Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Nicola Brasch' _publ_contact_author_address ; Department of Chemistry Kent State University School of Medical Sciences Kent OH 44242 UNITED STATES OF AMERICA ; _publ_contact_author_email NBRASCH@KENT.EDU _publ_section_title ; A Simple, Convenient Method to Synthesize Cobalamins: Synthesis of Homocysteinylcobalamin, N-Acetylcysteinylcobalamin, 2-N-acetylamino-2-carbomethoxyethanethiolatocobalamin, Sulfitocobalamin and Nitrocobalamin ; loop_ _publ_author_name 'Nicola Brasch' 'Roberto A. Chavez' 'Luciana Hannibal' 'W. Jacobsen' 'Clyde A. Smith' ; E.Suarez-Moreira ; # Attachment 'NACCblfinal.cif' data_nac7_init2 _database_code_depnum_ccdc_archive 'CCDC 615032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_absolute_configuration unk _chemical_formula_sum 'C67 H97 Co N14 Na O35 P S' _chemical_formula_weight 1819.54 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3387 1.2561 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 16.1530(10) _cell_length_b 21.0760(10) _cell_length_c 25.4490(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8663.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used N/A _cell_measurement_theta_min N/A _cell_measurement_theta_max N/A _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3816 _exptl_absorpt_coefficient_mu 0.339 _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 0.81797 _diffrn_radiation_type synchrotron _diffrn_radiation_source wiggler _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ADSC Q-315 CCD' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean 9.7 _diffrn_standards_number N/A _diffrn_standards_interval_count N/A _diffrn_standards_interval_time N/A _diffrn_standards_decay_% N/A _diffrn_reflns_number 17617 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1193 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 32.96 _reflns_number_total 17617 _reflns_number_gt 16106 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. Eighteen water molecules were located in an Fo-Fc map and included in refinement with no hydrogen atoms. ; _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^)+(0.1021P)^2^+41.8178P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.071(17) _refine_ls_number_reflns 17617 _refine_ls_number_parameters 1143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.1030 _refine_ls_wR_factor_ref 0.2645 _refine_ls_wR_factor_gt 0.2603 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 Co1 Co 0.78333(5) 0.39505(3) 0.76171(3) 0.0251(2) Uani 1 1 d . . . N21 N 0.6725(3) 0.3740(2) 0.74799(18) 0.0228(10) Uani 1 1 d . . . N22 N 0.7508(4) 0.4807(3) 0.7763(3) 0.0451(18) Uani 1 1 d . . . N23 N 0.9007(3) 0.4083(2) 0.7702(3) 0.0358(14) Uani 1 1 d . . . N24 N 0.8005(3) 0.3077(2) 0.75039(18) 0.0228(9) Uani 1 1 d . . . C1 C 0.6572(3) 0.3121(3) 0.7223(2) 0.0203(10) Uani 1 1 d . . . C2 C 0.5627(3) 0.3002(3) 0.7370(2) 0.0237(11) Uani 1 1 d . . . C3 C 0.5290(4) 0.3697(3) 0.7417(3) 0.0270(11) Uani 1 1 d . . . H3 H 0.487(3) 0.3713(3) 0.770(2) 0.032 Uiso 1 1 calc R . . C4 C 0.6052(3) 0.4043(3) 0.7592(2) 0.0282(12) Uani 1 1 d . . . C5 C 0.6034(4) 0.4661(3) 0.7867(3) 0.0375(17) Uani 1 1 d . . . C6 C 0.6728(5) 0.5016(4) 0.7921(3) 0.048(2) Uani 1 1 d . . . C7 C 0.6858(6) 0.5676(4) 0.8169(5) 0.073(4) Uani 1 1 d . . . C8 C 0.7613(5) 0.5902(4) 0.7874(6) 0.104(6) Uani 1 1 d . . . H8 H 0.807(6) 0.629(5) 0.817(4) 0.125 Uiso 1 1 calc R . . C9 C 0.8062(5) 0.5289(4) 0.7770(6) 0.085(5) Uani 1 1 d . . . C10 C 0.8897(6) 0.5218(4) 0.7769(7) 0.109(7) Uani 1 1 d . . . H10 H 0.925(6) 0.565(7) 0.7812(10) 0.131 Uiso 1 1 calc R . . C11 C 0.9352(5) 0.4664(4) 0.7718(5) 0.059(3) Uani 1 1 d . . . C12 C 1.0290(4) 0.4659(3) 0.7701(3) 0.0371(16) Uani 1 1 d . . . C13 C 1.0471(4) 0.3924(3) 0.7642(3) 0.0335(14) Uani 1 1 d . . . H13 H 1.075(3) 0.3806(14) 0.790(3) 0.040 Uiso 1 1 calc R . . C14 C 0.9612(4) 0.3621(3) 0.7675(3) 