# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Hong Liang' _publ_contact_author_email HONGLIANGBY1@YAHOO.COM _publ_section_title ; Microwave-Assisted Synthesis, Crystal Structure and Properties of a disc- like heptanuclear cobalt (II) cluster [Co7(immp)6(CH3O)6]*2ClO4 and a tetranuclear Heterometallic cubanic Cluster [NaCo3(L)3(OH)]2*CH3CN ; loop_ _publ_author_name 'Hong Liang' 'Shu Hua Zhang' 'Min-Hua Zhen' # Attachment 'co4.cif' data_666942 _database_code_depnum_ccdc_archive 'CCDC 666942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H56 Co4 O20' _chemical_formula_sum 'C40 H56 Co4 O20' _chemical_formula_weight 1092.57 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' 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 Tetragonal _symmetry_space_group_name_H-M 'I4(1)/a ' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 22.1046(16) _cell_length_b 22.1046(16) _cell_length_c 9.7539(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4765.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4894 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.99 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 1.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.491 _exptl_absorpt_correction_T_max 0.570 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11872 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.02 _reflns_number_total 2606 _reflns_number_gt 2015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0450P)^2^+7.1803P] 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 SHELXL _refine_ls_extinction_coef 0.0004(1) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2606 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.068435(15) 0.229728(14) 0.01418(3) 0.02681(13) Uani 1 1 d . . . O4 O 0.01968(7) 0.30830(7) 0.02378(16) 0.0261(4) Uani 1 1 d . . . O1 O 0.07736(9) 0.23651(8) -0.19776(19) 0.0385(5) Uani 1 1 d . . . O2 O 0.10464(8) 0.14588(8) 0.00351(17) 0.0306(4) Uani 1 1 d . . . O5 O 0.15035(8) 0.28110(9) 0.0344(2) 0.0420(5) Uani 1 1 d . . . H5A H 0.1502 0.3074 0.0980 0.063 Uiso 1 1 d R . . C2 C 0.11100(13) 0.13531(12) -0.2427(3) 0.0358(6) Uani 1 1 d . . . O3 O 0.13141(9) 0.03288(8) 0.0444(2) 0.0384(4) Uani 1 1 d . . . C7 C 0.11477(10) 0.11363(11) -0.1059(3) 0.0287(5) Uani 1 1 d . . . C6 C 0.13037(11) 0.05108(11) -0.0898(3) 0.0323(6) Uani 1 1 d . . . C9 C 0.03566(12) 0.35793(12) -0.0617(3) 0.0364(6) Uani 1 1 d . . . H9A H 0.0080 0.3917 -0.0445 0.055 Uiso 1 1 calc R . . H9B H 0.0328 0.3457 -0.1580 0.055 Uiso 1 1 calc R . . H9C H 0.0772 0.3705 -0.0413 0.055 Uiso 1 1 calc R . . C1 C 0.09266(14) 0.19546(13) -0.2763(3) 0.0410(7) Uani 1 1 d . . . H1A H 0.0922 0.2051 -0.3712 0.049 Uiso 1 1 calc R . . C3 C 0.12343(15) 0.09605(14) -0.3548(3) 0.0490(8) Uani 1 1 d . . . H3A H 0.1207 0.1112 -0.4457 0.059 Uiso 1 1 calc R . . C5 C 0.14209(14) 0.01497(13) -0.2007(3) 0.0436(7) Uani 1 1 d . . . H5B H 0.1525 -0.0263 -0.1865 0.052 Uiso 1 1 calc R . . C8 C 0.15812(18) -0.02459(13) 0.0715(4) 0.0591(9) Uani 1 1 d . . . H8A H 0.1564 -0.0329 0.1701 0.089 Uiso 1 1 calc R . . H8B H 0.2004 -0.0243 0.0412 0.089 Uiso 1 1 calc R . . H8C H 0.1359 -0.0561 0.0218 0.089 Uiso 1 1 calc R . . C4 C 0.13909(16) 0.03754(14) -0.3346(3) 0.0522(8) Uani 1 1 d . . . H4A H 0.1479 0.0121 -0.4104 0.063 Uiso 1 1 calc R . . C10 C 0.20845(16) 0.2718(2) -0.0161(5) 0.0800(14) Uani 1 1 d . . . H10A H 0.2349 0.3048 0.0141 0.120 Uiso 1 1 calc R . . H10B H 0.2073 0.2707 -0.1165 0.120 Uiso 1 1 calc R . . H10C H 0.2241 0.2332 0.0187 0.120 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 0.0317(2) 0.0275(2) 0.02125(19) 0.00000(13) 0.00325(13) 0.00137(13) O4 0.0320(9) 0.0249(8) 0.0215(8) 0.0016(6) 0.0009(7) 0.0005(6) O1 0.0574(12) 0.0326(10) 0.0255(9) 0.0015(8) 0.0054(8) 0.0091(8) O2 0.0363(10) 0.0302(9) 0.0252(9) -0.0005(7) 0.0019(7) 0.0045(7) O5 0.0358(10) 0.0459(11) 0.0443(11) -0.0132(9) 0.0124(9) -0.0050(9) C2 0.0423(15) 0.0366(14) 0.0284(13) -0.0020(11) 0.0051(11) 0.0073(11) O3 0.0421(11) 0.0318(10) 0.0413(11) 0.0067(8) -0.0010(9) 0.0026(8) C7 0.0234(12) 0.0341(13) 0.0285(12) -0.0033(10) 0.0011(10) 0.0018(10) C6 0.0267(13) 0.0329(14) 0.0373(14) 0.0006(11) -0.0002(11) -0.0010(10) C9 0.0437(16) 0.0336(14) 0.0320(14) 0.0070(11) 0.0062(12) -0.0004(11) C1 0.0586(19) 0.0426(16) 0.0218(13) 0.0019(11) 0.0070(12) 0.0090(13) C3 0.067(2) 0.0504(18) 0.0293(14) -0.0060(13) 0.0056(14) 0.0132(15) C5 0.0490(17) 0.0309(15) 0.0509(18) -0.0072(13) -0.0004(14) 0.0058(12) C8 0.085(3) 0.0308(16) 0.062(2) 0.0108(15) -0.0069(19) 0.0013(16) C4 0.070(2) 0.0474(18) 0.0398(17) -0.0152(14) 0.0049(15) 0.0136(16) C10 0.045(2) 0.092(3) 0.104(3) -0.043(3) 0.027(2) -0.0027(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.0215(17) . ? Co1 O4 2.0461(16) . ? Co1 O4 2.0803(16) 15 ? Co1 O1 2.0820(19) . ? Co1 O4 2.1234(17) 6_454 ? Co1 O5 2.1464(19) . ? O4 C9 1.422(3) . ? O4 Co1 2.0803(16) 12_666 ? O4 Co1 2.1234(17) 6_454 ? O1 C1 1.235(3) . ? O2 C7 1.303(3) . ? O5 C10 1.391(4) . ? O5 H5A 0.8500 . ? C2 C7 1.420(4) . ? C2 C3 1.423(4) . ? C2 C1 1.428(4) . ? O3 C6 1.370(3) . ? O3 C8 1.425(3) . ? C7 C6 1.434(3) . ? C6 C5 1.369(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C1 H1A 0.9500 . ? C3 C4 1.353(4) . ? C3 H3A 0.9500 . ? C5 C4 1.399(4) . ? C5 H5B 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C4 H4A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O4 171.53(7) . . ? O2 Co1 O4 95.72(7) . 15 ? O4 Co1 O4 83.82(7) . 15 ? O2 Co1 O1 88.70(7) . . ? O4 Co1 O1 91.97(7) . . ? O4 Co1 O1 175.45(7) 15 . ? O2 Co1 O4 90.14(7) . 6_454 ? O4 Co1 O4 81.42(7) . 6_454 ? O4 Co1 O4 81.94(7) 15 6_454 ? O1 Co1 O4 99.16(7) . 6_454 ? O2 Co1 O5 98.97(7) . . ? O4 Co1 O5 89.49(7) . . ? O4 Co1 O5 89.79(7) 15 . ? O1 Co1 O5 88.45(8) . . ? O4 Co1 O5 168.29(7) 6_454 . ? C9 O4 Co1 119.81(15) . . ? C9 O4 Co1 119.86(15) . 12_666 ? Co1 O4 Co1 97.68(7) . 12_666 ? C9 O4 Co1 120.48(15) . 6_454 ? Co1 O4 Co1 98.35(7) . 6_454 ? Co1 O4 Co1 95.30(6) 12_666 6_454 ? C1 O1 Co1 126.10(18) . . ? C7 O2 Co1 127.74(16) . . ? C10 O5 Co1 131.9(2) . . ? C10 O5 H5A 111.3 . . ? Co1 O5 H5A 115.2 . . ? C7 C2 C3 120.3(2) . . ? C7 C2 C1 123.1(2) . . ? C3 C2 C1 116.5(2) . . ? C6 O3 C8 116.5(2) . . ? O2 C7 C2 125.1(2) . . ? O2 C7 C6 118.6(2) . . ? C2 C7 C6 116.3(2) . . ? C5 C6 O3 125.5(2) . . ? C5 C6 C7 121.4(2) . . ? O3 C6 C7 113.1(2) . . ? O4 C9 H9A 109.5 . . ? O4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C1 C2 128.3(3) . . ? O1 C1 H1A 115.9 . . ? C2 C1 H1A 115.9 . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5B 119.3 . . ? C4 C5 H5B 119.3 . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? O5 C10 H10A 109.5 . . ? O5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 O5 H5A O2 0.85 2.06 2.823(2) 149.7 12_666 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.466 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.069 #==================================================================== # Attachment '689515.cif' data_689515 _database_code_depnum_ccdc_archive 'CCDC 689515' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H66 Cl2 Co7 N6 O26' _chemical_formula_weight 1698.54 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P-3 ' _symmetry_space_group_name_Hall ' -P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 14.1188(11) _cell_length_b 14.1188(11) _cell_length_c 9.6675(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1668.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1541 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 22.72 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.117 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 863 _exptl_absorpt_coefficient_mu 1.861 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 0.804 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7954 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1975 _reflns_number_gt 1452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0471P)^2^+22.7173P] 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 1975 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2457 _refine_ls_wR_factor_gt 0.2338 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _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 0.0889(9) 0.3437(8) 0.7011(12) 0.048(3) Uani 1 1 d . . . C2 C 0.2017(10) 0.4058(10) 0.7328(14) 0.061(3) Uani 1 1 d . . . C3 C 0.2364(13) 0.4696(12) 0.8500(17) 0.083(5) Uani 1 1 d . . . H3A H 0.3106 0.5087 0.8714 0.099 Uiso 1 1 calc R . . C4 C 0.1619(14) 0.4759(13) 0.9355(18) 0.089(5) Uani 1 1 d . . . H4A H 0.1859 0.5225 1.0116 0.107 Uiso 1 1 calc R . . C5 C 0.0545(14) 0.4147(12) 0.9089(16) 0.080(4) Uani 1 1 d . . . H5A H 0.0052 0.4162 0.9713 0.096 Uiso 1 1 calc R . . C6 C 0.0133(10) 0.3479(10) 0.7900(13) 0.058(3) Uani 1 1 d . . . C7 C -0.1029(11) 0.2899(10) 0.7656(16) 0.071(4) Uani 1 1 d . . . H7A H -0.1451 0.3041 0.8268 0.085 Uiso 1 1 calc R . . C8 C 0.3813(12) 0.4572(17) 0.645(2) 0.135(8) Uani 1 1 d . . . H8A H 0.4147 0.4355 0.5751 0.202 Uiso 1 1 calc R . . H8B H 0.4073 0.4507 0.7347 0.202 Uiso 1 1 calc R . . H8C H 0.4000 0.5318 0.6303 0.202 Uiso 1 1 calc R . . C9 C 0.0103(16) 0.1448(15) 0.244(3) 0.137(9) Uani 1 1 d . . . H9A H 0.0625 0.1313 0.1975 0.205 Uiso 1 1 calc R . . H9B H 0.0236 0.2165 0.2201 0.205 Uiso 1 1 calc R . . H9C H -0.0623 0.0912 0.2157 0.205 Uiso 1 1 calc R . . Cl1 Cl -0.3333 0.3333 0.6843(8) 0.0790(18) Uani 1 3 d S . . Co1 Co 0.0000 0.0000 