# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Lin, Jian-Bin' 'Xue, Wei' 'Zhang, Jie-Peng' 'Chen, Xiao-Ming' _publ_contact_author_name 'Zhang, Jie-Peng' _publ_contact_author_email zhangjp7@mail.sysu.edu.cn _publ_section_title ; An ionic porous coordination framework exhibiting high CO2 affinity and CO2/CH4 selectivity ; # Attachment 'all.cif' data_1-g _database_code_depnum_ccdc_archive 'CCDC 794764' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H38 Cl4 Co3 N10 O6' _chemical_formula_weight 965.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.4490(17) _cell_length_b 15.5529(13) _cell_length_c 13.6581(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.197(2) _cell_angle_gamma 90.00 _cell_volume 4343.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1638 _cell_measurement_theta_min 2.218 _cell_measurement_theta_max 23.9725 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 1.429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7440 _exptl_absorpt_correction_T_max 0.8703 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCd' _diffrn_measurement_method '\w scan' _diffrn_reflns_number 7790 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3721 _reflns_number_gt 2814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _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^)+(0.1420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3721 _refine_ls_number_parameters 236 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.2039 _refine_ls_wR_factor_gt 0.1786 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.013 _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 0.2500 0.2500 0.5000 0.0191(3) Uani 1 2 d S . . Co2 Co 0.15946(3) 0.11637(5) 0.63349(5) 0.0268(3) Uani 1 1 d . . . Cl1 Cl 0.12628(8) -0.01359(10) 0.57716(13) 0.0487(5) Uani 1 1 d . . . Cl2 Cl 0.10410(7) 0.15573(11) 0.76973(11) 0.0423(4) Uani 1 1 d . . . O1 O 0.34497(16) 0.2958(2) 0.4705(2) 0.0223(8) Uani 1 1 d . . . N1 N 0.2910(2) 0.1763(3) 0.6063(3) 0.0238(10) Uani 1 1 d . . . N2 N 0.2564(2) 0.1159(3) 0.6588(3) 0.0249(10) Uani 1 1 d . . . N3 N 0.3629(2) 0.0985(3) 0.6917(4) 0.0403(13) Uani 1 1 d . . . N4 N 0.2660(2) -0.1428(3) 0.8964(3) 0.0304(11) Uani 1 1 d . . . C1 C 0.4027(2) 0.2738(3) 0.5103(4) 0.0225(11) Uani 1 1 d . . . C2 C 0.4605(3) 0.3110(4) 0.4760(4) 0.0308(13) Uani 1 1 d . . . H2A H 0.4579 0.3508 0.4234 0.037 Uiso 1 1 calc R . . C3 C 0.5211(3) 0.2924(4) 0.5151(4) 0.0404(15) Uani 1 1 d . . . H3A H 0.5592 0.3200 0.4906 0.048 Uiso 1 1 calc R . . C4 C 0.5259(3) 0.2332(5) 0.5904(5) 0.0472(18) Uani 1 1 d . . . H4A H 0.5674 0.2193 0.6176 0.057 Uiso 1 1 calc R . . C5 C 0.4705(3) 0.1950(5) 0.6254(5) 0.0456(17) Uani 1 1 d . . . H5A H 0.4741 0.1550 0.6776 0.055 Uiso 1 1 calc R . . C6 C 0.4088(3) 0.2132(4) 0.5866(4) 0.0310(13) Uani 1 1 d . . . C7 C 0.3533(3) 0.1632(4) 0.6286(4) 0.0301(13) Uani 1 1 d . . . C8 C 0.3018(3) 0.0718(4) 0.7082(4) 0.0330(13) Uani 1 1 d . . . C9 C 0.2877(3) -0.0029(4) 0.7732(4) 0.0323(13) Uani 1 1 d . . . C10 C 0.2269(3) -0.0215(5) 0.8077(5) 0.0502(18) Uani 1 1 d . . . H10A H 0.1905 0.0135 0.7907 0.060 Uiso 1 1 calc R . . C11 C 0.2188(3) -0.0924(4) 0.8681(5) 0.0434(17) Uani 1 1 d . . . H11A H 0.1759 -0.1049 0.8903 0.052 Uiso 1 1 calc R . . C12 C 0.3251(4) -0.1245(5) 0.8619(6) 0.074(3) Uani 1 1 d . . . H12A H 0.3606 -0.1605 0.8803 0.088 Uiso 1 1 calc R . . C13 C 0.3373(3) -0.0567(6) 0.8015(7) 0.083(3) Uani 1 1 d . . . H13A H 0.3805 -0.0467 0.7789 0.100 Uiso 1 1 calc R . . N1S N 0.0000 -0.0079(5) 0.7500 0.0450(19) Uani 1 2 d S . . H1SG H -0.0274 0.0265 0.7832 0.054 Uiso 1 1 d R . . C1S C -0.0381(4) -0.0521(7) 0.6799(7) 0.094(4) Uani 1 1 d . . . H1SA H -0.0604 -0.0117 0.6385 0.141 Uiso 1 1 d R . . H1SB H -0.0100 -0.0876 0.6408 0.141 Uiso 1 1 d R . . H1SC H -0.0695 -0.0875 0.7128 0.141 Uiso 1 1 d R . . O1W O 0.4716(11) -0.0363(14) 0.5953(15) 0.371(12) Uiso 1 1 d . . . H1WA H 0.4343 -0.0543 0.5771 0.445 Uiso 1 1 d R . . H1WB H 0.4640 0.0103 0.6257 0.445 Uiso 1 1 d R . . O2W O 0.5000 -0.144(2) 0.7500 0.41(2) Uiso 1 2 d S . . H2WA H 0.4777 -0.1034 0.7247 0.498 Uiso 1 1 d R . . N1A N 0.2600(7) -0.2358(8) 0.5357(10) 0.075(4) Uiso 0.50 1 d PD A -1 H1AB H 0.2356 -0.2211 0.4806 0.090 Uiso 0.50 1 calc PR A -1 C3A C 0.2254(9) -0.2211(11) 0.6282(11) 0.081(5) Uiso 0.50 1 d PD A -1 H3AA H 0.2044 -0.1659 0.6273 0.121 Uiso 0.50 1 d PR A -1 H3AB H 0.1935 -0.2649 0.6407 0.121 Uiso 0.50 1 d PR A -1 H3AC H 0.2582 -0.2221 0.6787 0.121 Uiso 0.50 1 d PR A -1 C2A C 0.2789(10) -0.3274(9) 0.5389(16) 0.099(7) Uiso 0.50 1 d PD A -1 H2AA H 0.3002 -0.3423 0.4788 0.148 Uiso 0.50 1 d PR A -1 H2AB H 0.3104 -0.3264 0.5911 0.148 Uiso 0.50 1 d PR A -1 H2AC H 0.2457 -0.3693 0.5532 0.148 Uiso 0.50 1 d PR A -1 C1A C 0.3215(14) -0.192(2) 0.542(2) 0.132(10) Uiso 0.50 1 d P A -1 H1AA H 0.3637 -0.2177 0.5472 0.158 Uiso 0.50 1 calc PR A -1 O1A O 0.3078(12) -0.1146(11) 0.5380(18) 0.224(12) Uiso 0.50 1 d PD A -1 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 0.0224(5) 0.0161(5) 0.0190(6) -0.0003(4) -0.0007(4) -0.0002(4) Co2 0.0264(4) 0.0261(5) 0.0279(5) 0.0071(3) 0.0022(3) -0.0008(3) Cl1 0.0546(10) 0.0265(8) 0.0651(12) 0.0010(7) -0.0056(8) -0.0089(7) Cl2 0.0398(9) 