0.0276(12) Uani 1 1 d . . . C15 C 0.9476(3) 0.2973(3) 0.7639(3) 0.0253(11) Uani 1 1 d . . . C16 C 0.8652(3) 0.2716(2) 0.7545(2) 0.0198(10) Uani 1 1 d . . . C17 C 0.8415(3) 0.2019(2) 0.7486(2) 0.0211(11) Uani 1 1 d . . . C18 C 0.7536(4) 0.2066(3) 0.7246(2) 0.0250(12) Uani 1 1 d . . . H18 H 0.7591(6) 0.2120(5) 0.686(3) 0.030 Uiso 1 1 calc R . . C19 C 0.7230(3) 0.2698(3) 0.7483(2) 0.0231(11) Uani 1 1 d . . . H19 H 0.7049(14) 0.2613(7) 0.785(3) 0.028 Uiso 1 1 calc R . . C20 C 0.6725(3) 0.3143(3) 0.6628(2) 0.0201(10) Uani 1 1 d . . . H20A H 0.640(3) 0.349(2) 0.6472(8) 0.030 Uiso 1 1 calc R . . H20B H 0.655(3) 0.274(2) 0.6470(8) 0.030 Uiso 1 1 calc R . . H20C H 0.732(3) 0.321(2) 0.6561(4) 0.030 Uiso 1 1 calc R . . C25 C 0.5152(4) 0.2599(3) 0.6969(2) 0.0274(12) Uani 1 1 d . . . H25A H 0.522(3) 0.2767(17) 0.6640(18) 0.041 Uiso 1 1 calc R . . H25B H 0.460(3) 0.260(2) 0.7053(12) 0.041 Uiso 1 1 calc R . . H25C H 0.535(2) 0.219(2) 0.6974(14) 0.041 Uiso 1 1 calc R . . C26 C 0.5560(4) 0.2695(3) 0.7924(2) 0.0288(13) Uani 1 1 d . . . H26A H 0.5834(19) 0.235(2) 0.7926(2) 0.035 Uiso 1 1 calc R . . H26B H 0.5780(16) 0.2945(17) 0.8151(15) 0.035 Uiso 1 1 calc R . . C27 C 0.4665(4) 0.2559(3) 0.8086(3) 0.0328(14) Uani 1 1 d . . . O28 O 0.4137(4) 0.2974(3) 0.8109(3) 0.0566(16) Uani 1 1 d . . . N29 N 0.4513(5) 0.1977(4) 0.8201(4) 0.061(2) Uani 1 1 d . . . H29A H 0.4024 0.1866 0.8298 0.073 Uiso 1 1 calc R . . H29B H 0.4900 0.1698 0.8180 0.073 Uiso 1 1 calc R . . C30 C 0.4936(4) 0.4027(3) 0.6920(2) 0.0286(12) Uani 1 1 d . . . H30A H 0.5051 0.4478 0.6941 0.034 Uiso 1 1 calc R . . H30B H 0.5220 0.3863 0.6613 0.034 Uiso 1 1 calc R . . C31 C 0.4005(4) 0.3932(4) 0.6849(3) 0.0345(14) Uani 1 1 d . . . H31A H 0.3913(8) 0.356(3) 0.6763(7) 0.041 Uiso 1 1 calc R . . H31B H 0.3768(18) 0.3998(6) 0.713(2) 0.041 Uiso 1 1 calc R . . C32 C 0.3674(5) 0.4367(4) 0.6442(3) 0.0464(19) Uani 1 1 d . . . O33 O 0.3385(4) 0.4904(3) 0.6563(2) 0.0510(14) Uani 1 1 d . . . N34 N 0.3735(5) 0.4158(4) 0.5953(3) 0.059(2) Uani 1 1 d . . . H34A H 0.3572 0.4392 0.5696 0.071 Uiso 1 1 calc R . . H34B H 0.3937 0.3788 0.5892 0.071 Uiso 1 1 calc R . . C35 C 0.5180(5) 0.4856(4) 0.8063(3) 0.0464(19) Uani 1 1 d . . . H35A H 0.4880 0.4486 0.8174 0.070 Uiso 1 1 calc R . . H35B H 0.4883 0.5063 0.7785 0.070 Uiso 1 1 calc R . . H35C H 0.5238 0.5142 0.8354 0.070 Uiso 1 1 calc R . . C36 C 0.6136(6) 0.6167(4) 0.8144(5) 0.076(4) Uani 1 1 d . . . H36A H 0.5884 0.6153 0.7803 0.114 Uiso 1 1 calc R . . H36B H 0.6349 0.6585 0.8208 0.114 Uiso 1 1 calc R . . H36C H 0.5730 0.6065 0.8406 0.114 Uiso 1 1 calc R . . C37 C 0.7232(8) 0.5646(5) 0.8692(4) 0.067(3) Uani 1 1 d . . . H37A H 0.783(4) 0.526(3) 0.8686(4) 0.081 Uiso 1 1 calc R . . H37B H 0.750(2) 0.619(4) 0.8818(10) 0.081 Uiso 1 1 calc R . . C38 C 0.6699(8) 0.5462(5) 0.9035(6) 0.078(4) Uani 1 1 d . . . O39 O 0.6312(6) 0.5900(5) 0.9353(4) 0.095(3) Uani 1 1 d . . . N40 N 0.6404(6) 0.4841(9) 0.9175(3) 0.124(7) Uani 1 1 d . . . H40A H 0.6594 0.4512 0.9016 0.149 Uiso 1 1 calc R . . H40B H 0.6039 0.4799 0.9418 0.149 Uiso 1 1 calc R . . C41 C 0.7387(5) 0.6215(4) 0.7341(7) 0.092(5) Uani 1 1 d . . . H41A H 0.714(3) 0.661(4) 0.7410(10) 0.111 Uiso 1 1 calc R . . H41B H 0.699(4) 0.596(3) 0.7174(19) 0.111 Uiso 1 1 calc R . . C42 C 0.8122(5) 0.6328(5) 0.6948(9) 0.135(9) Uani 1 1 d . . . H42A H 0.8363 0.5922 0.6856 0.162 Uiso 1 1 calc R . . H42B H 0.8546 0.6576 0.7124 0.162 Uiso 1 1 calc R . . C43 C 0.7855(8) 0.6685(5) 0.6424(8) 0.098(5) Uani 1 1 d . . . O44 O 0.7231(6) 0.6907(4) 0.6406(6) 0.134(5) Uani 1 1 d . . . N45 N 0.8481(9) 0.6618(9) 0.6137(10) 0.216(14) Uani 1 1 d . . . H45A H 0.8485 0.6776 0.5826 0.259 Uiso 1 1 calc R . . H45B H 0.8905 0.6415 0.6253 0.259 Uiso 1 1 calc R . . C46 C 1.0626(4) 0.4915(3) 0.8216(3) 0.0363(15) Uani 1 1 d . . . H46A H 1.127(4) 0.490(3) 0.8209(9) 0.054 Uiso 1 1 calc R . . H46B H 1.041(3) 0.464(2) 0.8525(17) 0.054 Uiso 1 1 calc R . . H46C H 