#------------------------------------------------------------------------------ #$Date: 2013-01-31 11:31:55 +0000 (Thu, 31 Jan 2013) $ #$Revision: 72864 $ #$URL: svn://www.crystallography.net/cod/cif/7/10/88/7108861.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_7108861 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_name_full Chem.Commun. _journal_page_first 1606 _journal_volume 49 _journal_year 2012 _chemical_formula_moiety 'C20 H16 Cu F6 N4 Sn' _chemical_formula_sum 'C20 H16 Cu F6 N4 Sn' _chemical_formula_weight 608.60 _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 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_formula_units_Z 1 _cell_length_a 11.116(5) _cell_length_b 11.116(5) _cell_length_c 8.627(5) _cell_measurement_temperature 228(2) _cell_volume 1066.0(9) _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 0.995 _diffrn_measured_fraction_theta_max 0.995 _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 0.0557 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 5235 _diffrn_reflns_theta_full 66.53 _diffrn_reflns_theta_max 66.53 _diffrn_reflns_theta_min 3.98 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 5.587 _exptl_absorpt_correction_T_max 0.9726 _exptl_absorpt_correction_T_min 0.8965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2003)' _exptl_crystal_colour purple _exptl_crystal_density_diffrn 0.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 297 _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 0.687 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.092 _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 40 _refine_ls_number_reflns 603 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.188 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0317 _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^)+(0.0459P)^2^+0.0551P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.0748 _reflns_number_gt 584 _reflns_number_total 603 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c3cc37695h.txt _[local]_cod_data_source_block SNIFSIX-1-Cu _cod_database_code 7108861 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 Sn01 Sn 0.0000 0.0000 0.0000 0.0247(2) Uani 1 16 d S . . Cu1 Cu 0.0000 0.0000 0.5000 0.0190(3) Uani 1 16 d S . . F003 F 0.0000 0.0000 0.2284(4) 0.0309(8) Uani 1 8 d S . . N1 N 0.0000 0.1826(3) 0.5000 0.0257(7) Uani 1 4 d S . . F1 F 0.0543(5) 0.1661(4) 0.0000 0.0716(16) Uani 0.50 2 d SP . . C1 C 0.0000 0.4336(4) 0.5000 0.0349(10) Uani 1 4 d S . . C2A C 0.0385(6) 0.3677(4) 0.3733(5) 0.054(2) Uani 0.50 1 d P A -1 H2A H 0.0652 0.4076 0.2836 0.065 Uiso 0.50 1 calc PR A -1 C3A C 0.0379(5) 0.2448(4) 0.3785(5) 0.0458(16) Uani 0.50 1 d P A -1 H3A H 0.0657 0.2023 0.2914 0.055 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn01 0.0244(2) 0.0244(2) 0.0253(3) 0.000 0.000 0.000 Cu1 0.0127(3) 0.0127(3) 0.0314(6) 0.000 0.000 0.000 F003 0.0339(12) 0.0339(12) 0.0250(14) 0.000 0.000 0.000 N1 0.0259(17) 0.0140(15) 0.0373(17) 0.000 0.000 0.000 F1 0.124(5) 0.043(2) 0.047(2) 0.000 0.000 -0.032(2) C1 0.050(3) 0.017(2) 0.038(2) 0.000 0.000 0.000 C2A 0.101(6) 0.0213(19) 0.042(2) 0.0044(17) 0.026(3) -0.009(2) C3A 0.075(5) 0.0199(18) 0.043(2) -0.0062(17) 0.022(2) -0.0052(19) 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' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn 0.0259 5.4591 '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 Sn01 F003 180.0 . 