0.0559(10) 0.0313(9) 0.0047(7) 0.0076(6) 0.0073(7) O1 0.0254(19) 0.0185(18) 0.023(2) 0.0046(15) -0.0011(15) -0.0021(15) N1 0.025(2) 0.023(2) 0.023(2) 0.0004(18) 0.0030(19) -0.0030(18) N2 0.027(2) 0.022(2) 0.026(3) 0.0067(18) 0.0016(19) -0.0006(19) N3 0.026(2) 0.043(3) 0.053(4) 0.022(3) -0.005(2) 0.000(2) N4 0.030(2) 0.031(3) 0.030(3) 0.009(2) -0.003(2) -0.001(2) C1 0.025(3) 0.017(3) 0.025(3) -0.006(2) 0.003(2) -0.001(2) C2 0.034(3) 0.034(3) 0.025(3) 0.006(2) 0.000(2) 0.000(3) C3 0.027(3) 0.057(4) 0.037(4) 0.008(3) -0.001(3) -0.009(3) C4 0.027(3) 0.059(4) 0.055(4) 0.021(3) -0.006(3) -0.001(3) C5 0.035(3) 0.056(4) 0.046(4) 0.022(3) -0.005(3) -0.007(3) C6 0.025(3) 0.035(3) 0.033(3) 0.004(3) -0.005(2) -0.001(2) C7 0.033(3) 0.031(3) 0.026(3) 0.005(2) -0.001(2) -0.005(2) C8 0.035(3) 0.030(3) 0.034(3) 0.013(3) -0.003(3) -0.006(3) C9 0.027(3) 0.035(3) 0.034(3) 0.011(3) 0.000(2) -0.004(2) C10 0.036(3) 0.052(4) 0.063(5) 0.033(4) -0.003(3) 0.009(3) C11 0.030(3) 0.044(4) 0.057(4) 0.028(3) 0.005(3) 0.005(3) C12 0.034(4) 0.083(6) 0.104(7) 0.072(5) 0.007(4) 0.009(4) C13 0.030(4) 0.086(6) 0.133(8) 0.083(6) 0.001(4) -0.004(4) N1S 0.040(4) 0.041(4) 0.053(5) 0.000 -0.004(4) 0.000 C1S 0.067(6) 0.121(9) 0.093(7) -0.068(7) -0.018(5) 0.036(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.029(4) . ? Co1 N1 2.029(4) 7_556 ? Co1 O1 2.109(3) 7_556 ? Co1 O1 2.109(3) . ? Co1 N4 2.211(5) 6 ? Co1 N4 2.211(5) 4_556 ? Co2 O1 1.972(3) 7_556 ? Co2 N2 2.012(4) . ? Co2 Cl2 2.2656(17) . ? Co2 Cl1 2.2658(17) . ? O1 C1 1.343(6) . ? O1 Co2 1.972(3) 7_556 ? N1 C7 1.326(7) . ? N1 N2 1.377(6) . ? N2 C8 1.336(7) . ? N3 C8 1.336(7) . ? N3 C7 1.338(7) . ? N4 C11 1.303(7) . ? N4 C12 1.329(8) . ? N4 Co1 2.211(5) 4_546 ? C1 C2 1.399(7) . ? C1 C6 1.410(8) . ? C2 C3 1.378(8) . ? C2 H2A 0.9500 . ? C3 C4 1.383(9) . ? C3 H3A 0.9500 . ? C4 C5 1.367(9) . ? C4 H4A 0.9500 . ? C5 C6 1.396(8) . ? C5 H5A 0.9500 . ? C6 C7 1.491(8) . ? C8 C9 1.490(8) . ? C9 C10 1.363(8) . ? C9 C13 1.371(9) . ? C10 C11 1.386(9) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.362(9) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? N1S C1S 1.410(9) . ? N1S C1S 1.410(9) 2_556 ? N1S H1SG 0.8999 . ? C1S H1SA 0.9601 . ? C1S H1SB 0.9599 . ? C1S H1SC 0.9601 . ? O1W H1WA 0.8498 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? N1A C1A 1.43(3) . ? N1A C3A 1.467(9) . ? N1A C2A 1.477(9) . ? N1A H1AB 0.9300 . ? C3A H3AA 0.9601 . ? C3A H3AB 0.9600 . ? C3A H3AC 0.9600 . ? C2A H2AA 0.9600 . ? C2A H2AB 0.9600 . ? C2A H2AC 0.9600 . ? C1A O1A 1.24(3) . ? C1A H1AA 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(17) . 7_556 ? N1 Co1 O1 92.90(15) . 7_556 ? N1 Co1 O1 87.10(15) 7_556 7_556 ? N1 Co1 O1 87.10(15) . . ? N1 Co1 O1 92.90(15) 7_556 . ? O1 Co1 O1 180.00(7) 7_556 . ? N1 Co1 N4 88.29(17) . 6 ? N1 Co1 N4 91.71(17) 7_556 6 ? O1 Co1 N4 90.36(15) 7_556 6 ? O1 Co1 N4 89.64(15) . 6 ? N1 Co1 N4 91.71(17) . 4_556 ? N1 Co1 N4 88.29(17) 7_556 4_556 ? O1 Co1 N4 89.64(15) 7_556 4_556 ? O1 Co1 N4 90.36(15) . 4_556 ? N4 Co1 N4 180.000(1) 6 4_556 ? O1 Co2 N2 99.72(16) 7_556 . ? O1 Co2 Cl2 112.48(11) 7_556 . ? N2 Co2 Cl2 110.78(14) . . ? O1 Co2 Cl1 111.12(11) 7_556 . ? N2 Co2 Cl1 110.44(13) . . ? Cl2 Co2 Cl1 111.72(7) . . ? C1 O1 Co2 120.4(3) . 7_556 ? C1 O1 Co1 130.2(3) . . ? Co2 O1 Co1 109.36(16) 7_556 . ? C7 N1 N2 105.7(4) . . ? C7 N1 Co1 130.2(4) . . ? N2 N1 Co1 123.1(3) . . ? C8 N2 N1 104.9(4) . . ? C8 N2 Co2 140.5(4) . . ? N1 N2 Co2 114.5(3) . . ? C8 N3 C7 102.0(5) . . ? C11 N4 C12 116.0(5) . . ? C11 N4 Co1 122.2(4) . 4_546 ? C12 N4 Co1 121.7(4) . 4_546 ? O1 C1 C2 120.1(5) . . ? O1 C1 C6 123.0(5) . . ? C2 C1 C6 116.8(5) . . ? C3 C2 C1 122.9(5) . . ? C3 C2 H2A 118.5 . . ? C1 C2 H2A 118.5 . . ? C2 C3 C4 119.2(6) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 119.5(6) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 121.9(6) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 119.5(5) . . ? C5 C6 C7 115.9(5) . . ? C1 C6 C7 124.6(5) . . ? N1 C7 N3 113.7(5) . . ? N1 C7 C6 124.3(5) . . ? N3 C7 C6 122.0(5) . . ? N2 C8 N3 113.8(5) . . ? N2 C8 C9 124.4(5) . . ? N3 C8 C9 121.8(5) . . ? C10 C9 C13 116.6(6) . . ? C10 C9 C8 123.5(5) . . ? C13 C9 C8 119.9(5) . . ? C9 C10 C11 119.1(6) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? N4 C11 C10 124.5(6) . . ? N4 C11 H11A 117.8 . . ? C10 C11 H11A 117.8 . . ? N4 C12 C13 123.4(6) . . ? N4 C12 H12A 118.3 . . ? C13 C12 H12A 118.3 . . ? C12 C13 C9 120.4(6) . . ? C12 C13 H13A 119.8 . . ? C9 C13 H13A 119.8 . . ? C1S N1S C1S 121.7(11) . 2_556 ? C1S N1S H1SG 106.8 . . ? C1S N1S H1SG 107.0 2_556 . ? N1S C1S H1SA 110.0 . . ? N1S C1S H1SB 109.1 . . ? H1SA C1S H1SB 109.5 . . ? N1S C1S H1SC 109.3 . . ? H1SA C1S H1SC 109.4 . . ? H1SB C1S H1SC 109.5 . . ? H1WA O1W H1WB 104.9 . . ? C1A N1A C3A 107.7(15) . . ? C1A N1A C2A 102.9(16) . . ? C3A N1A C2A 104.5(14) . . ? C1A N1A H1AB 113.6 . . ? C3A N1A H1AB 113.6 . . ? C2A N1A H1AB 113.6 . . ? N1A C3A H3AA 110.2 . . ? N1A C3A H3AB 111.9 . . ? H3AA C3A H3AB 109.5 . . ? N1A C3A H3AC 106.2 . . ? H3AA C3A H3AC 109.5 . . ? H3AB C3A H3AC 109.5 . . ? N1A C2A H2AA 109.0 . . ? N1A C2A H2AB 100.4 . . ? H2AA C2A H2AB 109.5 . . ? N1A C2A H2AC 118.4 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? O1A C1A N1A 105(2) . . ? O1A C1A H1AA 127.5 . . ? N1A C1A H1AA 127.5 . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.152 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.133 #===============================END data_1-120K _database_code_depnum_ccdc_archive 'CCDC 794765' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H32 Cl4 Co3 N10 O3' _chemical_formula_weight 911.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.545(5) _cell_length_b 15.456(4) _cell_length_c 13.721(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.865(4) _cell_angle_gamma 90.00 _cell_volume 4356.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2443 _cell_measurement_theta_min 2.2085 _cell_measurement_theta_max 22.8945 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 1.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7748 _exptl_absorpt_correction_T_max 0.9199 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCd' _diffrn_measurement_method '\w scan' _diffrn_reflns_number 15296 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3852 _reflns_number_gt 2807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _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. The guest-free single-crystal 1 was prepared by heating a single-crystal of 1-g at 453 K for 4hrs. The alerts of A in checkcif report are caused by the guest-free crystal. ; _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^)+(0.1270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3852 _refine_ls_number_parameters 230 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.003 _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 0.2500 0.7500 1.5000 0.0220(3) Uani 1 2 d S . . Co2 Co 0.16021(3) 0.88315(5) 1.63351(5) 0.0306(3) Uani 1 1 d . . . Cl1 Cl 0.10635(8) 0.84241(11) 1.76863(11) 0.0488(5) Uani 1 1 d . . . Cl2 Cl 0.12743(9) 1.01490(10) 1.58012(14) 0.0558(5) Uani 1 1 d . . . O1 O 0.15604(16) 0.7967(2) 1.5283(2) 0.0248(8) Uani 1 1 d . . . N1 N 0.2092(2) 0.6772(3) 1.3929(3) 0.0281(10) Uani 1 1 d . . . N2 N 0.2435(2) 0.6176(3) 1.3404(3) 0.0313(11) Uani 1 1 d . . . N3 N 0.1376(2) 0.6010(3) 1.3033(4) 0.0423(13) Uani 1 1 d . . . N4 N 0.2336(2) 0.3573(3) 1.1021(3) 0.0345(11) Uani 1 1 d . . . C1 C 0.0984(3) 0.7737(3) 1.4884(4) 0.0279(12) Uani 1 1 d . . . C2 C 0.0407(3) 0.8106(4) 1.5232(4) 0.0383(14) Uani 1 1 d . . . H2A H 0.0437 0.8511 1.5752 0.046 Uiso 1 1 calc R . . C3 C -0.0204(3) 0.7906(5) 1.4851(5) 0.0488(17) Uani 1 1 d . . . H3A H -0.0583 0.8171 1.5104 0.059 Uiso 1 1 calc R . . C4 C -0.0252(3) 0.7314(5) 1.4099(5) 0.057(2) Uani 1 1 d . . . H4A H -0.0666 0.7175 1.3825 0.069 Uiso 1 1 calc R . . C5 C 0.0293(3) 0.6931(5) 1.3750(5) 0.0550(19) Uani 1 1 d . . . H5A H 0.0250 0.6513 1.3246 0.066 Uiso 1 1 calc R . . C6 C 0.0921(3) 0.7134(4) 1.4112(4) 0.0366(14) Uani 1 1 d . . . C7 C 0.1469(3) 0.6646(4) 1.3697(4) 0.0363(14) Uani 1 1 d . . . C8 C 0.1984(3) 0.5733(4) 1.2891(4) 0.0374(14) Uani 1 1 d . . . C9 C 0.2128(3) 0.5002(4) 1.2236(4) 0.0357(14) Uani 1 1 d . . . C10 C 0.2733(3) 0.4811(4) 1.1895(5) 0.0506(18) Uani 1 1 d . . . H10A H 0.3094 0.5169 1.2061 0.061 Uiso 1 1 calc R . . C11 C 0.2816(3) 0.4091(4) 1.1307(5) 0.0430(16) Uani 1 1 d . . . H11A H 0.3244 0.3961 1.1096 0.052 Uiso 1 1 calc R . . C12 C 0.1749(3) 0.3757(5) 1.1348(6) 0.059(2) Uani 1 1 d . . . H12A H 0.1398 0.3387 1.1167 0.071 Uiso 1 1 calc R . . C13 C 0.1618(3) 0.4461(5) 1.1942(6) 0.063(2) Uani 1 1 d . . . H13A H 0.1187 0.4574 1.2146 0.075 Uiso 1 1 calc R . . N1S N 0.0000 1.0049(5) 1.7500 0.049(2) Uani 1 2 d S . . H1SG H -0.0281 0.9702 1.7811 0.059 Uiso 1 1 d R . . C1S C 0.0359(4) 1.0479(7) 1.8209(8) 0.113(5) Uani 1 1 d . . . H1SA H 0.0571 1.0071 1.8634 0.170 Uiso 1 1 d R . . H1SB H 0.0680 1.0836 1.7905 0.170 Uiso 1 1 d R . . H1SC H 0.0071 1.0836 1.8580 0.170 Uiso 1 1 d R . . N1A N -0.2379(6) 0.7354(8) 1.5341(9) 0.084(4) Uiso 0.50 1 d PD A -1 H1AA H -0.2655 0.7235 1.4814 0.101 Uiso 0.50 1 calc PR A -1 C3A C -0.2751(8) 0.7265(10) 1.6253(11) 0.082(5) Uiso 0.50 1 d PD A -1 H3AA H -0.2884 0.6661 1.6336 0.123 Uiso 0.50 1 calc PR A -1 H3AB H -0.3139 0.7635 1.6218 0.123 Uiso 0.50 1 calc PR A -1 H3AC H -0.2477 0.7442 1.6809 0.123 Uiso 0.50 1 calc PR A -1 C2A C -0.2223(9) 0.8287(8) 1.5339(15) 0.100(6) Uiso 0.50 1 d PD A -1 H2AA H -0.1974 0.8428 1.4756 0.149 Uiso 0.50 1 calc PR A -1 H2AB H -0.1964 0.8430 1.5922 0.149 Uiso 0.50 1 calc PR A -1 H2AC H -0.2628 0.8623 1.5337 0.149 Uiso 0.50 1 calc PR A -1 C1A C -0.1845(8) 0.6833(10) 1.5286(15) 0.145(10) Uiso 0.50 1 d PD A -1 H1AB H -0.1411 0.7026 1.5201 0.174 Uiso 0.50 1 calc PR A -1 O1A O -0.2006(9) 0.6104(9) 1.5361(14) 0.179(9) Uiso 0.50 1 d PD A -1 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 0.0291(6) 0.0157(5) 0.0213(5) 0.0000(4) -0.0006(4) 0.0018(4) Co2 0.0333(5) 0.0264(4) 0.0323(5) -0.0087(3) 0.0033(3) 0.0004(3) Cl1 0.0503(10) 0.0598(11) 0.0367(9) -0.0037(7) 0.0092(7) -0.0110(8) Cl2 0.0691(12) 0.0272(8) 0.0710(12) -0.0024(8) -0.0058(9) 0.0117(7) O1 0.031(2) 0.0207(18) 0.0227(18) -0.0004(15) 0.0014(15) 0.0011(15) N1 0.031(2) 0.026(2) 0.028(2) -0.0083(19) 0.002(2) 0.0025(19) N2 0.032(3) 0.028(2) 0.033(3) -0.010(2) 