# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Dirk Volkmer' Denysenko D.Denysenko Tamas T.Werner Maciej M.Grzywa ; Institute of Physics, Chair of Solid State and Material Science Augsburg University Universitaetsstrasse 1, D-86135 Augsburg, Germany ; A.Puls Puls V.Hagen Volker G.Eickerling ; Rubokat GmbH D-44801 Bochum Germany ; J.Jelic Eickerling K.Reuter Jelena _publ_contact_author_address ; Institute of Physics, Chair of Solid State and Material Science Augsburg University Universitaetsstrasse 1, D-86135 Augsburg, Germany ; _publ_contact_author_email dirk.volkmer@uni-ulm.de _publ_contact_author_fax '+49 (0)821 598 5955' _publ_contact_author_phone '+49 (0)821 598 3006' #TrackingRef '- Co-MFU-4l.cif' _publ_contact_author_name 'Professor Dirk Volkmer' _publ_section_title ; Reversible gas-phase redox processes catalyzed by Co-exchanged MFU-4l(arge)' ; data_Co-MFU-4l _database_code_depnum_ccdc_archive 'CCDC 847582' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C36 H12 Cl4 Co4 N18 O6 Zn1' _chemical_formula_sum 'C36 H12 Cl4 Co4 N18 O6 Zn1' _chemical_formula_weight 1235.5 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.018 0.009 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Cl 0.364 0.702 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.031 0.018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.049 0.032 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Zn -1.549 0.678 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Co -2.365 3.614 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F m -3 m' _symmetry_space_group_name_Hall '-F 4;2;3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,z 3 -x,y,-z 4 x,-y,-z 5 z,x,y 6 z,-x,-y 7 -z,-x,y 8 -z,x,-y 9 y,z,x 10 -y,z,-x 11 y,-z,-x 12 -y,-z,x 13 y,x,-z 14 -y,-x,-z 15 y,-x,z 16 -y,x,z 17 x,z,-y 18 -x,z,y 19 -x,-z,-y 20 x,-z,y 21 z,y,-x 22 z,-y,x 23 -z,y,x 24 -z,-y,-x 25 -x,-y,-z 26 x,y,-z 27 x,-y,z 28 -x,y,z 29 -z,-x,-y 30 -z,x,y 31 z,x,-y 32 z,-x,y 33 -y,-z,-x 34 y,-z,x 35 -y,z,x 36 y,z,-x 37 -y,-x,z 38 y,x,z 39 -y,x,-z 40 y,-x,-z 41 -x,-z,y 42 x,-z,-y 43 x,z,y 44 -x,z,-y 45 -z,-y,x 46 -z,y,-x 47 z,-y,-x 48 z,y,x 49 x,y+1/2,z+1/2 50 -x,-y+1/2,z+1/2 51 -x,y+1/2,-z+1/2 52 x,-y+1/2,-z+1/2 53 z,x+1/2,y+1/2 54 z,-x+1/2,-y+1/2 55 -z,-x+1/2,y+1/2 56 -z,x+1/2,-y+1/2 57 y,z+1/2,x+1/2 58 -y,z+1/2,-x+1/2 59 y,-z+1/2,-x+1/2 60 -y,-z+1/2,x+1/2 61 y,x+1/2,-z+1/2 62 -y,-x+1/2,-z+1/2 63 y,-x+1/2,z+1/2 64 -y,x+1/2,z+1/2 65 x,z+1/2,-y+1/2 66 -x,z+1/2,y+1/2 67 -x,-z+1/2,-y+1/2 68 x,-z+1/2,y+1/2 69 z,y+1/2,-x+1/2 70 z,-y+1/2,x+1/2 71 -z,y+1/2,x+1/2 72 -z,-y+1/2,-x+1/2 73 -x,-y+1/2,-z+1/2 74 x,y+1/2,-z+1/2 75 x,-y+1/2,z+1/2 76 -x,y+1/2,z+1/2 77 -z,-x+1/2,-y+1/2 78 -z,x+1/2,y+1/2 79 z,x+1/2,-y+1/2 80 z,-x+1/2,y+1/2 81 -y,-z+1/2,-x+1/2 82 y,-z+1/2,x+1/2 83 -y,z+1/2,x+1/2 84 y,z+1/2,-x+1/2 85 -y,-x+1/2,z+1/2 86 y,x+1/2,z+1/2 87 -y,x+1/2,-z+1/2 88 y,-x+1/2,-z+1/2 89 -x,-z+1/2,y+1/2 90 x,-z+1/2,-y+1/2 91 x,z+1/2,y+1/2 92 -x,z+1/2,-y+1/2 93 -z,-y+1/2,x+1/2 94 -z,y+1/2,-x+1/2 95 z,-y+1/2,-x+1/2 96 z,y+1/2,x+1/2 97 x+1/2,y,z+1/2 98 -x+1/2,-y,z+1/2 99 -x+1/2,y,-z+1/2 100 x+1/2,-y,-z+1/2 101 z+1/2,x,y+1/2 102 z+1/2,-x,-y+1/2 103 -z+1/2,-x,y+1/2 104 -z+1/2,x,-y+1/2 105 y+1/2,z,x+1/2 106 -y+1/2,z,-x+1/2 107 y+1/2,-z,-x+1/2 108 -y+1/2,-z,x+1/2 109 y+1/2,x,-z+1/2 110 -y+1/2,-x,-z+1/2 111 y+1/2,-x,z+1/2 112 -y+1/2,x,z+1/2 113 x+1/2,z,-y+1/2 114 -x+1/2,z,y+1/2 115 -x+1/2,-z,-y+1/2 116 x+1/2,-z,y+1/2 117 z+1/2,y,-x+1/2 118 z+1/2,-y,x+1/2 119 -z+1/2,y,x+1/2 120 -z+1/2,-y,-x+1/2 121 -x+1/2,-y,-z+1/2 122 x+1/2,y,-z+1/2 123 x+1/2,-y,z+1/2 124 -x+1/2,y,z+1/2 125 -z+1/2,-x,-y+1/2 126 -z+1/2,x,y+1/2 127 z+1/2,x,-y+1/2 128 z+1/2,-x,y+1/2 129 -y+1/2,-z,-x+1/2 130 y+1/2,-z,x+1/2 131 -y+1/2,z,x+1/2 132 y+1/2,z,-x+1/2 133 -y+1/2,-x,z+1/2 134 y+1/2,x,z+1/2 135 -y+1/2,x,-z+1/2 136 y+1/2,-x,-z+1/2 137 -x+1/2,-z,y+1/2 138 x+1/2,-z,-y+1/2 139 x+1/2,z,y+1/2 140 -x+1/2,z,-y+1/2 141 -z+1/2,-y,x+1/2 142 -z+1/2,y,-x+1/2 143 z+1/2,-y,-x+1/2 144 z+1/2,y,x+1/2 145 x+1/2,y+1/2,z 146 -x+1/2,-y+1/2,z 147 -x+1/2,y+1/2,-z 148 x+1/2,-y+1/2,-z 149 z+1/2,x+1/2,y 150 z+1/2,-x+1/2,-y 151 -z+1/2,-x+1/2,y 152 -z+1/2,x+1/2,-y 153 y+1/2,z+1/2,x 154 -y+1/2,z+1/2,-x 155 y+1/2,-z+1/2,-x 156 -y+1/2,-z+1/2,x 157 y+1/2,x+1/2,-z 158 -y+1/2,-x+1/2,-z 159 y+1/2,-x+1/2,z 160 -y+1/2,x+1/2,z 161 x+1/2,z+1/2,-y 162 -x+1/2,z+1/2,y 163 -x+1/2,-z+1/2,-y 164 x+1/2,-z+1/2,y 165 z+1/2,y+1/2,-x 166 z+1/2,-y+1/2,x 167 -z+1/2,y+1/2,x 168 -z+1/2,-y+1/2,-x 169 -x+1/2,-y+1/2,-z 170 x+1/2,y+1/2,-z 171 x+1/2,-y+1/2,z 172 -x+1/2,y+1/2,z 173 -z+1/2,-x+1/2,-y 174 -z+1/2,x+1/2,y 175 z+1/2,x+1/2,-y 176 z+1/2,-x+1/2,y 177 -y+1/2,-z+1/2,-x 178 y+1/2,-z+1/2,x 179 -y+1/2,z+1/2,x 180 y+1/2,z+1/2,-x 181 -y+1/2,-x+1/2,z 182 y+1/2,x+1/2,z 183 -y+1/2,x+1/2,-z 184 y+1/2,-x+1/2,-z 185 -x+1/2,-z+1/2,y 186 x+1/2,-z+1/2,-y 187 x+1/2,z+1/2,y 188 -x+1/2,z+1/2,-y 189 -z+1/2,-y+1/2,x 190 -z+1/2,y+1/2,-x 191 z+1/2,-y+1/2,-x 192 z+1/2,y+1/2,x _cell_length_a 30.9950(7) _cell_length_b 30.9950(7) _cell_length_c 30.9950(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 29776.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'microcrystalline powder' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4768 _exptl_absorpt_coefficient_mu 4.434 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_source X-ray _diffrn_source_target Cu _diffrn_source_type 'fine-focus sealed tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_monochromator germanium _diffrn_measurement_device_type 'STOE STADI P' _diffrn_detector 'Meteor 1D' _diffrn_detector_type PSD _pd_meas_number_of_points 4300 _pd_meas_2theta_range_min 4.020 _pd_meas_2theta_range_max 90.000 _pd_meas_2theta_range_inc 0.02 _pd_proc_ls_special_details ; ? ; _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function '15 Legendre polynoms' _pd_proc_ls_pref_orient_corr 'March & Dollase' _pd_proc_ls_prof_R_factor 0.0137 _pd_proc_ls_prof_wR_factor 0.0224 _pd_proc_ls_prof_wR_expected 0.0435 _refine_special_details ; ? ; _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_gt 0.0608 _refine_ls_R_factor_all 0.0932 _refine_ls_wR_factor_ref 0.0807 _refine_ls_number_parameters 18 _refine_ls_number_restraints 6 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0287 _refine_ls_shift/su_mean 0.0035 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _pd_proc_2theta_range_min 4.02 _pd_proc_2theta_range_max 90 _pd_proc_2theta_range_inc 0.02 _pd_proc_wavelength ? _pd_block_diffractogram_id ? _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? _computing_data_collection 'Diffractometer software' _computing_cell_refinement PROSZKI _computing_structure_solution ? _computing_structure_refinement Jana2006 _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material Jana2006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co2 Co 0.3185(3) 0.3185(3) 0.181542 Uiso 0.013(6) 32 1 d . . . Cl1 Cl 0.356(2) 0.356(2) 0.144361 Uiso 0.05(2) 32 1 d . . . N1 N 0.3399(3) 0.2752(2) 0.224812 Uiso 0.018(10) 96 1 d . . . C1 C 0.38267(10) 0.2665(3) 0.233457 Uiso 0.047(15) 96 1 d . . . N2 N 0.3146(6) 0.25 0.25 Uiso 0.018(10) 48 1 d . . . C2 C 0.4215(2) 0.2826(2) 0.217351 Uiso 0.047(15) 96 1 d . . . C3 C 0.4612(2) 0.2669(2) 0.233142 Uiso 0.047(15) 96 1 d . . . O1 O 0.5 0.2834(4) 0.216589 Uiso 0.04(3) 48 1 d . . . Zn1 Zn 0.25 0.25 0.25 Uiso 0.04(2) 8 1 d . . . H1 H 0.421274 0.303866 0.196134 Uiso 0.038 96 1 d . . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co2 Cl1 . . 2.00(5) yes Co2 N1 . . 2.009(9) yes Co2 N1 . 104_555 2.009(9) yes Co2 N1 . 59_555 2.009(10) yes N1 N1 . 52_555 2.208(6) yes N1 N1 . 104_555 2.835(10) yes N1 N1 . 59_555 2.835(10) yes N1 C1 . . 1.380(10) yes N1 C1 . 52_555 2.260(9) yes N1 N2 . . 1.355(13) yes N1 C2 . . 2.552(11) yes N1 Zn1 . . 2.996(9) yes C1 C1 . 52_555 1.450(9) yes C1 N2 . . 2.232(18) yes C1 C2 . . 1.396(7) yes C1 C2 . 52_555 2.470(8) yes C1 C3 . . 2.433(7) yes C1 C3 . 52_555 2.839(7) yes N2 N2 . 5_555 2.830(19) yes N2 N2 . 54_555 2.830(19) yes N2 N2 . 9_555 2.830(19) yes N2 N2 . 106_555 2.830(19) yes N2 Zn1 . . 2.001(19) yes C2 C2 . 52_555 2.862(6) yes C2 C3 . . 1.410(8) yes C2 O1 . . 2.432(6) yes C3 C3 . 52_555 1.478(6) yes C3 C3 . 18_655 2.826(8) yes C3 C3 . 67_655 2.408(9) yes C3 O1 . . 1.406(7) yes C3 O1 . 52_555 2.511(9) yes O1 O1 . 52_555 2.929(12) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Co2 N1 . . . 125.4(17) yes Cl1 Co2 N1 . . 104_555 125.4(17) yes Cl1 Co2 N1 . . 59_555 125.4(11) yes Cl1 Co2 C1 . . . 103.6(17) yes Cl1 Co2 C1 . . 104_555 103.6(17) yes Cl1 Co2 C1 . . 59_555 103.6(10) yes Cl1 Co2 N2 . . . 147.0(17) yes Cl1 Co2 N2 . . 5_555 147.0(17) yes Cl1 Co2 N2 . . 106_555 147.0(11) yes N1 Co2 N1 . . 104_555 89.7(3) yes N1 Co2 N1 . . 59_555 89.7(5) yes N1 Co2 C1 . . . 21.9(3) yes N1 Co2 C1 . . 104_555 105.1(2) yes N1 Co2 C1 . . 59_555 105.1(4) yes N1 Co2 N2 . . . 21.6(4) yes N1 Co2 N2 . . 5_555 74.6(4) yes N1 Co2 N2 . . 106_555 74.6(4) yes N1 Co2 N1 104_555 . 59_555 89.7(5) yes N1 Co2 C1 104_555 . . 105.1(2) yes N1 Co2 C1 104_555 . 104_555 21.9(3) yes N1 Co2 C1 104_555 . 59_555 105.1(4) yes N1 Co2 N2 104_555 . . 74.6(4) yes N1 Co2 N2 104_555 . 5_555 21.6(4) yes N1 Co2 N2 104_555 . 106_555 74.6(4) yes N1 Co2 C1 59_555 . . 105.1(4) yes N1 Co2 C1 59_555 . 104_555 105.1(4) yes N1 Co2 C1 59_555 . 59_555 21.9(3) yes N1 Co2 N2 59_555 . . 74.6(4) yes N1 Co2 N2 59_555 . 5_555 74.6(4) yes N1 Co2 N2 59_555 . 106_555 21.6(4) yes C1 Co2 C1 . . 104_555 114.68(18) yes C1 Co2 C1 . . 59_555 114.7(3) yes C1 Co2 N2 . . . 43.5(4) yes C1 Co2 N2 . . 5_555 93.9(2) yes C1 Co2 N2 . . 106_555 93.9(3) yes C1 Co2 C1 104_555 . 59_555 114.7(3) yes C1 Co2 N2 104_555 . . 93.9(3) yes C1 Co2 N2 104_555 . 5_555 43.5(4) yes C1 Co2 N2 104_555 . 106_555 93.9(3) yes C1 Co2 N2 59_555 . . 93.9(3) yes C1 Co2 N2 59_555 . 5_555 93.9(3) yes C1 Co2 N2 59_555 . 106_555 43.5(4) yes N2 Co2 N2 . . 5_555 56.2(4) yes N2 Co2 N2 . . 106_555 56.2(4) yes N2 Co2 N2 5_555 . 106_555 56.2(4) yes Co2 N1 N1 . . 52_555 160.7(6) yes Co2 N1 N1 . . 104_555 45.1(3) yes Co2 N1 N1 . . 59_555 45.1(3) yes Co2 N1 C1 . . . 125.2(6) yes Co2 N1 C1 . . 52_555 163.3(5) yes Co2 N1 N2 . . . 125.3(9) yes Co2 N1 N2 . . 5_555 67.3(4) yes Co2 N1 N2 . . 106_555 67.3(4) yes Co2 N1 C2 . . . 101.9(4) yes Co2 N1 Zn1 . . . 92.3(4) yes N1 N1 N1 52_555 . 104_555 120.0(4) yes N1 N1 N1 52_555 . 59_555 120.0(4) yes N1 N1 C1 52_555 . . 74.1(4) yes N1 N1 N2 52_555 . 5_555 95.7(4) yes N1 N1 N2 52_555 . 106_555 95.7(4) yes N1 N1 C2 52_555 . . 97.4(4) yes N1 N1 Zn1 52_555 . . 68.4(3) yes N1 N1 N1 104_555 . 59_555 60.0(2) yes N1 N1 C1 104_555 . . 144.8(5) yes N1 N1 C1 104_555 . 52_555 145.07(19) yes N1 N1 N2 104_555 . . 89.9(7) yes N1 N1 N2 104_555 . 106_555 63.2(2) yes N1 N1 C2 104_555 . . 129.6(3) yes N1 N1 Zn1 104_555 . . 61.8(2) yes N1 N1 C1 59_555 . . 144.8(3) yes N1 N1 C1 59_555 . 52_555 145.1(3) yes N1 N1 N2 59_555 . . 89.9(7) yes N1 N1 N2 59_555 . 5_555 63.2(2) yes N1 N1 C2 59_555 . . 129.6(2) yes N1 N1 Zn1 59_555 . . 61.8(2) yes C1 N1 N2 . . . 109.5(8) yes C1 N1 N2 . . 5_555 151.7(3) yes C1 N1 N2 . . 106_555 151.7(5) yes C1 N1 Zn1 . . . 142.4(4) yes C1 N1 N2 52_555 . . 71.4(7) yes C1 N1 N2 52_555 . 5_555 126.9(2) yes C1 N1 N2 52_555 . 106_555 126.9(3) yes C1 N1 C2 52_555 . . 61.4(3) yes C1 N1 Zn1 52_555 . . 104.3(2) yes N2 N1 N2 . . 5_555 64.3(7) yes N2 N1 N2 . . 106_555 64.3(7) yes N2 N1 C2 . . . 132.8(8) yes N2 N1 N2 5_555 . 106_555 53.6(3) yes N2 N1 C2 5_555 . . 150.1(4) yes N2 N1 C2 106_555 . . 150.1(3) yes C2 N1 Zn1 . . . 165.7(2) yes Co2 C1 N1 . . 52_555 102.9(3) yes Co2 C1 C1 . . 52_555 138.83(18) yes Co2 C1 N2 . . . 67.8(2) yes Co2 C1 C2 . . . 100.8(4) yes N1 C1 N1 . . 52_555 70.0(3) yes N1 C1 C1 . . 52_555 105.9(3) yes N1 C1 C2 . . . 133.7(6) yes N1 C1 C1 52_555 . 52_555 35.9(2) yes N1 C1 C2 52_555 . . 156.3(4) yes C1 C1 N2 52_555 . . 71.0(2) yes C1 C1 C2 52_555 . . 120.4(3) yes N2 C1 C2 . . . 168.6(5) yes Co2 N2 Co2 . . 52_555 175.4(8) yes Co2 N2 N1 . . 52_555 142.3(11) yes Co2 N2 N1 . . 151_555 144.9(4) yes Co2 N2 N1 . . 