1.043(3) 0.538(3) 0.8267(12) 0.054 Uiso 1 1 calc R . . C47 C 1.0563(7) 0.5079(4) 0.7244(4) 0.056(2) Uani 1 1 d . . . H47A H 1.033(4) 0.486(2) 0.684(2) 0.084 Uiso 1 1 calc R . . H47B H 1.129(4) 0.511(3) 0.7236(17) 0.084 Uiso 1 1 calc R . . H47C H 1.028(4) 0.559(3) 0.7296(16) 0.084 Uiso 1 1 calc R . . C48 C 1.0924(4) 0.3741(3) 0.7150(3) 0.0330(14) Uani 1 1 d . . . H48A H 1.0652 0.3943 0.6854 0.040 Uiso 1 1 calc R . . H48B H 1.0871 0.3287 0.7103 0.040 Uiso 1 1 calc R . . C49 C 1.1853(4) 0.3914(3) 0.7131(3) 0.0417(16) Uani 1 1 d . . . H49A H 1.2097 0.3735 0.6815 0.050 Uiso 1 1 calc R . . H49B H 1.1911 0.4371 0.7112 0.050 Uiso 1 1 calc R . . C50 C 1.2313(3) 0.3672(3) 0.7601(3) 0.0323(13) Uani 1 1 d . . . O51 O 1.2538(3) 0.4029(2) 0.7959(2) 0.0466(13) Uani 1 1 d . . . N52 N 1.2474(3) 0.3059(2) 0.7600(3) 0.0335(11) Uani 1 1 d . . . H52A H 1.2746 0.2892 0.7856 0.040 Uiso 1 1 calc R . . H52B H 1.2308 0.2825 0.7344 0.040 Uiso 1 1 calc R . . C54 C 0.8401(4) 0.1710(3) 0.8036(3) 0.0319(13) Uani 1 1 d . . . H54A H 0.820(3) 0.129(2) 0.8008(4) 0.048 Uiso 1 1 calc R . . H54B H 0.805(3) 0.194(2) 0.8259(14) 0.048 Uiso 1 1 calc R . . H54C H 0.894(3) 0.171(2) 0.8176(12) 0.048 Uiso 1 1 calc R . . C53 C 1.0195(4) 0.2526(3) 0.7737(3) 0.0281(12) Uani 1 1 d . . . H53A H 1.0010 0.2174 0.7946 0.042 Uiso 1 1 calc R . . H53B H 1.0626 0.2748 0.7921 0.042 Uiso 1 1 calc R . . H53C H 1.0404 0.2374 0.7407 0.042 Uiso 1 1 calc R . . C55 C 0.9012(3) 0.1632(2) 0.7127(2) 0.0223(11) Uani 1 1 d . . . H55A H 0.9528 0.1566 0.7315 0.027 Uiso 1 1 calc R . . H55B H 0.8769 0.1218 0.7064 0.027 Uiso 1 1 calc R . . C56 C 0.9207(4) 0.1942(3) 0.6596(2) 0.0260(12) Uani 1 1 d . . . H56A H 0.871(3) 0.1893(4) 0.6349(14) 0.031 Uiso 1 1 calc R . . H56B H 0.9315(7) 0.242(3) 0.6649(4) 0.031 Uiso 1 1 calc R . . C57 C 0.9958(4) 0.1634(3) 0.6352(2) 0.0266(12) Uani 1 1 d . . . O58 O 1.0652(3) 0.1678(2) 0.6560(2) 0.0322(10) Uani 1 1 d . . . N59 N 0.9833(4) 0.1283(2) 0.5924(2) 0.0301(11) Uani 1 1 d . . . H59 H 0.940(5) 0.1245(5) 0.5822(13) 0.036 Uiso 1 1 calc R . . C60 C 0.6954(4) 0.1516(3) 0.7350(3) 0.0334(13) Uani 1 1 d . . . H60A H 0.6398 0.1642 0.7251 0.040 Uiso 1 1 calc R . . H60B H 0.6950 0.1430 0.7725 0.040 Uiso 1 1 calc R . . C61 C 0.7173(4) 0.0903(3) 0.7059(3) 0.0298(13) Uani 1 1 d . . . O62 O 0.7374(3) 0.0918(2) 0.6592(2) 0.0379(11) Uani 1 1 d . . . N63 N 0.7123(3) 0.0361(2) 0.7335(3) 0.0371(12) Uani 1 1 d . . . H63A H 0.7234 0.0005 0.7186 0.045 Uiso 1 1 calc R . . H63B H 0.6980 0.0371 0.7660 0.045 Uiso 1 1 calc R . . S1 S 0.75896(12) 0.37128(13) 0.84653(8) 0.0560(6) Uani 1 1 d . . . C71 C 0.8519(6) 0.3839(7) 0.8859(4) 0.072(3) Uani 1 1 d . . . H71A H 0.902(3) 0.425(3) 0.8604(18) 0.087 Uiso 1 1 calc R . . H71B H 0.8303(15) 0.411(2) 0.932(3) 0.087 Uiso 1 1 calc R . . C72 C 0.9001(6) 0.3215(6) 0.8972(4) 0.062(3) Uani 1 1 d . . . H72 H 0.918(2) 0.302(2) 0.861(4) 0.075 Uiso 1 1 calc R . . C73 C 0.9778(7) 0.3389(6) 0.9270(4) 0.074(3) Uani 1 1 d . . . O74 O 1.0378(6) 0.3598(6) 0.8981(5) 0.111(4) Uani 1 1 d . . . O75 O 0.9811(7) 0.3329(8) 0.9758(4) 0.129(5) Uani 1 1 d . . . H75 H 1.0287 0.3390 0.9858 0.193 Uiso 1 1 calc R . . N76 N 0.8512(6) 0.2757(6) 0.9245(4) 0.075(3) Uani 1 1 d . . . H76 H 0.778(8) 0.2909(17) 0.944(2) 0.089 Uiso 1 1 calc R . . C77 C 0.8816(7) 0.2164(8) 0.9302(5) 0.083(4) Uani 1 1 d . . . O78 O 0.9510(6) 0.1998(5) 0.9144(4) 0.098(3) Uani 1 1 d . . . C79 C 0.8262(11) 0.1654(9) 0.9549(6) 0.109(5) Uani 1 1 d . . . H79A H 0.767(7) 0.196(2) 0.994(4) 0.164 Uiso 1 1 calc R . . H79B H 0.880(4) 0.117(5) 0.983(5) 0.164 Uiso 1 1 calc R . . H79C H 0.777(6) 0.132(5) 0.912(3) 0.164 Uiso 1 1 calc R . . N1B N 0.8802(3) 0.4314(2) 0.6120(2) 0.0293(11) Uani 1 1 d . . . C2B C 0.8718(4) 0.4025(3) 0.6591(3) 0.0273(12) Uani 1 1 d . . . H2B H 0.912(3) 0.371(3) 0.6730(12) 0.033 Uiso 1 1 calc R . . N3B N 0.8040(3) 0.4205(2) 0.6848(2) 0.0236(10) Uani 1 1 d . . . C4B C 0.6875(4) 0.4924(3) 