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 'Mark Murrie' _publ_contact_author_address ; Department of Chemistry University of Glasgow Glasgow G12 8QQ UNITED KINGDOM ; _publ_contact_author_email MARKM@CHEM.GLA.AC.UK _publ_section_title ; Synthesis and structural characterisation of polynuclear cobalt complexes with partially-deprotonated Bis-tris ; loop_ _publ_author_name 'Mark Murrie' 'Alan Ferguson' 'Andrew Parkin' data_2 _database_code_depnum_ccdc_archive 'CCDC 601284' _audit_creation_date 06-05-20 _audit_creation_method CRYSTALS_ver_12.83 _oxford_structure_analysis_title 'CRYSTALS_cif in P -4 21 c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.2070(7) _cell_length_b 13.2070(7) _cell_length_c 12.5890(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2195.8(2) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P -4 21 c ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z y,-x,-z -x,-y,z -y,x,-z -x+1/2,y+1/2,-z+1/2 -y+1/2,-x+1/2,z+1/2 x+1/2,-y+1/2,-z+1/2 y+1/2,x+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C34 H70 Co5 N4 O22' _chemical_formula_moiety 'C34 H70 Co5 N4 O22' _chemical_compound_source ? _chemical_formula_weight 1181.61 _cell_measurement_reflns_used 301848 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1226 _exptl_absorpt_coefficient_mu 1.938 # Sheldrick geometric approximatio 0.75 0.82 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SORTAV (Blessing)' _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.82 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 2538 _reflns_number_total 2538 _diffrn_reflns_av_R_equivalents 0.087 _diffrn_reflns_theta_min 2.235 _diffrn_reflns_theta_max 27.550 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.550 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.53 _refine_diff_density_max 1.56 _refine_ls_number_reflns 2538 _refine_ls_number_restraints 3 _refine_ls_number_parameters 145 #_refine_ls_R_factor_ref 0.0646 _refine_ls_wR_factor_ref 0.1134 _refine_ls_goodness_of_fit_ref 0.8874 #_reflns_number_all 2538 _refine_ls_R_factor_all 0.0646 _refine_ls_wR_factor_all 0.1134 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1874 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_gt 0.1077 _refine_ls_shift/su_max 0.003078 _refine_ls_abs_structure_Flack 0.50(3) _refine_ls_abs_structure_details 'Flack (1983), 1104 Friedel-pairs' _chemical_absolute_configuration unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _publ_section_exptl_refinement ; The absolute configuration was arbitrarily assigned. All non-H atoms were refined anisotropically with the exception of the solvent molecule, which was refined isotropically as a methanol molecule disordered over 2 sites. The positions of all hydrogen atoms involved in hydrogen bonding were placed geometrically on hydrogen bonds and refined with distance restraints. No su's have been quoted for parameters involving these hydrogen atoms. All other hydrogen atoms were placed geometrically and refined as riding on their parent atoms. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Blessing, SORTAV ( ) Flack, H. D. (1983). Acta Cryst. A39, 876-881. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Co1 Co 0.52624(5) 0.39432(5) 0.22068(5) 0.0368 1.0000 Uani . . . . . . Co2 Co 0.5000 0.5000 0.0000 0.0396 1.0000 Uani S T . . . . C1 C 0.5410(4) 0.2125(4) 0.3073(5) 0.0560 1.0000 Uani . . . . . . N1 N 0.6591(3) 0.3399(3) 0.2311(3) 0.0435 1.0000 Uani . . . . . . O1 O 0.5922(2) 0.5220(2) 0.1994(2) 0.0372 1.0000 Uani . . . . . . C2 C 0.6505(5) 0.2316(4) 0.2708(5) 0.0536 1.0000 Uani . . . . . . O2 O 0.5343(3) 0.4150(3) 0.3721(2) 0.0401 1.0000 Uani D . . . . . O3 O 0.4719(3) 0.2653(2) 0.2435(3) 0.0521 1.0000 Uani . . . . . . C4 C 0.6844(4) 0.5216(4) 0.2550(4) 0.0441 1.0000 Uani . . . . . . O4 O 0.5266(3) 0.3708(3) 0.0735(2) 0.0441 1.0000 Uani . . . . . . C5 C 0.7045(4) 0.4174(4) 0.3058(4) 0.0487 1.0000 Uani . . . . . . C6 C 0.8183(4) 0.4061(5) 0.3238(5) 0.0573 1.0000 Uani . . . . . . C10 C 0.7006(5) 0.3403(4) 0.1180(4) 0.0536 1.0000 Uani . . . . . . O10 O 0.8467(3) 0.3234(3) 0.3868(3) 0.0668 1.0000 Uani D . . . . . C11 C 0.6138(5) 0.3113(4) 0.0461(4) 0.0508 1.0000 Uani . . . . . . C12 C 0.6378(4) 0.4080(5) 0.4059(4) 0.0476 1.0000 Uani . . . . . . C51 C 1.000000(10) 0.50000(10) 