9_555 144.9(4) yes Co2 N2 C1 . . . 68.7(3) yes Co2 N2 C1 . . 52_555 106.6(6) yes Co2 N2 N2 . . 5_555 61.9(3) yes Co2 N2 N2 . . 54_555 121.9(5) yes Co2 N2 N2 . . 9_555 121.9(5) yes Co2 N2 N2 . . 106_555 61.9(3) yes Co2 N2 Zn1 . . . 92.3(4) yes Co2 N2 N1 52_555 . . 142.3(11) yes Co2 N2 N1 52_555 . 104_555 144.9(4) yes Co2 N2 N1 52_555 . 59_555 144.9(4) yes Co2 N2 C1 52_555 . . 106.6(6) yes Co2 N2 C1 52_555 . 52_555 68.7(3) yes Co2 N2 N2 52_555 . 5_555 121.9(5) yes Co2 N2 N2 52_555 . 54_555 61.9(3) yes Co2 N2 N2 52_555 . 9_555 61.9(3) yes Co2 N2 N2 52_555 . 106_555 121.9(5) yes Co2 N2 Zn1 52_555 . . 92.3(4) yes N1 N2 N1 . . 52_555 109.2(14) yes N1 N2 N1 . . 151_555 151.6(5) yes N1 N2 N1 . . 104_555 64.6(4) yes N1 N2 N1 . . 9_555 151.6(4) yes N1 N2 N1 . . 59_555 64.6(4) yes N1 N2 C1 . . 52_555 73.6(9) yes N1 N2 N2 . . 5_555 90.1(5) yes N1 N2 N2 . . 54_555 144.8(4) yes N1 N2 N2 . . 9_555 144.8(4) yes N1 N2 N2 . . 106_555 90.1(5) yes N1 N2 Zn1 . . . 125.4(7) yes N1 N2 N1 52_555 . 151_555 64.6(4) yes N1 N2 N1 52_555 . 104_555 151.6(5) yes N1 N2 N1 52_555 . 9_555 64.6(4) yes N1 N2 N1 52_555 . 59_555 151.6(4) yes N1 N2 C1 52_555 . . 73.6(9) yes N1 N2 N2 52_555 . 5_555 144.8(4) yes N1 N2 N2 52_555 . 54_555 90.1(5) yes N1 N2 N2 52_555 . 9_555 90.1(5) yes N1 N2 N2 52_555 . 106_555 144.8(4) yes N1 N2 Zn1 52_555 . . 125.4(7) yes N1 N2 N1 151_555 . 104_555 134.3(6) yes N1 N2 N1 151_555 . 9_555 53.68(19) yes N1 N2 N1 151_555 . 59_555 106.9(4) yes N1 N2 C1 151_555 . . 128.9(5) yes N1 N2 C1 151_555 . 52_555 96.1(3) yes N1 N2 N2 151_555 . 5_555 110.6(6) yes N1 N2 N2 151_555 . 9_555 63.2(3) yes N1 N2 N2 151_555 . 106_555 84.3(4) yes N1 N2 Zn1 151_555 . . 67.1(3) yes N1 N2 N1 104_555 . 9_555 106.9(4) yes N1 N2 N1 104_555 . 59_555 53.68(19) yes N1 N2 C1 104_555 . . 96.1(3) yes N1 N2 C1 104_555 . 52_555 128.9(5) yes N1 N2 N2 104_555 . 54_555 110.6(6) yes N1 N2 N2 104_555 . 9_555 84.3(4) yes N1 N2 N2 104_555 . 106_555 63.2(3) yes N1 N2 Zn1 104_555 . . 67.1(3) yes N1 N2 N1 9_555 . 59_555 134.3(6) yes N1 N2 C1 9_555 . . 128.9(5) yes N1 N2 C1 9_555 . 52_555 96.1(2) yes N1 N2 N2 9_555 . 5_555 84.3(4) yes N1 N2 N2 9_555 . 54_555 63.2(3) yes N1 N2 N2 9_555 . 106_555 110.6(6) yes N1 N2 Zn1 9_555 . . 67.1(3) yes N1 N2 C1 59_555 . . 96.1(2) yes N1 N2 C1 59_555 . 52_555 128.9(5) yes N1 N2 N2 59_555 . 5_555 63.2(3) yes N1 N2 N2 59_555 . 54_555 84.3(4) yes N1 N2 N2 59_555 . 9_555 110.6(6) yes N1 N2 Zn1 59_555 . . 67.1(3) yes C1 N2 N2 . . 5_555 120.4(4) yes C1 N2 N2 . . 54_555 146.2(5) yes C1 N2 N2 . . 9_555 146.2(4) yes C1 N2 N2 . . 106_555 120.4(3) yes C1 N2 Zn1 . . . 161.0(2) yes C1 N2 N2 52_555 . 5_555 146.2(5) yes C1 N2 N2 52_555 . 54_555 120.4(4) yes C1 N2 N2 52_555 . 9_555 120.4(3) yes C1 N2 N2 52_555 . 106_555 146.2(4) yes C1 N2 Zn1 52_555 . . 161.0(2) yes N2 N2 N2 5_555 . 54_555 90.0(7) yes N2 N2 N2 5_555 . 9_555 60.0(4) yes N2 N2 N2 5_555 . 106_555 60.0(4) yes N2 N2 Zn1 5_555 . . 45.0(4) yes N2 N2 N2 54_555 . 9_555 60.0(4) yes N2 N2 N2 54_555 . 106_555 60.0(4) yes N2 N2 Zn1 54_555 . . 45.0(4) yes N2 N2 N2 9_555 . 106_555 90.0(7) yes N2 N2 Zn1 9_555 . . 45.0(4) yes N2 N2 Zn1 106_555 . . 45.0(4) yes N1 C2 C3 . . . 143.2(4) yes N1 C2 O1 . . . 173.4(3) yes C1 C2 C3 . . . 120.2(4) yes C1 C2 O1 . . . 150.4(4) yes C2 C3 C3 . . 52_555 119.4(5) yes C2 C3 O1 . . . 119.5(5) yes C2 C3 O1 . . 52_555 148.1(4) yes C3 C3 O1 52_555 . . 121.1(6) yes O1 C3 O1 . . 52_555 92.4(4) yes C2 O1 C2 . . 67_655 178.4(4) yes C2 O1 C3 . . 52_555 60.6(2) yes C2 O1 C3 . . 18_655 117.9(3) yes C2 O1 C3 . . 67_655 148.1(6) yes C2 O1 O1 . . 52_555 89.2(2) yes C2 O1 C3 67_655 . . 148.1(6) yes C2 O1 C3 67_655 . 52_555 117.9(3) yes C2 O1 C3 67_655 . 18_655 60.6(2) yes C2 O1 O1 67_655 . 52_555 89.2(2) yes C3 O1 C3 . . 18_655 87.6(5) yes C3 O1 C3 . . 67_655 117.9(7) yes C3 O1 O1 . . 52_555 58.9(4) yes C3 O1 C3 52_555 . 18_655 57.3(3) yes C3 O1 C3 52_555 . 67_655 87.6(5) yes C3 O1 O1 67_655 . 52_555 58.9(4) yes N1 Zn1 N1 . . 146_555 149.80(6) yes N1 Zn1 N1 . . 99_555 149.80(17) yes N1 Zn1 N1 . . 52_555 43.24(14) yes N1 Zn1 N1 . . 5_555 93.89(13) yes N1 Zn1 N1 . . 54_555 114.62(12) yes N1 Zn1 N1 . . 151_555 93.89(13) yes N1 Zn1 N1 . . 104_555 56.47(14) yes N1 Zn1 N1 . . 9_555 93.89(13) yes N1 Zn1 N1 . . 106_555 93.89(13) yes N1 Zn1 N1 . . 59_555 56.47(14) yes N1 Zn1 N1 . . 156_555 114.62(12) yes N1 Zn1 N2 . . 146_555 158.38(10) yes N1 Zn1 N2 . . 5_555 74.90(12) yes N1 Zn1 N2 . . 54_555 105.10(12) yes N1 Zn1 N2 . . 9_555 105.10(5) yes N1 Zn1 N2 . . 106_555 74.90(5) yes N1 Zn1 N1 146_555 . 99_555 43.24(14) yes N1 Zn1 N1 146_555 . 52_555 149.80(17) yes N1 Zn1 N1 146_555 . 5_555 93.89(13) yes N1 Zn1 N1 146_555 . 54_555 56.47(14) yes N1 Zn1 N1 146_555 . 151_555 93.89(13) yes N1 Zn1 N1 146_555 . 104_555 114.62(12) yes N1 Zn1 N1 146_555 . 9_555 114.62(12) yes N1 Zn1 N1 146_555 . 106_555 56.47(14) yes N1 Zn1 N1 146_555 . 59_555 93.89(13) yes N1 Zn1 N1 146_555 . 156_555 93.89(13) yes N1 Zn1 N2 146_555 . . 158.38(10) yes N1 Zn1 N2 146_555 . 5_555 105.10(12) yes N1 Zn1 N2 146_555 . 54_555 74.90(12) yes N1 Zn1 N2 146_555 . 9_555 105.10(5) yes N1 Zn1 N2 146_555 . 106_555 74.90(5) yes N1 Zn1 N1 99_555 . 52_555 149.80(6) yes N1 Zn1 N1 99_555 . 5_555 56.47(14) yes N1 Zn1 N1 99_555 . 54_555 93.89(13) yes N1 Zn1 N1 99_555 . 151_555 114.62(12) yes N1 Zn1 N1 99_555 . 104_555 93.89(13) yes N1 Zn1 N1 99_555 . 9_555 93.89(13) yes N1 Zn1 N1 99_555 . 106_555 93.89(13) yes N1 Zn1 N1 99_555 . 59_555 114.62(12) yes N1 Zn1 N1 99_555 . 156_555 56.47(14) yes N1 Zn1 N2 99_555 . . 158.38(10) yes N1 Zn1 N2 99_555 . 5_555 74.90(12) yes N1 Zn1 N2 99_555 . 54_555 105.10(12) yes N1 Zn1 N2 99_555 . 9_555 74.90(5) yes N1 Zn1 N2 99_555 . 106_555 105.10(5) yes N1 Zn1 N1 52_555 . 5_555 114.62(12) yes N1 Zn1 N1 52_555 . 54_555 93.89(13) yes N1 Zn1 N1 52_555 . 151_555 56.47(14) yes N1 Zn1 N1 52_555 . 104_555 93.89(13) yes N1 Zn1 N1 52_555 . 9_555 56.47(14) yes N1 Zn1 N1 52_555 . 106_555 114.62(12) yes N1 Zn1 N1 52_555 . 