0.5000 0.0476(9) Uani 1 6 d S . . Co2 Co -0.08719(11) 0.16555(11) 0.52235(17) 0.0481(5) Uani 1 1 d . . . O1 O 0.0592(6) 0.2838(6) 0.5868(8) 0.0510(19) Uani 1 1 d . . . O2 O 0.2660(7) 0.3887(7) 0.6395(10) 0.070(2) Uani 1 1 d . . . O3 O 0.0210(6) 0.1381(6) 0.3923(9) 0.0507(18) Uani 1 1 d . . . N1 N -0.1540(8) 0.2218(8) 0.6704(11) 0.062(3) Uani 1 1 d . . . H1 H -0.2277 0.1868 0.6831 0.093 Uiso 1 1 d R . . O4 O -0.3564(14) 0.2229(14) 0.635(2) 0.207(9) Uani 1 1 d . . . O5 O -0.3333 0.3333 0.829(2) 0.134(9) Uani 1 3 d S . . 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 0.048(6) 0.039(6) 0.063(7) -0.004(5) -0.015(5) 0.024(5) C2 0.058(8) 0.048(7) 0.074(9) -0.005(6) -0.014(6) 0.024(6) C3 0.071(9) 0.062(9) 0.112(13) -0.012(8) -0.034(9) 0.030(8) C4 0.097(12) 0.069(10) 0.112(13) -0.036(9) -0.033(10) 0.050(10) C5 0.107(13) 0.069(9) 0.080(10) -0.007(8) 0.010(9) 0.055(9) C6 0.065(8) 0.054(7) 0.066(8) -0.009(6) -0.006(6) 0.038(6) C7 0.065(8) 0.053(8) 0.098(11) 0.004(7) 0.018(8) 0.031(7) C8 0.051(9) 0.151(19) 0.138(17) -0.042(14) -0.012(10) 0.002(10) C9 0.099(14) 0.088(13) 0.22(3) -0.036(16) 0.004(16) 0.047(12) Cl1 0.069(2) 0.069(2) 0.098(5) 0.000 0.000 0.0347(12) Co1 0.0356(12) 0.0356(12) 0.072(3) 0.000 0.000 0.0178(6) Co2 0.0361(8) 0.0361(8) 0.0727(11) -0.0042(7) -0.0019(7) 0.0184(7) O1 0.043(4) 0.047(4) 0.063(5) -0.009(4) -0.001(4) 0.022(4) O2 0.044(5) 0.063(6) 0.095(7) -0.004(5) -0.009(5) 0.021(4) O3 0.048(4) 0.050(4) 0.056(5) -0.001(4) -0.002(4) 0.027(4) N1 0.042(5) 0.052(6) 0.086(8) -0.012(6) 0.005(5) 0.020(5) O4 0.133(14) 0.142(14) 0.33(3) -0.101(16) -0.091(16) 0.055(12) O5 0.162(15) 0.162(15) 0.079(15) 0.000 0.000 0.081(7) _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 O1 1.326(13) . ? C1 C6 1.394(16) . ? C1 C2 1.415(16) . ? C2 C3 1.377(19) . ? C2 O2 1.383(15) . ? C3 C4 1.38(2) . ? C3 H3A 0.9300 . ? C4 C5 1.34(2) . ? C4 H4A 0.9300 . ? C5 C6 1.415(18) . ? C5 H5A 0.9300 . ? C6 C7 1.439(18) . ? C7 N1 1.264(16) . ? C7 H7A 0.9300 . ? C8 O2 1.420(16) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O3 1.45(2) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? Cl1 O5 1.40(2) . ? Cl1 O4 1.503(17) . ? Cl1 O4 1.503(17) 2_565 ? Cl1 O4 1.503(17) 3_455 ? Co1 O3 2.096(8) 5_556 ? Co1 O3 2.096(8) 3 ? Co1 O3 2.096(8) 2 ? Co1 O3 2.096(8) 4_556 ? Co1 O3 2.096(8) . ? Co1 O3 2.096(8) 6_556 ? Co2 O1 1.999(7) . ? Co2 O3 2.040(8) 6_556 ? Co2 O1 2.054(7) 6_556 ? Co2 N1 2.078(10) . ? Co2 O3 2.157(8) . ? Co2 O2 2.328(9) 6_556 ? O1 Co2 2.054(7) 5_556 ? O2 Co2 2.328(9) 5_556 ? O3 Co2 2.040(8) 5_556 ? N1 H1 0.9101 . ? 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 C1 C6 122.4(10) . . ? O1 C1 C2 118.3(11) . . ? C6 C1 C2 119.3(11) . . ? C3 C2 O2 126.9(12) . . ? C3 C2 C1 120.4(13) . . ? O2 C2 C1 112.6(11) . . ? C4 C3 C2 120.2(14) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 119.8(15) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 122.8(15) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C1 C6 C5 117.4(12) . . ? C1 C6 C7 123.6(11) . . ? C5 C6 C7 119.0(13) . . ? N1 C7 C6 127.3(12) . . ? N1 C7 H7A 116.3 . . ? C6 C7 H7A 116.3 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O5 Cl1 O4 108.6(10) . . ? O5 Cl1 O4 108.6(10) . 