#------------------------------------------------------------------------------ #$Date: 2016-03-26 01:42:01 +0000 (Sat, 26 Mar 2016) $ #$Revision: 180192 $ #$URL: svn://www.crystallography.net/cod/cif/7/10/88/7108860.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_7108860 loop_ _publ_author_name 'Patrick Nugent' 'Vanessah Rhodus' 'Tony Pham' 'Brant Tudor' 'Katherine Forrest' 'Lukasz Wojtas' 'Brian Space' 'Michael Zaworotko' _publ_section_title ; Enhancement of CO2 selectivity in a pillared pcu MOM platform through pillar substitution ; _journal_issue 16 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1606 _journal_page_last 1608 _journal_paper_doi 10.1039/c3cc37695h _journal_volume 49 _journal_year 2013 _chemical_formula_moiety 'C20 H16 Cu F6 N4 Ti' _chemical_formula_sum 'C20 H16 Cu F6 N4 Ti' _chemical_formula_weight 537.81 _chemical_name_systematic ; ? ; _space_group_crystal_system tetragonal _space_group_IT_number 123 _space_group_name_Hall '-P 4 2' _space_group_name_H-M_alt 'P 4/m m m' _symmetry_space_group_name_Hall '-P 4 2' _symmetry_space_group_name_H-M 'P 4/m m m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2012-10-18 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 11.1001(6) _cell_length_b 11.1001(6) _cell_length_c 8.4055(7) _cell_measurement_temperature 228(2) _cell_volume 1035.66(12) _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 228(2) _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_device_type 'BRUKER SMART APEXII CCD' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_unetI/netI 0.0479 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 5175 _diffrn_reflns_theta_full 66.33 _diffrn_reflns_theta_max 66.32 _diffrn_reflns_theta_min 5.26 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.593 _exptl_absorpt_correction_T_max 0.9871 _exptl_absorpt_correction_T_min 0.9500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_crystal_colour purple _exptl_crystal_density_diffrn 0.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 269 _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _platon_squeeze_details ; ; _refine_diff_density_max 0.365 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 48 _refine_ls_number_reflns 573 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0362 _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^)+(0.0511P)^2^+0.8374P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1083 _refine_ls_wR_factor_ref 0.1095 _reflns_number_gt 522 _reflns_number_total 573 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c3cc37695h.txt _cod_data_source_block TIFSIX-1-Cu _cod_database_code 7108860 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, z' 3 'x, -y, -z' 4 '-x, y, -z' 5 '-y, -x, -z' 6 'y, x, -z' 7 'y, -x, z' 8 '-y, x, z' 9 '-x, -y, -z' 10 'x, y, -z' 11 '-x, y, z' 12 'x, -y, z' 13 