0.003(2) -0.001(2) N3 0.036(3) 0.044(3) 0.047(3) -0.021(2) -0.003(2) 0.002(2) N4 0.034(3) 0.031(3) 0.039(3) -0.007(2) 0.004(2) -0.001(2) C1 0.029(3) 0.025(3) 0.030(3) 0.004(2) -0.001(2) 0.002(2) C2 0.038(3) 0.039(3) 0.038(3) -0.007(3) 0.002(3) 0.006(3) C3 0.034(3) 0.061(4) 0.052(4) -0.009(3) 0.004(3) 0.008(3) C4 0.027(3) 0.080(5) 0.065(5) -0.033(4) -0.009(3) 0.007(3) C5 0.043(4) 0.066(5) 0.055(4) -0.033(4) -0.013(3) 0.009(3) C6 0.033(3) 0.038(3) 0.039(3) -0.008(3) -0.002(3) 0.003(3) C7 0.036(3) 0.039(3) 0.034(3) -0.008(3) 0.002(3) 0.003(3) C8 0.039(3) 0.031(3) 0.043(4) -0.013(3) 0.001(3) 0.002(3) C9 0.035(3) 0.033(3) 0.038(3) -0.010(3) -0.005(3) 0.000(2) C10 0.044(4) 0.053(4) 0.055(4) -0.031(3) 0.004(3) -0.007(3) C11 0.035(3) 0.042(4) 0.052(4) -0.024(3) 0.002(3) -0.003(3) C12 0.039(4) 0.058(5) 0.081(5) -0.040(4) 0.003(4) -0.008(3) C13 0.045(4) 0.057(5) 0.087(6) -0.044(4) 0.002(4) -0.001(3) N1S 0.042(4) 0.046(5) 0.059(5) 0.000 -0.003(4) 0.000 C1S 0.061(6) 0.147(10) 0.131(9) -0.095(8) -0.022(6) 0.038(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.023(4) 7_568 ? Co1 N1 2.023(4) . ? Co1 O1 2.102(3) . ? Co1 O1 2.102(3) 7_568 ? Co1 N4 2.200(5) 6_566 ? Co1 N4 2.200(5) 4_557 ? Co2 O1 1.968(3) . ? Co2 N2 2.005(5) 7_568 ? Co2 Cl2 2.2632(18) . ? Co2 Cl1 2.2628(17) . ? O1 C1 1.346(6) . ? N1 C7 1.328(7) . ? N1 N2 1.371(6) . ? N2 C8 1.342(7) . ? N2 Co2 2.005(5) 7_568 ? N3 C8 1.338(7) . ? N3 C7 1.352(7) . ? N4 C12 1.324(8) . ? N4 C11 1.326(7) . ? N4 Co1 2.200(4) 4_547 ? C1 C2 1.404(8) . ? C1 C6 1.415(8) . ? C2 C3 1.387(8) . ? C2 H2A 0.9500 . ? C3 C4 1.381(9) . ? C3 H3A 0.9500 . ? C4 C5 1.361(9) . ? C4 H4A 0.9500 . ? C5 C6 1.409(8) . ? C5 H5A 0.9500 . ? C6 C7 1.477(8) . ? C8 C9 1.478(8) . ? C9 C10 1.367(8) . ? C9 C13 1.394(9) . ? C10 C11 1.387(8) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.388(9) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? N1S C1S 1.382(9) 2_558 ? N1S C1S 1.382(9) . ? N1S H1SG 0.8999 . ? C1S H1SA 0.9599 . ? C1S H1SB 0.9599 . ? C1S H1SC 0.9601 . ? N1A C1A 1.364(9) . ? N1A C2A 1.477(9) . ? N1A C3A 1.484(9) . ? N1A H1AA 0.9300 . ? C3A H3AA 0.9800 . ? C3A H3AB 0.9800 . ? C3A H3AC 0.9800 . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C1A O1A 1.178(9) . ? C1A H1AB 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.000(1) 7_568 . ? N1 Co1 O1 92.69(15) 7_568 . ? N1 Co1 O1 87.31(15) . . ? N1 Co1 O1 87.31(15) 7_568 7_568 ? N1 Co1 O1 92.69(15) . 7_568 ? O1 Co1 O1 180.000(1) . 7_568 ? N1 Co1 N4 91.30(18) 7_568 6_566 ? N1 Co1 N4 88.70(18) . 6_566 ? O1 Co1 N4 89.48(15) . 6_566 ? O1 Co1 N4 90.52(15) 7_568 6_566 ? N1 Co1 N4 88.70(18) 7_568 4_557 ? N1 Co1 N4 91.30(18) . 4_557 ? O1 Co1 N4 90.52(15) . 4_557 ? O1 Co1 N4 89.48(15) 7_568 4_557 ? N4 Co1 N4 180.000(1) 6_566 4_557 ? O1 Co2 N2 99.15(16) . 7_568 ? O1 Co2 Cl2 111.35(11) . . ? N2 Co2 Cl2 110.55(14) 7_568 . ? O1 Co2 Cl1 113.30(11) . . ? N2 Co2 Cl1 110.20(14) 7_568 . ? Cl2 Co2 Cl1 111.64(7) . . ? C1 O1 Co2 120.4(3) . . ? C1 O1 Co1 129.8(3) . . ? Co2 O1 Co1 109.78(16) . . ? C7 N1 N2 106.1(4) . . ? C7 N1 Co1 130.0(4) . . ? N2 N1 Co1 123.0(3) . . ? C8 N2 N1 105.2(4) . . ? C8 N2 Co2 139.6(4) . 7_568 ? N1 N2 Co2 115.1(3) . 7_568 ? C8 N3 C7 102.0(5) . . ? C12 N4 C11 116.6(5) . . ? C12 N4 Co1 121.8(4) . 4_547 ? C11 N4 Co1 121.5(4) . 4_547 ? O1 C1 C2 119.7(5) . . ? O1 C1 C6 123.3(5) . . ? C2 C1 C6 117.0(5) . . ? C3 C2 C1 123.0(6) . . ? C3 C2 H2A 118.5 . . ? C1 C2 H2A 118.5 . . ? C4 C3 C2 118.9(6) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C5 C4 C3 120.0(6) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 122.2(6) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C5 C6 C1 118.9(5) . . ? C5 C6 C7 116.7(5) . . ? C1 C6 C7 124.3(5) . . ? N1 C7 N3 113.2(5) . . ? N1 C7 C6 124.8(5) . . ? N3 C7 C6 122.0(5) . . ? N3 C8 N2 113.6(5) . . ? N3 C8 C9 121.9(5) . . ? N2 C8 C9 124.5(5) . . ? C10 C9 C13 117.1(6) . . ? C10 C9 C8 124.3(5) . . ? C13 C9 C8 118.6(6) . . ? C9 C10 C11 119.5(6) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? N4 C11 C10 124.0(6) . . ? N4 C11 H11A 118.0 . . ? C10 C11 H11A 118.0 . . ? N4 C12 C13 123.5(6) . . ? N4 C12 H12A 118.2 . . ? C13 C12 H12A 118.2 . . ? C12 C13 C9 119.3(6) . . ? C12 C13 H13A 120.4 . . ? C9 C13 H13A 120.4 . . ? C1S N1S C1S 122.5(12) 2_558 . ? C1S N1S H1SG 106.4 2_558 . ? C1S N1S H1SG 107.0 . . ? N1S C1S H1SA 110.1 . . ? N1S C1S H1SB 109.4 . . ? H1SA C1S H1SB 109.5 . . ? N1S C1S H1SC 108.8 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C1A N1A C2A 113.8(9) . . ? C1A N1A C3A 114.7(9) . . ? C2A N1A C3A 101.9(13) . . ? C1A N1A H1AA 108.7 . . ? C2A N1A H1AA 108.7 . . ? C3A N1A H1AA 108.7 . . ? N1A C3A H3AA 109.5 . . ? N1A C3A H3AB 109.5 . . ? H3AA C3A H3AB 109.5 . . ? N1A C3A H3AC 109.5 . . ? H3AA C3A H3AC 109.5 . . ? H3AB C3A H3AC 109.5 . . ? N1A C2A H2AA 109.5 . . ? N1A C2A H2AB 109.5 . . ? H2AA C2A H2AB 109.5 . . ? N1A C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? O1A C1A N1A 109.5(10) . . ? O1A C1A H1AB 125.3 . . ? N1A C1A H1AB 125.3 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.261 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.116 #===============================END data_1-293K _database_code_depnum_ccdc_archive 'CCDC 794766' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H32 Cl4 Co3 N10 O3' _chemical_formula_weight 911.