2_565 ? O4 Cl1 O4 110.3(10) . 2_565 ? O5 Cl1 O4 108.6(10) . 3_455 ? O4 Cl1 O4 110.3(10) . 3_455 ? O4 Cl1 O4 110.3(10) 2_565 3_455 ? O3 Co1 O3 82.5(3) 5_556 3 ? O3 Co1 O3 180.0(4) 5_556 2 ? O3 Co1 O3 97.5(3) 3 2 ? O3 Co1 O3 97.5(3) 5_556 4_556 ? O3 Co1 O3 82.5(3) 3 4_556 ? O3 Co1 O3 82.5(3) 2 4_556 ? O3 Co1 O3 82.5(3) 5_556 . ? O3 Co1 O3 97.5(3) 3 . ? O3 Co1 O3 97.5(3) 2 . ? O3 Co1 O3 180.000(1) 4_556 . ? O3 Co1 O3 97.5(3) 5_556 6_556 ? O3 Co1 O3 180.0(2) 3 6_556 ? O3 Co1 O3 82.5(3) 2 6_556 ? O3 Co1 O3 97.5(3) 4_556 6_556 ? O3 Co1 O3 82.5(3) . 6_556 ? O1 Co2 O3 108.7(3) . 6_556 ? O1 Co2 O1 167.12(17) . 6_556 ? O3 Co2 O1 80.1(3) 6_556 6_556 ? O1 Co2 N1 86.8(3) . . ? O3 Co2 N1 101.4(4) 6_556 . ? O1 Co2 N1 100.9(4) 6_556 . ? O1 Co2 O3 78.6(3) . . ? O3 Co2 O3 82.3(4) 6_556 . ? O1 Co2 O3 93.7(3) 6_556 . ? N1 Co2 O3 165.3(4) . . ? O1 Co2 O2 98.5(3) . 6_556 ? O3 Co2 O2 151.8(3) 6_556 6_556 ? O1 Co2 O2 71.8(3) 6_556 6_556 ? N1 Co2 O2 87.3(4) . 6_556 ? O3 Co2 O2 96.0(3) . 6_556 ? C1 O1 Co2 131.1(7) . . ? C1 O1 Co2 122.2(7) . 5_556 ? Co2 O1 Co2 102.8(3) . 5_556 ? C2 O2 C8 118.9(12) . . ? C2 O2 Co2 113.6(7) . 5_556 ? C8 O2 Co2 127.4(10) . 5_556 ? C9 O3 Co2 116.3(9) . 5_556 ? C9 O3 Co1 125.5(9) . . ? Co2 O3 Co1 99.0(3) 5_556 . ? C9 O3 Co2 117.3(9) . . ? Co2 O3 Co2 98.0(3) 5_556 . ? Co1 O3 Co2 95.4(3) . . ? C7 N1 Co2 126.6(9) . . ? C7 N1 H1 112.2 . . ? Co2 N1 H1 120.0 . . ? 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 N1 H1 O4 0.91 2.17 2.89(2) 135.1 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.145 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.139 # Attachment '689516.cif' data_co _database_code_depnum_ccdc_archive 'CCDC 689516' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H43 Co3 N6 Na O16 S3), (C2 H3 N)' _chemical_formula_sum 'C74 H89 Co6 N13 Na2 O32 S6' _chemical_formula_weight 2264.50 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' Na Na 0.0362 0.0249 '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 trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.1568(12) _cell_length_b 17.1568(12) _cell_length_c 27.247(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6945.9(11) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2606 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 24.87 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3480 _exptl_absorpt_coefficient_mu 1.282 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10304 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2719 _reflns_number_gt 1833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0952P)^2^+44.0845P] 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 2719 _refine_ls_number_parameters 207 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1455 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.028 _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 Co1 Co 0.74294(5) 0.28783(5) 0.08484(3) 0.0224(3) Uani 1 1 d . . . Na1 Na 0.6667 0.3333 0.18674(13) 0.0321(9) Uani 1 3 d S . . S1 S 0.73787(11) 0.15633(10) -0.00067(6) 