0.5058(9) 0.1223 1.0000 Uiso DS . . . . . O60 O 0.9736(7) 0.4119(6) 0.5501(7) 0.0815 0.5000 Uiso D . . . . . H10 H 0.8888 0.2783 0.3414 0.0500 1.0000 Uiso DR . . . . . H11 H 0.5263 0.1405 0.3039 0.0500 1.0000 Uiso R . . . . . H12 H 0.5337 0.2332 0.3818 0.0500 1.0000 Uiso R . . . . . H21 H 0.6972 0.2212 0.3289 0.0500 1.0000 Uiso R . . . . . H22 H 0.6682 0.1846 0.2133 0.0500 1.0000 Uiso R . . . . . H41 H 0.6812 0.5723 0.3101 0.0500 1.0000 Uiso R . . . . . H42 H 0.7385 0.5382 0.2063 0.0500 1.0000 Uiso R . . . . . H61 H 0.8529 0.4003 0.2554 0.0500 1.0000 Uiso R . . . . . H62 H 0.8432 0.4668 0.3589 0.0500 1.0000 Uiso R . . . . . H101 H 0.7247 0.4078 0.1004 0.0500 1.0000 Uiso R . . . . . H102 H 0.7561 0.2931 0.1116 0.0500 1.0000 Uiso R . . . . . H121 H 0.6493 0.3447 0.4414 0.0500 1.0000 Uiso R . . . . . H122 H 0.6536 0.4631 0.4551 0.0500 1.0000 Uiso R . . . . . H111 H 0.6328 0.3217 -0.0265 0.0500 1.0000 Uiso R . . . . . H112 H 0.5985 0.2393 0.0543 0.0500 1.0000 Uiso R . . . . . H2 H 0.4923 0.4728 0.3983 0.0500 0.5000 Uiso DR . . . . . H60 H 0.9481 0.3726 0.4871 0.0500 0.5000 Uiso DR . . . . . H511 H 1.0271 0.5469 0.5613 0.1467 0.5000 Uiso R . . . . . H512 H 1.0532 0.4878 0.4508 0.1467 0.5000 Uiso R . . . . . H513 H 0.9391 0.5311 0.4717 0.1467 0.5000 Uiso 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 0.0423(4) 0.0299(3) 0.0383(3) 0.0002(3) 0.0001(3) -0.0003(3) Co2 0.0416(5) 0.0416(5) 0.0356(6) 0.0000 0.0000 0.0000 C1 0.060(4) 0.035(3) 0.072(4) 0.011(3) 0.002(3) -0.002(2) N1 0.053(3) 0.033(2) 0.044(2) -0.002(2) 0.003(2) 0.0101(18) O1 0.0366(18) 0.0296(17) 0.0454(17) -0.0010(13) 0.0016(14) -0.0013(15) C2 0.069(4) 0.036(3) 0.056(3) 0.006(3) 0.006(3) 0.013(3) O2 0.044(2) 0.040(2) 0.0364(15) 0.0065(14) 0.0057(15) 0.0073(16) O3 0.056(2) 0.0286(17) 0.072(3) 0.0042(16) -0.0014(19) 0.0012(16) C4 0.038(3) 0.038(3) 0.057(3) -0.006(2) 0.002(2) -0.003(2) O4 0.054(2) 0.040(2) 0.0378(16) -0.0030(14) -0.0007(16) 0.0068(18) C5 0.046(3) 0.047(3) 0.053(3) -0.005(2) -0.004(2) 0.006(2) C6 0.044(3) 0.058(4) 0.071(3) -0.006(3) -0.006(3) 0.009(3) C10 0.060(4) 0.048(3) 0.054(3) 0.002(3) 0.015(3) 0.018(3) O10 0.071(3) 0.065(3) 0.065(3) 0.008(2) 0.002(2) 0.025(2) C11 0.065(4) 0.044(3) 0.043(3) -0.007(2) 0.006(3) 0.012(3) C12 0.048(3) 0.051(3) 0.043(3) -0.002(3) -0.008(2) 0.012(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.638(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . Co1 3_665 2.8763(13) yes Co1 . O1 3_665 1.934(3) yes Co1 . Co2 . 3.1283(7) yes Co1 . C1 . 2.644(6) yes Co1 . N1 . 1.901(4) yes Co1 . O1 . 1.917(3) yes Co1 . O2 . 1.928(3) yes Co1 . O3 . 1.871(3) yes Co1 . O4 . 1.878(3) yes Co1 . C5 . 2.604(6) yes Co2 . O4 4_655 1.972(3) yes Co2 . O4 2_565 1.972(3) yes Co2 . O4 3_665 1.972(3) yes Co2 . O4 . 1.972(3) yes C1 . C2 . 1.538(8) yes C1 . O3 . 1.402(7) yes C1 . H11 . 0.972 no C1 . H12 . 0.982 no N1 . C2 . 1.519(7) yes N1 . C5 . 1.514(7) yes N1 . C10 . 1.525(7) yes O1 . C4 . 1.404(6) yes C2 . H21 . 0.967 no C2 . H22 . 0.981 no O2 . C12 . 1.435(6) yes O2 . H2 . 1.000 no C4 . C5 . 1.540(8) yes C4 . H41 . 0.966 no C4 . H42 . 0.966 no O4 . C11 . 1.437(7) yes C5 . C6 . 1.528(8) yes C5 . C12 . 1.542(8) yes C6 . O10 . 1.400(7) yes C6 . H61 . 0.978 no C6 . H62 . 0.972 no C10 . C11 . 1.510(8) yes C10 . H101 . 0.972 no C10 . H102 . 0.965 no O10 . H10 . 0.995 no C11 . H111 . 0.958 no C11 . H112 . 0.977 no C12 . H121 . 0.961 no C12 . H122 . 0.978 no C51 . O60 3_765 1.336(7) yes C51 . O60 . 1.336(7) yes O60 . H60 . 1.005 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Co1 3_665 Co1 . O1 3_665 41.46(9) yes Co1 3_665 Co1 . Co2 . 62.631(12) yes O1 3_665 Co1 . Co2 . 62.12(9) yes Co1 3_665 Co1 . C1 . 154.03(13) yes O1 3_665 Co1 . C1 . 129.47(16) yes Co2 . Co1 . C1 . 141.22(13) yes Co1 3_665 Co1 . N1 . 126.12(13) yes O1 3_665 Co1 . N1 . 166.51(16) yes Co2 . Co1 . N1 . 109.39(13) yes C1 . Co1 . N1 . 63.89(18) yes Co1 3_665 Co1 . O1 . 41.91(10) yes O1 3_665 Co1 . O1 . 81.13(14) yes Co2 . Co1 . O1 . 62.21(9) yes C1 . Co1 . O1 . 145.36(17) yes N1 . Co1 . O1 . 85.57(17) yes Co1 3_665 Co1 . O2 . 82.86(10) yes O1 3_665 Co1 . O2 . 95.77(14) yes Co2 . Co1 . O2 . 145.15(11) yes C1 . Co1 . O2 . 73.56(17) yes N1 . Co1 . O2 . 86.26(16) yes Co1 3_665 Co1 . O3 . 142.31(12) yes O1 3_665 Co1 . O3 . 103.37(15) yes Co2 . Co1 . O3 . 