59_555 93.89(13) yes N1 Zn1 N1 52_555 . 156_555 93.89(13) yes N1 Zn1 N2 52_555 . 146_555 158.38(10) yes N1 Zn1 N2 52_555 . 5_555 105.10(12) yes N1 Zn1 N2 52_555 . 54_555 74.90(12) yes N1 Zn1 N2 52_555 . 9_555 74.90(5) yes N1 Zn1 N2 52_555 . 106_555 105.10(5) yes N1 Zn1 N1 5_555 . 54_555 149.80(6) yes N1 Zn1 N1 5_555 . 151_555 149.80(17) yes N1 Zn1 N1 5_555 . 104_555 43.24(14) yes N1 Zn1 N1 5_555 . 9_555 93.89(13) yes N1 Zn1 N1 5_555 . 106_555 114.62(12) yes N1 Zn1 N1 5_555 . 59_555 93.89(13) yes N1 Zn1 N1 5_555 . 156_555 56.47(14) yes N1 Zn1 N2 5_555 . . 105.10(5) yes N1 Zn1 N2 5_555 . 146_555 74.90(5) yes N1 Zn1 N2 5_555 . 54_555 158.38(10) yes N1 Zn1 N2 5_555 . 9_555 74.90(12) yes N1 Zn1 N2 5_555 . 106_555 105.10(12) yes N1 Zn1 N1 54_555 . 151_555 43.24(14) yes N1 Zn1 N1 54_555 . 104_555 149.80(17) yes N1 Zn1 N1 54_555 . 9_555 93.89(13) yes N1 Zn1 N1 54_555 . 106_555 56.47(14) yes N1 Zn1 N1 54_555 . 59_555 93.89(13) yes N1 Zn1 N1 54_555 . 156_555 114.62(12) yes N1 Zn1 N2 54_555 . . 105.10(5) yes N1 Zn1 N2 54_555 . 146_555 74.90(5) yes N1 Zn1 N2 54_555 . 5_555 158.38(10) yes N1 Zn1 N2 54_555 . 9_555 105.10(12) yes N1 Zn1 N2 54_555 . 106_555 74.90(12) yes N1 Zn1 N1 151_555 . 104_555 149.80(6) yes N1 Zn1 N1 151_555 . 9_555 56.47(14) yes N1 Zn1 N1 151_555 . 106_555 93.89(13) yes N1 Zn1 N1 151_555 . 59_555 114.62(12) yes N1 Zn1 N1 151_555 . 156_555 93.89(13) yes N1 Zn1 N2 151_555 . . 74.90(5) yes N1 Zn1 N2 151_555 . 146_555 105.10(5) yes N1 Zn1 N2 151_555 . 5_555 158.38(10) yes N1 Zn1 N2 151_555 . 9_555 74.90(12) yes N1 Zn1 N2 151_555 . 106_555 105.10(12) yes N1 Zn1 N1 104_555 . 9_555 114.62(12) yes N1 Zn1 N1 104_555 . 106_555 93.89(13) yes N1 Zn1 N1 104_555 . 59_555 56.47(14) yes N1 Zn1 N1 104_555 . 156_555 93.89(13) yes N1 Zn1 N2 104_555 . . 74.90(5) yes N1 Zn1 N2 104_555 . 146_555 105.10(5) yes N1 Zn1 N2 104_555 . 54_555 158.38(10) yes N1 Zn1 N2 104_555 . 9_555 105.10(12) yes N1 Zn1 N2 104_555 . 106_555 74.90(12) yes N1 Zn1 N1 9_555 . 106_555 149.80(6) yes N1 Zn1 N1 9_555 . 59_555 149.80(17) yes N1 Zn1 N1 9_555 . 156_555 43.24(14) yes N1 Zn1 N2 9_555 . . 74.90(12) yes N1 Zn1 N2 9_555 . 146_555 105.10(12) yes N1 Zn1 N2 9_555 . 5_555 105.10(5) yes N1 Zn1 N2 9_555 . 54_555 74.90(5) yes N1 Zn1 N2 9_555 . 106_555 158.38(10) yes N1 Zn1 N1 106_555 . 59_555 43.24(14) yes N1 Zn1 N1 106_555 . 156_555 149.80(17) yes N1 Zn1 N2 106_555 . . 105.10(12) yes N1 Zn1 N2 106_555 . 146_555 74.90(12) yes N1 Zn1 N2 106_555 . 5_555 105.10(5) yes N1 Zn1 N2 106_555 . 54_555 74.90(5) yes N1 Zn1 N2 106_555 . 9_555 158.38(10) yes N1 Zn1 N1 59_555 . 156_555 149.80(6) yes N1 Zn1 N2 59_555 . . 74.90(12) yes N1 Zn1 N2 59_555 . 146_555 105.10(12) yes N1 Zn1 N2 59_555 . 5_555 74.90(5) yes N1 Zn1 N2 59_555 . 54_555 105.10(5) yes N1 Zn1 N2 59_555 . 9_555 158.38(10) yes N1 Zn1 N2 156_555 . . 105.10(12) yes N1 Zn1 N2 156_555 . 146_555 74.90(12) yes N1 Zn1 N2 156_555 . 5_555 74.90(5) yes N1 Zn1 N2 156_555 . 54_555 105.10(5) yes N1 Zn1 N2 156_555 . 106_555 158.38(10) yes N2 Zn1 N2 . . 146_555 180.0(5) yes N2 Zn1 N2 . . 5_555 90 yes N2 Zn1 N2 . . 54_555 90 yes N2 Zn1 N2 . . 9_555 90 yes N2 Zn1 N2 . . 106_555 90 yes N2 Zn1 N2 146_555 . 5_555 90 yes N2 Zn1 N2 146_555 . 54_555 90 yes N2 Zn1 N2 146_555 . 9_555 90 yes N2 Zn1 N2 146_555 . 106_555 90 yes N2 Zn1 N2 5_555 . 54_555 180.0(5) yes N2 Zn1 N2 5_555 . 9_555 90 yes N2 Zn1 N2 5_555 . 106_555 90 yes N2 Zn1 N2 54_555 . 9_555 90 yes N2 Zn1 N2 54_555 . 106_555 90 yes N2 Zn1 N2 9_555 . 106_555 180.0(5) yes #END # Attachment '- Co-MFU4.cif' data_Co-MFU4 _database_code_depnum_ccdc_archive 'CCDC 847583' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H6 Cl4 Co5 N18' _chemical_formula_sum 'C18 H6 Cl4 Co5 N18' _chemical_formula_weight 910.8 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co -2.365 3.614 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Cl 0.364 0.702 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.031 0.018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' C 0.018 0.009 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F m -3 m' _symmetry_space_group_name_Hall '-F 4;2;3' _symmetry_Int_Tables_number 225 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,z 3 -x,y,-z 4 x,-y,-z 5 z,x,y 6 z,-x,-y 7 -z,-x,y 8 -z,x,-y 9 y,z,x 10 -y,z,-x 11 y,-z,-x 12 -y,-z,x 13 y,x,-z 14 -y,-x,-z 15 y,-x,z 16 -y,x,z 17 x,z,-y 18 -x,z,y 19 -x,-z,-y 20 x,-z,y 21 z,y,-x 22 z,-y,x 23 -z,y,x 24 -z,-y,-x 25 -x,-y,-z 26 x,y,-z 27 x,-y,z 28 -x,y,z 29 -z,-x,-y 30 -z,x,y 31 z,x,-y 32 z,-x,y 33 -y,-z,-x 34 y,-z,x 35 -y,z,x 36 y,z,-x 37 -y,-x,z 38 y,x,z 39 -y,x,-z 40 y,-x,-z 41 -x,-z,y 42 x,-z,-y 43 x,z,y 44 -x,z,-y 45 -z,-y,x 46 -z,y,-x 47 z,-y,-x 48 z,y,x 49 x,y+1/2,z+1/2 50 -x,-y+1/2,z+1/2 51 -x,y+1/2,-z+1/2 52 x,-y+1/2,-z+1/2 53 z,x+1/2,y+1/2 54 z,-x+1/2,-y+1/2 55 -z,-x+1/2,y+1/2 56 -z,x+1/2,-y+1/2 57 y,z+1/2,x+1/2 58 -y,z+1/2,-x+1/2 59 y,-z+1/2,-x+1/2 60 -y,-z+1/2,x+1/2 61 y,x+1/2,-z+1/2 62 -y,-x+1/2,-z+1/2 63 y,-x+1/2,z+1/2 64 -y,x+1/2,z+1/2 65 x,z+1/2,-y+1/2 66 -x,z+1/2,y+1/2 67 -x,-z+1/2,-y+1/2 68 x,-z+1/2,y+1/2 69 z,y+1/2,-x+1/2 70 z,-y+1/2,x+1/2 71 -z,y+1/2,x+1/2 72 -z,-y+1/2,-x+1/2 73 -x,-y+1/2,-z+1/2 74 x,y+1/2,-z+1/2 75 x,-y+1/2,z+1/2 76 -x,y+1/2,z+1/2 77 -z,-x+1/2,-y+1/2 78 -z,x+1/2,y+1/2 79 z,x+1/2,-y+1/2 80 z,-x+1/2,y+1/2 81 -y,-z+1/2,-x+1/2 82 y,-z+1/2,x+1/2 83 -y,z+1/2,x+1/2 84 y,z+1/2,-x+1/2 85 -y,-x+1/2,z+1/2 86 y,x+1/2,z+1/2 87 -y,x+1/2,-z+1/2 88 y,-x+1/2,-z+1/2 89 -x,-z+1/2,y+1/2 90 x,-z+1/2,-y+1/2 91 x,z+1/2,y+1/2 92 -x,z+1/2,-y+1/2 93 -z,-y+1/2,x+1/2 94 -z,y+1/2,-x+1/2 95 z,-y+1/2,-x+1/2 96 z,y+1/2,x+1/2 97 x+1/2,y,z+1/2 98 -x+1/2,-y,z+1/2 99 -x+1/2,y,-z+1/2 100 x+1/2,-y,-z+1/2 101 z+1/2,x,y+1/2 102 z+1/2,-x,-y+1/2 103 -z+1/2,-x,y+1/2 104 -z+1/2,x,-y+1/2 105 y+1/2,z,x+1/2 106 -y+1/2,z,-x+1/2 107 y+1/2,-z,-x+1/2 108 -y+1/2,-z,x+1/2 109 y+1/2,x,-z+1/2 110 -y+1/2,-x,-z+1/2 111 y+1/2,-x,z+1/2 112 -y+1/2,x,z+1/2 113 x+1/2,z,-y+1/2 114 -x+1/2,z,y+1/2 115 -x+1/2,-z,-y+1/2 116 x+1/2,-z,y+1/2 117 z+1/2,y,-x+1/2 118 z+1/2,-y,x+1/2 