9 F1 Sn01 F003 90.0 3 . F1 Sn01 F003 90.0 11 . F1 Sn01 F003 90.0 15 . F1 Sn01 F003 90.0 7 . F1 Sn01 F003 90.0 . . F1 Sn01 F003 90.0 13 . F1 Sn01 F003 90.0 5 . F1 Sn01 F003 90.0 9 . F1 Sn01 F003 90.0 11 9 F1 Sn01 F003 90.0 3 9 F1 Sn01 F003 90.0 15 9 F1 Sn01 F003 90.0 7 9 F1 Sn01 F003 90.0 . 9 F1 Sn01 F003 90.0 13 9 F1 Sn01 F003 90.0 5 9 F1 Sn01 F003 90.0 9 9 F1 Sn01 F1 143.8(3) 9 11 F1 Sn01 F1 90.0 5 11 F1 Sn01 F1 90.0 13 11 F1 Sn01 F1 143.8(3) . 3 F1 Sn01 F1 36.2(3) 9 3 F1 Sn01 F1 90.0 5 3 F1 Sn01 F1 90.0 13 3 F1 Sn01 F1 180.0(3) 13 5 F1 Sn01 F1 126.2(3) . 5 F1 Sn01 F1 53.8(3) . 13 F1 Sn01 F1 180.0 . 9 F1 Sn01 F1 36.2(3) . 11 F1 Sn01 F1 53.8(3) 5 9 F1 Sn01 F1 126.2(3) 13 9 F1 Sn01 F1 90.0 . 7 F1 Sn01 F1 36.2(3) 13 7 F1 Sn01 F1 143.8(3) 5 7 F1 Sn01 F1 126.2(3) 3 15 F1 Sn01 F1 36.2(3) 5 15 F1 Sn01 F1 90.0 9 15 F1 Sn01 F1 53.8(3) 11 15 F1 Sn01 F1 143.8(3) 13 15 F1 Sn01 F1 90.0 . 15 F1 Sn01 F1 180.0(3) 11 3 F1 Sn01 F1 180.0(3) 15 7 F1 Sn01 F1 90.0 9 7 F1 Sn01 F1 126.2(3) 11 7 F1 Sn01 F1 53.8(3) 3 7 F003 Cu1 F003 180.0 9_556 . N1 Cu1 F003 90.0 . 9_556 N1 Cu1 F003 90.0 13 9_556 N1 Cu1 F003 90.0 5_556 9_556 N1 Cu1 F003 90.0 9_556 9_556 N1 Cu1 F003 90.0 . . N1 Cu1 F003 90.0 9_556 . N1 Cu1 F003 90.0 5_556 . N1 Cu1 F003 90.0 13 . N1 Cu1 N1 90.0 5_556 9_556 N1 Cu1 N1 90.0 13 9_556 N1 Cu1 N1 180.0 13 5_556 N1 Cu1 N1 180.0 9_556 . N1 Cu1 N1 90.0 5_556 . N1 Cu1 N1 90.0 13 . Sn01 F003 Cu1 180.0 . . C3A N1 Cu1 121.5(2) . . C3A N1 Cu1 121.5(2) 10_556 . C3A N1 Cu1 121.5(2) 4_556 . C3A N1 Cu1 121.5(2) 11 . C3A N1 C3A 104.6(4) . 10_556 C3A N1 C3A 117.1(5) . 4_556 C3A N1 C3A 104.6(4) 4_556 11 C3A N1 C3A 117.1(5) 10_556 11 F1 F1 Sn01 63.12(17) 13 . F1 F1 Sn01 71.88(17) 11 . F1 F1 F1 135.0 11 13 C2A C1 C1 122.0(2) 11 9_566 C2A C1 C1 122.0(2) . 9_566 C2A C1 C1 122.0(2) 10_556 9_566 C2A C1 C1 122.0(2) 4_556 9_566 C2A C1 C2A 104.4(5) . 10_556 C2A C1 C2A 116.1(5) 11 10_556 C2A C1 C2A 104.4(5) 11 4_556 C2A C1 C2A 116.1(5) . 4_556 C3A C2A C1 120.1(4) . . N1 C3A C2A 123.3(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sn01 F003 1.971(3) . Sn01 F003 1.971(3) 9 Sn01 F1 1.942(5) 3 Sn01 F1 1.942(5) 15 Sn01 F1 1.942(5) 7 Sn01 F1 1.942(5) . Sn01 F1 1.942(5) 13 Sn01 F1 1.942(5) 5 Sn01 F1 1.942(5) 11 Sn01 F1 1.942(5) 9 Cu1 F003 2.343(3) 9_556 Cu1 F003 2.343(3) . Cu1 N1 2.030(3) . Cu1 N1 2.030(3) 13 Cu1 N1 2.030(3) 5_556 Cu1 N1 2.030(3) 9_556 N1 C3A 1.325(5) 4_556 N1 C3A 1.325(5) 11 N1 C3A 1.325(5) . N1 C3A 1.325(5) 10_556 F1 F1 1.757(11) 13 F1 F1 1.208(12) 11 C1 C1 1.476(8) 9_566 C1 C2A 1.383(5) 4_556 C1 C2A 1.383(5) 10_556 C1 C2A 1.383(5) . C1 C2A 1.383(5) 11 C2A C3A 1.367(6) . 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 -0.027 0.495 -0.019 544 224 ' '