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.787(2) _cell_length_b 15.4366(18) _cell_length_c 13.7906(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.899(2) _cell_angle_gamma 90.00 _cell_volume 4424.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1386 _cell_measurement_theta_min 2.1995 _cell_measurement_theta_max 20.284 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7816 _exptl_absorpt_correction_T_max 0.9161 _exptl_absorpt_process_details SADABS _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 'Bruker Apex CCd' _diffrn_measurement_method '\w scan' _diffrn_reflns_number 10532 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3737 _reflns_number_gt 2296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _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. The guest-free single-crystal 1 was prepared by heating a single-crystal of 1-g at 453 K for 4hrs. The alerts of A in checkcif report are caused by the guest-free crystal. ; _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^)+(0.1300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3737 _refine_ls_number_parameters 222 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.2219 _refine_ls_wR_factor_gt 0.1834 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 0.5000 0.0337(4) Uani 1 2 d S . . Co2 Co 0.33970(5) 0.11743(6) 0.36782(7) 0.0455(4) Uani 1 1 d . . . Cl1 Cl 0.39195(11) 0.15839(16) 0.23320(16) 0.0728(7) Uani 1 1 d . . . Cl2 Cl 0.37385(12) -0.01363(13) 0.4203(2) 0.0798(8) Uani 1 1 d . . . O1 O 0.3432(2) 0.2042(3) 0.4725(3) 0.0366(11) Uani 1 1 d . . . N1 N 0.2895(3) 0.3244(3) 0.6057(4) 0.0400(14) Uani 1 1 d . . . N2 N 0.2554(3) 0.3829(4) 0.6586(4) 0.0448(15) Uani 1 1 d . . . N3 N 0.3599(3) 0.4002(4) 0.6946(5) 0.0615(19) Uani 1 1 d . . . N4 N 0.2655(3) 0.6426(3) 0.8968(5) 0.0482(16) Uani 1 1 d . . . C1 C 0.3999(3) 0.2280(4) 0.5116(5) 0.0390(17) Uani 1 1 d . . . C2 C 0.4567(4) 0.1915(5) 0.4787(6) 0.056(2) Uani 1 1 d . . . H2A H 0.4544 0.1510 0.4289 0.067 Uiso 1 1 calc R . . C3 C 0.5157(4) 0.2127(6) 0.5166(7) 0.070(3) Uani 1 1 d . . . H3A H 0.5524 0.1869 0.4921 0.084 Uiso 1 1 calc R . . C4 C 0.5211(4) 0.2720(7) 0.5910(7) 0.083(3) Uani 1 1 d . . . H4A H 0.5612 0.2869 0.6167 0.100 Uiso 1 1 calc R . . C5 C 0.4670(4) 0.3081(6) 0.6256(7) 0.070(3) Uani 1 1 d . . . H5A H 0.4706 0.3480 0.6760 0.084 Uiso 1 1 calc R . . C6 C 0.4055(4) 0.2878(5) 0.5887(5) 0.0490(19) Uani 1 1 d . . . C7 C 0.3515(4) 0.3355(5) 0.6299(5) 0.0491(19) Uani 1 1 d . . . C8 C 0.2996(4) 0.4280(5) 0.7097(6) 0.051(2) Uani 1 1 d . . . C9 C 0.2859(4) 0.5006(5) 0.7748(6) 0.051(2) Uani 1 1 d . . . C10 C 0.2268(4) 0.5209(5) 0.8071(7) 0.069(3) Uani 1 1 d . . . H10A H 0.1914 0.4875 0.7891 0.083 Uiso 1 1 calc R . . C11 C 0.2195(4) 0.5927(5) 0.8678(7) 0.067(2) Uani 1 1 d . . . H11A H 0.1783 0.6053 0.8888 0.080 Uiso 1 1 calc R . . C12 C 0.3234(4) 0.6218(6) 0.8651(8) 0.085(3) Uani 1 1 d . . . H12A H 0.3580 0.6559 0.8849 0.101 Uiso 1 1 calc R . . C13 C 0.3352(5) 0.5532(6) 0.8049(8) 0.092(4) Uani 1 1 d . . . H13A H 0.3768 0.5431 0.7840 0.111 Uiso 1 1 d R . . N1S N 0.5000 -0.0009(7) 0.2500 0.078(3) Uiso 1 2 d S . . H1SG H 0.5281 0.0338 0.2198 0.094 Uiso 1 1 d R . . C1S C 0.5342(7) -0.0451(8) 0.3212(10) 0.133(5) Uiso 1 1 d . . . H1SA H 0.5550 -0.0048 0.3646 0.200 Uiso 1 1 d R . . H1SB H 0.5051 -0.0808 0.3569 0.200 Uiso 1 1 d R . . H1SC H 0.5661 -0.0808 0.2914 0.200 Uiso 1 1 d R . . N1A N 0.7352(13) 0.2588(17) 0.5252(18) 0.200(13) Uiso 0.50 1 d PD A -1 H1AA H 0.7780 0.2558 0.5122 0.240 Uiso 0.50 1 calc PR A -1 C3A C 0.7080(15) 0.1913(15) 0.462(2) 0.165(12) Uiso 0.50 1 d PD A -1 H3AA H 0.7091 0.2100 0.3961 0.247 Uiso 0.50 1 calc PR A -1 H3AB H 0.6642 0.1804 0.4802 0.247 Uiso 0.50 1 calc PR A -1 H3AC H 0.7327 0.1391 0.4699 0.247 Uiso 0.50 1 calc PR A -1 C2A C 0.7318(17) 0.218(2) 0.624(2) 0.185(14) Uiso 0.50 1 d PD A -1 H2AA H 0.7478 0.2582 0.6720 0.278 Uiso 0.50 1 calc PR A -1 H2AB H 0.7575 0.1664 0.6258 0.278 Uiso 0.50 1 calc PR A -1 H2AC H 0.6879 0.2037 0.6378 0.278 Uiso 0.50 1 calc PR A -1 O1A O 0.6868(19) 0.3592(17) 0.450(3) 0.35(2) Uiso 0.50 1 d PD A -1 C1A C 0.723(2) 0.3406(15) 0.513(3) 0.59(8) Uiso 0.50 1 d PD A -1 H1AB H 0.7415 0.3825 0.5532 0.703 Uiso 0.50 1 calc PR A -1 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 0.0437(8) 0.0213(6) 0.0358(8) -0.0013(5) -0.0031(6) 0.0024(5) Co2 0.0503(7) 0.0363(5) 0.0500(7) -0.0117(4) 0.0025(5) 0.0023(4) Cl1 0.0751(16) 0.0879(16) 0.0556(14) -0.0010(12) 0.0124(12) -0.0100(12) Cl2 0.0935(18) 0.0404(11) 0.105(2) 0.0019(11) -0.0038(14) 0.0154(11) O1 0.044(3) 0.028(2) 0.037(3) -0.005(2) -0.005(2) 0.004(2) N1 0.045(4) 0.030(3) 0.044(4) -0.009(3) 0.003(3) 0.006(3) N2 0.045(4) 0.040(3) 0.050(4) -0.017(3) -0.001(3) 0.001(3) N3 0.049(4) 0.052(4) 0.083(5) -0.030(4) -0.006(4) 0.001(3) N4 0.052(4) 0.037(3) 0.056(4) -0.016(3) -0.005(3) -0.005(3) C1 0.049(5) 0.029(3) 0.040(4) 0.003(3) -0.001(4) 0.009(3) C2 0.056(5) 0.054(5) 0.058(6) -0.021(4) -0.005(4) 0.001(4) C3 0.049(5) 0.084(6) 0.077(7) -0.023(5) -0.004(5) 0.006(5) C4 