.011(3) 0.008(3) -0.011(3) C8 0.048(4) 0.045(4) 0.058(5) 0.000 0.000 -0.011(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 Co O1 2.135(5) . ? Co O1 2.135(5) 9_557 ? Co N1 2.191(4) 2 ? Co N1 2.191(4) 10_557 ? Co N1 2.191(4) 9_557 ? Co N1 2.191(4) . ? O1 H1A 0.8210 . ? O2 C6 1.226(7) . ? O3 H301 0.8260 . ? O3 H302 0.8354 . ? O4 H401 0.891(17) . ? O5 H501 0.87(2) . ? N1 C5 1.348(6) . ? N1 C1 1.351(6) . ? N2 C6 1.374(7) . ? N2 C3 1.393(6) . ? N2 H2A 0.8600 . ? N3 C6 1.342(7) . ? N3 C7 1.448(6) . ? N3 H3 0.8600 . ? C1 C2 1.363(7) . ? C1 H1 0.9300 . ? C2 C3 1.391(7) . ? C2 H2 0.9300 . ? C3 C4 1.376(7) . ? C4 C5 1.369(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.485(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C7 1.485(7) 10_556 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 O1 Co O1 180.000(1) . 9_557 ? O1 Co N1 88.28(14) . 2 ? O1 Co N1 91.72(14) 9_557 2 ? O1 Co N1 91.72(14) . 10_557 ? O1 Co N1 88.28(14) 9_557 10_557 ? N1 Co N1 180.000(1) 2 10_557 ? O1 Co N1 88.28(14) . 9_557 ? O1 Co N1 91.72(14) 9_557 9_557 ? N1 Co N1 94.9(2) 2 9_557 ? N1 Co N1 85.1(2) 10_557 9_557 ? O1 Co N1 91.72(14) . . ? O1 Co N1 88.28(14) 9_557 . ? N1 Co N1 85.1(2) 2 . ? N1 Co N1 94.9(2) 10_557 . ? N1 Co N1 180.000(1) 9_557 . ? Co O1 H1A 106.8 . . ? H301 O3 H302 117.1 . . ? C5 N1 C1 114.9(4) . . ? C5 N1 Co 124.6(3) . . ? C1 N1 Co 120.5(3) . . ? C6 N2 C3 127.3(5) . . ? C6 N2 H2A 116.4 . . ? C3 N2 H2A 116.4 . . ? C6 N3 C7 122.9(5) . . ? C6 N3 H3 118.6 . . ? C7 N3 H3 118.6 . . ? N1 C1 C2 124.6(4) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 119.5(5) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 116.8(5) . . ? C4 C3 N2 118.2(5) . . ? C2 C3 N2 124.9(5) . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 124.0(5) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? O2 C6 N3 123.0(5) . . ? O2 C6 N2 123.6(5) . . ? N3 C6 N2 113.4(5) . . ? N3 C7 C8 114.8(5) . . ? N3 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N3 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? C7 C8 C7 109.2(6) . 10_556 ? C7 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 10_556 . ? C7 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 10_556 . ? H8A C8 H8B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co N1 C5 142.6(5) . . . . ? O1 Co N1 C5 -37.4(5) 9_557 . . . ? N1 Co N1 C5 -129.3(5) 2 . . . ? N1 Co N1 C5 50.7(5) 10_557 . . . ? N1 Co N1 C5 15.6(5) 9_557 . . . ? O1 Co N1 C1 -37.5(4) . . . . ? O1 Co N1 C1 142.5(4) 9_557 . . . ? N1 Co N1 C1 50.6(3) 2 . . . ? N1 Co N1 C1 -129.4(3) 10_557 . . . ? N1 Co N1 C1 -164.6(5) 9_557 . . . ? C5 N1 C1 C2 -1.3(8) . . . . ? Co N1 C1 C2 178.8(4) . . . . ? N1 C1 C2 C3 0.1(9) . . . . ? C1 C2 C3 C4 -0.1(9) . . . . ? C1 C2 C3 N2 -177.8(6) . . . . ? C6 N2 C3 C4 166.5(7) . . . . ? C6 N2 C3 C2 -15.8(11) . . . . ? C2 C3 C4 C5 1.4(10) . . . . ? N2 C3 C4 C5 179.3(6) . . . . ? C1 N1 C5 C4 2.7(9) . . . . ? Co N1 C5 C4 -177.4(5) . . . . ? C3 C4 C5 N1 -2.9(11) . . . . ? C7 N3 C6 O2 7.7(11) . . . . ? C7 N3 C6 N2 -174.8(6) . . . . ? C3 N2 C6 O2 -4.1(12) . . . . ? C3 N2 C6 N3 178.5(6) . . . . ? C6 N3 C7 C8 -95.4(8) . . . . ? N3 C7 C8 C7 -177.6(4) . . . 