'y, x, z' 14 '-y, -x, z' 15 '-y, x, -z' 16 'y, -x, -z' 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 Cu1 Cu 0.0000 0.0000 0.0000 0.0200(4) Uani 1 16 d S . . Ti2 Ti 0.0000 0.0000 0.5000 0.0288(4) Uani 1 16 d SD . . F003 F 0.0000 0.0000 0.2787(4) 0.0352(8) Uani 1 8 d S . . C1 C 0.0000 0.4328(4) 0.0000 0.0350(10) Uani 1 4 d S . . N2 N 0.0000 0.1824(3) 0.0000 0.0268(7) Uani 1 4 d S . . F1 F 0.1183(9) 0.1183(9) 0.5000 0.048(7) Uani 0.375 4 d SPD . . C2 C 0.0422(6) 0.3676(4) 0.1264(6) 0.0548(19) Uani 0.50 1 d P A -1 H2 H 0.0722 0.4077 0.2165 0.066 Uiso 0.50 1 calc PR A -1 C4 C 0.0410(5) 0.2451(4) 0.1226(6) 0.0499(16) Uani 0.50 1 d P A -1 H4 H 0.0707 0.2029 0.2113 0.060 Uiso 0.50 1 calc PR A -1 F2 F 0.0709(12) 0.1523(12) 0.5000 0.039(6) Uani 0.25 2 d SPD . . F3 F 0.0000 0.1676(16) 0.5000 0.043(10) Uani 0.125 4 d SPD . . 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 Cu1 0.0165(4) 0.0165(4) 0.0269(6) 0.000 0.000 0.000 Ti2 0.0322(6) 0.0322(6) 0.0221(8) 0.000 0.000 0.000 F003 0.0425(13) 0.0425(13) 0.0205(17) 0.000 0.000 0.000 C1 0.048(3) 0.021(2) 0.036(2) 0.000 0.000 0.000 N2 0.0278(17) 0.0195(16) 0.0332(18) 0.000 0.000 0.000 F1 0.048(10) 0.048(10) 0.050(6) 0.000 0.000 -0.009(10) C2 0.102(6) 0.024(2) 0.038(2) -0.0009(17) -0.028(2) -0.008(2) C4 0.085(5) 0.024(2) 0.041(3) 0.0064(18) -0.027(2) -0.004(2) F2 0.040(14) 0.032(7) 0.044(6) 0.000 0.000 -0.009(9) F3 0.05(3) 0.037(15) 0.041(14) 0.000 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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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 F003 Cu1 F003 180.0 . 9 N2 Cu1 F003 90.0 9 . N2 Cu1 F003 90.0 13 9 N2 Cu1 F003 90.0 9 9 N2 Cu1 F003 90.0 5 . N2 Cu1 F003 90.0 . 9 N2 Cu1 F003 90.0 5 9 N2 Cu1 F003 90.0 13 . N2 Cu1 F003 90.0 . . N2 Cu1 N2 90.0 . 5 N2 Cu1 N2 180.0 13 5 N2 Cu1 N2 90.0 13 . N2 Cu1 N2 90.0 5 9 N2 Cu1 N2 180.0 . 9 N2 Cu1 N2 90.0 13 9 F003 Ti2 F003 180.0 9_556 . F003 Ti2 F2 90.000(1) . 13 F003 Ti2 F2 90.000(1) 9_556 13 F003 Ti2 F2 90.000(1) 9_556 . F003 Ti2 F2 90.000(1) . . F1 Ti2 F003 90.0 3_556 . F1 Ti2 F003 90.0 11 . F1 Ti2 F003 90.000(1) 9_556 9_556 F1 Ti2 F003 90.0 11 9_556 F1 Ti2 F003 90.000(1) 9_556 . F1 Ti2 F003 90.000(1) . 9_556 F1 Ti2 F003 90.0 3_556 9_556 F1 Ti2 F003 90.000(1) . . F1 Ti2 F1 90.000(1) . 3_556 F1 Ti2 F1 90.000(1) 9_556 3_556 F1 Ti2 F1 180.000(1) 11 3_556 F1 Ti2 F1 180.0(9) . 9_556 F1 Ti2 F1 90.0 . 11 F1 Ti2 F1 90.0 9_556 11 F1 Ti2 F2 70.0(5) 11 . F1 Ti2 F2 70.0(5) 3_556 13 F1 Ti2 F2 20.0(5) . 13 F1 Ti2 F2 110.0(5) 3_556 . F1 Ti2 F2 110.0(5) 11 13 F1 Ti2 F2 160.0(5) 9_556 . F1 Ti2 F2 20.0(5) . . F1 Ti2 F2 160.0(5) 9_556 13 F1 Ti2 F3 45.000(1) 11 5_556 F1 Ti2 F3 135.000(2) 3_556 5_556 F1 Ti2 F3 45.000(1) . . F1 Ti2 F3 135.000(1) 9_556 . F1 Ti2 F3 45.0 3_556 9_556 F1 Ti2 F3 135.000(2) 11 9_556 F1 Ti2 F3 45.000(1) 9_556 9_556 F1 Ti2 F3 135.000(1) . 