0.6534(3) 0.0310(13) Uani 1 1 d . . . H4B H 0.657(3) 0.4877(6) 0.680(3) 0.037 Uiso 1 1 calc R . . C5B C 0.6609(4) 0.5296(3) 0.6126(3) 0.0366(15) Uani 1 1 d . . . C6B C 0.7133(5) 0.5396(3) 0.5687(4) 0.0441(17) Uani 1 1 d . . . C7B C 0.7867(5) 0.5090(3) 0.5633(3) 0.0428(16) Uani 1 1 d . . . H7B H 0.824(4) 0.5142(6) 0.529(3) 0.051 Uiso 1 1 calc R . . C8B C 0.8110(4) 0.4699(3) 0.6054(3) 0.0306(13) Uani 1 1 d . . . C9B C 0.7632(4) 0.4626(3) 0.6504(3) 0.0268(12) Uani 1 1 d . . . C10B C 0.5754(5) 0.5586(4) 0.6132(4) 0.0459(18) Uani 1 1 d . . . H10A H 0.5789(7) 0.599(3) 0.606(3) 0.069 Uiso 1 1 calc R . . H10B H 0.553(2) 0.554(3) 0.644(2) 0.069 Uiso 1 1 calc R . . H10C H 0.544(3) 0.540(3) 0.590(2) 0.069 Uiso 1 1 calc R . . C11B C 0.6848(6) 0.5805(5) 0.5238(4) 0.060(2) Uani 1 1 d . . . H11A H 0.628(5) 0.568(3) 0.514(2) 0.090 Uiso 1 1 calc R . . H11B H 0.722(4) 0.575(3) 0.493(2) 0.090 Uiso 1 1 calc R . . H11C H 0.685(5) 0.626(3) 0.5347(13) 0.090 Uiso 1 1 calc R . . C1R C 0.9325(4) 0.4098(3) 0.5701(3) 0.0343(14) Uani 1 1 d . . . H1R H 0.9384(7) 0.444(3) 0.542(3) 0.041 Uiso 1 1 calc R . . C2R C 0.9008(4) 0.3485(3) 0.5449(3) 0.0253(12) Uani 1 1 d . . . H2R H 0.871(3) 0.3551(8) 0.523(3) 0.030 Uiso 1 1 calc R . . C3R C 0.9817(4) 0.3209(3) 0.5241(3) 0.0293(12) Uani 1 1 d . . . H3R H 0.9984(15) 0.3423(19) 0.492(3) 0.035 Uiso 1 1 calc R . . C4R C 1.0423(4) 0.3360(3) 0.5690(3) 0.0362(15) Uani 1 1 d . . . H4R H 1.0387(5) 0.302(3) 0.596(3) 0.043 Uiso 1 1 calc R . . C5R C 1.1312(5) 0.3450(5) 0.5537(4) 0.053(2) Uani 1 1 d . . . O6R O 1.0108(3) 0.3946(3) 0.5915(2) 0.0398(11) Uani 1 1 d . . . O7R O 0.8654(3) 0.31072(19) 0.58330(18) 0.0270(9) Uani 1 1 d . . . H7R H 0.8359 0.2838 0.5695 0.041 Uiso 1 1 calc R . . O8RA O 1.1442(8) 0.3943(8) 0.5234(6) 0.066(4) Uani 0.50 1 d P . . H8RA H 1.1284 0.3863 0.4935 0.098 Uiso 0.50 1 calc PR . . O8RB O 1.1768(8) 0.3663(8) 0.5885(6) 0.071(4) Uani 0.50 1 d P . . H8RB H 1.2113 0.3900 0.5754 0.107 Uiso 0.50 1 calc PR . . P1 P 1.00830(10) 0.22052(9) 0.46348(6) 0.0326(4) Uani 1 1 d . . . O2P O 0.9751(3) 0.2540(2) 0.51586(17) 0.0322(10) Uani 1 1 d . . . O3P O 1.0238(3) 0.1519(3) 0.48459(18) 0.0369(11) Uani 1 1 d . . . O4P O 0.9393(3) 0.2133(3) 0.4243(2) 0.0431(12) Uani 1 1 d . . . O5P O 1.0856(3) 0.2528(3) 0.44612(19) 0.0465(13) Uani 1 1 d . . . C65 C 1.0515(4) 0.0965(3) 0.5642(3) 0.0382(15) Uani 1 1 d . . . H65A H 1.0300(14) 0.056(3) 0.5475(11) 0.046 Uiso 1 1 calc R . . H65B H 1.096(3) 0.0844(9) 0.5901(17) 0.046 Uiso 1 1 calc R . . C66 C 1.0882(4) 0.1382(4) 0.5224(3) 0.0379(16) Uani 1 1 d . . . H66 H 1.1112(19) 0.184(4) 0.5404(15) 0.045 Uiso 1 1 calc R . . C67 C 1.1596(5) 0.1043(5) 0.4932(3) 0.055(2) Uani 1 1 d . . . H67A H 1.189(3) 0.137(2) 0.466(3) 0.082 Uiso 1 1 calc R . . H67B H 1.1351(17) 0.064(3) 0.471(3) 0.082 Uiso 1 1 calc R . . H67C H 1.205(4) 0.088(3) 0.5215(18) 0.082 Uiso 1 1 calc R . . Na1 Na 1.1653(8) 0.3989(7) 0.9523(7) 0.164(8) Uani 0.65(3) 1 d P . . OW1 O 1.2056(4) 0.2435(3) 0.6590(2) 0.0493(13) Uani 1 1 d . . . OW2 O 0.7530(3) 0.2386(3) 0.5323(2) 0.0447(12) Uani 1 1 d . . . OW3 O 0.8016(4) 0.2859(3) 0.4301(2) 0.0493(13) Uani 1 1 d . . . OW4 O 0.920(2) 0.2508(10) 1.0555(6) 0.287(18) Uani 1 1 d . . . OW5 O 0.5162(8) 0.4491(6) 0.9905(5) 0.055(5) Uani 0.51(3) 1 d P . . OW6 O 0.8123(5) 0.1153(4) 0.5580(4) 0.094(3) Uani 1 1 d . . . OW7 O 1.2898(12) 0.4886(7) 0.5024(5) 0.158(6) Uani 1 1 d . . . OW8 O 0.5262(15) 0.3491(9) 0.9302(15) 0.293(17) Uani 1 1 d . . . OW9 O 0.6861(8) 0.2863(6) 0.9717(8) 0.170(7) Uani 1 1 d . . . OW10 O 0.7049(19) 0.7674(12) 0.5779(10) 0.087(11) Uani 0.35(3) 1 d P . . OW11 O 0.3935(5) 0.6203(4) 0.6506(4) 0.093(3) Uani 1 1 d . . . OW12 O 1.3278(16) 0.3891(9) 0.8872(7) 0.243(13) Uani 1 1 d . . . OW13 O 0.9959(8) 0.0783(7) 0.9060(5) 0.137(5) Uani 1 1 d . . . OW14 O 0.7525(15) 0.0038(14) 0.5768(10) 0.085(10) Uani 0.34(3) 1 d P . . OW15 O 1.0988(9) 0.3707(6) 0.4040(6) 0.137(5) Uani 1 1 d . . . OW16 O 0.3896(11) 0.4976(10) 0.9447(7) 0.185(8) Uani 1 1 d . . . OW17 O 1.1055(10) 0.3262(8) 1.0536(9) 0.199(10) Uani 1 1 d . . . OW18 O 0.1705(12) 0.5025(7) 0.6075(8) 0.186(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0168(3) 0.0197(3) 0.0387(4) -0.0189(3) -0.0090(3) 0.0113(3) N21 0.018(2) 0.028(2) 0.022(2) -0.0137(18) -0.0045(17) 0.0123(17) N22 0.028(3) 0.036(3) 0.071(4) -0.039(3) -0.024(3) 0.022(2) N23 0.020(2) 0.024(3) 0.063(4) -0.027(2) -0.021(2) 0.0141(19) N24 0.011(2) 0.030(2) 0.027(2) -0.0050(18) 0.0000(17) 0.0057(16) C1 0.015(2) 0.020(3) 0.026(3) -0.007(2) 0.000(2) 0.0047(18) C2 0.019(3) 0.026(3) 0.026(3) -0.005(2) -0.002(2) -0.0006(19) C3 0.018(3) 0.032(3) 0.031(3) 0.002(2) 0.003(2) 0.006(2) C4 0.017(3) 0.042(3) 0.026(3) -0.004(3) -0.001(2) 0.013(2) C5 0.031(3) 0.043(4) 0.039(3) -0.025(3) -0.010(3) 0.030(3) C6 0.032(4) 0.045(4) 0.068(5) -0.039(4) -0.030(3) 0.030(3) C7 0.061(6) 0.048(5) 0.112(8) -0.060(5) -0.053(6) 0.045(4) C8 0.033(5) 0.045(5) 0.235(16) -0.098(8) -0.063(7) 0.032(4) C9 0.041(5) 0.035(4) 0.180(12) -0.072(6) -0.052(6) 0.027(3) C10 0.033(4) 0.031(4) 0.262(19) -0.073(7) -0.060(7) 0.015(3) C11 0.026(4) 0.032(4) 0.119(8) -0.041(4) -0.030(4) 0.008(3) C12 0.030(3) 0.019(3) 0.062(4) -0.016(3) -0.017(3) 0.008(2) C13 0.021(3) 0.016(3) 0.063(4) -0.010(3) -0.020(3) 0.002(2) C14 0.023(3) 0.024(3) 0.036(3) -0.008(2) -0.011(2) 0.012(2) C15 0.015(2) 0.023(3) 0.038(3) -0.013(2) -0.004(2) 0.0059(19) C16 0.022(3) 0.016(2) 0.022(2) -0.0049(19) -0.002(2) 0.0067(18) C17 0.020(2) 0.013(2) 0.030(3) -0.001(2) 0.005(2) 0.0036(18) C18 0.019(3) 0.017(3) 0.039(3) -0.003(2) 0.003(2) 0.0037(19) C19 0.016(2) 0.026(3) 0.027(3) -0.006(2) 0.002(2) 0.008(2) C20 0.015(2) 0.023(3) 0.023(2) -0.008(2) 0.0026(19) -0.0017(19) C25 0.017(3) 0.029(3) 0.036(3) -0.001(2) -0.001(2) -0.005(2) C26 0.019(3) 0.038(3) 0.029(3) 0.008(3) 0.004(2) 0.007(2) C27 0.021(3) 0.047(4) 0.030(3) 0.011(3) 0.001(2) 0.005(3) O28 0.029(3) 0.068(4) 0.073(4) 0.026(3) 0.017(3) 0.016(3) N29 0.037(4) 0.048(4) 0.096(6) 0.010(4) 0.018(4) 0.004(3) C30 0.017(3) 0.033(3) 0.036(3) 0.001(2) 0.000(2) 0.002(2) C31 0.018(3) 0.042(3) 0.043(3) 0.005(3) -0.006(2) 0.004(3) C32 0.023(3) 0.058(5) 0.058(5) 0.013(4) -0.012(3) -0.003(3) O33 0.053(3) 0.038(3) 0.062(3) 0.006(3) -0.007(3) 0.010(2) N34 0.049(4) 0.074(5) 0.055(4) 0.007(4) -0.008(3) 0.018(4) C35 0.035(4) 0.058(5) 0.047(4) -0.018(3) -0.002(3) 0.027(3) C36 0.065(6) 0.057(5) 0.106(8) -0.057(6) -0.053(6) 0.051(5) C37 0.080(7) 0.054(5) 0.068(6) -0.028(5) -0.020(6) 0.015(5) C38 0.067(7) 0.045(5) 0.123(10) 0.007(6) -0.051(7) -0.024(5) O39 0.099(7) 0.094(6) 0.090(6) -0.035(5) 0.021(5) 0.029(5) N40 0.058(6) 0.29(2) 0.027(4) -0.026(7) -0.014(4) 0.019(9) C41 0.020(4) 0.026(4) 0.231(17) -0.048(7) -0.009(6) 0.012(3) C42 0.014(4) 0.050(6) 0.34(3) -0.113(11) 0.035(8) -0.014(4) C43 0.052(6) 0.031(4) 0.209(17) -0.032(7) 0.028(9) -0.001(4) O44 0.096(7) 0.055(4) 0.252(14) 0.009(6) 0.118(9) 0.012(5) N45 0.087(9) 0.199(18) 0.36(3) -0.20(2) 0.127(15) -0.073(11) C46 0.021(3) 0.032(3) 0.056(4) -0.024(3) -0.005(3) -0.001(2) C47 0.073(6) 0.027(4) 0.068(6) -0.006(3) -0.010(5) 0.009(4) C48 0.021(3) 0.015(3) 0.063(4) -0.004(3) -0.010(3) -0.001(2) C49 0.025(3) 0.030(3) 0.069(5) -0.008(3) -0.009(3) -0.002(3) C50 0.012(3) 0.030(3) 0.056(4) -0.004(3) -0.004(3) -0.005(2) O51 0.030(2) 0.035(3) 0.075(4) -0.019(3) -0.009(2) 0.004(2) N52 0.027(3) 0.025(2) 0.049(3) -0.005(2) -0.005(2) 0.0014(19) C54 0.026(3) 0.036(3) 0.034(3) 0.003(3) 0.004(3) 0.006(2) C53 0.020(3) 0.021(3) 0.043(3) -0.003(2) -0.002(2) 0.007(2) C55 0.019(3) 0.016(2) 0.033(3) -0.004(2) -0.001(2) 0.0050(19) C56 0.027(3) 0.021(3) 0.030(3) 0.003(2) 0.009(2) 0.014(2) C57 0.029(3) 0.013(2) 0.037(3) 0.004(2) 0.011(2) 0.007(2) O58 0.022(2) 0.028(2) 0.047(3) -0.0044(19) 0.0047(19) 0.0030(16) N59 0.024(3) 0.025(2) 0.041(3) -0.007(2) 0.003(2) 0.0085(19) C60 0.025(3) 0.027(3) 