0.043(5) 0.109(8) 0.096(8) -0.047(6) -0.013(5) 0.002(5) C5 0.052(5) 0.081(6) 0.078(7) -0.038(5) -0.012(5) 0.012(5) C6 0.048(5) 0.050(4) 0.048(5) -0.009(4) 0.000(4) 0.005(4) C7 0.051(5) 0.048(4) 0.048(5) -0.013(4) 0.000(4) 0.002(4) C8 0.058(5) 0.043(4) 0.051(5) -0.011(4) -0.003(4) -0.002(4) C9 0.052(5) 0.047(4) 0.054(5) -0.023(4) -0.006(4) 0.002(4) C10 0.054(5) 0.068(5) 0.085(7) -0.049(5) 0.004(5) -0.012(4) C11 0.048(5) 0.066(5) 0.085(7) -0.035(5) 0.006(5) -0.004(4) C12 0.052(6) 0.077(6) 0.125(9) -0.058(6) 0.005(6) -0.015(5) C13 0.057(6) 0.084(7) 0.136(10) -0.067(7) 0.001(6) 0.001(5) _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 N1 2.020(6) . ? Co1 N1 2.020(6) 7_556 ? Co1 O1 2.102(4) . ? Co1 O1 2.102(4) 7_556 ? Co1 N4 2.211(6) 6_565 ? Co1 N4 2.211(6) 4_546 ? Co2 O1 1.970(4) . ? Co2 N2 2.004(6) 7_556 ? Co2 Cl1 2.256(2) . ? Co2 Cl2 2.259(2) . ? O1 C1 1.339(8) . ? N1 C7 1.337(9) . ? N1 N2 1.368(7) . ? N2 C8 1.344(9) . ? N2 Co2 2.004(6) 7_556 ? N3 C8 1.344(9) . ? N3 C7 1.349(9) . ? N4 C11 1.286(9) . ? N4 C12 1.326(10) . ? N4 Co1 2.211(6) 4_556 ? C1 C2 1.391(10) . ? C1 C6 1.412(10) . ? C2 C3 1.364(11) . ? C2 H2A 0.9300 . ? C3 C4 1.379(11) . ? C3 H3A 0.9300 . ? C4 C5 1.349(11) . ? C4 H4A 0.9300 . ? C5 C6 1.404(10) . ? C5 H5A 0.9300 . ? C6 C7 1.464(10) . ? C8 C9 1.467(10) . ? C9 C10 1.350(11) . ? C9 C13 1.366(11) . ? C10 C11 1.399(11) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C13 1.370(11) . ? C12 H12A 0.9300 . ? C13 H13A 0.9299 . ? N1S C1S 1.384(13) 2_655 ? N1S C1S 1.384(13) . ? N1S H1SG 0.9000 . ? C1S H1SA 0.9599 . ? C1S H1SB 0.9598 . ? C1S H1SC 0.9598 . ? N1A C1A 1.298(9) . ? N1A C3A 1.463(10) . ? N1A C2A 1.506(10) . ? N1A H1AA 0.9100 . ? C3A H3AA 0.9600 . ? C3A H3AB 0.9600 . ? C3A H3AC 0.9600 . ? C2A H2AA 0.9600 . ? C2A H2AB 0.9600 . ? C2A H2AC 0.9600 . ? O1A C1A 1.181(10) . ? C1A H1AB 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.0(2) . 7_556 ? N1 Co1 O1 87.46(19) . . ? N1 Co1 O1 92.54(19) 7_556 . ? N1 Co1 O1 92.54(19) . 7_556 ? N1 Co1 O1 87.46(19) 7_556 7_556 ? O1 Co1 O1 180.0 . 7_556 ? N1 Co1 N4 88.7(2) . 6_565 ? N1 Co1 N4 91.3(2) 7_556 6_565 ? O1 Co1 N4 89.6(2) . 6_565 ? O1 Co1 N4 90.45(19) 7_556 6_565 ? N1 Co1 N4 91.3(2) . 4_546 ? N1 Co1 N4 88.7(2) 7_556 4_546 ? O1 Co1 N4 90.45(19) . 4_546 ? O1 Co1 N4 89.6(2) 7_556 4_546 ? N4 Co1 N4 180.00(18) 6_565 4_546 ? O1 Co2 N2 99.2(2) . 7_556 ? O1 Co2 Cl1 113.57(15) . . ? N2 Co2 Cl1 109.72(19) 7_556 . ? O1 Co2 Cl2 111.51(14) . . ? N2 Co2 Cl2 111.07(18) 7_556 . ? Cl1 Co2 Cl2 111.19(10) . . ? C1 O1 Co2 120.2(4) . . ? C1 O1 Co1 130.0(4) . . ? Co2 O1 Co1 109.7(2) . . ? C7 N1 N2 106.7(5) . . ? C7 N1 Co1 129.3(5) . . ? N2 N1 Co1 123.5(4) . . ? C8 N2 N1 105.4(6) . . ? C8 N2 Co2 139.6(5) . 7_556 ? N1 N2 Co2 114.8(4) . 7_556 ? C8 N3 C7 103.2(6) . . ? C11 N4 C12 115.2(7) . . ? C11 N4 Co1 122.3(5) . 4_556 ? C12 N4 Co1 122.4(5) . 4_556 ? O1 C1 C2 120.3(6) . . ? O1 C1 C6 123.0(6) . . ? C2 C1 C6 116.7(7) . . ? C3 C2 C1 122.8(7) . . ? C3 C2 H2A 118.6 . . ? C1 C2 H2A 118.6 . . ? C2 C3 C4 120.4(8) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 118.6(8) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? C4 C5 C6 122.6(8) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C1 118.9(7) . . ? C5 C6 C7 116.5(7) . . ? C1 C6 C7 124.4(7) . . ? N1 C7 N3 112.0(6) . . ? N1 C7 C6 125.5(6) . . ? N3 C7 C6 122.5(7) . . ? N2 C8 N3 112.7(6) . . ? N2 C8 C9 125.4(7) . . ? N3 C8 C9 122.0(7) . . ? C10 C9 C13 116.3(7) . . ? C10 C9 C8 124.4(7) . . ? C13 C9 C8 119.3(7) . . ? C9 C10 C11 119.3(7) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? N4 C11 C10 125.0(8) . . ? N4 C11 H11A 117.5 . . ? C10 C11 H11A 117.5 . . ? N4 C12 C13 124.0(8) . . ? N4 C12 H12A 118.0 . . ? C13 C12 H12A 118.0 . . ? C12 C13 C9 120.2(9) . . ? C12 C13 H13A 119.6 . . ? C9 C13 H13A 120.1 . . ? C1S N1S C1S 120.9(14) 2_655 . ? C1S N1S H1SG 107.1 2_655 . ? C1S N1S H1SG 107.0 . . ? N1S C1S H1SA 110.1 . . ? N1S C1S H1SB 109.1 . . ? H1SA C1S H1SB 109.5 . . ? N1S C1S H1SC 109.2 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C1A N1A C3A 123.0(9) . . ? C1A N1A C2A 120.5(12) . . ? C3A N1A C2A 102(3) . . ? C1A N1A H1AA 102.6 . . ? C3A N1A H1AA 102.6 . . ? C2A N1A H1AA 102.5 . . ? N1A C3A H3AA 109.5 . . ? N1A C3A H3AB 109.5 . . ? H3AA C3A H3AB 109.5 . . ? N1A C3A H3AC 109.5 . . ? H3AA C3A H3AC 109.5 . . ? H3AB C3A H3AC 109.5 . . ? N1A C2A H2AA 109.5 . . ? N1A C2A H2AB 109.5 . . ? H2AA C2A H2AB 109.5 . . ? N1A C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? O1A C1A N1A 116.9(9) . . ? O1A C1A H1AB 121.6 . . ? N1A C1A H1AB 121.6 . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.137 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.130 #===============================END data_1-CO2 _database_code_depnum_ccdc_archive 'CCDC 794767' #TrackingRef 'all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Cl4 Co3 N10 O5' _chemical_formula_weight 955.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.471(2) _cell_length_b 15.3812(17) _cell_length_c 13.8175(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.271(2) _cell_angle_gamma 90.00 _cell_volume 4350.