120.03(12) yes C1 . Co1 . O3 . 30.47(17) yes N1 . Co1 . O3 . 89.95(18) yes Co1 3_665 Co1 . O4 . 99.26(11) yes O1 3_665 Co1 . O4 . 87.71(15) yes Co2 . Co1 . O4 . 36.69(11) yes C1 . Co1 . O4 . 104.88(17) yes N1 . Co1 . O4 . 90.16(18) yes Co1 3_665 Co1 . C5 . 95.97(13) yes O1 3_665 Co1 . C5 . 136.16(15) yes Co2 . Co1 . C5 . 114.40(13) yes C1 . Co1 . C5 . 82.53(19) yes N1 . Co1 . C5 . 35.08(18) yes O1 . Co1 . O2 . 89.34(14) yes O1 . Co1 . O3 . 175.49(15) yes O2 . Co1 . O3 . 89.89(15) yes O1 . Co1 . O4 . 90.35(14) yes O2 . Co1 . O4 . 176.42(16) yes O3 . Co1 . O4 . 90.15(16) yes O1 . Co1 . C5 . 62.84(16) yes O2 . Co1 . C5 . 61.78(16) yes O3 . Co1 . C5 . 112.97(17) yes O4 . Co1 . C5 . 114.99(17) yes O4 4_655 Co2 . O4 2_565 124.03(18) yes O4 4_655 Co2 . O4 3_665 102.72(8) yes O4 2_565 Co2 . O4 3_665 102.72(8) yes O4 4_655 Co2 . Co1 3_665 115.65(10) yes O4 2_565 Co2 . Co1 3_665 113.61(10) yes O4 3_665 Co2 . Co1 3_665 34.68(9) yes O4 4_655 Co2 . Co1 . 113.61(10) yes O4 2_565 Co2 . Co1 . 115.65(10) yes O4 3_665 Co2 . Co1 . 89.36(9) yes Co1 3_665 Co2 . Co1 . 54.74(2) yes O4 4_655 Co2 . Co1 2_565 89.36(9) yes O4 2_565 Co2 . Co1 2_565 34.68(9) yes O4 3_665 Co2 . Co1 2_565 115.65(10) yes Co1 3_665 Co2 . Co1 2_565 142.060(16) yes Co1 . Co2 . Co1 2_565 142.060(16) yes O4 4_655 Co2 . Co1 4_655 34.68(9) yes O4 2_565 Co2 . Co1 4_655 89.36(9) yes O4 3_665 Co2 . Co1 4_655 113.61(10) yes Co1 3_665 Co2 . Co1 4_655 142.060(16) yes Co1 . Co2 . Co1 4_655 142.060(16) yes O4 4_655 Co2 . O4 . 102.72(8) yes O4 2_565 Co2 . O4 . 102.72(8) yes O4 3_665 Co2 . O4 . 124.03(18) yes Co1 3_665 Co2 . O4 . 89.36(9) yes Co1 . Co2 . O4 . 34.68(9) yes Co1 2_565 Co2 . Co1 4_655 54.74(2) yes Co1 2_565 Co2 . O4 . 113.61(10) yes Co1 4_655 Co2 . O4 . 115.65(10) yes Co1 . C1 . C2 . 78.3(3) yes Co1 . C1 . O3 . 42.6(2) yes C2 . C1 . O3 . 111.1(4) yes Co1 . C1 . H11 . 148.9 no C2 . C1 . H11 . 109.6 no O3 . C1 . H11 . 109.4 no Co1 . C1 . H12 . 97.7 no C2 . C1 . H12 . 109.4 no O3 . C1 . H12 . 110.2 no H11 . C1 . H12 . 107.1 no Co1 . N1 . C2 . 108.0(3) yes Co1 . N1 . C5 . 98.8(3) yes C2 . N1 . C5 . 117.5(4) yes Co1 . N1 . C10 . 105.4(3) yes C2 . N1 . C10 . 109.7(4) yes C5 . N1 . C10 . 115.8(4) yes Co1 3_665 O1 . Co1 . 96.63(14) yes Co1 3_665 O1 . C4 . 129.4(3) yes Co1 . O1 . C4 . 108.7(3) yes C1 . C2 . N1 . 108.8(4) yes C1 . C2 . H21 . 110.4 no N1 . C2 . H21 . 109.6 no C1 . C2 . H22 . 109.9 no N1 . C2 . H22 . 109.6 no H21 . C2 . H22 . 108.5 no Co1 . O2 . C12 . 109.7(3) yes Co1 . O2 . H2 . 113.9 no C12 . O2 . H2 . 118.6 no C1 . O3 . Co1 . 106.9(3) yes O1 . C4 . C5 . 111.1(4) yes O1 . C4 . H41 . 108.5 no C5 . C4 . H41 . 109.2 no O1 . C4 . H42 . 108.9 no C5 . C4 . H42 . 109.8 no H41 . C4 . H42 . 109.3 no Co2 . O4 . Co1 . 108.64(17) yes Co2 . O4 . C11 . 120.3(3) yes Co1 . O4 . C11 . 109.2(3) yes C4 . C5 . N1 . 106.1(4) yes C4 . C5 . Co1 . 77.2(3) yes N1 . C5 . Co1 . 46.2(2) yes C4 . C5 . C6 . 108.6(5) yes N1 . C5 . C6 . 114.6(4) yes Co1 . C5 . C6 . 159.9(4) yes C4 . C5 . C12 . 108.2(4) yes N1 . C5 . C12 . 103.1(5) yes Co1 . C5 . C12 . 79.1(3) yes C6 . C5 . C12 . 115.6(5) yes C5 . C6 . O10 . 115.1(5) yes C5 . C6 . H61 . 109.6 no O10 . C6 . H61 . 108.2 no C5 . C6 . H62 . 108.6 no O10 . C6 . H62 . 107.2 no H61 . C6 . H62 . 107.9 no N1 . C10 . C11 . 106.6(5) yes N1 . C10 . H101 . 109.5 no C11 . C10 . H101 . 110.1 no N1 . C10 . H102 . 110.4 no C11 . C10 . H102 . 111.2 no H101 . C10 . H102 . 108.9 no C6 . O10 . H10 . 107.0 no C10 . C11 . O4 . 109.0(4) yes C10 . C11 . H111 . 109.7 no O4 . C11 . H111 . 111.1 no C10 . C11 . H112 . 109.9 no O4 . C11 . H112 . 109.9 no H111 . C11 . H112 . 107.1 no C5 . C12 . O2 . 107.3(4) yes C5 . C12 . H121 . 111.1 no O2 . C12 . H121 . 110.1 no C5 . C12 . H122 . 109.7 no O2 . C12 . H122 . 110.1 no H121 . C12 . H122 . 108.6 no O60 3_765 C51 . O60 . 130.7(13) yes C51 . O60 . H60 . 102.0 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O10 . H10 . O3 7_555 164 0.99 1.64 2.607(2) yes O2 . H2 . O2 3_665 141 1.00 1.56 2.421(2) yes O60 . H60 . O10 . 