0.0354(4) Uani 1 1 d . . . C1 C 0.8500(5) 0.2425(5) -0.0088(3) 0.0536(19) Uani 1 1 d . . . H1B H 0.8868 0.2331 0.0148 0.064 Uiso 1 1 calc R . . H1A H 0.8691 0.2355 -0.0412 0.064 Uiso 1 1 calc R . . C2 C 0.8703(5) 0.3370(4) -0.0040(2) 0.0429(16) Uani 1 1 d . . . H2B H 0.9308 0.3768 -0.0160 0.051 Uiso 1 1 calc R . . H2A H 0.8290 0.3455 -0.0245 0.051 Uiso 1 1 calc R . . C3 C 0.9327(4) 0.4303(4) 0.0654(2) 0.0326(14) Uani 1 1 d . . . H3 H 0.9838 0.4583 0.0457 0.039 Uiso 1 1 d R . . C4 C 0.9395(4) 0.4680(4) 0.1146(2) 0.0311(13) Uani 1 1 d . . . C5 C 1.0257(4) 0.5225(4) 0.1324(2) 0.0397(15) Uani 1 1 d . . . H5 H 1.0749 0.5348 0.1129 0.048 Uiso 1 1 calc R . . C6 C 1.0393(5) 0.5591(5) 0.1791(3) 0.0507(19) Uani 1 1 d . . . H6 H 1.0974 0.5957 0.1910 0.061 Uiso 1 1 calc R . . C7 C 0.9657(4) 0.5405(4) 0.2079(2) 0.0441(17) Uani 1 1 d . . . H7 H 0.9745 0.5655 0.2391 0.053 Uiso 1 1 calc R . . C8 C 0.8793(4) 0.4852(4) 0.1909(2) 0.0329(14) Uani 1 1 d . . . C9 C 0.8638(4) 0.4498(3) 0.14299(19) 0.0257(12) Uani 1 1 d . . . C10 C 0.8126(6) 0.5034(7) 0.2633(3) 0.082(3) Uani 1 1 d U . . H10A H 0.8432 0.4857 0.2864 0.124 Uiso 1 1 calc R . . H10B H 0.7545 0.4881 0.2760 0.124 Uiso 1 1 calc R . . H10C H 0.8473 0.5672 0.2580 0.124 Uiso 1 1 calc R . . C11 C 0.8667(4) 0.2741(4) 0.1713(2) 0.0351(14) Uani 1 1 d . . . C12 C 0.9327(5) 0.3042(5) 0.2106(3) 0.0492(18) Uani 1 1 d . . . H12A H 0.9762 0.3667 0.2060 0.074 Uiso 1 1 calc R . . H12B H 0.9625 0.2695 0.2102 0.074 Uiso 1 1 calc R . . H12C H 0.9030 0.2963 0.2415 0.074 Uiso 1 1 calc R . . C13 C 0.6667 0.3333 0.9449(7) 0.089(6) Uani 0.25 3 d SPDU . . H13 H 0.7121 0.3780 0.9550 0.133 Uiso 0.25 1 d PR . . C14 C 0.6667 0.3333 0.9002(6) 0.089(6) Uani 0.25 3 d SPDU . . C13' C 0.6667 0.3333 0.8555(7) 0.089(6) Uani 0.25 3 d SPD . . H13' H 0.6446 0.3651 0.8480 0.133 Uiso 0.25 1 d PR . . C14' C 0.6667 0.3333 0.9002(6) 0.089(6) Uani 0.25 3 d SPD . . N1 N 0.8635(3) 0.3625(3) 0.04691(17) 0.0287(11) Uani 1 1 d . . . N2 N 0.8153(4) 0.2519(3) 0.14025(19) 0.0370(13) Uani 1 1 d . . . N3 N 0.6667 0.3333 0.8496(7) 0.055(4) Uani 0.25 3 d SPDU . . N3' N 0.6667 0.3333 0.9508(7) 0.055(4) Uani 0.25 3 d SPDU . . O1 O 0.7794(2) 0.3991(2) 0.12751(13) 0.0226(8) Uani 1 1 d . . . O2 O 0.8021(3) 0.4577(3) 0.21805(15) 0.0424(11) Uani 1 1 d . . . O3 O 0.6667 0.3333 0.0493(2) 0.0224(14) Uani 1 3 d S . . H3A H 0.6667 0.3333 0.0181 0.034 Uiso 1 3 d SR . . O4 O 0.6851(4) 0.1575(5) -0.04009(19) 0.0793(18) Uani 1 1 d . . . O5 O 0.7083(3) 0.1719(3) 0.04685(14) 0.0358(10) Uani 1 1 d . . . O6 O 0.7421(4) 0.0744(4) 0.0005(2) 0.0750(17) Uani 1 1 d U . . 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 0.0223(4) 0.0220(4) 0.0237(4) -0.0011(3) 0.0008(3) 0.0116(3) Na1 0.0369(14) 0.0369(14) 0.022(2) 0.000 0.000 0.0184(7) S1 0.0386(9) 0.0318(8) 0.0307(8) -0.0074(6) 0.0039(7) 0.0137(7) C1 0.055(5) 0.057(5) 0.050(4) -0.006(4) 0.016(4) 0.029(4) C2 0.047(4) 0.044(4) 0.032(3) 0.005(3) 0.019(3) 0.019(3) C3 0.021(3) 0.030(3) 0.041(4) 0.005(3) 0.005(3) 0.009(3) C4 0.027(3) 0.025(3) 0.039(3) 0.001(3) -0.003(3) 0.012(3) C5 0.029(3) 0.033(3) 0.052(4) -0.003(3) -0.005(3) 0.011(3) C6 