9_556 F1 Ti2 F3 45.000(1) 9_556 5_556 F1 Ti2 F3 135.000(2) 3_556 . F1 Ti2 F3 45.000(1) . 13 F1 Ti2 F3 135.000(1) 9_556 13 F1 Ti2 F3 45.000(1) 11 . F1 Ti2 F3 135.000(1) . 5_556 F1 Ti2 F3 45.000(1) 3_556 13 F1 Ti2 F3 135.000(2) 11 13 F2 Ti2 F2 40.1(10) . 13 F3 Ti2 F003 90.0 . 9_556 F3 Ti2 F003 90.0 13 9_556 F3 Ti2 F003 90.0 9_556 9_556 F3 Ti2 F003 90.0 5_556 9_556 F3 Ti2 F003 90.0 . . F3 Ti2 F003 90.0 9_556 . F3 Ti2 F003 90.0 13 . F3 Ti2 F003 90.0 5_556 . F3 Ti2 F2 25.0(5) 13 13 F3 Ti2 F2 65.0(5) . 13 F3 Ti2 F2 65.0(5) 13 . F3 Ti2 F2 115.0(5) 5_556 . F3 Ti2 F2 115.0(5) 9_556 13 F3 Ti2 F2 155.0(5) 5_556 13 F3 Ti2 F2 155.0(5) 9_556 . F3 Ti2 F2 25.0(5) . . F3 Ti2 F3 90.000(2) 13 . F3 Ti2 F3 90.000(1) 5_556 . F3 Ti2 F3 180.000(1) 9_556 . F3 Ti2 F3 180.000(1) 13 5_556 F3 Ti2 F3 90.0 13 9_556 F3 Ti2 F3 90.000(2) 5_556 9_556 Ti2 F003 Cu1 180.0 . . C2 C1 C1 122.0(3) . 9_565 C2 C1 C1 122.0(2) 4 9_565 C2 C1 C1 122.0(2) 11 9_565 C2 C1 C1 122.0(3) 10 9_565 C2 C1 C2 116.1(5) 4 . C2 C1 C2 101.9(5) . 10 C2 C1 C2 116.1(5) 10 11 C2 C1 C2 101.9(5) 4 11 C4 N2 Cu1 121.7(2) 11 . C4 N2 Cu1 121.7(2) . . C4 N2 Cu1 121.7(2) 4 . C4 N2 Cu1 121.7(2) 10 . C4 N2 C4 116.6(5) . 4 C4 N2 C4 102.2(5) 11 4 C4 N2 C4 116.6(5) 11 10 C4 N2 C4 102.2(5) . 10 F2 F1 Ti2 80.6(18) . . F2 F1 Ti2 80.6(18) 13 . F2 F1 F2 161(4) 13 . F2 F1 F3 148(3) . 13 F2 F1 F3 148(3) 13 . F3 F1 Ti2 67.6(10) . . F3 F1 Ti2 67.6(10) 13 . F3 F1 F3 135.2(19) 13 . C1 C2 H2 119.8 . . C4 C2 C1 120.5(4) . . C4 C2 H2 119.8 . . N2 C4 C2 123.1(4) . . N2 C4 H4 118.4 . . C2 C4 H4 118.4 . . F1 F2 Ti2 79.3(19) . . F1 F2 F2 144.4(18) . 11 F1 F2 F3 157(2) . . F2 F2 Ti2 70.0(5) 13 . F2 F2 Ti2 65.0(5) 11 . F2 F2 F2 135.000(2) 13 11 F3 F2 Ti2 77.2(13) . . F3 F2 F2 147.1(13) . 13 F1 F3 Ti2 67.4(10) . . F1 F3 Ti2 67.4(10) 11 . F1 F3 F1 134.8(19) . 11 F2 F3 Ti2 77.9(13) . . F2 F3 Ti2 77.9(13) 11 . F2 F3 F1 145(2) 11 . F2 F3 F1 145(2) . 11 F2 F3 F2 156(3) . 11 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 F003 2.343(3) 9 Cu1 F003 2.343(3) . Cu1 N2 2.025(3) 13 Cu1 N2 2.025(3) . Cu1 N2 2.025(3) 5 Cu1 N2 2.025(3) 9 Ti2 F003 1.860(3) 9_556 Ti2 F003 1.860(3) . Ti2 F1 1.858(15) 3_556 Ti2 F1 1.858(15) . Ti2 F1 1.858(15) 9_556 Ti2 F1 1.858(15) 11 Ti2 F2 1.865(10) . Ti2 F2 1.865(10) 13 Ti2 F3 1.860(18) 9_556 Ti2 F3 1.860(18) 5_556 Ti2 F3 1.860(18) 13 Ti2 F3 1.860(18) . C1 C1 1.492(8) 9_565 C1 C2 1.368(5) 10 C1 C2 1.368(5) 11 C1 C2 1.368(5) . C1 C2 1.368(5) 4 N2 C4 1.324(5) 4 N2 C4 1.324(5) 10 N2 C4 1.324(5) . N2 C4 1.324(5) 11 F1 F2 0.648(16) . F1 F2 0.648(16) 13 F1 F3 1.423(8) . F1 F3 1.423(8) 13 C2 H2 0.9400 . C2 C4 1.360(7) . C4 H4 0.9400 . F2 F2 1.57(3) 11 F2 F2 1.28(3) 13 F2 F3 0.805(14) . F3 F1 1.423(8) 11 F3 F2 0.805(14) 11 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 _platon_squeeze_void_content 1 0.459 0.497 -0.059 546 150 ' '