156 1.01 1.95 2.899(2) yes data_1 _database_code_depnum_ccdc_archive 'CCDC 601285' _audit_creation_date 06-05-20 _audit_creation_method CRYSTALS_ver_12.83 _oxford_structure_analysis_title 'sx030 in P 21/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.1331(2) _cell_length_b 12.2948(2) _cell_length_c 18.9290(3) _cell_angle_alpha 90 _cell_angle_beta 94.0590(10) _cell_angle_gamma 90 _cell_volume 3048.78(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C42 H102 Co4 N4 Na2 O30' _chemical_formula_moiety 'C42 H102 Co4 N4 Na2 O30' _chemical_compound_source ? _chemical_formula_weight 1424.99 _cell_measurement_reflns_used 65077 _cell_measurement_theta_min 0 _cell_measurement_theta_max 30 _cell_measurement_temperature 100 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 1.172 # Sheldrick geometric approximatio 0.70 0.79 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.79 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 59541 _reflns_number_total 8879 _diffrn_reflns_av_R_equivalents 0.071 # Number of reflections with Friedels Law is 8879 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8889 _diffrn_reflns_theta_min 1.828 _diffrn_reflns_theta_max 29.995 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.995 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.68 _refine_diff_density_max 2.16 _refine_ls_number_reflns 8878 _refine_ls_number_restraints 0 _refine_ls_number_parameters 334 #_refine_ls_R_factor_ref 0.0835 _refine_ls_wR_factor_ref 0.1241 _refine_ls_goodness_of_fit_ref 0.8519 #_reflns_number_all 8878 _refine_ls_R_factor_all 0.0835 _refine_ls_wR_factor_all 0.1241 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5432 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_gt 0.1173 _refine_ls_shift/su_max 0.001254 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _publ_section_exptl_refinement ; All non-hydrogen atoms were refined anisotropically, except for the free solvent molecules, where they were refined isotropically. Hydrogen atoms bound to carbon atoms were placed geometrically, and refined as riding groups. Hydrogen-bonding hydrogen atoms were placed along the hydrogen bond 1\A away from the donor atom and refined as riding groups. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Co1 Co 1.01057(3) 0.13913(3) 0.63063(2) 0.0094 1.0000 Uani . . . . . . Co2 Co 0.98417(3) 0.01187(3) 0.73500(2) 0.0099 1.0000 Uani . . . . . . Na3 Na 1.03039(9) -0.08330(10) 0.56661(6) 0.0141 1.0000 Uani . . . . . . O4 O 0.91965(15) 0.01782(17) 0.64043(10) 0.0102 1.0000 Uani . . . . . . C5 C 0.8123(2) 0.0329(3) 0.64780(16) 0.0131 1.0000 Uani . . . . . . O6 O 1.10252(15) 0.03643(17) 0.68121(10) 0.0112 1.0000 Uani . . . . . . O7 O 0.97822(15) 0.16782(17) 0.72663(10) 0.0110 1.0000 Uani . . . . . . N8 N 0.85181(18) -0.0090(2) 0.77336(13) 0.0111 1.0000 Uani . . . . . . C9 C 0.8851(2) -0.1011(3) 0.82395(16) 0.0148 1.0000 Uani . . . . . . C10 C 0.9274(2) -0.1896(3) 0.77874(16) 0.0159 1.0000 Uani . . . . . . O12 O 1.03815(16) 0.01000(18) 0.82996(11) 0.0148 1.0000 Uani . . . . . . O13 O 1.05653(15) 0.10219(17) 0.54175(10) 0.0116 1.0000 Uani . . . . . . C14 C 1.1631(2) 0.1218(3) 0.54554(16) 0.0140 1.0000 Uani . . . . . . N15 N 1.11381(18) 0.2465(2) 0.64046(13) 0.0106 1.0000 Uani . . . . . . C16 C 1.1550(2) 0.2192(3) 0.71539(15) 0.0121 1.0000 Uani . . . . . . O17 O 0.91780(15) 0.24438(17) 0.59167(11) 0.0121 1.0000 Uani . . . . . . O18 O 1.17371(17) -0.1564(2) 0.52435(12) 0.0237 1.0000 Uani D . . . . . O19 O 0.7101(2) 0.1862(2) 0.88072(13) 0.0332 1.0000 Uani . . . . . . O21 O 1.33315(17) 0.2665(2) 0.71529(12) 0.0208 1.0000 Uani . . . . . . O22 O 0.98618(18) -0.25315(19) 0.61862(12) 0.0208 1.0000 Uani D . . . . . O23 O 0.71533(17) -0.1748(2) 0.82222(11) 0.0201 1.0000 Uani D . . . . . C24 C 1.0632(2) 0.2240(3) 0.76139(15) 0.0139 1.0000 Uani . . . . . . C25 C 1.1870(2) 0.0988(3) 0.71273(16) 0.0142 1.0000 Uani . . . . . . C26 C 1.1866(2) 0.2303(3) 0.58247(16) 0.0146 1.0000 Uani . . . . . . C27 C 0.8016(2) -0.1485(3) 0.86761(16) 0.0191 1.0000 Uani . . . . . . C28 C 1.2800(3) -0.1621(3) 0.53234(19) 0.0249 1.0000 Uani . . . . . . C29 C 1.0566(3) -0.3434(3) 0.62675(19) 0.0311 1.0000 Uani . . . . . . C30 C 1.0610(2) 0.3544(3) 0.63069(16) 0.0141 1.0000 Uani . . . . . . C31 C 1.2402(2) 0.2938(3) 0.74455(17) 0.0180 1.0000 Uani . . . . . . C32 C 0.8176(2) 0.0913(3) 0.80894(17) 0.0170 1.0000 Uani . . . . . . C33 C 1.2176(3) 0.0183(3) 0.95789(18) 0.0262 1.0000 Uiso . . . . . . C34 C 0.9751(2) -0.0542(3) 0.87105(17) 0.0186 1.0000 Uani . . . . . . C35 C 0.7117(3) 0.0916(3) 0.83659(19) 0.0238 1.0000 Uani . . . . . . C36 