0.032(4) 0.044(4) 0.069(5) -0.006(4) -0.021(4) 0.014(3) C7 0.048(4) 0.043(4) 0.037(4) -0.008(3) -0.022(3) 0.020(3) C8 0.031(3) 0.035(3) 0.034(3) 0.000(3) -0.008(3) 0.018(3) C9 0.029(3) 0.020(3) 0.027(3) -0.001(2) -0.011(2) 0.012(3) C10 0.069(5) 0.108(6) 0.056(5) -0.035(5) 0.000(4) 0.033(5) C11 0.040(4) 0.033(3) 0.041(4) 0.009(3) 0.005(3) 0.025(3) C12 0.051(4) 0.051(4) 0.050(4) -0.007(3) -0.017(3) 0.029(4) C13 0.097(6) 0.097(6) 0.072(9) 0.000 0.000 0.048(3) C14 0.097(6) 0.097(6) 0.072(9) 0.000 0.000 0.048(3) C13' 0.097(6) 0.097(6) 0.072(9) 0.000 0.000 0.048(3) C14' 0.097(6) 0.097(6) 0.072(9) 0.000 0.000 0.048(3) N1 0.031(3) 0.027(3) 0.029(3) 0.000(2) 0.002(2) 0.015(2) N2 0.041(3) 0.032(3) 0.043(3) 0.008(2) -0.003(3) 0.022(3) N3 0.057(4) 0.057(4) 0.051(6) 0.000 0.000 0.029(2) N3' 0.057(4) 0.057(4) 0.051(6) 0.000 0.000 0.029(2) O1 0.0217(19) 0.0217(19) 0.024(2) -0.0029(15) -0.0049(15) 0.0108(16) O2 0.046(3) 0.051(3) 0.028(2) -0.015(2) -0.008(2) 0.023(2) O3 0.025(2) 0.025(2) 0.018(3) 0.000 0.000 0.0124(10) O4 0.069(4) 0.115(5) 0.048(3) -0.013(3) -0.019(3) 0.042(4) O5 0.041(2) 0.027(2) 0.034(2) -0.0077(18) 0.0073(19) 0.0125(19) O6 0.101(4) 0.057(3) 0.078(4) -0.001(3) 0.030(3) 0.048(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 Co1 O1 2.048(3) . ? Co1 O5 2.048(4) . ? Co1 O3 2.070(3) . ? Co1 N1 2.082(5) . ? Co1 O1 2.170(3) 3_665 ? Co1 N2 2.228(5) . ? Na1 O1 2.331(4) 3_665 ? Na1 O1 2.331(4) . ? Na1 O1 2.331(4) 2_655 ? Na1 O2 2.392(4) 3_665 ? Na1 O2 2.392(4) . ? Na1 O2 2.392(4) 2_655 ? Na1 Co1 3.325(3) 3_665 ? Na1 Co1 3.325(3) 2_655 ? S1 O4 1.411(6) . ? S1 O6 1.444(5) . ? S1 O5 1.464(4) . ? S1 C1 1.759(7) . ? C1 C2 1.484(9) . ? C1 H1B 0.9700 . ? C1 H1A 0.9700 . ? C2 N1 1.478(7) . ? C2 H2B 0.9700 . ? C2 H2A 0.9700 . ? C3 N1 1.279(7) . ? C3 C4 1.467(8) . ? C3 H3 0.9300 . ? C4 C5 1.383(8) . ? C4 C9 1.407(8) . ? C5 C6 1.387(9) . ? C5 H5 0.9300 . ? C6 C7 1.381(10) . ? C6 H6 0.9300 . ? C7 C8 1.380(8) . ? C7 H7 0.9300 . ? C8 O2 1.379(7) . ? C8 C9 1.408(8) . ? C9 O1 1.332(6) . ? C10 O2 1.422(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.141(8) . ? C11 C12 1.453(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.218(10) . ? C13 H13 0.8200 . ? C14 C13' 1.218(10) . ? C14 N3' 1.378(10) . ? C14 N3 1.379(10) . ? C13' N3 1.05(3) 16_656 ? C13' C13' 1.21(4) 16_656 ? C13' H13' 0.8299 . ? N3 N3 0.89(4) 16_656 ? N3 C13' 1.05(3) 16_656 ? N3 H13' 0.8057 . ? N3' H13 0.7815 . ? O1 Co1 2.170(3) 2_655 ? O3 Co1 2.070(3) 3_665 ? O3 Co1 2.070(3) 2_655 ? O3 H3A 0.8501 . ? 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 O5 175.52(15) . . ? O1 Co1 O3 82.53(14) . . ? O5 Co1 O3 101.41(16) . . ? O1 Co1 N1 87.81(16) . . ? O5 Co1 N1 93.65(17) . . ? O3 Co1 N1 98.97(16) . . ? O1 Co1 O1 87.32(19) . 3_665 ? O5 Co1 O1 91.27(15) . 3_665 ? O3 Co1 O1 79.63(14) . 3_665 ? N1 Co1 O1 175.07(16) . 3_665 ? O1 Co1 N2 85.45(16) . . ? O5 Co1 N2 90.32(18) . . ? O3 Co1 N2 165.1(2) . . ? N1 Co1 N2 89.28(18) . . ? O1 Co1 N2 91.10(16) 3_665 . ? O1 Na1 O1 77.35(16) 3_665 . ? O1 Na1 O1 77.35(16) 3_665 2_655 ? O1 Na1 O1 77.35(16) . 2_655 ? O1 Na1 O2 67.33(13) 3_665 3_665 ? O1 Na1 O2 111.15(14) . 