10_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O3 0.82 2.10 2.631(10) 122.5 16 O5 H501 Cl 0.87(2) 2.35(3) 3.198(7) 165(7) 14_456 O4 H401 O5 0.891(17) 1.997(17) 2.861(13) 163(6) . O3 H302 O2 0.84 2.06 2.789(10) 146.3 . N3 H3 Cl 0.86 2.54 3.346(5) 156.1 . N2 H2A Cl 0.86 2.43 3.261(5) 164.0 . C2 H2 O2 0.93 2.33 2.889(7) 118.2 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.495 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.087 ################################## data_CoL2SO4 _database_code_depnum_ccdc_archive 'CCDC 739488' #TrackingRef '1D_interpenetration.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 Co N12 O16 S' _chemical_formula_weight 927.83 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' S S 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.53(4) _cell_length_b 18.26(4) _cell_length_c 21.45(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.11(3) _cell_angle_gamma 90.00 _cell_volume 8389(29) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3896 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8545 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18137 _diffrn_reflns_av_R_equivalents 0.1341 _diffrn_reflns_av_sigmaI/netI 0.1619 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 23.52 _reflns_number_total 6112 _reflns_number_gt 2828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _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 ? _computing_publication_material ? _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. For the compound {[CoL2(H2O)2]SO4?8H2O}n (4), the sulfate anions are severely disordered with solvent water molecules. Increasing the exposure time of the crystal to X-rays at 173K did not ameliorate the quality of data in this case. Repeated measurements of the unit cell dimensions from different single crystals at 173K confirmed the main composition and structure of 4. But it is still difficult to determine the accurate positions of solvent molecules. Thus, eight unidentified peaks within void spaces were modeled as isolated oxygen atoms O11 to O18. The occupancy factors for these oxygen atoms have been carefully refined to avoid new high residuary peaks. Isotropic refinement was applied to these atoms with similar environment. Finally, the Ueq values of O11-O17 are below 0.3. The disordered sulfate group was divided into two parts; the same anisotropic displacements were used to O7-O10 and O7A-O10A. And hydrogen atoms were not included for the crystalline water molecules (O11?O18). ; _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^)+(0.1984P)^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 6112 _refine_ls_number_parameters 552 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1990 _refine_ls_R_factor_gt 0.1029 _refine_ls_wR_factor_ref 0.3458 _refine_ls_wR_factor_gt 0.2693 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.006 _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 Co1 Co 0.5000 1.25956(10) 0.7500 0.0328(6) Uani 1 2 d S . . Co2 Co 0.5000 0.72753(11) 0.7500 0.0331(6) Uani 1 2 d