C 0.9760(2) 0.3366(3) 0.57326(17) 0.0154 1.0000 Uani . . . . . . C37 C 0.7829(2) -0.0377(3) 0.70912(15) 0.0128 1.0000 Uani . . . . . . O38 O 0.8784(4) 0.3328(4) 0.9182(2) 0.0915 1.0000 Uiso . . . . . . C39 C 0.9353(4) 0.2705(5) 0.9704(3) 0.0613 1.0000 Uiso . . . . . . O40 O 0.9509(5) 0.5460(5) 0.8848(3) 0.1303 1.0000 Uiso . . . . . . H42 H 0.7958 0.1073 0.6593 0.0166 1.0000 Uiso R . . . . . H43 H 0.7746 0.0107 0.6036 0.0166 1.0000 Uiso R . . . . . H44 H 0.9651 -0.2426 0.8095 0.0205 1.0000 Uiso R . . . . . H45 H 0.8708 -0.2234 0.7512 0.0205 1.0000 Uiso R . . . . . H46 H 1.2011 0.0616 0.5707 0.0179 1.0000 Uiso R . . . . . H47 H 1.1870 0.1246 0.4978 0.0179 1.0000 Uiso R . . . . . H48 H 1.0829 0.1912 0.8066 0.0179 1.0000 Uiso R . . . . . H49 H 1.0468 0.2973 0.7695 0.0179 1.0000 Uiso R . . . . . H50 H 1.2070 0.0727 0.7598 0.0176 1.0000 Uiso R . . . . . H51 H 1.2465 0.0880 0.6863 0.0176 1.0000 Uiso R . . . . . H52 H 1.2587 0.2347 0.6005 0.0185 1.0000 Uiso R . . . . . H53 H 1.1733 0.2873 0.5468 0.0185 1.0000 Uiso R . . . . . H54 H 0.8273 -0.2159 0.8922 0.0237 1.0000 Uiso R . . . . . H55 H 0.7815 -0.0957 0.9024 0.0237 1.0000 Uiso R . . . . . H56 H 1.1072 0.4109 0.6171 0.0175 1.0000 Uiso R . . . . . H57 H 1.0316 0.3747 0.6733 0.0175 1.0000 Uiso R . . . . . H58 H 1.2477 0.2866 0.7956 0.0234 1.0000 Uiso R . . . . . H59 H 1.2208 0.3695 0.7331 0.0234 1.0000 Uiso R . . . . . H60 H 0.8645 0.1073 0.8498 0.0214 1.0000 Uiso R . . . . . H61 H 0.8203 0.1486 0.7744 0.0214 1.0000 Uiso R . . . . . H62 H 1.0161 -0.1140 0.8925 0.0229 1.0000 Uiso R . . . . . H63 H 0.9494 -0.0130 0.9093 0.0229 1.0000 Uiso R . . . . . H64 H 0.7000 0.0255 0.8643 0.0288 1.0000 Uiso R . . . . . H65 H 0.6590 0.0960 0.7965 0.0288 1.0000 Uiso R . . . . . H66 H 0.9290 0.3990 0.5695 0.0196 1.0000 Uiso R . . . . . H67 H 1.0041 0.3267 0.5277 0.0196 1.0000 Uiso R . . . . . H68 H 0.7929 -0.1149 0.6970 0.0163 1.0000 Uiso R . . . . . H69 H 0.7133 -0.0246 0.7179 0.0163 1.0000 Uiso R . . . . . H281 H 1.3007 -0.2348 0.5358 0.0302 1.0000 Uiso R . . . . . H282 H 1.3027 -0.1231 0.5742 0.0302 1.0000 Uiso R . . . . . H283 H 1.3057 -0.1308 0.4912 0.0302 1.0000 Uiso R . . . . . H291 H 1.0256 -0.4012 0.5991 0.0378 1.0000 Uiso R . . . . . H292 H 1.0654 -0.3668 0.6759 0.0378 1.0000 Uiso R . . . . . H293 H 1.1234 -0.3260 0.6098 0.0378 1.0000 Uiso R . . . . . H18 H 0.9939 -0.2040 0.6607 0.0500 1.0000 Uiso DR . . . . . H20 H 0.6431 0.2189 0.8914 0.0500 1.0000 Uiso R . . . . . H22 H 1.3824 0.3183 0.7403 0.0500 1.0000 Uiso R . . . . . H13 H 1.1582 0.0081 0.8624 0.0500 1.0000 Uiso R . . . . . H331 H 1.2785 0.0516 0.9784 0.0323 1.0000 Uiso R . . . . . H332 H 1.2046 -0.0455 0.9830 0.0323 1.0000 Uiso R . . . . . H333 H 1.1610 0.0687 0.9643 0.0323 1.0000 Uiso R . . . . . O20 O 1.22780(19) -0.0045(2) 0.88625(13) 0.0257 1.0000 Uiso . . . . . . H19 H 1.1539 -0.1873 0.4765 0.0500 1.0000 Uiso DR . . . . . O11 O 0.99440(15) -0.14175(17) 0.73200(11) 0.0133 1.0000 Uani . . . . . . H1 H 0.6611 -0.1958 0.8541 0.0500 1.0000 Uiso DR . . . . . H2 H 0.9288 0.4691 0.8930 0.0500 1.0000 Uiso R . . . . . H3 H 0.8294 0.2741 0.9020 0.0500 1.0000 Uiso R . . . . . C41 C 1.0296(6) 0.5265(7) 0.8452(4) 0.1132 1.0000 Uiso . . . . . . H411 H 1.0612 0.5971 0.8322 0.1358 1.0000 Uiso R . . . . . H412 H 1.0814 0.4813 0.8731 0.1358 1.0000 Uiso R . . . . . H413 H 1.0053 0.4867 0.8011 0.1358 1.0000 Uiso R . . . . . H391 H 0.9907 0.3163 0.9940 0.0736 1.0000 Uiso R . . . . . H392 H 0.8889 0.2446 1.0065 0.0736 1.0000 Uiso R . . . . . H393 H 0.9662 0.2064 0.9474 0.0736 1.0000 Uiso 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 0.00905(19) 0.0097(2) 0.00991(19) -0.00057(16) 0.00303(14) -0.00016(16) Co2 0.00902(19) 0.0114(2) 0.00963(18) 0.00012(16) 0.00241(14) -0.00008(17) Na3 0.0160(6) 0.0132(6) 0.0133(6) 0.0003(5) 0.0035(5) 0.0004(5) O4 0.0083(10) 0.0108(11) 0.0117(10) -0.0004(8) 0.0020(8) -0.0011(8) C5 0.0084(14) 0.0154(16) 0.0156(15) 0.0005(12) 0.0022(11) 0.0005(12) O6 0.0097(10) 0.0125(11) 0.0115(10) -0.0011(8) 0.0015(8) -0.0002(8) O7 0.0125(10) 0.0098(11) 0.0108(10) -0.0010(8) 0.0020(8) -0.0026(8) N8 0.0100(12) 0.0113(13) 0.0124(12) -0.0002(10) 0.0032(9) 0.0006(10) C9 0.0157(16) 0.0163(16) 0.0129(14) 0.0033(12) 0.0046(12) -0.0012(13) C10 0.0147(16) 0.0150(16) 0.0188(16) 0.0050(13) 0.0067(12) 0.0015(13) O12 