0.049(4) -0.007(3) -0.001(3) -0.001(2) C61 0.014(3) 0.018(3) 0.057(4) -0.001(2) 0.004(3) -0.006(2) O62 0.044(3) 0.028(2) 0.042(3) -0.0023(19) -0.005(2) -0.0046(19) N63 0.029(3) 0.022(2) 0.060(4) 0.007(2) 0.006(3) 0.004(2) S1 0.0316(10) 0.0955(17) 0.0409(10) -0.0273(10) -0.0061(8) 0.0217(10) C71 0.038(5) 0.127(10) 0.052(5) -0.039(6) -0.014(4) 0.026(5) C72 0.038(4) 0.109(8) 0.040(4) -0.008(5) -0.004(4) -0.003(5) C73 0.060(7) 0.103(9) 0.060(6) -0.004(6) -0.027(5) 0.013(6) O74 0.064(5) 0.148(9) 0.122(8) 0.051(7) -0.032(5) -0.034(6) O75 0.082(6) 0.227(14) 0.078(6) -0.040(7) -0.047(5) 0.024(8) N76 0.062(6) 0.106(8) 0.056(5) 0.006(5) -0.006(4) 0.020(5) C77 0.051(6) 0.137(12) 0.063(6) 0.017(7) 0.001(5) -0.022(7) O78 0.063(5) 0.127(8) 0.105(7) 0.042(6) 0.008(5) 0.024(5) C79 0.103(11) 0.140(14) 0.085(9) 0.008(9) 0.026(8) -0.020(10) N1B 0.023(3) 0.015(2) 0.050(3) -0.003(2) 0.005(2) -0.0009(18) C2B 0.019(3) 0.011(2) 0.052(4) -0.004(2) -0.001(2) 0.0037(19) N3B 0.012(2) 0.0099(19) 0.049(3) -0.0023(19) -0.0051(19) 0.0046(15) C4B 0.023(3) 0.021(3) 0.049(4) -0.002(3) -0.001(3) 0.001(2) C5B 0.027(3) 0.025(3) 0.058(4) 0.000(3) -0.005(3) 0.010(2) C6B 0.035(4) 0.030(3) 0.067(5) 0.009(3) 0.002(4) 0.000(3) C7B 0.040(4) 0.020(3) 0.068(5) 0.003(3) 0.000(4) 0.000(3) C8B 0.022(3) 0.016(3) 0.054(4) -0.004(3) -0.006(3) 0.000(2) C9B 0.022(3) 0.015(2) 0.043(3) -0.003(2) -0.009(2) -0.0003(19) C10B 0.030(4) 0.036(4) 0.072(5) 0.005(4) -0.006(3) 0.017(3) C11B 0.057(5) 0.053(5) 0.070(6) 0.023(4) 0.007(5) 0.018(4) C1R 0.023(3) 0.024(3) 0.056(4) -0.002(3) 0.002(3) -0.002(2) C2R 0.019(3) 0.018(3) 0.039(3) -0.003(2) 0.000(2) 0.001(2) C3R 0.026(3) 0.028(3) 0.034(3) -0.001(2) 0.003(2) 0.000(2) C4R 0.025(3) 0.036(3) 0.048(4) -0.013(3) 0.006(3) 0.006(3) C5R 0.027(4) 0.064(5) 0.068(6) -0.012(5) 0.013(4) -0.009(3) O6R 0.021(2) 0.043(3) 0.056(3) -0.015(2) -0.001(2) 0.000(2) O7R 0.022(2) 0.0194(19) 0.040(2) -0.0067(17) 0.0037(17) -0.0014(15) O8RA 0.042(7) 0.083(10) 0.071(8) -0.022(8) 0.000(6) -0.011(7) O8RB 0.031(6) 0.091(11) 0.092(10) -0.042(8) -0.007(6) 0.006(6) P1 0.0195(7) 0.0508(10) 0.0274(7) -0.0092(7) 0.0029(6) 0.0079(7) O2P 0.032(2) 0.035(2) 0.030(2) -0.0030(18) 0.0106(18) 0.0045(18) O3P 0.029(2) 0.049(3) 0.033(2) -0.016(2) -0.0005(19) 0.010(2) O4P 0.026(2) 0.068(4) 0.035(2) -0.003(2) -0.006(2) 0.005(2) O5P 0.031(3) 0.079(4) 0.030(2) -0.006(2) 0.008(2) -0.001(3) C65 0.031(3) 0.039(4) 0.045(4) -0.018(3) 0.007(3) 0.012(3) C66 0.030(3) 0.054(4) 0.030(3) -0.019(3) 0.000(3) 0.019(3) C67 0.034(4) 0.078(6) 0.051(4) -0.014(4) 0.005(3) 0.018(4) Na1 0.118(10) 0.146(11) 0.228(17) 0.040(10) -0.083(10) -0.053(8) OW1 0.042(3) 0.038(3) 0.068(3) -0.016(2) 0.010(3) -0.010(2) OW2 0.023(2) 0.062(3) 0.048(3) -0.010(2) -0.007(2) -0.004(2) OW3 0.046(3) 0.053(3) 0.049(3) 0.009(2) 0.002(2) 0.005(2) OW4 0.57(5) 0.198(18) 0.090(9) -0.048(10) -0.077(17) 0.20(3) OW5 0.043(7) 0.069(9) 0.054(7) 0.003(6) 0.002(5) -0.010(6) OW6 0.064(5) 0.089(6) 0.129(8) -0.022(5) -0.035(5) 0.024(4) OW7 0.25(2) 0.130(10) 0.090(7) -0.016(7) 0.032(10) 0.007(12) OW8 0.20(2) 0.128(14) 0.55(5) -0.01(2) 0.15(3) 0.027(14) OW9 0.106(9) 0.104(8) 0.30(2) -0.043(11) 0.090(12) -0.037(7) OW10 0.11(2) 0.076(16) 0.076(16) 0.016(11) 0.009(14) 0.021(14) OW11 0.057(4) 0.081(5) 0.142(8) -0.050(5) 0.026(5) -0.010(4) OW12 0.37(3) 0.174(15) 0.185(15) -0.083(13) -0.179(19) 0.127(18) OW13 0.100(8) 0.186(13) 0.126(9) 0.023(9) 0.031(7) 0.058(8) OW14 0.057(14) 0.11(2) 0.089(18) -0.023(14) -0.002(12) 0.019(13) OW15 0.142(11) 0.109(8) 0.159(11) -0.011(8) 0.086(9) -0.034(8) OW16 0.142(13) 0.25(2) 0.161(14) -0.070(14) -0.008(11) -0.062(13) OW17 0.111(10) 0.164(14) 0.32(3) -0.105(16) -0.066(14) 0.039(10) OW18 0.207(17) 0.098(9) 0.25(2) 0.006(11) -0.106(16) -0.032(10) _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 N21 1.878(5) . ? Co1 N24 1.884(5) . ? Co1 N22 1.916(5) . ? Co1 N23 1.929(5) . ? Co1 N3B 2.058(6) . ? Co1 S1 2.250(2) . ? N21 C4 1.292(7) . ? N21 