S . . S S 0.25022(15) 0.0021(4) 0.50654(17) 0.114(2) Uani 1 1 d D . . O1 O 0.5934(3) 1.2630(4) 0.7283(3) 0.0447(18) Uani 1 1 d . . . H1B H 0.6116 1.3048 0.7315 0.080 Uiso 1 1 d R . . H1 H 0.6005 1.2296 0.7016 0.080 Uiso 1 1 d R . . O2 O 0.4809(3) 0.7239(4) 0.8449(3) 0.0479(19) Uani 1 1 d . . . H2C H 0.4937 0.6909 0.8714 0.080 Uiso 1 1 d R . . H2 H 0.4486 0.7513 0.8469 0.080 Uiso 1 1 d R . . O3 O 0.5199(4) 0.9231(5) 0.5747(4) 0.067(2) Uani 1 1 d . . . O4 O 0.5086(3) 0.5968(4) 0.5781(3) 0.0504(19) Uani 1 1 d . . . O5 O 0.3288(3) 0.3899(4) 0.7604(3) 0.0476(19) Uani 1 1 d . . . O6 O 0.3249(4) 0.0632(5) 0.7710(4) 0.066(2) Uani 1 1 d . . . O7 O 0.3040(7) -0.0434(12) 0.5166(9) 0.190(5) Uani 0.700(13) 1 d PD A 1 O8 O 0.1903(7) -0.0358(13) 0.5070(9) 0.190(5) Uani 0.700(13) 1 d PD A 1 O9 O 0.2464(9) 0.0364(13) 0.4445(7) 0.190(5) Uani 0.700(13) 1 d PD A 1 O10 O 0.2554(9) 0.0589(11) 0.5565(8) 0.190(5) Uani 0.700(13) 1 d PD A 1 O7A O 0.3012(13) -0.012(2) 0.5527(15) 0.190(5) Uani 0.300(13) 1 d PD A 2 O8A O 0.220(2) -0.0698(15) 0.4860(19) 0.190(5) Uani 0.300(13) 1 d PD A 2 O9A O 0.2695(16) 0.037(2) 0.4508(13) 0.190(5) Uani 0.300(13) 1 d PD A 2 O10A O 0.2014(16) 0.045(2) 0.5335(17) 0.190(5) Uani 0.300(13) 1 d PD A 2 O11 O 0.1410(11) 0.1114(15) 0.5770(11) 0.130(8) Uani 0.50 1 d PU . . O12 O 0.1691(7) 0.8863(9) 0.6068(7) 0.170(6) Uani 1 1 d U . . O13 O 0.254(3) 0.227(3) 0.951(3) 0.30(3) Uani 0.50 1 d PU . . O14 O 0.3333(9) 0.0864(13) 0.9022(9) 0.099(6) Uani 0.50 1 d PU . . O15 O 0.3459(6) 0.1970(10) 0.8563(6) 0.164(5) Uani 1 1 d U . . O16 O 0.6106(6) 0.7678(8) 0.5970(7) 0.152(5) Uani 1 1 d U . . O17 O 0.6485(6) 0.9013(9) 0.5837(6) 0.155(5) Uani 1 1 d U . . O18 O 0.2500 0.2500 0.5000 0.58(5) Uani 1 2 d SU . . N1 N 0.4777(4) 1.1714(5) 0.6836(3) 0.036(2) Uani 1 1 d . . . N2 N 0.4323(4) 0.9942(5) 0.5630(4) 0.049(2) Uani 1 1 d . . . H2A H 0.3942 0.9963 0.5437 0.058 Uiso 1 1 calc R . . N3 N 0.4377(4) 0.8889(5) 0.5078(4) 0.053(3) Uani 1 1 d . . . H3 H 0.3990 0.8995 0.4931 0.064 Uiso 1 1 calc R . . N4 N 0.4364(4) 0.6193(5) 0.4964(4) 0.056(3) Uani 1 1 d . . . H4 H 0.4014 0.6042 0.4755 0.067 Uiso 1 1 calc R . . N5 N 0.4327(4) 0.5130(5) 0.5483(4) 0.047(2) Uani 1 1 d . . . H5 H 0.4006 0.5046 0.5202 0.057 Uiso 1 1 calc R . . N6 N 0.4729(4) 0.3464(5) 0.6817(4) 0.037(2) Uani 1 1 d . . . N7 N 0.4310(3) 0.6413(5) 0.7248(4) 0.037(2) Uani 1 1 d . . . N8 N 0.2997(4) 0.4739(5) 0.6835(4) 0.047(2) Uani 1 1 d . . . H8 H 0.2734 0.4817 0.6499 0.056 Uiso 1 1 calc R . . N9 N 0.2455(4) 0.3666(5) 0.6889(4) 0.053(3) Uani 1 1 d . . . H9 H 0.2231 0.3814 0.6544 0.064 Uiso 1 1 calc R . . N10 N 0.2597(4) 0.0986(5) 0.6861(5) 0.062(3) Uani 1 1 d . . . H10 H 0.2468 0.0888 0.6467 0.075 Uiso 1 1 calc R . . N11 N 0.3142(4) -0.0072(5) 0.6821(4) 0.050(2) Uani 1 1 d . . . H11 H 0.2950 -0.0093 0.6438 0.060 Uiso 1 1 calc R . . N12 N 0.4338(3) -0.1842(5) 0.7285(4) 0.040(2) Uani 1 1 d . . . C1 C 0.5185(4) 1.1184(6) 0.6766(5) 0.039(3) Uani 1 1 d . . . H1A H 0.5584 1.1225 0.6997 0.047 Uiso 1 1 calc R . . C2 C 0.5080(4) 1.0588(6) 0.6391(4) 0.039(3) Uani 1 1 d . . . H2B H 0.5395 1.0228 0.6371 0.047 Uiso 