0.0145(11) 0.0199(12) 0.0099(10) 0.0021(9) 0.0001(8) -0.0033(9) O13 0.0089(10) 0.0131(11) 0.0131(10) -0.0021(8) 0.0040(8) 0.0001(9) C14 0.0107(14) 0.0157(16) 0.0164(15) -0.0021(12) 0.0062(12) -0.0010(12) N15 0.0080(12) 0.0116(13) 0.0125(12) -0.0017(10) 0.0033(9) -0.0010(10) C16 0.0112(15) 0.0127(15) 0.0123(14) -0.0022(11) 0.0009(11) -0.0015(12) O17 0.0106(10) 0.0118(11) 0.0144(10) -0.0010(9) 0.0037(8) 0.0004(9) O18 0.0149(12) 0.0343(15) 0.0221(12) -0.0121(11) 0.0027(10) 0.0011(11) O19 0.0293(15) 0.0411(17) 0.0295(14) -0.0128(13) 0.0039(12) 0.0110(13) O21 0.0138(11) 0.0250(14) 0.0237(12) -0.0082(10) 0.0027(9) -0.0061(10) O22 0.0315(14) 0.0135(12) 0.0178(11) 0.0009(9) 0.0051(10) -0.0016(10) O23 0.0169(12) 0.0257(13) 0.0182(11) 0.0010(10) 0.0053(9) -0.0075(10) C24 0.0145(15) 0.0144(16) 0.0131(14) -0.0042(12) 0.0029(12) -0.0044(13) C25 0.0112(15) 0.0174(16) 0.0140(14) 0.0004(12) 0.0004(12) -0.0020(13) C26 0.0135(15) 0.0160(16) 0.0152(14) 0.0000(12) 0.0073(12) -0.0017(13) C27 0.0193(17) 0.0220(18) 0.0167(15) 0.0027(14) 0.0061(13) -0.0030(14) C28 0.0195(18) 0.029(2) 0.0261(18) -0.0062(15) 0.0000(14) 0.0032(15) C29 0.048(3) 0.020(2) 0.0251(19) -0.0013(15) 0.0032(17) 0.0054(18) C30 0.0136(15) 0.0096(15) 0.0197(15) 0.0007(12) 0.0049(12) -0.0001(12) C31 0.0164(16) 0.0207(18) 0.0172(15) -0.0038(13) 0.0031(13) -0.0042(14) C32 0.0189(16) 0.0176(17) 0.0154(15) -0.0031(13) 0.0064(13) -0.0003(14) C34 0.0177(17) 0.0229(18) 0.0155(15) 0.0047(13) 0.0018(13) -0.0029(14) C35 0.0240(18) 0.0193(18) 0.0297(19) 0.0020(15) 0.0139(15) 0.0051(15) C36 0.0148(15) 0.0125(16) 0.0195(15) -0.0004(12) 0.0039(12) 0.0013(12) C37 0.0076(14) 0.0170(16) 0.0141(14) 0.0007(12) 0.0017(11) -0.0004(12) O11 0.0130(11) 0.0115(11) 0.0160(10) 0.0025(9) 0.0047(8) 0.0018(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.18482(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . Co2 . 2.5628(6) yes Co1 . Na3 . 3.0100(13) yes Co1 . O4 . 1.928(2) yes Co1 . O6 . 1.951(2) yes Co1 . O7 . 1.9278(19) yes Co1 . O13 . 1.883(2) yes Co1 . N15 . 1.892(2) yes Co1 . C16 . 2.590(3) yes Co1 . O17 . 1.891(2) yes Co2 . O4 . 1.927(2) yes Co2 . O6 . 1.941(2) yes Co2 . O7 . 1.925(2) yes Co2 . N8 . 1.948(2) yes Co2 . C9 . 2.601(3) yes Co2 . O12 . 1.885(2) yes Co2 . O11 . 1.895(2) yes Na3 . O13 2_756 2.287(2) yes Na3 . Na3 2_756 3.302(2) yes Na3 . O4 . 2.429(2) yes Na3 . O6 . 2.735(2) yes Na3 . O13 . 2.359(2) yes Na3 . O18 . 2.281(2) yes Na3 . O22 . 2.398(3) yes O4 . C5 . 1.438(3) yes C5 . C37 . 1.521(4) yes C5 . H42 . 0.968 no C5 . H43 . 0.980 no O6 . C25 . 1.443(4) yes O7 . C24 . 1.432(3) yes N8 . C9 . 1.527(4) yes N8 . C32 . 1.489(4) yes N8 . C37 . 1.505(4) yes C9 . C10 . 1.515(4) yes C9 . C27 . 1.534(4) yes C9 . C34 . 1.542(5) yes C10 . H44 . 0.983 no C10 . H45 . 0.970 no C10 . O11 . 1.419(3) yes O12 . C34 . 1.416(4) yes O13 . C14 . 1.417(3) yes C14 . C26 . 1.528(4) yes C14 . H46 . 0.995 no C14 . H47 . 0.979 no N15 . C16 . 1.519(4) yes N15 . C26 . 1.519(4) yes N15 . C30 . 1.502(4) yes C16 . C24 . 1.537(4) yes C16 . C25 . 1.540(4) yes C16 . C31 . 1.521(4) yes O17 . C36 . 1.425(4) yes O18 . C28 . 1.396(4) yes O18 . H19 . 1.000 no O19 . C35 . 1.434(4) yes O19 . H20 . 1.001 no O21 . C31 . 1.416(4) yes O21 . H22 . 1.002 no O22 . C29 . 1.446(4) yes O22 . H18 . 1.000 no O23 . C27 . 1.410(4) yes O23 . H1 . 1.000 no C24 . H48 . 0.965 no C24 . H49 . 0.942 no C25 . H50 . 0.966 no C25 . H51 . 0.966 no C26 . H52 . 0.985 no C26 . H53 . 0.980 no C27 . H54 . 0.999 no C27 . H55 . 0.974 no C28 . H281 . 0.935 no C28 . H282 . 0.955 no C28 . H283 . 0.952 no C29 . H291 . 0.955 no C29 . H292 . 0.973 no C29 . H293 . 0.979 no C30 . C36 . 1.518(4) yes C30 . H56 . 0.968 no C30 . H57 . 0.953 no C31 . H58 . 0.969 no C31 . H59 . 0.985 no C32 . C35 . 1.521(4) yes C32 . H60 . 0.974 no C32 . H61 . 0.964 no C33 . H331 . 0.957 no C33 . H332 . 0.938 no C33 . H333 . 0.982 no C33 . O20 . 1.400(4) yes C34 . H62 . 0.983 no C34 . H63 . 0.964 no C35 . H64 . 0.984 no C35 . H65 . 0.991 no C36 . H66 . 0.985 no C36 . H67 . 0.969 no C37 . H68 . 0.988 no C37 . H69 . 0.955 no O38 . C39 . 1.420(6) yes O38 . H3 . 1.001 no C39 . H391 . 1.000 no C39 . H392 . 1.000 no C39 . H393 . 1.000 no O40 . H2 . 1.004 no O40 . C41 . 1.341(8) yes H13 . O20 . 1.002 no C41 . H411 . 1.000 no C41 . H412 . 