#------------------------------------------------------------------------------ #$Date: 2014-03-15 13:45:36 +0200 (Sat, 15 Mar 2014) $ #$Revision: 106525 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/00/7110011.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_7110011 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 Se2' _chemical_formula_weight 678.29 _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 37.4018(2) _cell_length_b 37.4018(2) _cell_length_c 37.4018(2) _cell_measurement_temperature 100(2) _cell_volume 52321.2(5) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_number 44602 _diffrn_reflns_theta_full 69.86 _diffrn_reflns_theta_max 69.86 _diffrn_reflns_theta_min 3.34 _exptl_absorpt_coefficient_mu 2.420 _exptl_crystal_colour orange _exptl_crystal_density_diffrn 0.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 8064 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.467 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 76 _refine_ls_number_reflns 2475 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.109 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0609 _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^)+(0.1240P)^2^+112.4551P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2033 _refine_ls_wR_factor_ref 0.2089 _reflns_number_gt 2252 _reflns_number_total 2475 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c3cc45180a.txt _[local]_cod_data_source_block 2x(guest) _[local]_cod_cif_authors_sg_H-M Fm-3m _cod_database_code 7110011 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 0.0000 0.2500 0.2500 0.0309(3) Uani 1 8 d S N1 N 0.03790(6) 0.22348(5) 0.27652(5) 0.0365(6) Uani 1 2 d S C1 C 0.03851(11) 0.22077(13) 0.31249(11) 0.0396(9) Uani 0.50 1 d P C2 C 0.06564(11) 0.20315(12) 0.33109(12) 0.0408(9) Uani 0.50 1 d P C3 C 0.09338(8) 0.18735(6) 0.31265(6) 0.0392(7) Uani 1 2 d S C4 C 0.09237(11) 0.18917(13) 0.27474(11) 0.0415(10) Uani 0.50 1 d P C5 C 0.06484(11) 0.20665(13) 0.25806(12) 0.0413(10) Uani 0.50 1 d P C6 C 0.12378(8) 0.16956(6) 0.33044(6) 0.0397(7) Uani 1 2 d S C7 C 0.13892(6) 0.13892(6) 0.31562(8) 0.0412(7) Uani 1 2 d S H7A H 0.1282 0.1282 0.2952 0.049 Uiso 1 2 calc SR N2 N 0.0000 0.21326(6) 0.21326(6) 0.0350(7) Uani 1 4 d S C8 C 0.0000 0.19152(11) 0.19152(11) 0.0570(12) Uani 1 4 d S Se1 Se 0.0000 0.157764(15) 0.157764(15) 0.1251(6) 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 0.0210(4) 0.0359(4) 0.0359(4) -0.0032(3) 0.000 0.000 N1 0.0274(11) 0.0411(8) 0.0411(8) -0.0059(10) 0.0017(7) -0.0017(7) C1 0.0266(18) 0.053(2) 0.039(2) -0.0042(18) -0.0011(16) 0.0024(16) C2 0.035(2) 0.049(2) 0.038(2) -0.0017(18) 0.0005(16) 0.0037(17) C3 0.0306(14) 0.0435(10) 0.0435(10) -0.0067(12) -0.0044(9) 0.0044(9) C4 0.0323(19) 0.055(3) 0.037(2) -0.0074(18) -0.0045(16) 0.0109(18) C5 0.030(2) 0.052(3) 0.042(2) -0.0053(19) 0.0044(17) 0.0030(18) C6 0.0354(15) 0.0419(10) 0.0419(10) -0.0016(12) -0.0044(9) 0.0044(9) C7 0.0416(10) 0.0416(10) 0.0402(15) -0.0060(9) -0.0060(9) 0.0032(13) N2 0.0234(15) 0.0408(11) 0.0408(11) -0.0034(15) 0.000 0.000 C8 0.048(3) 0.0615(19) 0.0615(19) -0.010(3) 0.000 0.000 Se1 0.1521(10) 0.1116(6) 0.1116(6) -0.0732(7) 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' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 '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(2) 121 . N2 Fe1 N1 90.0 121 . N2 Fe1 N1 90.0 . . N2 Fe1 N1 90.0 121 28 N2 Fe1 N1 90.0 . 