1 1 calc R . . C3 C 0.4501(4) 1.0513(6) 0.6035(5) 0.035(2) Uani 1 1 d . . . C4 C 0.4070(4) 1.1056(6) 0.6100(5) 0.045(3) Uani 1 1 d . . . H4A H 0.3665 1.1033 0.5877 0.054 Uiso 1 1 calc R . . C5 C 0.4234(5) 1.1627(6) 0.6491(5) 0.041(3) Uani 1 1 d . . . H5A H 0.3931 1.2000 0.6518 0.049 Uiso 1 1 calc R . . C6 C 0.4677(5) 0.9349(6) 0.5496(5) 0.046(3) Uani 1 1 d . . . C7 C 0.4648(6) 0.8237(6) 0.4858(5) 0.056(3) Uani 1 1 d . . . H7A H 0.5099 0.8234 0.5008 0.067 Uiso 1 1 calc R . . H7B H 0.4608 0.8247 0.4395 0.067 Uiso 1 1 calc R . . C8 C 0.4360(6) 0.7548(6) 0.5067(5) 0.048(3) Uani 1 1 d . . . H8A H 0.3905 0.7557 0.4941 0.058 Uiso 1 1 calc R . . H8B H 0.4428 0.7513 0.5530 0.058 Uiso 1 1 calc R . . C9 C 0.4644(6) 0.6893(6) 0.4781(5) 0.058(3) Uani 1 1 d . . . H9A H 0.4586 0.6940 0.4319 0.069 Uiso 1 1 calc R . . H9B H 0.5099 0.6885 0.4914 0.069 Uiso 1 1 calc R . . C10 C 0.4627(5) 0.5787(6) 0.5437(5) 0.043(3) Uani 1 1 d . . . C11 C 0.4478(5) 0.4575(5) 0.5931(4) 0.036(2) Uani 1 1 d . . . C12 C 0.5046(4) 0.4543(6) 0.6291(4) 0.041(3) Uani 1 1 d . . . H12 H 0.5360 0.4899 0.6251 0.049 Uiso 1 1 calc R . . C13 C 0.5139(4) 0.3980(6) 0.6710(5) 0.042(3) Uani 1 1 d . . . H13 H 0.5537 0.3955 0.6949 0.050 Uiso 1 1 calc R . . C14 C 0.4188(5) 0.3518(6) 0.6448(5) 0.043(3) Uani 1 1 d . . . H14 H 0.3881 0.3156 0.6498 0.052 Uiso 1 1 calc R . . C15 C 0.4039(5) 0.4051(6) 0.6005(5) 0.041(3) Uani 1 1 d . . . H15 H 0.3645 0.4055 0.5760 0.049 Uiso 1 1 calc R . . C16 C 0.4227(4) 0.5893(6) 0.7653(5) 0.042(3) Uani 1 1 d . . . H16 H 0.4485 0.5907 0.8040 0.050 Uiso 1 1 calc R . . C17 C 0.3803(4) 0.5334(6) 0.7572(5) 0.044(3) Uani 1 1 d . . . H17 H 0.3762 0.4992 0.7898 0.053 Uiso 1 1 calc R . . C18 C 0.3430(4) 0.5276(6) 0.6995(5) 0.037(3) Uani 1 1 d . . . C19 C 0.3500(5) 0.5822(6) 0.6571(5) 0.046(3) Uani 1 1 d . . . H19 H 0.3245 0.5829 0.6181 0.055 Uiso 1 1 calc R . . C20 C 0.3949(5) 0.6372(6) 0.6711(5) 0.048(3) Uani 1 1 d . . . H20 H 0.3996 0.6735 0.6402 0.058 Uiso 1 1 calc R . . C21 C 0.2936(5) 0.4091(6) 0.7149(5) 0.040(3) Uani 1 1 d . . . C22 C 0.2306(5) 0.2975(6) 0.7171(5) 0.047(3) Uani 1 1 d . . . H22A H 0.1846 0.2919 0.7137 0.057 Uiso 1 1 calc R . . H22B H 0.2461 0.2987 0.7622 0.057 Uiso 1 1 calc R . . C23 C 0.2584(5) 0.2312(6) 0.6872(5) 0.048(3) Uani 1 1 d . . . H23A H 0.2466 0.2319 0.6414 0.057 Uiso 1 1 calc R . . H23B H 0.3046 0.2330 0.6949 0.057 Uiso 1 1 calc R . . C24 C 0.2355(6) 0.1632(7) 0.7139(6) 0.065(4) Uani 1 1 d . . . H24A H 0.2480 0.1626 0.7596 0.078 Uiso 1 1 calc R . . H24B H 0.1894 0.1624 0.7071 0.078 Uiso 1 1 calc R . . C25 C 0.3010(5) 0.0520(6) 0.7173(6) 0.047(3) Uani 1 1 d . . . C26 C 0.3545(5) -0.0645(6) 0.7001(5) 0.045(3) Uani 1 1 d . . . C27 C 0.3889(4) -0.0729(6) 0.7600(5) 0.042(3) Uani 1 1 d . . . H27 H 0.3854 -0.0379 0.7922 0.051 Uiso 1 1 calc R . . C28 C 0.4267(4) -0.1317(6) 0.7702(5) 0.042(3) Uani 1 1 d . . . H28 H 0.4500 -0.1359 0.8102 0.051 Uiso 1 1 calc R . . C29 C 0.4004(5) -0.1752(6) 0.6727(5) 0.044(3) Uani 1 1 d . . . H29 H 0.4043 -0.2118 0.6420 0.053 Uiso 1 1 calc R . . C30 C 0.3622(5) -0.1195(6) 0.6566(5) 0.046(3) Uani 1 1 d . . . H30 