1.000 no C41 . H413 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Co2 . Co1 . Na3 . 77.05(3) yes Co2 . Co1 . O4 . 48.31(6) yes Na3 . Co1 . O4 . 53.67(6) yes Co2 . Co1 . O6 . 48.65(6) yes Na3 . Co1 . O6 . 62.70(6) yes O4 . Co1 . O6 . 79.52(8) yes Co2 . Co1 . O7 . 48.26(6) yes Na3 . Co1 . O7 . 125.23(7) yes O4 . Co1 . O7 . 82.62(8) yes O6 . Co1 . O7 . 79.97(9) yes Co2 . Co1 . O13 . 127.66(7) yes Na3 . Co1 . O13 . 51.59(7) yes O4 . Co1 . O13 . 98.01(9) yes O6 . Co1 . O13 . 93.21(9) yes O7 . Co1 . O13 . 172.95(9) yes Co2 . Co1 . N15 . 119.03(8) yes Na3 . Co1 . N15 . 126.28(8) yes O4 . Co1 . N15 . 167.11(10) yes O6 . Co1 . N15 . 89.37(10) yes O7 . Co1 . N15 . 89.07(9) yes Co2 . Co1 . C16 . 83.55(7) yes Na3 . Co1 . C16 . 120.96(7) yes O4 . Co1 . C16 . 131.74(9) yes O6 . Co1 . C16 . 62.70(9) yes O7 . Co1 . C16 . 63.07(9) yes Co2 . Co1 . O17 . 126.86(6) yes Na3 . Co1 . O17 . 122.44(7) yes O4 . Co1 . O17 . 100.41(9) yes O6 . Co1 . O17 . 173.58(9) yes O7 . Co1 . O17 . 93.64(9) yes O13 . Co1 . N15 . 89.05(10) yes O13 . Co1 . C16 . 112.22(9) yes N15 . Co1 . C16 . 35.49(10) yes O13 . Co1 . O17 . 93.15(9) yes N15 . Co1 . O17 . 89.90(10) yes C16 . Co1 . O17 . 113.87(9) yes Co1 . Co2 . O4 . 48.34(6) yes Co1 . Co2 . O6 . 48.98(6) yes O4 . Co2 . O6 . 79.78(8) yes Co1 . Co2 . O7 . 48.35(6) yes O4 . Co2 . O7 . 82.71(9) yes O6 . Co2 . O7 . 80.29(9) yes Co1 . Co2 . N8 . 122.73(8) yes O4 . Co2 . N8 . 90.34(9) yes O6 . Co2 . N8 . 170.05(9) yes O7 . Co2 . N8 . 97.44(10) yes Co1 . Co2 . C9 . 157.81(7) yes O4 . Co2 . C9 . 114.47(9) yes O6 . Co2 . C9 . 151.46(10) yes O7 . Co2 . C9 . 124.44(9) yes N8 . Co2 . C9 . 35.69(10) yes Co1 . Co2 . O12 . 132.86(7) yes O4 . Co2 . O12 . 175.73(9) yes O6 . Co2 . O12 . 103.95(9) yes O7 . Co2 . O12 . 95.79(9) yes N8 . Co2 . O12 . 85.89(10) yes Co1 . Co2 . O11 . 124.87(6) yes O4 . Co2 . O11 . 92.15(9) yes O6 . Co2 . O11 . 94.49(9) yes O7 . Co2 . O11 . 173.22(8) yes N8 . Co2 . O11 . 86.97(10) yes C9 . Co2 . O12 . 63.12(10) yes C9 . Co2 . O11 . 61.78(9) yes O12 . Co2 . O11 . 89.64(9) yes O13 2_756 Na3 . Co1 . 113.66(7) yes O13 2_756 Na3 . Na3 2_756 45.57(6) yes Co1 . Na3 . Na3 2_756 73.79(4) yes O13 2_756 Na3 . O4 . 106.66(8) yes Co1 . Na3 . O4 . 39.74(5) yes Na3 2_756 Na3 . O4 . 89.98(7) yes O13 2_756 Na3 . O6 . 152.72(9) yes Co1 . Na3 . O6 . 39.34(5) yes Na3 2_756 Na3 . O6 . 108.86(7) yes O4 . Na3 . O6 . 57.05(7) yes O13 2_756 Na3 . O13 . 89.41(8) yes Co1 . Na3 . O13 . 38.72(5) yes Na3 2_756 Na3 . O13 . 43.84(6) yes O4 . Na3 . O13 . 73.83(7) yes O6 . Na3 . O13 . 65.84(7) yes O13 2_756 Na3 . O18 . 91.00(9) yes Co1 . Na3 . O18 . 126.60(8) yes Na3 2_756 Na3 . O18 . 97.90(8) yes O4 . Na3 . O18 . 161.05(9) yes O6 . Na3 . O18 . 104.01(8) yes O13 2_756 Na3 . O22 . 99.20(9) yes Co1 . Na3 . O22 . 126.56(7) yes Na3 2_756 Na3 . O22 . 143.26(9) yes O4 . Na3 . O22 . 92.14(8) yes O6 . Na3 . O22 . 102.91(8) yes O13 . Na3 . O18 . 100.12(9) yes O13 . Na3 . O22 . 165.24(9) yes O18 . Na3 . O22 . 91.76(10) yes Na3 . O4 . Co1 . 86.59(8) yes Na3 . O4 . Co2 . 105.85(9) yes Co1 . O4 . Co2 . 83.35(8) yes Na3 . O4 . C5 . 138.81(18) yes Co1 . O4 . C5 . 121.82(18) yes Co2 . O4 . C5 . 106.53(16) yes O4 . C5 . C37 . 107.7(2) yes O4 . C5 . H42 . 112.4 no C37 . C5 . H42 . 107.1 no O4 . C5 . H43 . 108.8 no C37 . C5 . H43 . 110.6 no H42 . C5 . H43 . 110.3 no Co1 . O6 . Co2 . 82.37(8) yes Co1 . O6 . Na3 . 77.96(7) yes Co2 . O6 . Na3 . 95.00(8) yes Co1 . O6 . C25 . 106.85(17) yes Co2 . O6 . C25 . 119.12(17) yes Na3 . O6 . C25 . 145.81(17) yes Co1 . O7 . Co2 . 83.39(8) yes Co1 . O7 . C24 . 107.74(16) yes Co2 . O7 . C24 . 114.62(18) yes Co2 . N8 . C9 . 96.20(17) yes Co2 . N8 . C32 . 111.44(19) yes C9 . N8 . C32 . 114.3(2) yes Co2 . N8 . C37 . 103.35(17) yes C9 . N8 . C37 . 117.5(2) yes C32 . N8 . C37 . 112.1(2) yes N8 . C9 . Co2 . 48.10(12) yes N8 . C9 . C10 . 106.2(2) yes Co2 . C9 . C10 . 78.32(16) yes N8 . C9 . C27 . 115.9(3) yes Co2 . C9 . C27 . 163.9(2) yes C10 . C9 . C27 . 109.6(3) yes N8 . C9 . C34 . 105.0(2) yes Co2 . C9 . C34 . 77.07(17) yes C10 . C9 . C34 . 107.4(3) yes C27 . C9 . C34 . 112.2(3) yes C9 . C10 . H44 . 109.3 no C9 . C10 . H45 . 108.2 no H44 . C10 . H45 . 111.7 no C9 . C10 . O11 . 108.8(3) yes H44 . C10 . O11 . 109.6 no H45 . C10 . O11 . 109.1 no Co2 . O12 . C34 . 109.61(18) yes Na3 2_756 O13 . Na3 . 90.59(8) yes Na3 2_756 O13 . Co1 . 