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1388 _cell_measurement_theta_min 2.214 _cell_measurement_theta_max 22.3935 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1932 _exptl_absorpt_coefficient_mu 1.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8021 _exptl_absorpt_correction_T_max 0.8825 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCd' _diffrn_measurement_method '\w scan' _diffrn_reflns_number 9080 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3838 _reflns_number_gt 2630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Bruker AXS Inc., 1998.' _computing_cell_refinement 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_data_reduction 'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.' _computing_structure_solution 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_molecular_graphics 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _computing_publication_material 'SHELXTL Ver. 6.12, (Sheldrick, 2000)' _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. The alerts of A in checkcif report are caused by the two-fold disorder of Hdmf cations. ; _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^)+(0.1300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3838 _refine_ls_number_parameters 242 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2100 _refine_ls_wR_factor_gt 0.1827 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.015 _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 0.2500 0.2500 0.5000 0.0187(3) Uani 1 2 d S . . Co2 Co 0.34035(4) 0.11553(6) 0.36824(6) 0.0265(3) Uani 1 1 d . . . Cl1 Cl 0.39570(8) 0.15559(13) 0.23403(13) 0.0428(5) Uani 1 1 d . . . Cl2 Cl 0.37290(9) -0.01615(12) 0.42296(15) 0.0476(5) Uani 1 1 d . . . O1 O 0.15498(19) 0.2965(3) 0.5283(3) 0.0228(9) Uani 1 1 d . . . N1 N 0.2093(2) 0.1758(3) 0.3943(4) 0.0240(11) Uani 1 1 d . . . N2 N 0.2437(2) 0.1159(3) 0.3416(4) 0.0242(12) Uani 1 1 d . . . N3 N 0.1374(3) 0.1001(3) 0.3059(4) 0.0314(13) Uani 1 1 d . . . N4 N 0.2336(2) -0.1422(3) 0.1019(4) 0.0268(12) Uani 1 1 d . . . C1 C 0.0968(3) 0.2739(4) 0.4878(4) 0.0231(13) Uani 1 1 d . . . C2 C 0.0396(3) 0.3107(4) 0.5244(5) 0.0280(14) Uani 1 1 d . . . H2A H 0.0424 0.3508 0.5766 0.034 Uiso 1 1 calc R . . C3 C -0.0215(3) 0.2899(5) 0.4862(5) 0.0338(16) Uani 1 1 d . . . H3A H -0.0597 0.3165 0.5113 0.041 Uiso 1 1 calc R . . C4 C -0.0264(3) 0.2310(5) 0.4126(5) 0.0406(19) Uani 1 1 d . . . H4A H -0.0680 0.2163 0.3865 0.049 Uiso 1 1 calc R . . C5 C 0.0290(3) 0.1933(5) 0.3765(5) 0.0375(17) Uani 1 1 d . . . H5A H 0.0252 0.1519 0.3258 0.045 Uiso 1 1 calc R . . C6 C 0.0914(3) 0.2143(4) 0.4125(4) 0.0259(14) Uani 1 1 d . . . C7 C 0.1464(3) 0.1642(4) 0.3710(4) 0.0248(14) Uani 1 1 d . . . C8 C 0.1986(3) 0.0719(4) 0.2901(5) 0.0294(15) Uani 1 1 d . . . C9 C 0.2124(3) -0.0011(4) 0.2253(4) 0.0250(14) Uani 1 1 d . . . C10 C 0.1626(4) -0.0498(5) 0.1903(6) 0.048(2) Uani 1 1 d . . . H10A H 0.1190 -0.0358 0.2075 0.057 Uiso 1 1 calc R . . C11 C 0.1741(4) -0.1195(5) 0.1301(6) 0.047(2) Uani 1 1 d . . . H11A H 0.1379 -0.1527 0.1079 0.057 Uiso 1 1 calc R . . C12 C 0.2821(3) -0.0936(5) 0.1334(6) 0.048(2) Uani 1 1 d . . . H12A H 0.3251 -0.1078 0.1134 0.058 Uiso 1 1 calc R . . C13 C 0.2738(3) -0.0224(5) 0.1946(6) 0.050(2) Uani 1 1 d . . . H13A H 0.3104 0.0110 0.2148 0.060 Uiso 1 1 calc R . . N1S N 0.5000 -0.0084(6) 0.2500 0.047(2) Uani 1 2 d S . . H1SD H 0.4723 0.0263 0.2825 0.056 Uiso 1 1 d R . . C1S C 0.4627(5) -0.0547(7) 0.1814(8) 0.093(4) Uani 1 1 d . . . H1SA H 0.4830 -0.1100 0.1704 0.139 Uiso 1 1 d R . . H1SB H 0.4192 -0.0635 0.2053 0.139 Uiso 1 1 d R . . H1SC H 0.4608 -0.0228 0.1217 0.139 Uiso 1 1 d R . . N1A N -0.2340(6) -0.2484(8) 0.0501(10) 0.063(4) Uiso 0.50 1 d PD A -1 H1AA H -0.2590 -0.2373 -0.0049 0.075 Uiso 0.50 1 calc PR A -1 C3A C -0.2768(7) -0.2261(11) 0.1333(11) 0.064(5) Uiso 0.50 1 d PD A -1 H3AA H -0.2830 -0.1630 0.1360 0.096 Uiso 0.50 1 calc PR A -1 H3AB H -0.2564 -0.2462 0.1936 0.096 Uiso 0.50 1 calc PR A -1 H3AC H -0.3193 -0.2546 0.1250 0.096 Uiso 0.50 1 calc PR A -1 C2A C -0.2283(9) -0.3426(8) 0.0554(16) 0.084(6) Uiso 0.50 1 d PD A -1 H2AA H -0.2007 -0.3633 0.0024 0.126 Uiso 0.50 1 calc PR A -1 H2AB H -0.2717 -0.3689 0.0499 0.126 Uiso 0.50 1 calc PR A -1 H2AC H -0.2085 -0.3590 0.1175 0.126 Uiso 0.50 1 calc PR A -1 C1A C -0.1797(7) -0.2008(10) 0.0398(13) 0.078(6) Uiso 0.50 1 d PD A -1 H1AB H -0.1368 -0.2235 0.0330 0.093 Uiso 0.50 1 calc PR A -1 O1A O -0.1937(12) -0.1250(10) 0.040(2) 0.264(17) Uiso 0.50 1 d PD A -1 O2C O -0.1109(9) -0.0784(14) 0.0578(16) 0.138(7) Uiso 0.50 1 d PD A -1 O1C O -0.0055(9) -0.0442(14) 0.1077(17) 0.147(8) Uiso 0.50 1 d PD A -1 C1C C -0.0591(11) -0.055(3) 0.083(3) 0.184(17) Uiso 0.50 1 d PD A -1 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 0.0243(6) 0.0146(6) 0.0173(6) -0.0003(4) 0.0004(4) 0.0017(4) Co2 0.0272(5) 0.0241(5) 0.0282(5) -0.0074(4) 0.0025(4) 0.0010(4) Cl1 0.0407(10) 0.0572(13) 0.0306(9) -0.0036(8) 0.0066(8) -0.0098(9) Cl2 0.0554(12) 0.0242(10) 0.0631(13) -0.0028(9) -0.0079(9) 0.0110(8) O1 0.027(2) 0.019(2) 0.023(2) -0.0028(18) -0.0016(17) 0.0036(18) N1 0.024(3) 0.026(3) 0.022(3) -0.005(2) 0.002(2) 0.001(2) N2 0.031(3) 0.016(3) 0.026(3) -0.004(2) 0.002(2) 0.000(2) N3 0.029(3) 0.027(3) 