H 0.3405 -0.1173 0.6158 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0330(11) 0.0284(13) 0.0352(11) 0.000 -0.0048(8) 0.000 Co2 0.0331(11) 0.0321(13) 0.0326(11) 0.000 -0.0034(8) 0.000 S 0.046(2) 0.241(7) 0.049(2) 0.011(3) -0.0141(17) -0.011(3) O1 0.038(4) 0.033(5) 0.062(5) -0.008(4) 0.003(3) 0.000(3) O2 0.061(5) 0.042(5) 0.040(4) 0.008(3) -0.001(3) 0.006(4) O3 0.066(5) 0.052(6) 0.081(6) -0.021(5) 0.001(5) 0.016(4) O4 0.059(5) 0.036(5) 0.052(5) -0.004(4) -0.009(4) -0.006(4) O5 0.044(4) 0.046(5) 0.050(5) 0.007(4) -0.007(4) -0.005(3) O6 0.070(6) 0.061(7) 0.068(6) -0.015(5) 0.009(5) 0.013(5) O7 0.119(8) 0.285(17) 0.152(9) -0.004(8) -0.056(7) -0.010(8) O8 0.119(8) 0.285(17) 0.152(9) -0.004(8) -0.056(7) -0.010(8) O9 0.119(8) 0.285(17) 0.152(9) -0.004(8) -0.056(7) -0.010(8) O10 0.119(8) 0.285(17) 0.152(9) -0.004(8) -0.056(7) -0.010(8) O7A 0.119(8) 0.285(17) 0.152(9) -0.004(8) -0.056(7) -0.010(8) O8A 0.119(8) 0.285(17) 0.152(9) -0.004(8) -0.056(7) -0.010(8) O9A 0.119(8) 0.285(17) 0.152(9) -0.004(8) -0.056(7) -0.010(8) O10A 0.119(8) 0.285(17) 0.152(9) -0.004(8) -0.056(7) -0.010(8) O11 0.123(11) 0.137(12) 0.132(11) -0.035(9) 0.028(9) -0.001(9) O12 0.183(9) 0.192(10) 0.136(8) 0.017(7) 0.029(7) -0.041(8) O13 0.29(3) 0.30(3) 0.30(3) 0.008(10) 0.029(11) -0.010(10) O14 0.100(9) 0.101(11) 0.097(9) 0.002(8) 0.011(8) -0.009(8) O15 0.145(8) 0.202(10) 0.149(8) 0.041(8) 0.034(7) -0.012(8) O16 0.124(8) 0.191(10) 0.148(8) 0.000(7) 0.039(7) -0.037(7) O17 0.144(8) 0.170(10) 0.152(8) 0.018(7) 0.018(7) 0.003(7) O18 0.58(5) 0.58(5) 0.57(5) 0.001(10) 0.061(12) 0.004(10) N1 0.038(5) 0.036(6) 0.034(5) -0.003(4) 0.000(4) 0.005(4) N2 0.045(5) 0.043(7) 0.056(6) -0.007(5) -0.008(4) 0.004(5) N3 0.072(6) 0.024(6) 0.062(6) -0.008(5) -0.001(5) -0.001(5) N4 0.073(6) 0.035(6) 0.056(6) 0.003(5) -0.008(5) -0.006(5) N5 0.058(6) 0.034(6) 0.046(5) 0.005(4) -0.017(4) 0.006(4) N6 0.041(5) 0.032(6) 0.037(5) 0.002(4) -0.002(4) 0.001(4) N7 0.037(5) 0.031(6) 0.041(5) 0.013(4) -0.003(4) 0.001(4) N8 0.042(5) 0.036(6) 0.059(6) 0.000(5) -0.010(4) -0.004(4) N9 0.036(5) 0.043(7) 0.077(7) 0.000(5) -0.008(5) -0.006(4) N10 0.073(7) 0.040(7) 0.073(7) -0.010(5) 0.004(6) 0.013(5) N11 0.058(6) 0.026(6) 0.064(6) -0.006(5) -0.004(5) 0.009(5) N12 0.038(5) 0.044(6) 0.038(5) -0.008(4) 0.000(4) 0.002(4) C1 0.037(6) 0.029(7) 0.049(7) -0.006(5) -0.002(5) -0.002(5) C2 0.037(6) 0.035(7) 0.043(6) 0.000(5) -0.009(5) 0.010(5) C3 0.043(6) 0.019(6) 0.046(6) -0.001(5) 0.009(5) -0.006(5) C4 0.035(6) 0.044(8) 0.052(7) -0.005(6) -0.010(5) 0.004(5) C5 0.047(6) 0.020(6) 0.055(7) -0.009(5) -0.001(5) 0.003(5) C6 0.059(7) 0.032(7) 0.046(7) -0.007(5) 0.004(6) 0.007(6) C7 0.090(9) 0.034(8) 0.043(7) -0.004(6) 0.006(6) 0.002(6) C8 0.077(8) 0.032(7) 0.037(6) 0.000(5) 0.010(6) 0.005(6) C9 0.099(9) 0.033(8) 0.043(7) 0.009(6) 0.014(6) 0.004(7) C10 0.074(8) 0.014(6) 0.040(7) -0.008(5) 0.006(6) -0.009(6) C11 0.056(7) 0.018(6) 0.032(6) 0.001(5) -0.004(5) -0.001(5) C12 0.042(6) 0.035(7) 0.044(6) -0.002(5) -0.002(5) -0.006(5) C13 0.029(5) 0.047(8) 0.046(6) 0.007(6) -0.012(5) -0.001(5) C14 0.043(6) 0.028(7) 0.057(7) 