C1 1.479(7) . ? N22 C9 1.354(12) . ? N22 C6 1.395(9) . ? N23 C11 1.346(10) . ? N23 C14 1.381(7) . ? N24 C16 1.297(7) . ? N24 C19 1.486(7) . ? C1 C20 1.534(8) . ? C1 C19 1.538(7) . ? C1 C2 1.590(8) . ? C2 C25 1.534(8) . ? C2 C26 1.555(8) . ? C2 C3 1.567(8) . ? C3 C4 1.499(9) . ? C3 C30 1.553(9) . ? C4 C5 1.480(9) . ? C5 C6 1.354(12) . ? C5 C35 1.525(9) . ? C6 C7 1.543(10) . ? C7 C37 1.464(14) . ? C7 C8 1.51(2) . ? C7 C36 1.560(9) . ? C8 C9 1.505(9) . ? C8 C41 1.55(2) . ? C9 C10 1.358(12) . ? C10 C11 1.386(10) . ? C11 C12 1.516(10) . ? C12 C46 1.517(10) . ? C12 C47 1.528(13) . ? C12 C13 1.582(8) . ? C13 C48 1.502(11) . ? C13 C14 1.530(9) . ? C14 C15 1.386(8) . ? C15 C16 1.457(8) . ? C15 C53 1.516(7) . ? C16 C17 1.525(7) . ? C17 C54 1.543(8) . ? C17 C18 1.548(8) . ? C17 C55 1.559(7) . ? C18 C60 1.516(8) . ? C18 C19 1.545(7) . ? C26 C27 1.529(9) . ? C27 O28 1.222(9) . ? C27 N29 1.286(11) . ? C30 C31 1.528(8) . ? C31 C32 1.484(10) . ? C32 O33 1.262(11) . ? C32 N34 1.324(12) . ? C37 C38 1.285(19) . ? C38 O39 1.378(17) . ? C38 N40 1.44(2) . ? C41 C42 1.570(19) . ? C42 C43 1.59(3) . ? C43 O44 1.113(16) . ? C43 N45 1.254(17) . ? C48 C49 1.545(9) . ? C49 C50 1.498(11) . ? C50 O51 1.236(9) . ? C50 N52 1.320(8) . ? C55 C56 1.533(8) . ? C56 C57 1.510(8) . ? C57 O58 1.243(8) . ? C57 N59 1.333(9) . ? N59 C65 1.475(8) . ? C60 C61 1.530(8) . ? C61 O62 1.231(9) . ? C61 N63 1.344(8) . ? S1 C71 1.825(9) . ? C71 C72 1.554(17) . ? C72 N76 1.426(15) . ? C72 C73 1.511(14) . ? C73 O75 1.250(16) . ? C73 O74 1.294(16) . ? O74 Na1 2.611(14) . ? N76 C77 1.351(19) . ? C77 O78 1.241(16) . ? C77 C79 1.53(2) . ? N1B C2B 1.352(9) . ? N1B C8B 1.391(8) . ? N1B C1R 1.435(9) . ? C2B N3B 1.330(8) . ? N3B C9B 1.409(8) . ? C4B C5B 1.371(10) . ? C4B C9B 1.377(8) . ? C5B C6B 1.417(11) . ? C5B C10B 1.511(9) . ? C6B C7B 1.357(11) . ? C6B C11B 1.504(12) . ? C7B C8B 1.406(11) . ? C8B C9B 1.391(10) . ? C1R O6R 1.415(8) . ? C1R C2R 1.531(8) . ? C2R O7R 1.384(8) . ? C2R C3R 1.525(8) . ? C3R O2P 1.429(8) . ? C3R C4R 1.538(10) . ? C4R O6R 1.453(8) . ? C4R C5R 1.501(10) . ? C5R O8RB 1.236(16) . ? C5R O8RA 1.310(19) . ? P1 O5P 1.489(6) . ? P1 O4P 1.504(5) . ? P1 O3P 1.564(6) . ? P1 O2P 1.600(4) . ? O3P C66 1.446(8) . ? C65 C66 1.502(11) . ? C66 C67 1.548(9) . ? Na1 OW14 2.68(3) 4_756 ? Na1 OW7 2.79(2) 2_765 ? OW7 Na1 2.79(2) 2_764 ? OW14 Na1 2.68(3) 4_746 ? 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 N21 Co1 N24 83.2(2) . . ? N21 Co1 N22 89.9(2) . . ? N24 Co1 N22 172.1(3) . . ? N21 Co1 N23 173.0(2) . . ? N24 Co1 N23 90.8(2) . . ? N22 Co1 N23 96.4(2) . . ? N21 Co1 N3B 92.3(2) . . ? N24 Co1 N3B 94.91(19) . . ? N22 Co1 N3B 89.1(3) . . ? N23 Co1 N3B 84.8(2) . . ? N21 Co1 S1 87.65(16) . . ? N24 Co1 S1 87.42(16) . . ? N22 Co1 S1 88.6(2) . . ? N23 Co1 S1 95.5(2) . . ? N3B Co1 S1 177.64(14) . . ? C4 N21 C1 113.1(5) . . ? C4 N21 Co1 130.1(4) . . ? C1 N21 Co1 116.7(3) . . ? C9 N22 C6 110.8(6) . . ? C9 N22 Co1 121.9(5) . . ? C6 N22 Co1 127.0(6) . . ? C11 N23 C14 110.5(5) . . ? C11 N23 Co1 122.7(4) . . ? C14 N23 Co1 126.0(4) . . ? C16 N24 C19 111.5(5) . . ? C16 N24 Co1 132.8(4) . . ? C19 N24 Co1 114.0(3) . . ? N21 C1 C20 112.5(5) . . ? N21 C1 C19 101.8(4) . . ? C20 C1 C19 109.3(4) . . ? N21 C1 C2 101.3(4) . . ? C20 C1 C2 113.1(4) . . ? C19 C1 C2 118.0(5) . . ? C25 C2 C26 109.8(5) . . ? C25 C2 C3 113.2(5) . . ? C26 C2 C3 107.1(5) . . ? C25 C2 C1 114.3(5) . . ? C26 C2 C1 110.3(5) . . ? C3 C2 C1 101.7(4) . . ? C4 C3 C30 109.0(5) . . ? C4 C3 C2 101.1(4) . . ? C30 C3 C2 119.0(5) . . ? N21 C4 C5 123.8(6) . . ? N21 C4 C3 112.6(5) . . ? C5 C4 C3 123.6(5) . . ? C6 C5 C4 121.2(6) . . ? C6 C5 C35 124.5(6) . . ? C4 C5 C35 114.3(7) . . ? C5 C6 N22 122.9(6) . . ? C5 C6 C7 130.8(7) . . ? N22 C6 C7 106.2(7) . . ? C37 C7 C8 97.6(9) . . ? C37 C7 C6 112.9(8) . . ? C8 C7 C6 101.1(7) . . ? C37 C7 C36 112.0(8) . . ? C8 C7 C36 112.0(10) . . ? C6 C7 C36 118.6(7) . . ? C9 C8 C7 101.9(9) . . ? C9 