0.038(3) -0.008(3) -0.001(2) 0.001(2) N4 0.031(3) 0.024(3) 0.025(3) -0.009(2) -0.002(2) 0.000(2) C1 0.030(3) 0.017(3) 0.022(3) 0.006(3) 0.000(3) 0.000(3) C2 0.028(3) 0.025(3) 0.031(4) -0.002(3) 0.003(3) 0.008(3) C3 0.023(3) 0.038(4) 0.041(4) -0.006(3) 0.000(3) 0.006(3) C4 0.027(4) 0.056(5) 0.039(4) -0.020(4) -0.005(3) 0.001(3) C5 0.031(4) 0.046(5) 0.036(4) -0.016(3) -0.011(3) 0.008(3) C6 0.029(3) 0.025(3) 0.024(3) 0.001(3) -0.003(3) 0.007(3) C7 0.027(3) 0.031(4) 0.017(3) -0.004(3) 0.003(2) 0.001(3) C8 0.035(4) 0.024(4) 0.030(4) -0.005(3) 0.002(3) -0.002(3) C9 0.030(3) 0.020(3) 0.025(3) -0.003(3) -0.003(3) 0.003(3) C10 0.032(4) 0.047(5) 0.064(5) -0.031(4) 0.006(4) 0.003(3) C11 0.033(4) 0.050(5) 0.059(5) -0.040(4) -0.002(4) -0.001(3) C12 0.028(4) 0.059(5) 0.058(5) -0.032(4) 0.003(4) 0.000(4) C13 0.030(4) 0.051(5) 0.069(5) -0.038(4) -0.001(4) -0.007(3) N1S 0.043(5) 0.042(6) 0.056(6) 0.000 0.000(4) 0.000 C1S 0.062(6) 0.112(10) 0.104(9) -0.080(8) -0.022(6) 0.029(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.029(5) 7_556 ? Co1 N1 2.029(5) . ? Co1 O1 2.111(4) . ? Co1 O1 2.111(4) 7_556 ? Co1 N4 2.202(5) 6_556 ? Co1 N4 2.202(5) 4 ? Co2 O1 1.970(4) 7_556 ? Co2 N2 2.010(5) . ? Co2 Cl1 2.2633(19) . ? Co2 Cl2 2.261(2) . ? O1 C1 1.358(7) . ? O1 Co2 1.970(4) 7_556 ? N1 C7 1.338(8) . ? N1 N2 1.372(7) . ? N2 C8 1.346(8) . ? N3 C7 1.346(8) . ? N3 C8 1.344(8) . ? N4 C12 1.314(9) . ? N4 C11 1.328(8) . ? N4 Co1 2.202(5) 4_545 ? C1 C6 1.391(9) . ? C1 C2 1.399(8) . ? C2 C3 1.392(9) . ? C2 H2A 0.9500 . ? C3 C4 1.365(9) . ? C3 H3A 0.9500 . ? C4 C5 1.370(9) . ? C4 H4A 0.9500 . ? C5 C6 1.405(9) . ? C5 H5A 0.9500 . ? C6 C7 1.482(8) . ? C8 C9 1.464(9) . ? C9 C10 1.353(9) . ? C9 C13 1.367(9) . ? C10 C11 1.378(9) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.395(10) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? N1S C1S 1.408(9) . ? N1S C1S 1.408(9) 2_655 ? N1S H1SD 0.8999 . ? C1S H1SA 0.9598 . ? C1S H1SB 0.9601 . ? C1S H1SC 0.9599 . ? N1A C1A 1.339(8) . ? N1A C2A 1.456(9) . ? N1A C3A 1.488(9) . ? N1A H1AA 0.9300 . ? C3A H3AA 0.9800 . ? C3A H3AB 0.9800 . ? C3A H3AC 0.9800 . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C1A O1A 1.200(9) . ? C1A H1AB 0.9500 . ? O1A O2C 1.86(3) . ? O2C C1C 1.169(9) . ? O1C C1C 1.162(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.000(1) 7_556 . ? N1 Co1 O1 92.96(17) 7_556 . ? N1 Co1 O1 87.04(17) . . ? N1 Co1 O1 87.04(17) 7_556 7_556 ? N1 Co1 O1 92.96(17) . 7_556 ? O1 Co1 O1 180.0 . 7_556 ? N1 Co1 N4 91.5(2) 7_556 6_556 ? N1 Co1 N4 88.5(2) . 6_556 ? O1 Co1 N4 89.62(17) . 6_556 ? O1 Co1 N4 90.38(17) 7_556 6_556 ? N1 Co1 N4 88.5(2) 7_556 4 ? N1 Co1 N4 91.5(2) . 4 ? O1 Co1 N4 90.38(17) . 4 ? O1 Co1 N4 89.62(17) 7_556 4 ? N4 Co1 N4 180.00(18) 6_556 4 ? O1 Co2 N2 100.11(18) 7_556 . ? O1 Co2 Cl1 112.62(13) 7_556 . ? N2 Co2 Cl1 110.18(16) . . ? O1 Co2 Cl2 111.06(13) 7_556 . ? N2 Co2 Cl2 110.60(15) . . ? Cl1 Co2 Cl2 111.72(8) . . ? C1 O1 Co2 120.9(4) . 7_556 ? C1 O1 Co1 130.1(4) . . ? Co2 O1 Co1 109.00(18) 7_556 . ? C7 N1 N2 106.1(5) . . ? C7 N1 Co1 129.8(4) . . ? N2 N1 Co1 123.4(4) . . ? C8 N2 N1 105.4(5) . . ? C8 N2 Co2 140.2(4) . . ? N1 N2 Co2 114.3(4) . . ? C7 N3 C8 102.7(5) . . ? C12 N4 C11 116.4(6) . . ? C12 N4 Co1 121.5(5) . 4_545 ? C11 N4 Co1 121.9(4) . 4_545 ? O1 C1 C6 123.0(5) . . ? O1 C1 C2 118.8(6) . . ? C6 C1 C2 118.2(6) . . ? C1 C2 C3 121.5(6) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C4 C3 C2 119.9(6) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 119.6(6) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C4 C5 C6 121.8(6) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C1 C6 C5 119.0(6) . . ? C1 C6 C7 125.0(5) . . ? C5 C6 C7 115.8(6) . . ? N3 C7 N1 112.8(5) . . ? N3 C7 C6 122.5(5) . . ? N1 C7 C6 124.7(6) . . ? N3 C8 N2 112.9(5) . . ? N3 C8 C9 122.0(6) . . ? N2 C8 C9 125.0(6) . . ? C10 C9 C13 116.6(6) . . ? C10 C9 C8 119.7(6) . . ? C13 C9 C8 123.6(6) . . ? C9 C10 C11 121.1(7) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? N4 C11 C10 122.8(6) . . ? N4 C11 H11A 118.6 . . ? C10 C11 H11A 118.6 . . ? N4 C12 C13 123.6(7) . . ? N4 C12 H12A 118.2 . . ? C13 C12 H12A 118.2 . . ? C9 C13 C12 119.4(6) . . ? C9 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C1S N1S C1S 119.3(12) . 2_655 ? C1S N1S H1SD 107.1 . . ? C1S N1S H1SD 107.8 2_655 . ? N1S C1S H1SA 108.6 . . ? N1S C1S H1SB 109.9 . . ? H1SA C1S H1SB 109.5 . . ? N1S C1S H1SC 109.9 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C1A N1A C2A 118.8(10) . . ? C1A N1A C3A 116.7(9) . . ? C2A N1A C3A 103.8(13) . . ? C1A N1A H1AA 105.5 . . ? C2A N1A H1AA 105.5 . . ? C3A N1A H1AA 105.5 . . ? N1A C3A H3AA 109.5 . . ? N1A C3A H3AB 109.5 . . ? H3AA C3A H3AB 109.5 . . ? N1A C3A H3AC 109.5 . . ? H3AA C3A H3AC 109.5 . . ? H3AB C3A H3AC 109.5 . . ? N1A C2A H2AA 109.5 . . ? N1A C2A H2AB 109.5 . . ? H2AA C2A H2AB 109.5 . . ? N1A C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? O1A C1A N1A 109.4(10) . . ? O1A C1A H1AB 125.3 . . ? N1A C1A H1AB 125.3 . . ? C1A O1A O2C 99.1(18) . . ? C1C O2C O1A 170(3) . . ? O1C C1C O2C 170(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.669 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.136