#------------------------------------------------------------------------------ #$Date: 2014-03-15 13:45:36 +0200 (Sat, 15 Mar 2014) $ #$Revision: 106525 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/00/7110010.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7110010 loop_ _publ_author_name 'Feng Shao' 'Jia Li' 'Jia-Ping Tong' 'Jian Zhang' 'Ming-Guang Chen' 'Zhiping Zheng' 'Rong-Bin Huang' 'Lan-Sun Zheng' 'Jun Tao' _publ_section_title ; A boracite metal-organic framework displaying selective gas sorption and guest-dependent spin-crossover behaviour ; _journal_name_full Chem.Commun. _journal_page_first 10730 _journal_volume 49 _journal_year 2013 _chemical_formula_sum 'C30 H20 Fe N6 S2' _chemical_formula_weight 584.49 _chemical_name_systematic ; ? ; _space_group_IT_number 225 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-F 4 2 3' _symmetry_space_group_name_H-M 'F m -3 m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 24 _cell_length_a 37.4447(4) _cell_length_b 37.4447(4) _cell_length_c 37.4447(4) _cell_measurement_temperature 120(2) _cell_volume 52501.4(10) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 41134 _diffrn_reflns_theta_full 62.14 _diffrn_reflns_theta_max 62.14 _diffrn_reflns_theta_min 3.34 _exptl_absorpt_coefficient_mu 1.906 _exptl_crystal_colour red _exptl_crystal_density_diffrn 0.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 7200 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.810 _refine_diff_density_min -4.807 _refine_diff_density_rms 0.099 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 76 _refine_ls_number_reflns 2086 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.133 _refine_ls_R_factor_all 0.1456 _refine_ls_R_factor_gt 0.1294 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1551P)^2^+845.7126P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3534 _refine_ls_wR_factor_ref 0.3696 _reflns_number_gt 1729 _reflns_number_total 2086 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c3cc45180a.txt _[local]_cod_data_source_block 1x(guest) _[local]_cod_cif_authors_sg_H-M Fm-3m _cod_database_code 7110010 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'y, -x+1/2, z+1/2' '-y, x+1/2, z+1/2' 'x, z+1/2, -y+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'x, -z+1/2, y+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' '-z, y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, -z+1/2' '-y+1/2, -x, -z+1/2' 'y+1/2, -x, z+1/2' '-y+1/2, x, z+1/2' 'x+1/2, z, -y+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' 'y+1/2, -x+1/2, z' '-y+1/2, x+1/2, z' 'x+1/2, z+1/2, -y' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'x+1/2, -z+1/2, y' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' '-z+1/2, y+1/2, x' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-z, -x+1/2, -y+1/2' '-z, x+1/2, y+1/2' 'z, x+1/2, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' '-y, -x+1/2, z+1/2' 'y, x+1/2, z+1/2' '-y, x+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' '-x, -z+1/2, y+1/2' 'x, -z+1/2, -y+1/2' 'x, z+1/2, y+1/2' '-x, z+1/2, -y+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' 'z, -y+1/2, -x+1/2' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' '-z+1/2, -x, -y+1/2' '-z+1/2, x, y+1/2' 'z+1/2, x, -y+1/2' 'z+1/2, -x, y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/2, -z, x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' '-y+1/2, -x, z+1/2' 'y+1/2, x, z+1/2' '-y+1/2, x, -z+1/2' 'y+1/2, -x, -z+1/2' '-x+1/2, -z, y+1/2' 'x+1/2, -z, -y+1/2' 'x+1/2, z, y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' 'z+1/2, -y, -x+1/2' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/2, y' 'z+1/2, x+1/2, -y' 'z+1/2, -x+1/2, y' '-y+1/2, -z+1/2, -x' 'y+1/2, -z+1/2, x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' '-y+1/2, x+1/2, -z' 'y+1/2, -x+1/2, -z' '-x+1/2, -z+1/2, y' 'x+1/2, -z+1/2, -y' 'x+1/2, z+1/2, y' '-x+1/2, z+1/2, -y' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, -x' 'z+1/2, y+1/2, x' 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 