3_665 ? O1 Na1 O2 139.95(15) 2_655 3_665 ? O1 Na1 O2 139.95(15) 3_665 . ? O1 Na1 O2 67.33(13) . . ? O1 Na1 O2 111.15(14) 2_655 . ? O2 Na1 O2 108.01(14) 3_665 . ? O1 Na1 O2 111.15(14) 3_665 2_655 ? O1 Na1 O2 139.95(15) . 2_655 ? O1 Na1 O2 67.33(13) 2_655 2_655 ? O2 Na1 O2 108.01(14) 3_665 2_655 ? O2 Na1 O2 108.01(14) . 2_655 ? O1 Na1 Co1 37.53(9) 3_665 3_665 ? O1 Na1 Co1 79.53(13) . 3_665 ? O1 Na1 Co1 40.55(9) 2_655 3_665 ? O2 Na1 Co1 100.76(12) 3_665 3_665 ? O2 Na1 Co1 141.99(15) . 3_665 ? O2 Na1 Co1 85.35(12) 2_655 3_665 ? O1 Na1 Co1 79.53(13) 3_665 2_655 ? O1 Na1 Co1 40.55(9) . 2_655 ? O1 Na1 Co1 37.53(9) 2_655 2_655 ? O2 Na1 Co1 141.99(15) 3_665 2_655 ? O2 Na1 Co1 85.35(12) . 2_655 ? O2 Na1 Co1 100.76(11) 2_655 2_655 ? Co1 Na1 Co1 56.89(6) 3_665 2_655 ? O4 S1 O6 112.0(4) . . ? O4 S1 O5 112.8(3) . . ? O6 S1 O5 110.5(3) . . ? O4 S1 C1 109.4(4) . . ? O6 S1 C1 104.7(4) . . ? O5 S1 C1 107.0(3) . . ? C2 C1 S1 117.9(5) . . ? C2 C1 H1B 107.8 . . ? S1 C1 H1B 107.8 . . ? C2 C1 H1A 107.8 . . ? S1 C1 H1A 107.8 . . ? H1B C1 H1A 107.2 . . ? N1 C2 C1 113.4(5) . . ? N1 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? N1 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? H2B C2 H2A 107.7 . . ? N1 C3 C4 126.4(5) . . ? N1 C3 H3 116.7 . . ? C4 C3 H3 116.9 . . ? C5 C4 C9 120.8(6) . . ? C5 C4 C3 116.3(5) . . ? C9 C4 C3 122.9(5) . . ? C4 C5 C6 120.7(6) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 119.2(6) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C8 C7 C6 120.8(6) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? O2 C8 C7 125.0(6) . . ? O2 C8 C9 114.1(5) . . ? C7 C8 C9 120.9(6) . . ? O1 C9 C4 123.6(5) . . ? O1 C9 C8 119.0(5) . . ? C4 C9 C8 117.4(5) . . ? O2 C10 H10A 109.5 . . ? O2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 178.8(6) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13 109.5 . . ? C13' C14 C13 180.000(17) . . ? C13' C14 N3' 180.000(8) . . ? C13 C14 N3' 0.000(6) . . ? C13' C14 N3 0.000(5) . . ? C13 C14 N3 180.000(8) . . ? N3' C14 N3 180.000(8) . . ? N3 C13' C13' 0.001(5) 16_656 16_656 ? N3 C13' H13' 75.8 16_656 . ? C13' C13' H13' 75.8 16_656 . ? C14 C13' H13' 104.2 . . ? C3 N1 C2 117.6(5) . . ? C3 N1 Co1 123.4(4) . . ? C2 N1 Co1 119.1(4) . . ? C11 N2 Co1 148.7(5) . . ? N3 N3 C13' 0.001(6) 16_656 16_656 ? N3 N3 H13' 87.0 16_656 . ? C13' N3 H13' 87.0 16_656 . ? C14 N3 H13' 93.0 . . ? C14 N3' H13 98.4 . . ? C9 O1 Co1 120.9(3) . . ? C9 O1 Co1 121.8(3) . 2_655 ? Co1 O1 Co1 97.27(14) . 2_655 ? C9 O1 Na1 117.7(3) . . ? Co1 O1 Na1 98.57(14) . . ? Co1 O1 Na1 95.15(14) 2_655 . ? C8 O2 C10 116.1(5) . . ? C8 O2 Na1 116.9(3) . . ? C10 O2 Na1 126.9(5) . . ? Co1 O3 Co1 99.83(18) . 3_665 ? Co1 O3 Co1 99.83(18) . 2_655 ? Co1 O3 Co1 99.83(18) 3_665 2_655 ? Co1 O3 H3A 117.9 . . ? Co1 O3 H3A 117.9 3_665 . ? Co1 O3 H3A 117.9 2_655 . ? S1 O5 Co1 131.7(3) . . ? 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 N3' H13 O4 0.78 2.42 3.197(7) 170.7 2_656 O3 H3A N3' 0.85 1.83 2.68(2) 180.0 1_554 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.510 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.113