130.88(11) yes Na3 . O13 . Co1 . 89.69(8) yes Na3 2_756 O13 . C14 . 119.42(17) yes Na3 . O13 . C14 . 108.14(17) yes Co1 . O13 . C14 . 106.96(17) yes O13 . C14 . C26 . 109.8(2) yes O13 . C14 . H46 . 111.0 no C26 . C14 . H46 . 110.6 no O13 . C14 . H47 . 109.8 no C26 . C14 . H47 . 108.9 no H46 . C14 . H47 . 106.6 no Co1 . N15 . C16 . 98.20(17) yes Co1 . N15 . C26 . 108.69(18) yes C16 . N15 . C26 . 116.4(2) yes Co1 . N15 . C30 . 106.43(18) yes C16 . N15 . C30 . 116.2(2) yes C26 . N15 . C30 . 109.6(2) yes N15 . C16 . Co1 . 46.31(12) yes N15 . C16 . C24 . 106.2(2) yes Co1 . C16 . C24 . 78.25(16) yes N15 . C16 . C25 . 105.2(2) yes Co1 . C16 . C25 . 78.71(16) yes C24 . C16 . C25 . 106.4(2) yes N15 . C16 . C31 . 114.2(2) yes Co1 . C16 . C31 . 160.4(2) yes C24 . C16 . C31 . 111.0(2) yes C25 . C16 . C31 . 113.3(3) yes Co1 . O17 . C36 . 107.33(17) yes Na3 . O18 . C28 . 145.7(2) yes Na3 . O18 . H19 . 107.4 no C28 . O18 . H19 . 105.9 no C35 . O19 . H20 . 119.5 no C31 . O21 . H22 . 102.1 no Na3 . O22 . C29 . 122.7(2) yes Na3 . O22 . H18 . 77.7 no C29 . O22 . H18 . 110.6 no C27 . O23 . H1 . 105.5 no C16 . C24 . O7 . 109.8(2) yes C16 . C24 . H48 . 108.4 no O7 . C24 . H48 . 110.9 no C16 . C24 . H49 . 109.0 no O7 . C24 . H49 . 110.9 no H48 . C24 . H49 . 107.8 no C16 . C25 . O6 . 108.7(2) yes C16 . C25 . H50 . 110.2 no O6 . C25 . H50 . 110.9 no C16 . C25 . H51 . 112.5 no O6 . C25 . H51 . 109.8 no H50 . C25 . H51 . 104.8 no C14 . C26 . N15 . 109.2(2) yes C14 . C26 . H52 . 111.4 no N15 . C26 . H52 . 112.4 no C14 . C26 . H53 . 106.8 no N15 . C26 . H53 . 108.2 no H52 . C26 . H53 . 108.6 no C9 . C27 . O23 . 109.4(2) yes C9 . C27 . H54 . 109.6 no O23 . C27 . H54 . 108.9 no C9 . C27 . H55 . 110.5 no O23 . C27 . H55 . 108.7 no H54 . C27 . H55 . 109.7 no O18 . C28 . H281 . 109.8 no O18 . C28 . H282 . 108.4 no H281 . C28 . H282 . 110.5 no O18 . C28 . H283 . 107.4 no H281 . C28 . H283 . 109.1 no H282 . C28 . H283 . 111.6 no O22 . C29 . H291 . 105.6 no O22 . C29 . H292 . 111.2 no H291 . C29 . H292 . 108.8 no O22 . C29 . H293 . 112.2 no H291 . C29 . H293 . 109.8 no H292 . C29 . H293 . 109.2 no N15 . C30 . C36 . 105.7(2) yes N15 . C30 . H56 . 112.0 no C36 . C30 . H56 . 110.8 no N15 . C30 . H57 . 109.8 no C36 . C30 . H57 . 108.8 no H56 . C30 . H57 . 109.6 no C16 . C31 . O21 . 110.4(3) yes C16 . C31 . H58 . 109.1 no O21 . C31 . H58 . 109.9 no C16 . C31 . H59 . 108.5 no O21 . C31 . H59 . 110.8 no H58 . C31 . H59 . 108.1 no N8 . C32 . C35 . 118.1(3) yes N8 . C32 . H60 . 109.4 no C35 . C32 . H60 . 105.6 no N8 . C32 . H61 . 105.8 no C35 . C32 . H61 . 108.0 no H60 . C32 . H61 . 109.8 no H331 . C33 . H332 . 109.3 no H331 . C33 . H333 . 107.3 no H332 . C33 . H333 . 107.3 no H331 . C33 . O20 . 110.1 no H332 . C33 . O20 . 110.9 no H333 . C33 . O20 . 111.8 no C9 . C34 . O12 . 110.2(2) yes C9 . C34 . H62 . 109.5 no O12 . C34 . H62 . 108.6 no C9 . C34 . H63 . 109.6 no O12 . C34 . H63 . 111.7 no H62 . C34 . H63 . 107.1 no C32 . C35 . O19 . 104.7(3) yes C32 . C35 . H64 . 111.2 no O19 . C35 . H64 . 110.5 no C32 . C35 . H65 . 110.0 no O19 . C35 . H65 . 111.3 no H64 . C35 . H65 . 109.1 no C30 . C36 . O17 . 108.7(2) yes C30 . C36 . H66 . 111.4 no O17 . C36 . H66 . 107.0 no C30 . C36 . H67 . 110.4 no O17 . C36 . H67 . 111.2 no H66 . C36 . H67 . 108.1 no C5 . C37 . N8 . 108.2(2) yes C5 . C37 . H68 . 109.1 no N8 . C37 . H68 . 109.3 no C5 . C37 . H69 . 109.6 no N8 . C37 . H69 . 110.4 no H68 . C37 . H69 . 110.3 no C39 . O38 . H3 . 96.8 no O38 . C39 . H391 . 109.7 no O38 . C39 . H392 . 109.4 no H391 . C39 . H392 . 109.5 no O38 . C39 . H393 . 109.4 no H391 . C39 . H393 . 109.5 no H392 . C39 . H393 . 109.5 no H2 . O40 . C41 . 99.2 no H13 . O20 . C33 . 105.0 no C10 . O11 . Co2 . 110.28(18) yes O40 . C41 . H411 . 109.4 no O40 . C41 . H412 . 109.0 no H411 . C41 . H412 . 109.5 no O40 . C41 . H413 . 110.0 no H411 . C41 . H413 . 109.5 no H412 . C41 . H413 . 109.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O22 . H18 . O11 . 170 1.00 1.55 2.542(2) yes O19 . H20 . O22 3_656 158 1.00 1.73 2.684(2) yes O21 . H22 . O11 3_756 151 1.00 1.74 2.660(2) yes O20 . H13 . O12 . 170 1.00 1.65 2.645(2) yes O18 . H19 . O17 2_756 160 1.00 1.69 2.658(2) yes O23 . H1 . O17 3_646 168 1.00 1.68 2.666(2) yes O40 . H2 . O38 . 172 1.00 1.88 2.875(2) yes O38 . H3 . O19 . 165 1.00 1.92 2.901(2) yes