28 N1 Fe1 N1 89.40(14) . 28 N2 Fe1 N1 90.0 121 100 N2 Fe1 N1 90.0 . 100 N1 Fe1 N1 90.60(14) . 100 N1 Fe1 N1 180.0(2) 28 100 N2 Fe1 N1 90.0 121 121 N2 Fe1 N1 90.0 . 121 N1 Fe1 N1 180.00(13) . 121 N1 Fe1 N1 90.60(14) 28 121 N1 Fe1 N1 89.40(14) 100 121 C1 N1 C1 81.4(4) . 138 C1 N1 C5 64.4(3) . 138 C1 N1 C5 117.0(3) 138 138 C1 N1 C5 117.0(3) . . C1 N1 C5 64.4(3) 138 . C5 N1 C5 85.6(4) 138 . C1 N1 Fe1 123.1(2) . . C1 N1 Fe1 123.1(2) 138 . C5 N1 Fe1 120.0(2) 138 . C5 N1 Fe1 120.0(2) . . N1 C1 C2 123.0(4) . . N1 C1 C5 58.6(3) . 138 C2 C1 C5 90.6(3) . 138 N1 C1 C1 49.3(2) . 138 C2 C1 C1 91.1(3) . 138 C5 C1 C1 92.1(2) 138 138 N1 C1 C4 88.9(3) . 138 C2 C1 C4 48.0(3) . 138 C5 C1 C4 42.6(2) 138 138 C1 C1 C4 92.12(17) 138 138 C3 C2 C1 120.0(4) . . C3 C2 C4 58.9(3) . 138 C1 C2 C4 88.4(3) . 138 C3 C2 C2 48.9(2) . 138 C1 C2 C2 88.9(3) . 138 C4 C2 C2 91.9(2) 138 138 C3 C2 C5 88.2(3) . 138 C1 C2 C5 45.8(3) . 138 C4 C2 C5 42.6(2) 138 138 C2 C2 C5 90.78(18) 138 138 C2 C3 C2 82.1(4) 138 . C2 C3 C4 117.3(3) 138 138 C2 C3 C4 64.9(3) . 138 C2 C3 C4 64.9(3) 138 . C2 C3 C4 117.3(3) . . C4 C3 C4 84.5(4) 138 . C2 C3 C6 123.2(3) 138 . C2 C3 C6 123.2(3) . . C4 C3 C6 119.5(2) 138 . C4 C3 C6 119.5(2) . . C5 C4 C3 119.8(4) . . C5 C4 C2 89.5(3) . 138 C3 C4 C2 56.2(3) . 138 C5 C4 C4 89.1(3) . 138 C3 C4 C4 47.8(2) . 138 C2 C4 C4 88.1(2) 138 138 C5 C4 C1 45.9(3) . 138 C3 C4 C1 86.7(3) . 138 C2 C4 C1 43.6(2) 138 138 C4 C4 C1 87.88(17) 138 138 C4 C5 N1 122.8(4) . . C4 C5 C1 91.5(4) . 138 N1 C5 C1 57.0(3) . 138 C4 C5 C5 90.9(3) . 138 N1 C5 C5 47.2(2) . 138 C1 C5 C5 87.9(2) 138 138 C4 C5 C2 47.9(3) . 138 N1 C5 C2 88.3(3) . 138 C1 C5 C2 43.6(2) 138 138 C5 C5 C2 89.22(18) 138 138 C7 C6 C7 119.3(3) 35 . C7 C6 C3 120.30(15) 35 . C7 C6 C3 120.30(15) . . C6 C7 C6 120.7(3) . 56 C8 N2 Fe1 180.0(4) . . N2 C8 Se1 180.0(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Fe1 N2 1.943(3) 121 Fe1 N2 1.943(3) . Fe1 N1 1.994(2) . Fe1 N1 1.994(2) 28 Fe1 N1 1.994(2) 100 Fe1 N1 1.994(2) 121 N1 C1 1.350(5) . N1 C1 1.350(5) 138 N1 C5 1.374(5) 138 N1 C5 1.374(5) . C1 C2 1.396(6) . C1 C5 1.452(6) 138 C1 C1 1.759(9) 138 C1 C4 2.022(6) 138 C2 C3 1.379(5) . C2 C4 1.503(6) 138 C2 C2 1.811(9) 138 C2 C5 2.024(7) 138 C3 C2 1.379(5) 138 C3 C4 1.420(5) 138 C3 C4 1.420(5) . C3 C6 1.476(4) . C4 C5 1.370(6) . C4 C2 1.503(6) 138 C4 C4 1.909(9) 138 C4 C1 2.022(6) 138 C5 C1 1.452(6) 138 C5 C5 1.867(9) 138 C5 C2 2.024(7) 138 C6 C7 1.393(2) 35 C6 C7 1.393(2) . C7 C6 1.393(2) 56 N2 C8 1.150(7) . C8 Se1 1.786(6) . _journal_paper_doi 10.1039/c3cc45180a