119 -z+1/2,y,x+1/2 120 -z+1/2,-y,-x+1/2 121 -x+1/2,-y,-z+1/2 122 x+1/2,y,-z+1/2 123 x+1/2,-y,z+1/2 124 -x+1/2,y,z+1/2 125 -z+1/2,-x,-y+1/2 126 -z+1/2,x,y+1/2 127 z+1/2,x,-y+1/2 128 z+1/2,-x,y+1/2 129 -y+1/2,-z,-x+1/2 130 y+1/2,-z,x+1/2 131 -y+1/2,z,x+1/2 132 y+1/2,z,-x+1/2 133 -y+1/2,-x,z+1/2 134 y+1/2,x,z+1/2 135 -y+1/2,x,-z+1/2 136 y+1/2,-x,-z+1/2 137 -x+1/2,-z,y+1/2 138 x+1/2,-z,-y+1/2 139 x+1/2,z,y+1/2 140 -x+1/2,z,-y+1/2 141 -z+1/2,-y,x+1/2 142 -z+1/2,y,-x+1/2 143 z+1/2,-y,-x+1/2 144 z+1/2,y,x+1/2 145 x+1/2,y+1/2,z 146 -x+1/2,-y+1/2,z 147 -x+1/2,y+1/2,-z 148 x+1/2,-y+1/2,-z 149 z+1/2,x+1/2,y 150 z+1/2,-x+1/2,-y 151 -z+1/2,-x+1/2,y 152 -z+1/2,x+1/2,-y 153 y+1/2,z+1/2,x 154 -y+1/2,z+1/2,-x 155 y+1/2,-z+1/2,-x 156 -y+1/2,-z+1/2,x 157 y+1/2,x+1/2,-z 158 -y+1/2,-x+1/2,-z 159 y+1/2,-x+1/2,z 160 -y+1/2,x+1/2,z 161 x+1/2,z+1/2,-y 162 -x+1/2,z+1/2,y 163 -x+1/2,-z+1/2,-y 164 x+1/2,-z+1/2,y 165 z+1/2,y+1/2,-x 166 z+1/2,-y+1/2,x 167 -z+1/2,y+1/2,x 168 -z+1/2,-y+1/2,-x 169 -x+1/2,-y+1/2,-z 170 x+1/2,y+1/2,-z 171 x+1/2,-y+1/2,z 172 -x+1/2,y+1/2,z 173 -z+1/2,-x+1/2,-y 174 -z+1/2,x+1/2,y 175 z+1/2,x+1/2,-y 176 z+1/2,-x+1/2,y 177 -y+1/2,-z+1/2,-x 178 y+1/2,-z+1/2,x 179 -y+1/2,z+1/2,x 180 y+1/2,z+1/2,-x 181 -y+1/2,-x+1/2,z 182 y+1/2,x+1/2,z 183 -y+1/2,x+1/2,-z 184 y+1/2,-x+1/2,-z 185 -x+1/2,-z+1/2,y 186 x+1/2,-z+1/2,-y 187 x+1/2,z+1/2,y 188 -x+1/2,z+1/2,-y 189 -z+1/2,-y+1/2,x 190 -z+1/2,y+1/2,-x 191 z+1/2,-y+1/2,-x 192 z+1/2,y+1/2,x _cell_length_a 21.7309(4) _cell_length_b 21.7309(4) _cell_length_c 21.7309(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10262.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'microcrystalline powder' _exptl_crystal_colour blue _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_diffrn 1.1787 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3501 _exptl_absorpt_coefficient_mu 14.554 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_source X-ray _diffrn_source_target Cu _diffrn_source_type 'fine-focus sealed tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_monochromator germanium _diffrn_measurement_device 'STOE STADI P' _diffrn_measurement_device_type Bragg-Brentano _diffrn_detector 'Meteor 1D' _diffrn_detector_type PSD _pd_meas_number_of_points 4300 _pd_meas_2theta_range_min 4.020 _pd_meas_2theta_range_max 90.000 _pd_meas_2theta_range_inc 0.02 _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.0130 _pd_proc_ls_prof_wR_factor 0.0182 _pd_proc_ls_prof_wR_expected 0.0437 _refine_special_details ; ? ; _refine_ls_R_factor_gt 0.1592 _refine_ls_wR_factor_gt 0.1408 _refine_ls_R_factor_all 0.1498 _refine_ls_wR_factor_ref 0.1474 _refine_ls_number_parameters 2 _refine_ls_number_restraints 3 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment constr _refine_ls_shift/su_max 0.0109 _refine_ls_shift/su_mean 0.0079 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _pd_proc_2theta_range_min 4.02 _pd_proc_2theta_range_max 90 _pd_proc_2theta_range_inc 0.02 _pd_proc_wavelength ? _computing_data_collection 'Diffractometer software' _computing_cell_refinement PROSZKI _computing_structure_solution ? _computing_structure_refinement Jana2006 _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material Jana2006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.25 0.25 0.25 Uiso 0.014(4) 8 1.000 d . . . Co2 Co 0.3411(2) 0.3411(2) 0.3411(2) Uiso 0.014(4) 32 1.000 d . . . Cl Cl 0.3946(3) 0.3946(3) 0.3946(3) Uiso 0.044(10) 32 1.000 d . . . N1 N 0.2863(2) 0.3877(4) 0.2863(2) Uiso 0.043(10) 96 1 d . . . N2 N 0.25 0.35536(10) 0.25 Uiso 0.043(10) 48 1 d . . . C1 C 0.2741(4) 0.4474(2) 0.2741(4) Uiso 0.051(10) 96 1 d . . . C2 C 0.2999(6) 0.5 0.2999(6) Uiso 0.051(10) 48 1 d . . . H2 H 0.3302 0.5 0.3302 Uiso 0.038 48 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 ? ? ? ? ? ? ? ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 N2 . . 2.290(2) yes Co1 N2 . 146_555 2.290(2) yes Co1 N2 . 5_555 2.290(2) yes Co1 N2 . 54_555 2.290(2) yes Co1 N2 . 9_555 2.290(2) yes Co1 N2 . 106_555 2.290(2) yes Co2 Cl . . 2.014(8) yes Co2 N1 . . 1.965(7) yes Co2 N1 . 5_555 1.965(7) yes Co2 N1 . 9_555 1.965(7) yes Co2 N2 . . 2.818(4) yes Co2 N2 . 5_555 2.818(4) yes Co2 N2 . 9_555 2.818(4) yes Co2 C1 . . 3.094(8) yes Co2 C1 . 5_555 3.094(8) yes Co2 C1 . 9_555 3.094(8) yes N1 N1 . 99_555 2.233(6) yes N1 N1 . 5_555 3.116(10) yes N1 N1 . 9_555 3.116(10) yes N1 N2 . . 1.319(6) yes N1 C1 . . 1.350(10) yes N1 C1 . 99_555 2.266(10) yes N1 C2 . . 2.476(9) yes N2 C1 . . 2.133(5) yes N2 C1 . 99_555 2.133(5) yes C1 C1 . 99_555 1.484(12) yes C1 C2 . . 1.391(10) yes C2 H2 . . 0.930(13) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 Co1 N2 . . 146_555 180.0(5) yes N2 Co1 N2 . . 5_555 90 yes N2 Co1 N2 . . 54_555 90 yes N2 Co1 N2 . . 9_555 90 yes N2 Co1 N2 . . 106_555 90 yes N2 Co1 N2 146_555 . 5_555 90 yes N2 Co1 N2 146_555 . 54_555 90 yes N2 Co1 N2 146_555 . 9_555 90 yes N2 Co1 N2 146_555 . 106_555 90 yes N2 Co1 N2 5_555 . 54_555 180.0(5) yes N2 Co1 N2 5_555 . 9_555 90 yes N2 Co1 N2 5_555 . 106_555 90 yes N2 Co1 N2 54_555 . 9_555 90 yes N2 Co1 N2 54_555 . 106_555 90 yes N2 Co1 N2 9_555 . 106_555 180.0(5) yes Cl Co2 N1 . . . 113.7(4) yes Cl Co2 N1 . . 5_555 113.7(4) yes Cl Co2 N1 . . 9_555 113.7(4) yes Cl Co2 N2 . . . 138.4(3) yes Cl Co2 N2 . . 5_555 138.4(3) yes Cl Co2 N2 . . 9_555 138.4(3) yes Cl Co2 C1 . . . 96.5(3) yes Cl Co2 C1 . . 5_555 96.5(3) yes Cl Co2 C1 . . 9_555 96.5(3) yes N1 Co2 N1 . . 5_555 104.9(3) yes N1 Co2 N1 . . 9_555 104.9(3) yes N1 Co2 N2 . . 5_555 90.1(3) yes N1 Co2 N2 . . 9_555 90.1(3) yes N1 Co2 C1 . . 5_555 114.2(3) yes N1 Co2 C1 . . 9_555 114.2(3) yes N1 Co2 N1 5_555 . 9_555 104.9(3) yes N1 Co2 N2 5_555 . . 90.1(3) yes N1 Co2 N2 5_555 . 9_555 90.1(3) yes N1 Co2 C1 5_555 . . 114.2(3) yes N1 Co2 C1 5_555 . 9_555 114.2(3) yes N1 Co2 N2 9_555 . . 90.1(3) yes N1 Co2 N2 9_555 . 5_555 90.1(3) yes N1 Co2 C1 9_555 . . 114.2(3) yes N1 Co2 C1 9_555 . 5_555 114.2(3) yes N2 Co2 N2 . . 5_555 70.14(11) yes N2 Co2 N2 . . 