0.007(5) -0.004(5) -0.005(5) C15 0.042(6) 0.027(7) 0.052(7) 0.008(5) -0.008(5) 0.006(5) C16 0.039(6) 0.038(7) 0.047(6) 0.004(6) -0.005(5) -0.001(5) C17 0.050(6) 0.041(8) 0.039(6) 0.013(5) -0.004(5) 0.000(5) C18 0.029(5) 0.024(6) 0.056(7) -0.002(5) -0.006(5) 0.004(4) C19 0.051(7) 0.037(8) 0.046(7) 0.000(5) -0.019(5) -0.006(5) C20 0.056(7) 0.041(8) 0.044(7) 0.004(5) -0.011(6) -0.009(6) C21 0.037(6) 0.025(7) 0.056(7) -0.001(5) 0.004(5) 0.008(5) C22 0.033(6) 0.024(7) 0.086(8) -0.001(6) 0.013(5) 0.005(5) C23 0.044(6) 0.032(7) 0.065(7) -0.011(6) 0.001(5) -0.007(5) C24 0.060(7) 0.032(8) 0.106(10) 0.009(7) 0.024(7) 0.001(6) C25 0.035(6) 0.026(7) 0.077(9) 0.000(6) 0.001(6) -0.004(5) C26 0.049(7) 0.028(7) 0.057(7) 0.005(6) 0.004(6) -0.005(5) C27 0.034(6) 0.044(8) 0.048(7) -0.017(5) 0.003(5) -0.003(5) C28 0.037(6) 0.041(8) 0.047(7) -0.001(6) -0.005(5) 0.005(5) C29 0.055(7) 0.037(7) 0.036(6) -0.016(5) -0.012(5) 0.002(5) C30 0.051(7) 0.047(8) 0.038(6) 0.000(6) -0.001(5) 0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.113(7) 2_656 ? Co1 O1 2.113(7) . ? Co1 N1 2.170(9) . ? Co1 N1 2.170(9) 2_656 ? Co1 N6 2.196(9) 2_666 ? Co1 N6 2.196(9) 1_565 ? Co2 O2 2.121(8) . ? Co2 O2 2.121(8) 2_656 ? Co2 N12 2.169(9) 2_666 ? Co2 N12 2.169(9) 1_565 ? Co2 N7 2.193(9) . ? Co2 N7 2.193(9) 2_656 ? S O7A 1.422(16) . ? S O7 1.423(13) . ? S O9A 1.453(17) . ? S O9 1.464(13) . ? S O8 1.465(13) . ? S O10A 1.479(17) . ? S O10 1.487(13) . ? S O8A 1.512(17) . ? O3 C6 1.214(12) . ? O4 C10 1.215(12) . ? O5 C21 1.221(11) . ? O6 C25 1.228(12) . ? N1 C5 1.324(12) . ? N1 C1 1.326(12) . ? N2 C6 1.373(14) . ? N2 C3 1.384(13) . ? N3 C6 1.343(13) . ? N3 C7 1.428(14) . ? N4 C10 1.332(13) . ? N4 C9 1.485(14) . ? N5 C10 1.371(13) . ? N5 C11 1.411(13) . ? N6 C13 1.326(12) . ? N6 C14 1.340(12) . ? N6 Co1 2.196(9) 1_545 ? N7 C16 1.312(13) . ? N7 C20 1.322(12) . ? N8 C18 1.370(13) . ? N8 C21 1.376(13) . ? N9 C21 1.365(13) . ? N9 C22 1.452(14) . ? N10 C25 1.356(14) . ? N10 C24 1.444(15) . ? N11 C25 1.366(14) . ? N11 C26 1.388(13) . ? N12 C28 1.331(13) . ? N12 C29 1.340(11) . ? N12 Co2 2.169(9) 1_545 ? C1 C2 1.357(14) . ? C2 C3 1.397(13) . ? C3 C4 1.376(14) . ? C4 C5 1.360(14) . ? C7 C8 1.493(15) . ? C8 C9 1.503(15) . ? C11 C15 1.366(14) . ? C11 C12 1.377(13) . ? C12 C13 1.367(14) . ? C14 C15 1.374(14) . ? C16 C17 1.369(14) . ? C17 C18 1.405(13) . ? C18 C19 1.370(14) . ? C19 C20 1.404(15) . ? C22 C23 1.522(15) . ? C23 C24 1.473(15) . ? C26 C30 1.392(15) . ? C26 C27 1.423(14) . ? C27 C28 1.349(14) . ? C29 C30 1.330(14) . ? 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 O1 Co1 O1 176.6(4) 2_656 . ? O1 Co1 N1 91.0(3) 2_656 . ? O1 Co1 N1 91.5(3) . . ? O1 Co1 N1 91.5(3) 2_656 2_656 ? O1 Co1 N1 91.0(3) . 2_656 ? N1 Co1 N1 84.2(5) . 2_656 ? O1 Co1 N6 91.3(3) 2_656 2_666 ? O1 Co1 N6 86.3(3) . 2_666 ? N1 Co1 N6 177.2(3) . 2_666 ? N1 Co1 N6 94.2(3) 2_656 2_666 ? O1 Co1 N6 86.3(3) 2_656 1_565 ? O1 Co1 N6 91.3(3) . 1_565 ? N1 Co1 N6 94.2(3) . 1_565 ? N1 Co1 N6 177.2(3) 2_656 1_565 ? N6 Co1 N6 87.5(5) 2_666 1_565 ? O2 Co2 O2 176.4(4) . 2_656 ? O2 Co2 N12 90.5(3) . 2_666 ? O2 Co2 N12 92.1(3) 2_656 2_666 ? O2 Co2 N12 92.1(3) . 