C8 C41 108.9(11) . . ? C7 C8 C41 112.3(7) . . ? N22 C9 C10 125.0(7) . . ? N22 C9 C8 109.2(8) . . ? C10 C9 C8 125.0(7) . . ? C9 C10 C11 128.3(8) . . ? N23 C11 C10 123.5(7) . . ? N23 C11 C12 113.9(6) . . ? C10 C11 C12 122.6(7) . . ? C11 C12 C46 109.3(7) . . ? C11 C12 C47 107.8(7) . . ? C46 C12 C47 110.4(6) . . ? C11 C12 C13 101.2(5) . . ? C46 C12 C13 111.4(6) . . ? C47 C12 C13 116.1(6) . . ? C48 C13 C14 112.3(5) . . ? C48 C13 C12 114.9(6) . . ? C14 C13 C12 103.7(5) . . ? N23 C14 C15 125.8(6) . . ? N23 C14 C13 110.4(5) . . ? C15 C14 C13 123.6(5) . . ? C14 C15 C16 121.5(5) . . ? C14 C15 C53 118.6(5) . . ? C16 C15 C53 119.8(5) . . ? N24 C16 C15 122.1(5) . . ? N24 C16 C17 110.8(5) . . ? C15 C16 C17 127.1(4) . . ? C16 C17 C54 108.8(5) . . ? C16 C17 C18 102.0(4) . . ? C54 C17 C18 111.8(5) . . ? C16 C17 C55 114.0(4) . . ? C54 C17 C55 108.6(4) . . ? C18 C17 C55 111.6(5) . . ? C60 C18 C19 113.1(5) . . ? C60 C18 C17 116.8(5) . . ? C19 C18 C17 101.2(4) . . ? N24 C19 C1 106.6(4) . . ? N24 C19 C18 102.0(4) . . ? C1 C19 C18 123.6(5) . . ? C27 C26 C2 112.9(5) . . ? O28 C27 N29 122.6(7) . . ? O28 C27 C26 122.6(7) . . ? N29 C27 C26 114.9(6) . . ? C31 C30 C3 113.6(5) . . ? C32 C31 C30 110.8(6) . . ? O33 C32 N34 123.7(8) . . ? O33 C32 C31 121.2(8) . . ? N34 C32 C31 115.1(8) . . ? C38 C37 C7 110.7(11) . . ? C37 C38 O39 120.1(9) . . ? C37 C38 N40 131.7(13) . . ? O39 C38 N40 108.3(13) . . ? C8 C41 C42 116.3(10) . . ? C41 C42 C43 113.6(10) . . ? O44 C43 N45 139(2) . . ? O44 C43 C42 118.6(15) . . ? N45 C43 C42 102.5(18) . . ? C13 C48 C49 116.1(6) . . ? C50 C49 C48 112.1(6) . . ? O51 C50 N52 122.7(7) . . ? O51 C50 C49 121.9(6) . . ? N52 C50 C49 115.4(6) . . ? C56 C55 C17 114.9(4) . . ? C57 C56 C55 110.2(4) . . ? O58 C57 N59 121.8(5) . . ? O58 C57 C56 121.2(6) . . ? N59 C57 C56 116.9(6) . . ? C57 N59 C65 122.4(6) . . ? C18 C60 C61 114.6(5) . . ? O62 C61 N63 122.8(6) . . ? O62 C61 C60 120.5(6) . . ? N63 C61 C60 116.7(6) . . ? C71 S1 Co1 110.5(4) . . ? C72 C71 S1 113.0(8) . . ? N76 C72 C73 112.3(9) . . ? N76 C72 C71 112.6(9) . . ? C73 C72 C71 107.7(10) . . ? O75 C73 O74 124.5(11) . . ? O75 C73 C72 120.7(12) . . ? O74 C73 C72 114.8(9) . . ? C73 O74 Na1 113.5(9) . . ? C77 N76 C72 118.5(10) . . ? O78 C77 N76 123.7(12) . . ? O78 C77 C79 117.5(15) . . ? N76 C77 C79 118.8(13) . . ? C2B N1B C8B 106.8(5) . . ? C2B N1B C1R 125.1(5) . . ? C8B N1B C1R 124.6(6) . . ? N3B C2B N1B 112.9(5) . . ? C2B N3B C9B 105.1(5) . . ? C2B N3B Co1 121.7(4) . . ? C9B N3B Co1 132.7(4) . . ? C5B C4B C9B 119.8(7) . . ? C4B C5B C6B 119.7(6) . . ? C4B C5B C10B 120.7(7) . . ? C6B C5B C10B 119.6(7) . . ? C7B C6B C5B 122.1(7) . . ? C7B C6B C11B 117.6(8) . . ? C5B C6B C11B 120.1(7) . . ? C6B C7B C8B 116.5(8) . . ? N1B C8B C9B 106.4(6) . . ? N1B C8B C7B 131.1(7) . . ? C9B C8B C7B 122.5(6) . . ? C4B C9B C8B 119.2(6) . . ? C4B C9B N3B 132.0(6) . . ? C8B C9B N3B 108.7(5) . . ? O6R C1R N1B 108.1(6) . . ? O6R C1R C2R 105.7(5) . . ? N1B C1R C2R 112.5(5) . . ? O7R C2R C3R 112.3(5) . . ? O7R C2R C1R 109.1(5) . . ? C3R C2R C1R 100.4(5) . . ? O2P C3R C2R 111.3(5) . . ? O2P C3R C4R 111.1(5) . . ? C2R C3R C4R 102.0(5) . . ? O6R C4R C5R 109.3(6) . . ? O6R C4R C3R 104.3(5) . . ? C5R C4R C3R 116.3(7) . . ? O8RB C5R O8RA 92.3(12) . . ? O8RB C5R C4R 115.4(10) . . ? O8RA C5R C4R 113.9(10) . . ? C1R O6R C4R 110.6(5) . . ? O5P P1 O4P 118.1(3) . . ? O5P P1 O3P 113.0(3) . . ? O4P P1 O3P 104.7(3) . . ? O5P P1 O2P 109.1(3) . . ? O4P P1 O2P 110.4(3) . . ? O3P P1 O2P 100.1(2) . . ? C3R O2P P1 122.1(4) . . ? C66 O3P P1 121.8(5) . . ? N59 C65 C66 111.9(6) . . ? O3P C66 C65 107.7(6) . . ? O3P C66 C67 108.0(5) . . ? C65 C66 C67 111.4(7) . . ? O74 Na1 OW14 120.3(8) . 4_756 ? O74 Na1 OW7 135.6(8) . 2_765 ? OW14 Na1 OW7 45.3(7) 4_756 2_765 ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 29.40 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.303 _refine_diff_density_min -1.073 _refine_diff_density_rms 0.136