9_555 70.14(11) yes N2 Co2 C1 . . . 41.98(15) yes N2 Co2 C1 . . 5_555 104.2(2) yes N2 Co2 C1 . . 9_555 104.2(2) yes N2 Co2 N2 5_555 . 9_555 70.14(11) yes N2 Co2 C1 5_555 . . 104.2(2) yes N2 Co2 C1 5_555 . 5_555 41.98(15) yes N2 Co2 C1 5_555 . 9_555 104.2(2) yes N2 Co2 C1 9_555 . . 104.2(2) yes N2 Co2 C1 9_555 . 5_555 104.2(2) yes N2 Co2 C1 9_555 . 9_555 41.98(15) yes C1 Co2 C1 . . 5_555 118.8(3) yes C1 Co2 C1 . . 9_555 118.8(3) yes C1 Co2 C1 5_555 . 9_555 118.8(3) yes Co2 N1 N1 . . 99_555 149.0(5) yes Co2 N1 N2 . . . 116.8(6) yes Co2 N1 C1 . . . 137.1(6) yes Co2 N1 C1 . . 99_555 176.1(5) yes Co2 N1 C2 . . . 111.3(4) yes N1 N1 N1 99_555 . 5_555 120.0(3) yes N1 N1 N1 99_555 . 9_555 120.0(3) yes N1 N1 C1 99_555 . . 73.9(5) yes N1 N1 C2 99_555 . . 99.7(5) yes N1 N1 N1 5_555 . 9_555 60.0(2) yes N1 N1 N2 5_555 . . 92.6(4) yes N1 N1 C1 5_555 . . 144.9(5) yes N1 N1 C1 5_555 . 99_555 144.6(3) yes N1 N1 C2 5_555 . . 127.8(4) yes N1 N1 N2 9_555 . . 92.6(4) yes N1 N1 C1 9_555 . . 144.9(5) yes N1 N1 C1 9_555 . 99_555 144.6(3) yes N1 N1 C2 9_555 . . 127.8(4) yes N2 N1 C1 . . . 106.1(5) yes N2 N1 C1 . . 99_555 67.1(3) yes N2 N1 C2 . . . 131.9(5) yes C1 N1 C2 99_555 . . 64.8(4) yes Co1 N2 Co2 . . . 83.70(10) yes Co1 N2 Co2 . . 99_555 83.70(10) yes Co1 N2 N1 . . . 122.2(3) yes Co1 N2 N1 . . 99_555 122.2(3) yes Co1 N2 C1 . . . 159.6(2) yes Co1 N2 C1 . . 99_555 159.6(2) yes Co2 N2 Co2 . . 99_555 167.40(15) yes Co2 N2 N1 . . 99_555 154.1(4) yes Co2 N2 C1 . . . 75.9(2) yes Co2 N2 C1 . . 99_555 116.7(2) yes Co2 N2 N1 99_555 . . 154.1(4) yes Co2 N2 C1 99_555 . . 116.7(2) yes Co2 N2 C1 99_555 . 99_555 75.9(2) yes N1 N2 N1 . . 99_555 115.6(5) yes N1 N2 C1 . . 99_555 78.1(4) yes N1 N2 C1 99_555 . . 78.1(4) yes Co2 C1 N1 . . 99_555 96.8(3) yes Co2 C1 N2 . . . 62.07(16) yes Co2 C1 C1 . . 99_555 131.7(3) yes Co2 C1 C2 . . . 103.6(6) yes N1 C1 N1 . . 99_555 71.2(4) yes N1 C1 C1 . . 99_555 106.1(5) yes N1 C1 C2 . . . 129.2(8) yes N1 C1 C2 99_555 . . 159.6(7) yes N2 C1 C1 . . 99_555 69.6(3) yes N2 C1 C2 . . . 165.6(7) yes C1 C1 C2 99_555 . . 124.7(6) yes N1 C2 N1 . . 22_565 160.6(6) yes N1 C2 C1 . . 22_565 135.6(8) yes N1 C2 C1 22_565 . . 135.6(8) yes C1 C2 C1 . . 22_565 110.5(10) yes data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- compound3.cif' #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'May 25 13:04:00 2011' _audit_creation_method 'PLATON option' _audit_update_record ; UPDATED 06.10.2011 by author GE ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence 'Georg Eickerling' _publ_contact_author_address # address of author for correspondence ; Universit\"at Augsburg Universit\"atsstrasse 1 86159 Augsburg ; _publ_contact_author_email georg.eickerling@physik.uni-augsburg.de _publ_contact_author_fax '(+49) (0)821-5983227' _publ_contact_author_phone '(+49) (0)821-5983362' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission ? Please consider this CIF submission for publication as a Regular Structural Paper in Acta Crystallographica C. ; #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ; _journal_techeditor_code ? _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Reversible gas-phase redox processes catalyzed by Co-exchanged MFU-4l(arge) ; _publ_section_title_footnote ; ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Dmytro Denysenko' ; Chair of Solid State and Material Science Universit\"at Augsburg D-86159 Augsburg Germany ; 'Tamas Werner' ; Chair of Solid State and Material Science Universit\"at Augsburg D-86159 Augsburg Germany ; 'Maciej Grzywa' ; Chair of Solid State and Material Science Universit\"at Augsburg D-86159 Augsburg Germany ; 'Angela Puls' ; Rubotherm GmbH D-44799 Bochum Germany ; 'Volker Hagen' ; Rubokat GmbH D-44801 Bochum Germany ; 'Georg Eickerling' ; Chair of Chemical Physics and Materials Science Universit\"at Augsburg D-86159 Augsburg Germany ; ; J.Jelic ; ; Dept. Chemie Technische Universi\"at M\"unchen D-85747 Garching Germany ; 'Dirk Volkmer' ; Chair of Solid State and Material Science Universit\"at Augsburg D-86159 Augsburg Germany ; #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; # Insert blank lines between references _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C. Guagliardi, A., Moliterni, A.G.G., Polidori, G. & Spagna, R. (1999) J. Appl. Cryst. 32, 115-119. Sheldrick, G.M. (1997). SHELXL97. University of G"ottingen, Germany. Spek, A. L. "PLATON", A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands, (2006). Wilson, A.J.C. (1992). Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; #=============================================================================== data_co5 _database_code_depnum_ccdc_archive 'CCDC 847498' #TrackingRef '- compound3.cif' #=============================================================================== # 5. CHEMICAL DATA #=============================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C48 H48 Cl4 Co5 N18' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C48 H48 Cl4 Co5 N18' _chemical_formula_weight 1313.49 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3050 0.6296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0998 0.0984 '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' C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA #=============================================================================== _symmetry_cell_setting Cubic _symmetry_space_group_name_Hall '-F 4vw 2vw 3' _symmetry_space_group_name_H-M 'F d -3 m' _symmetry_Int_Tables_number 227 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,1/4+x,1/4+z 3 3/4-x,1/4-y,1/2+z 4 3/4+y,-x,3/4+z 5 x,1/4-y,1/4-z 6 3/4+y,1/4+x,1/2-z 7 3/4-x,y,3/4-z 8 -y,-x,-z 9 z,x,y 10 -x,1/4+z,1/4+y 11 3/4-z,1/4-x,1/2+y 12 3/4+x,-z,3/4+y 13 z,1/4-x,1/4-y 14 3/4+x,1/4+z,1/2-y 15 3/4-z,x,3/4-y 16 -x,-z,-y 17 y,z,x 18 -z,-y,-x 19 1/2-z,3/4+y,1/4+x 20 3/4+z,3/4+y,-x 21 1/4+z,-y,1/4+x 22 y,1/4-z,1/4-x 23 1/4-y,3/4-z,1/2+x 24 1/4-y,z,1/4-x 25 -x,-y,-z 26 y,3/4-x,3/4-z 27 