1_565 ? O2 Co2 N12 90.5(3) 2_656 1_565 ? N12 Co2 N12 84.0(5) 2_666 1_565 ? O2 Co2 N7 91.1(3) . . ? O2 Co2 N7 86.3(3) 2_656 . ? N12 Co2 N7 177.4(3) 2_666 . ? N12 Co2 N7 93.9(3) 1_565 . ? O2 Co2 N7 86.3(3) . 2_656 ? O2 Co2 N7 91.1(3) 2_656 2_656 ? N12 Co2 N7 93.9(3) 2_666 2_656 ? N12 Co2 N7 177.4(3) 1_565 2_656 ? N7 Co2 N7 88.2(4) . 2_656 ? O7A S O7 39.7(18) . . ? O7A S O9A 112.7(15) . . ? O7 S O9A 95(2) . . ? O7A S O9 132.5(18) . . ? O7 S O9 110.7(10) . . ? O9A S O9 19.8(17) . . ? O7A S O8 121.5(19) . . ? O7 S O8 115.3(13) . . ? O9A S O8 122.8(18) . . ? O9 S O8 104.1(9) . . ? O7A S O10A 110.8(15) . . ? O7 S O10A 148.4(17) . . ? O9A S O10A 111.5(16) . . ? O9 S O10A 99(2) . . ? O8 S O10A 65.6(17) . . ? O7A S O10 68.6(18) . . ? O7 S O10 107.5(9) . . ? O9A S O10 106(2) . . ? O9 S O10 110.4(12) . . ? O8 S O10 108.8(10) . . ? O10A S O10 49.3(16) . . ? O7A S O8A 108.6(16) . . ? O7 S O8A 81.8(19) . . ? O9A S O8A 107.0(14) . . ? O9 S O8A 97(2) . . ? O8 S O8A 40.4(16) . . ? O10A S O8A 105.9(14) . . ? O10 S O8A 144.4(19) . . ? C5 N1 C1 113.9(9) . . ? C5 N1 Co1 125.2(7) . . ? C1 N1 Co1 120.8(6) . . ? C6 N2 C3 127.1(9) . . ? C6 N3 C7 123.8(10) . . ? C10 N4 C9 121.9(10) . . ? C10 N5 C11 127.0(9) . . ? C13 N6 C14 113.5(8) . . ? C13 N6 Co1 119.6(6) . 1_545 ? C14 N6 Co1 126.8(7) . 1_545 ? C16 N7 C20 115.3(9) . . ? C16 N7 Co2 119.5(7) . . ? C20 N7 Co2 125.2(7) . . ? C18 N8 C21 126.2(9) . . ? C21 N9 C22 121.0(9) . . ? C25 N10 C24 123.8(11) . . ? C25 N11 C26 127.1(10) . . ? C28 N12 C29 115.0(9) . . ? C28 N12 Co2 120.9(7) . 1_545 ? C29 N12 Co2 124.0(7) . 1_545 ? N1 C1 C2 125.5(9) . . ? C1 C2 C3 119.1(10) . . ? C4 C3 N2 117.5(9) . . ? C4 C3 C2 116.4(10) . . ? N2 C3 C2 126.1(9) . . ? C5 C4 C3 118.8(9) . . ? N1 C5 C4 126.3(10) . . ? O3 C6 N3 122.9(11) . . ? O3 C6 N2 123.7(10) . . ? N3 C6 N2 113.3(10) . . ? N3 C7 C8 113.9(10) . . ? C7 C8 C9 110.4(10) . . ? N4 C9 C8 112.5(9) . . ? O4 C10 N4 124.3(10) . . ? O4 C10 N5 123.6(10) . . ? N4 C10 N5 112.1(10) . . ? C15 C11 C12 119.3(9) . . ? C15 C11 N5 118.1(9) . . ? C12 C11 N5 122.6(9) . . ? C13 C12 C11 117.4(10) . . ? N6 C13 C12 126.4(9) . . ? N6 C14 C15 125.8(10) . . ? C11 C15 C14 117.6(9) . . ? N7 C16 C17 126.3(10) . . ? C16 C17 C18 118.6(10) . . ? N8 C18 C19 118.3(9) . . ? N8 C18 C17 125.8(10) . . ? C19 C18 C17 115.9(10) . . ? C18 C19 C20 120.1(10) . . ? N7 C20 C19 123.7(10) . . ? O5 C21 N9 122.9(10) . . ? O5 C21 N8 123.7(10) . . ? N9 C21 N8 113.4(9) . . ? N9 C22 C23 113.7(9) . . ? C24 C23 C22 110.1(10) . . ? N10 C24 C23 112.3(10) . . ? O6 C25 N10 123.1(11) . . ? O6 C25 N11 124.1(10) . . ? N10 C25 N11 112.8(11) . . ? N11 C26 C30 118.3(10) . . ? N11 C26 C27 125.7(10) . . ? C30 C26 C27 116.0(10) . . ? C28 C27 C26 118.6(10) . . ? N12 C28 C27 125.1(10) . . ? C30 C29 N12 125.8(10) . . ? C29 C30 C26 119.5(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 N1 C5 32.8(8) 2_656 . . . ? O1 Co1 N1 C5 -144.9(8) . . . . ? N1 Co1 N1 C5 124.2(9) 2_656 . . . ? N6 Co1 N1 C5 178(100) 2_666 . . . ? N6 Co1 N1 C5 -53.5(8) 1_565 . . . ? O1 Co1 N1 C1 -144.1(8) 2_656 . . . ? O1 Co1 N1 C1 38.2(8) . . . . ? N1 