Fe1 Fe 0.5000 0.2500 0.2500 0.0398(8) Uani 1 8 d S N1 N 0.46213(14) 0.22342(10) 0.22342(10) 0.0339(13) Uani 1 2 d S C1 C 0.4350(2) 0.2419(3) 0.2073(3) 0.040(2) Uani 0.50 1 d P C1' C 0.4612(3) 0.2207(3) 0.1873(3) 0.039(2) Uani 0.50 1 d P C2 C 0.4077(3) 0.2254(2) 0.1882(3) 0.041(2) Uani 0.50 1 d P C2' C 0.4333(3) 0.2036(3) 0.1685(3) 0.043(2) Uani 0.50 1 d P C3 C 0.40622(17) 0.18764(13) 0.18764(13) 0.0362(16) Uani 1 2 d S C4 C 0.37561(17) 0.16995(13) 0.16995(13) 0.0349(16) Uani 1 2 d S C5 C 0.36063(13) 0.13937(13) 0.18451(17) 0.0355(16) Uani 1 2 d S H5A H 0.3715 0.1285 0.2047 0.043 Uiso 1 2 calc SR N2 N 0.5000 0.28660(15) 0.21340(15) 0.0335(18) Uani 1 4 d S C6 C 0.5000 0.3080(2) 0.1920(2) 0.056(3) Uani 1 4 d S S1 S 0.5000 0.33923(7) 0.16077(7) 0.127(2) Uani 1 4 d S loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0319(13) 0.0437(9) 0.0437(9) 0.0038(10) 0.000 0.000 N1 0.027(3) 0.0371(19) 0.0371(19) 0.002(2) -0.0011(16) -0.0011(16) C1 0.025(5) 0.055(6) 0.038(5) 0.004(5) -0.010(4) 0.000(4) C1' 0.032(5) 0.039(5) 0.046(6) -0.003(5) -0.004(4) -0.005(4) C2 0.039(5) 0.028(5) 0.056(6) 0.005(4) -0.009(5) -0.007(4) C2' 0.033(5) 0.050(6) 0.044(6) -0.002(5) -0.004(4) -0.006(5) C3 0.034(4) 0.037(2) 0.037(2) 0.006(3) -0.002(2) -0.002(2) C4 0.030(4) 0.037(2) 0.037(2) 0.004(3) -0.002(2) -0.002(2) C5 0.038(2) 0.038(2) 0.030(3) 0.008(2) -0.008(2) 0.000(3) N2 0.028(4) 0.036(3) 0.036(3) 0.008(4) 0.000 0.000 C6 0.045(7) 0.062(5) 0.062(5) 0.014(7) 0.000 0.000 S1 0.159(5) 0.111(3) 0.111(3) 0.076(3) 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N2 Fe1 N2 180.0(5) . 121_655 N2 Fe1 N1 90.0 . 28 N2 Fe1 N1 90.000(1) 121_655 28 N2 Fe1 N1 90.000(1) . 121_655 N2 Fe1 N1 90.000(1) 121_655 121_655 N1 Fe1 N1 90.4(3) 28 121_655 N2 Fe1 N1 90.000(1) . . N2 Fe1 N1 90.000(1) 121_655 . N1 Fe1 N1 89.6(3) 28 . N1 Fe1 N1 180.0(4) 121_655 . N2 Fe1 N1 90.0 . 100_655 N2 Fe1 N1 90.0 121_655 100_655 N1 Fe1 N1 180.0(4) 28 100_655 N1 Fe1 N1 89.6(3) 121_655 100_655 N1 Fe1 N1 90.4(3) . 100_655 C1' N1 C1' 81.4(9) . 115 C1' N1 C1 65.1(6) . . C1' N1 C1 116.8(7) 115 . C1' N1 C1 116.8(7) . 115 C1' N1 C1 65.1(6) 115 115 C1 N1 C1 84.0(9) . 115 C1' N1 Fe1 123.5(5) . . C1' N1 Fe1 123.5(5) 115 . C1 N1 Fe1 119.7(5) . . C1 N1 Fe1 119.7(5) 115 . N1 C1 C2 123.2(9) . . N1 C1 C1' 57.0(6) . . C2 C1 C1' 89.5(8) . . N1 C1 C1 48.0(4) . 115 C2 C1 C1 92.8(6) . 115 C1' C1 C1 88.7(5) . 115 N1 C1' C2' 123.4(9) . . N1 C1' C1 58.0(6) . . C2' C1' C1 90.3(8) . . N1 C1' C1' 49.3(4) . 115 C2' C1' C1' 91.9(6) . 115 C1 C1' C1' 91.3(5) . 115 N1 C1' C2 90.2(6) . . C2' C1' C2 46.6(6) . . C1 C1' C2 43.7(5) . . C1' C1' C2 92.9(4) 115 . C1 C2 C3 118.7(8) . . C1 C2 C2' 91.4(8) . . C3 C2 C2' 57.3(6) . . C1 C2 C2 87.2(6) . 115 C3 C2 C2 45.9(5) . 115 C2' C2 C2 87.8(6) . 115 C1 C2 C1' 46.8(6) . . C3 C2 C1' 87.2(6) . . C2' C2 C1' 44.6(5) . . C2 C2 C1' 87.1(4) 115 . C3 C2' C1' 118.7(9) . . C3 C2' C2 59.8(6) . . C1' C2' C2 88.8(8) . . C3 C2' C2' 47.6(5) . 115 C1' C2' C2' 88.1(6) . 115 C2 C2' C2' 92.2(6) . 115 C2' C3 C2' 84.8(9) . 115 C2' C3 C2 118.9(8) . 115 C2' C3 C2 63.0(6) 115 115 C2' C3 C2 63.0(6) . . C2' C3 C2 118.9(8) 115 . C2 C3 C2 88.1(9) 115 . C2' C3 C4 122.1(6) . . C2' C3 C4 122.1(6) 115 . C2 C3 C4 119.0(5) 115 . C2 C3 C4 119.0(5) . . C5 C4 C5 119.1(6) 58 . C5 C4 C3 120.5(3) 58 . C5 C4 C3 120.5(3) . . C4 C5 C4 120.9(6) 79 . C6 N2 Fe1 180.0(8) . . N2 C6 S1 180.0(11) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Fe1 N2 1.938(8) . Fe1 N2 1.938(8) 121_655 Fe1 N1 1.998(5) 28 Fe1 N1 1.998(5) 121_655 Fe1 N1 1.998(5) . Fe1 N1 1.998(5) 100_655 N1 C1' 1.355(11) . N1 C1' 1.355(11) 115 N1 C1 1.370(10) . N1 C1 1.370(10) 115 C1 C2 1.389(13) . C1 C1' 1.466(14) . C1 C1 1.833(19) 115 C1' C2' 1.413(13) . C1' C1' 1.767(19) 115 C1' C2 2.010(14) . C2 C3 1.416(10) . C2 C2' 1.461(14) . C2 C2 1.970(19) 115 C2' C3 1.379(11) . C2' C2' 1.86(2) 115 C3 C2' 1.379(11) 115 C3 C2 1.416(10) 115 C3 C4 1.480(9) . C4 C5 1.387(4) 58 C4 C5 1.387(4) . C5 C4 1.387(4) 79 N2 C6 1.134(14) . C6 S1 1.653(13) . _journal_paper_doi 10.1039/c3cc45180a