1/4+x,3/4+y,1/2-z 28 1/4-y,x,1/4-z 29 -x,3/4+y,3/4+z 30 1/4-y,3/4-x,1/2+z 31 1/4+x,-y,1/4+z 32 y,x,z 33 -z,-x,-y 34 x,3/4-z,3/4-y 35 1/4+z,3/4+x,1/2-y 36 1/4-x,z,1/4-y 37 -z,3/4+x,3/4+y 38 1/4-x,3/4-z,1/2+y 39 1/4+z,-x,1/4+y 40 x,z,y 41 -y,-z,-x 42 z,y,x 43 1/2+z,1/4-y,3/4-x 44 1/4-z,1/4-y,x 45 3/4-z,y,3/4-x 46 -y,3/4+z,3/4+x 47 3/4+y,1/4+z,1/2-x 48 3/4+y,-z,3/4+x 49 x,1/2+y,1/2+z 50 -y,3/4+x,3/4+z 51 3/4-x,3/4-y,z 52 3/4+y,1/2-x,1/4+z 53 x,3/4-y,3/4-z 54 3/4+y,3/4+x,-z 55 3/4-x,1/2+y,1/4-z 56 -y,1/2-x,1/2-z 57 z,1/2+x,1/2+y 58 -x,3/4+z,3/4+y 59 3/4-z,3/4-x,y 60 3/4+x,1/2-z,1/4+y 61 z,3/4-x,3/4-y 62 3/4+x,3/4+z,-y 63 3/4-z,1/2+x,1/4-y 64 -x,1/2-z,1/2-y 65 y,1/2+z,1/2+x 66 -z,1/2-y,1/2-x 67 1/2-z,1/4+y,3/4+x 68 3/4+z,1/4+y,1/2-x 69 1/4+z,1/2-y,3/4+x 70 y,3/4-z,3/4-x 71 1/4-y,1/4-z,x 72 1/4-y,1/2+z,3/4-x 73 -x,1/2-y,1/2-z 74 y,1/4-x,1/4-z 75 1/4+x,1/4+y,-z 76 1/4-y,1/2+x,3/4-z 77 -x,1/4+y,1/4+z 78 1/4-y,1/4-x,z 79 1/4+x,1/2-y,3/4+z 80 y,1/2+x,1/2+z 81 -z,1/2-x,1/2-y 82 x,1/4-z,1/4-y 83 1/4+z,1/4+x,-y 84 1/4-x,1/2+z,3/4-y 85 -z,1/4+x,1/4+y 86 1/4-x,1/4-z,y 87 1/4+z,1/2-x,3/4+y 88 x,1/2+z,1/2+y 89 -y,1/2-z,1/2-x 90 z,1/2+y,1/2+x 91 1/2+z,3/4-y,1/4-x 92 1/4-z,3/4-y,1/2+x 93 3/4-z,1/2+y,1/4-x 94 -y,1/4+z,1/4+x 95 3/4+y,3/4+z,-x 96 3/4+y,1/2-z,1/4+x 97 1/2+x,y,1/2+z 98 1/2-y,1/4+x,3/4+z 99 1/4-x,1/4-y,z 100 1/4+y,-x,1/4+z 101 1/2+x,1/4-y,3/4-z 102 1/4+y,1/4+x,-z 103 1/4-x,y,1/4-z 104 1/2-y,-x,1/2-z 105 1/2+z,x,1/2+y 106 1/2-x,1/4+z,3/4+y 107 1/4-z,1/4-x,y 108 1/4+x,-z,1/4+y 109 1/2+z,1/4-x,3/4-y 110 1/4+x,1/4+z,-y 111 1/4-z,x,1/4-y 112 1/2-x,-z,1/2-y 113 1/2+y,z,1/2+x 114 1/2-z,-y,1/2-x 115 -z,3/4+y,3/4+x 116 1/4+z,3/4+y,1/2-x 117 3/4+z,-y,3/4+x 118 1/2+y,1/4-z,3/4-x 119 3/4-y,3/4-z,x 120 3/4-y,z,3/4-x 121 1/2-x,-y,1/2-z 122 1/2+y,3/4-x,1/4-z 123 3/4+x,3/4+y,-z 124 3/4-y,x,3/4-z 125 1/2-x,3/4+y,1/4+z 126 3/4-y,3/4-x,z 127 3/4+x,-y,3/4+z 128 1/2+y,x,1/2+z 129 1/2-z,-x,1/2-y 130 1/2+x,3/4-z,1/4-y 131 3/4+z,3/4+x,-y 132 3/4-x,z,3/4-y 133 1/2-z,3/4+x,1/4+y 134 3/4-x,3/4-z,y 135 3/4+z,-x,3/4+y 136 1/2+x,z,1/2+y 137 1/2-y,-z,1/2-x 138 1/2+z,y,1/2+x 139 z,1/4-y,1/4-x 140 3/4-z,1/4-y,1/2+x 141 1/4-z,y,1/4-x 142 1/2-y,3/4+z,1/4+x 143 1/4+y,1/4+z,-x 144 1/4+y,-z,1/4+x 145 1/2+x,1/2+y,z 146 1/2-y,3/4+x,1/4+z 147 1/4-x,3/4-y,1/2+z 148 1/4+y,1/2-x,3/4+z 149 1/2+x,3/4-y,1/4-z 150 1/4+y,3/4+x,1/2-z 151 1/4-x,1/2+y,3/4-z 152 1/2-y,1/2-x,-z 153 1/2+z,1/2+x,y 154 1/2-x,3/4+z,1/4+y 155 1/4-z,3/4-x,1/2+y 156 1/4+x,1/2-z,3/4+y 157 1/2+z,3/4-x,1/4-y 158 1/4+x,3/4+z,1/2-y 159 1/4-z,1/2+x,3/4-y 160 1/2-x,1/2-z,-y 161 1/2+y,1/2+z,x 162 1/2-z,1/2-y,-x 163 -z,1/4+y,1/4+x 164 1/4+z,1/4+y,-x 165 3/4+z,1/2-y,1/4+x 166 1/2+y,3/4-z,1/4-x 167 3/4-y,1/4-z,1/2+x 168 3/4-y,1/2+z,1/4-x 169 1/2-x,1/2-y,-z 170 1/2+y,1/4-x,3/4-z 171 3/4+x,1/4+y,1/2-z 172 3/4-y,1/2+x,1/4-z 173 1/2-x,1/4+y,3/4+z 174 3/4-y,1/4-x,1/2+z 175 3/4+x,1/2-y,1/4+z 176 1/2+y,1/2+x,z 177 1/2-z,1/2-x,-y 178 1/2+x,1/4-z,3/4-y 179 3/4+z,1/4+x,1/2-y 180 3/4-x,1/2+z,1/4-y 181 1/2-z,1/4+x,3/4+y 182 3/4-x,1/4-z,1/2+y 183 3/4+z,1/2-x,1/4+y 184 1/2+x,1/2+z,y 185 1/2-y,1/2-z,-x 186 1/2+z,1/2+y,x 187 z,3/4-y,3/4-x 188 3/4-z,3/4-y,x 189 1/4-z,1/2+y,3/4-x 190 1/2-y,1/4+z,3/4+x 191 1/4+y,3/4+z,1/2-x 192 1/4+y,1/2-z,3/4+x _cell_length_a 23.5130(1) _cell_length_b 23.5130(1) _cell_length_c 23.5130(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 12999.42(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 4491 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 21.78 _cell_special_details ; ; _exptl_crystal_description block _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 5320 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'SADABS-2008/1-Bruker AXS, Karlsruhe 2009' _exptl_absorpt_correction_T_min 0.95520 _exptl_absorpt_correction_T_max 0.96133 #=============================================================================== # 7. EXPERIMENTAL DATA #=============================================================================== _exptl_special_details ; Diffractometer operator G. Eickerling scanspeed 2 x 30 s per film 645 Films measured in 2 data sets set 1 and 2: omega-scan with delta_omega = 0.5 ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Ag K\a' _diffrn_radiation_source 'MicroFocus IuS (Incoatec)' _diffrn_radiation_monochromator 'montel multilayer optic (Incoatec)' _diffrn_measurement_device_type 'SMART APEX 2 CCD (Bruker)' _diffrn_measurement_method omega-scans _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 66.7 # 33.3 for binned mode _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 28354 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 23.66 _diffrn_reflns_theta_full 23.66 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 999 _reflns_number_gt 909 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2009)' _computing_data_reduction 'APEX2 (Bruker AXS, 2009)' _computing_structure_solution 'SIR-97 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2006)' _computing_publication_material 'PLATON (Spek, 2006)' #=============================================================================== # 8. REFINEMENT DATA #=============================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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. Solvent molecule contributions have been removed from the intensity data via the SQUEEZE routine as implemented in PLATON. Voids with volumes of 164 and 64 A^3 have been located in the unit cell containing approx. 73 and 1 electrons, respectively (see list at the end of this file). This electron count indicates the presence of one bromobenzene solvent molecule inside each of the 16 larger cavities. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.042200P)^2^+60.342499P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 999 _refine_ls_number_parameters 52 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.329 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.062 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS #=============================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Co1 Co Uani 0.62500 0.12500 0.12500 1.000 0.0134(1) . . Co2 Co Uani 0.71149(1) 0.03851(1) 0.03851(1) 1.000 0.0145(1) . . Cl3 Cl Uani 0.76598(2) -0.01598(2) -0.01598(2) 1.000 0.0236(1) . . N1 N Uani 0.62500 0.12500 0.03203(11) 1.000 0.0165(5) . . N2 N Uani 0.65795(6) 0.09205(6) -0.00031(8) 1.000 0.0182(4) . . C1 C Uani 0.64591(7) 0.10409(7) -0.05562(10) 1.000 0.0201(5) . . C2 C Uani 0.66808(7) 0.08192(7) -0.10673(11) 1.000 0.0247(5) . . C3 C Uani 0.64682(7) 0.10318(7) -0.15687(10) 1.000 0.0255(5) . . C4 C Uani 0.66835(8) 0.08165(8) -0.21306(11) 1.000 0.0293(6) . . H2 H Uiso 0.6978(10) 0.0522(10) -0.1061(14) 1.000 0.027(8) . . H4A H Uiso 0.6976(12) 0.0524(12) -0.2071(15) 1.000 0.038(9) . . H4B H Uiso 0.6844(10) 0.1105(11) -0.2350(11) 1.000 0.040(7) . . 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 0.0134(2) 0.0134(2) 0.0134(2) 0.0000 0.0000 0.0000 Co2 0.0145(2) 0.0145(2) 0.0145(2) -0.0010(1) 0.0010(1) 0.0010(1) Cl3 0.0236(2) 0.0236(2) 0.0236(2) -0.0048(2) 0.0048(2) 0.0048(2) N1 0.0168(8) 0.0168(8) 0.0158(12) 0.0000 0.0000 0.0017(9) N2 0.0202(6) 0.0202(6) 0.0141(8) -0.0013(5) 0.0013(5) 0.0030(7) C1 0.0229(7) 0.0229(7) 0.0145(10) 0.0002(5) -0.0002(5) 0.0039(9) C2 0.0283(8) 0.0283(8) 0.0176(11) -0.0007(6) 0.0007(6) 0.0109(10) C3 0.0301(8) 0.0301(8) 0.0162(11) -0.0011(6) 0.0011(6) 0.0106(11) C4 0.0358(9) 0.0358(9) 0.0163(11) -0.0015(6) 0.0015(6) 0.0155(12) #=============================================================================== # 10. MOLECULAR GEOMETRY #=============================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.186(3) . . yes Co1 N1 2.186(3) . 5_555 yes Co1 N1 2.186(3) . 36_655 yes Co1 N1 2.186(3) . 43_555 yes Co1 N1 2.186(3) . 45_555 yes Co1 N1 2.186(3) . 82_555 yes Co2 Cl3 2.2192(6) . . yes Co2 N2 2.0007(16) . . yes Co2 N2 2.0007(16) . 40_555 yes Co2 N2 2.0007(16) . 45_555 yes N1 N2 1.334(2) . . yes N1 N2 1.334(2) . 99_655 yes N2 C1 1.361(3) . . yes C1 C2 1.410(3) . . no C1 C1 1.391(2) . 99_655 no C2 C3 1.375(3) . . no C3 C4 1.503(3) . . no C3 C3 1.451(2) . 99_655 no C2 H2 0.99(2) . . no C4 H4A 0.98(3) . . no C4 H4B 0.93(3) . . no C4 H4B 0.93(3) . 126_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00 . . 5_555 yes N1 Co1 N1 90.00 . . 36_655 yes N1 Co1 N1 90.00 . . 43_555 yes N1 Co1 N1 90.00 . . 45_555 yes N1 Co1 N1 90.00 . . 82_555 yes N1 Co1 N1 90.00 5_555 . 36_655 yes N1 Co1 N1 90.00 5_555 . 43_555 yes N1 Co1 N1 90.00 5_555 . 45_555 yes N1 Co1 N1 90.00 5_555 . 82_555 yes N1 Co1 N1 90.00 36_655 . 43_555 yes N1 Co1 N1 90.00 36_655 . 45_555 yes N1 Co1 N1 180.00 36_655 . 82_555 yes N1 Co1 N1 180.00 43_555 . 45_555 yes N1 Co1 N1 90.00 43_555 . 82_555 yes N1 Co1 N1 90.00 45_555 . 82_555 yes Cl3 Co2 N2 117.59(5) . . . yes Cl3 Co2 N2 117.59(5) . . 40_555 yes Cl3 Co2 N2 117.59(5) . . 45_555 yes N2 Co2 N2 100.27(7) . . 40_555 yes N2 Co2 N2 100.27(7) . . 45_555 yes N2 Co2 N2 100.27(7) 40_555 . 45_555 yes Co1 N1 N2 124.76(12) . . . yes Co1 N1 N2 124.76(12) . . 99_655 yes N2 N1 N2 110.5(2) . . 99_655 yes Co2 N2 N1 118.09(15) . . . yes Co2 N2 C1 134.26(13) . . . yes N1 N2 C1 107.65(15) . . . yes N2 C1 C2 131.36(16) . . . yes N2 C1 C1 107.11(18) . . 99_655 yes C1 C1 C2 121.5(2) 99_655 . . no C1 C2 C3 117.52(16) . . . no C2 C3 C4 120.60(16) . . . no C2 C3 C3 121.0(2) . . 99_655 no C3 C3 C4 118.45(19) 99_655 . . no C1 C2 H2 120.7(19) . . . no C3 C2 H2 121.8(19) . . . no C3 C4 H4A 110(2) . . . no C3 C4 H4B 112.2(16) . . . no C3 C4 H4B 112.2(16) . . 126_555 no H4A C4 H4B 108(2) . . . no H4A C4 H4B 108(2) . . 126_555 no H4B C4 H4B 106(2) . . 126_555 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl3 Co2 N2 N1 -180.00(8) . . . . no Cl3 Co2 N2 C1 0.00(17) . . . . no Co1 N1 N2 Co2 0.00(12) . . . . no Co1 N1 N2 C1 -180.00(8) . . . . no Co2 N2 C1 C2 0.0(3) . . . . no N1 N2 C1 C2 -179.98(16) . . . . no N2 C1 C2 C3 179.98(18) . . . . no C1 C2 C3 C4 180.00(16) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl3 H2 3.10(3) . . no Cl3 H2 3.10(3) . 40_555 no Cl3 H2 3.10(3) . 45_555 no Cl3 H2 3.10(3) . 45_555 no Cl3 H2 3.10(3) . 40_555 no N1 N1 3.092(3) . 36_655 no N1 N1 3.092(3) . 36_655 no N1 N1 3.092(3) . 43_555 no N1 N1 3.092(3) . 45_555 no N1 N1 3.092(3) . 45_555 no N1 N1 3.092(3) . 45_555 no N1 N1 3.092(3) . 82_555 no N1 N1 3.092(3) . 82_555 no N1 N1 3.092(3) . 36_655 no N1 N1 3.092(3) . 82_555 no N1 N1 3.092(3) . 36_655 no N1 N1 3.092(3) . 43_555 no N1 N1 3.092(3) . 45_555 no N1 N1 3.092(3) . 43_555 no N1 N1 3.092(3) . 43_555 no N1 N1 3.092(3) . 82_555 no N2 N2 3.071(2) . 40_555 no N2 N2 3.071(2) . 45_555 no N2 N2 3.071(2) . 45_555 no N2 N2 3.071(2) . 40_555 no C4 H4B 2.82(2) . 99_655 no C4 H4B 2.82(2) . 176_545 no H2 Cl3 3.10(3) . . no H2 H4A 2.38(5) . . no H4A H2 2.38(5) . . no H4A H4A 2.48(4) . 47_555 no H4A H4A 2.48(4) . 106_654 no H4A H4A 2.48(4) . 114_555 no H4B C4 2.82(2) . 99_655 no H4B C4 2.82(2) . 99_655 no H4B H4B 2.46(3) . 176_545 no #=============================================================================== # 11. RESULTS OF PLATON SQUEEZE #=============================================================================== loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 164.1 72.7 2 0.000 0.250 0.750 164.2 73.3 3 0.000 0.500 0.000 164.1 72.7 4 0.000 0.750 0.250 164.2 73.3 5 0.125 0.125 0.125 64.1 1.4 6 0.125 0.625 0.625 64.1 1.4 7 0.250 0.250 0.500 164.1 73.3 8 0.250 0.500 0.250 164.2 73.3 9 0.250 0.750 1.000 164.1 73.3 10 0.250 1.000 0.750 164.2 73.3 11 0.375 0.375 0.875 64.1 1.5 12 0.375 0.875 0.375 64.1 1.5 13 0.500 0.000 0.000 164.1 72.7 14 0.500 0.250 0.250 164.2 73.3 15 0.500 0.500 0.500 164.1 72.7 16 0.500 0.750 0.750 164.2 73.3 17 0.625 0.125 0.625 64.1 1.4 18 0.625 0.625 0.125 64.1 1.4 19 0.750 0.250 1.000 164.1 73.3 20 0.750 0.500 0.750 164.2 73.3 21 0.750 0.750 0.500 164.1 73.3 22 0.750 1.000 0.250 164.2 73.3 23 0.875 0.375 0.375 64.1 1.5 24 0.875 0.875 0.875 64.1 1.5 # END of Crystallographic Information File