Co1 N1 C1 -52.6(7) 2_656 . . . ? N6 Co1 N1 C1 1(7) 2_666 . . . ? N6 Co1 N1 C1 129.6(8) 1_565 . . . ? O2 Co2 N7 C16 -33.9(8) . . . . ? O2 Co2 N7 C16 143.6(8) 2_656 . . . ? N12 Co2 N7 C16 -163(6) 2_666 . . . ? N12 Co2 N7 C16 -126.1(8) 1_565 . . . ? N7 Co2 N7 C16 52.4(7) 2_656 . . . ? O2 Co2 N7 C20 144.8(8) . . . . ? O2 Co2 N7 C20 -37.7(8) 2_656 . . . ? N12 Co2 N7 C20 16(7) 2_666 . . . ? N12 Co2 N7 C20 52.6(8) 1_565 . . . ? N7 Co2 N7 C20 -128.9(9) 2_656 . . . ? C5 N1 C1 C2 -1.1(15) . . . . ? Co1 N1 C1 C2 176.1(8) . . . . ? N1 C1 C2 C3 1.0(16) . . . . ? C6 N2 C3 C4 180.0(10) . . . . ? C6 N2 C3 C2 -0.5(17) . . . . ? C1 C2 C3 C4 -0.9(15) . . . . ? C1 C2 C3 N2 179.6(9) . . . . ? N2 C3 C4 C5 -179.3(9) . . . . ? C2 C3 C4 C5 1.1(15) . . . . ? C1 N1 C5 C4 1.4(15) . . . . ? Co1 N1 C5 C4 -175.7(8) . . . . ? C3 C4 C5 N1 -1.5(17) . . . . ? C7 N3 C6 O3 -3.7(18) . . . . ? C7 N3 C6 N2 179.3(10) . . . . ? C3 N2 C6 O3 3.6(18) . . . . ? C3 N2 C6 N3 -179.4(9) . . . . ? C6 N3 C7 C8 112.2(13) . . . . ? N3 C7 C8 C9 176.2(9) . . . . ? C10 N4 C9 C8 -96.4(13) . . . . ? C7 C8 C9 N4 -178.8(9) . . . . ? C9 N4 C10 O4 5.0(17) . . . . ? C9 N4 C10 N5 -173.7(9) . . . . ? C11 N5 C10 O4 2.0(17) . . . . ? C11 N5 C10 N4 -179.3(9) . . . . ? C10 N5 C11 C15 163.4(10) . . . . ? C10 N5 C11 C12 -16.8(16) . . . . ? C15 C11 C12 C13 -0.1(15) . . . . ? N5 C11 C12 C13 -179.9(9) . . . . ? C14 N6 C13 C12 2.3(16) . . . . ? Co1 N6 C13 C12 178.4(8) 1_545 . . . ? C11 C12 C13 N6 -1.7(17) . . . . ? C13 N6 C14 C15 -1.4(15) . . . . ? Co1 N6 C14 C15 -177.1(8) 1_545 . . . ? C12 C11 C15 C14 0.9(15) . . . . ? N5 C11 C15 C14 -179.3(9) . . . . ? N6 C14 C15 C11 -0.1(17) . . . . ? C20 N7 C16 C17 -0.9(16) . . . . ? Co2 N7 C16 C17 177.9(8) . . . . ? N7 C16 C17 C18 2.7(17) . . . . ? C21 N8 C18 C19 168.2(10) . . . . ? C21 N8 C18 C17 -13.8(16) . . . . ? C16 C17 C18 N8 178.2(10) . . . . ? C16 C17 C18 C19 -3.8(14) . . . . ? N8 C18 C19 C20 -178.4(10) . . . . ? C17 C18 C19 C20 3.4(15) . . . . ? C16 N7 C20 C19 0.5(15) . . . . ? Co2 N7 C20 C19 -178.3(8) . . . . ? C18 C19 C20 N7 -1.9(17) . . . . ? C22 N9 C21 O5 4.6(16) . . . . ? C22 N9 C21 N8 -177.7(8) . . . . ? C18 N8 C21 O5 -3.5(17) . . . . ? C18 N8 C21 N9 178.8(9) . . . . ? C21 N9 C22 C23 -97.4(12) . . . . ? N9 C22 C23 C24 -173.8(10) . . . . ? C25 N10 C24 C23 111.3(13) . . . . ? C22 C23 C24 N10 178.8(9) . . . . ? C24 N10 C25 O6 -4.9(18) . . . . ? C24 N10 C25 N11 176.6(10) . . . . ? C26 N11 C25 O6 1.4(18) . . . . ? C26 N11 C25 N10 179.8(10) . . . . ? C25 N11 C26 C30 -179.0(10) . . . . ? C25 N11 C26 C27 1.6(17) . . . . ? N11 C26 C27 C28 -179.6(10) . . . . ? C30 C26 C27 C28 1.0(15) . . . . ? C29 N12 C28 C27 0.7(15) . . . . ? Co2 N12 C28 C27 176.7(8) 1_545 . . . ? C26 C27 C28 N12 -1.3(16) . . . . ? C28 N12 C29 C30 0.2(16) . . . . ? Co2 N12 C29 C30 -175.7(9) 1_545 . . . ? N12 C29 C30 C26 -0.4(18) . . . . ? N11 C26 C30 C29 -179.7(10) . . . . ? C27 C26 C30 C29 -0.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 23.52 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.436 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.123 ###########################end