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#$Date: 2016-03-22 12:20:51 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178946 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/75/4117562.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_4117562
loop_
_publ_author_name
'Stephen D. Burd'
'Shengqian Ma'
'Jason A. Perman'
'Benjamin J. Sikora'
'Randall Q. Snurr'
'Praveen K. Thallapally'
'Jian Tian'
'Lukasz Wojtas'
'Michael J. Zaworotko'
_publ_section_title
;
 Highly Selective Carbon Dioxide Uptake by [Cu(bpy-n)2(SiF6)] (bpy-1 =
 4,4'-Bipyridine; bpy-2 = 1,2-Bis(4-pyridyl)ethene)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3663
_journal_page_last               3666
_journal_paper_doi               10.1021/ja211340t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C24 H20 Cu F6 N4 Si'
_chemical_formula_weight         570.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_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            2
_cell_length_a                   18.8471(11)
_cell_length_b                   18.8471(11)
_cell_length_c                   7.9975(5)
_cell_measurement_reflns_used    3091
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      29.76
_cell_volume                     2840.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19133
_diffrn_reflns_theta_full        68.01
_diffrn_reflns_theta_max         68.01
_diffrn_reflns_theta_min         4.69
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6154
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.666
_exptl_crystal_description       block
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1433
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0686
_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/[σ²(Fo²)+(0.1022P)²+4.7858P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.1956
_reflns_number_gt                1331
_reflns_number_total             1433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211340t_si_003.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               4117562
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x+1/2, -y+1/2, z'
'y+1/2, x+1/2, -z'
'-y, -x, -z'
'-x, -y, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'
'x-1/2, y-1/2, -z'
'-y-1/2, -x-1/2, z'
'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 0.2500 0.2500 0.43281(11) 0.0141(4) Uani 1 8 d S . .
Si1 Si 0.2500 0.2500 -0.0655(2) 0.0226(5) Uani 1 8 d S . .
F1 F 0.2500 0.2500 0.1505(5) 0.0231(9) Uani 1 8 d S . .
F2 F 0.2500 0.2500 -0.2705(6) 0.0395(12) Uani 1 8 d S . .
F3A F 0.2500 0.3392(5) -0.0620(12) 0.021(3) Uani 0.25 2 d SPU . .
F3B F 0.3133(7) 0.3133(7) -0.067(2) 0.021(4) Uani 0.25 2 d SPU . .
F3C F 0.2894(5) 0.3305(5) -0.0637(10) 0.029(3) Uani 0.25 1 d PU . .
N1 N 0.32549(12) 0.17451(12) 0.4369(4) 0.0246(7) Uani 1 2 d S . .
C1 C 0.3291(3) 0.1249(3) 0.3110(7) 0.0325(12) Uani 0.50 1 d P A -1
H1 H 0.2971 0.1288 0.2197 0.039 Uiso 0.50 1 calc PR A -1
C2 C 0.3765(4) 0.0707(3) 0.3113(7) 0.0393(15) Uani 0.50 1 d PU A -1
H2 H 0.3753 0.0345 0.2285 0.047 Uiso 0.50 1 calc PR A -1
C4 C 0.4224(3) 0.1172(4) 0.5638(7) 0.0390(15) Uani 0.50 1 d PU A -1
H4 H 0.4532 0.1153 0.6578 0.047 Uiso 0.50 1 calc PR A -1
C5 C 0.3712(3) 0.1694(3) 0.5565(6) 0.0308(13) Uani 0.50 1 d P A -1
H5 H 0.3695 0.2034 0.6440 0.037 Uiso 0.50 1 calc PR A -1
C3 C 0.4296 0.0703 0.4454 0.0435(16) Uani 1 2 d SU A -1
C6 C 0.48428(19) 0.01572(19) 0.4417(6) 0.067(2) Uani 1 2 d SU . .
H6 H 0.4985 0.0015 0.3328 0.081 Uiso 1 2 calc SR A .
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'
Si Si 0.2541 0.3302 '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
N1 Cu1 N1 89.988(3) 2 6
N1 Cu1 N1 178.13(17) 2 3
N1 Cu1 N1 89.982(4) 6 3
N1 Cu1 N1 89.983(3) 2 .
N1 Cu1 N1 178.13(17) 6 .
N1 Cu1 N1 89.986(3) 3 .
N1 Cu1 F1 90.94(8) 2 .
N1 Cu1 F1 90.94(8) 6 .
N1 Cu1 F1 90.94(8) 3 .
N1 Cu1 F1 90.94(8) . .
N1 Cu1 F2 89.06(8) 2 1_556
N1 Cu1 F2 89.06(8) 6 1_556
N1 Cu1 F2 89.07(8) 3 1_556
N1 Cu1 F2 89.07(8) . 1_556
F1 Cu1 F2 180.0 . 1_556
F2 Si1 F3A 91.0(3) . 13_565
F2 Si1 F3A 91.0(3) . .
F3A Si1 F3A 178.1(7) 13_565 .
F2 Si1 F3A 91.0(3) . 3
F3A Si1 F3A 89.986(13) 13_565 3
F3A Si1 F3A 89.982(12) . 3
F2 Si1 F3A 91.0(3) . 2
F3A Si1 F3A 89.986(12) 13_565 2
F3A Si1 F3A 89.982(13) . 2
F3A Si1 F3A 178.1(7) 3 2
F2 Si1 F3B 89.5(6) . 2
F3A Si1 F3B 135.000(9) 13_565 2
F3A Si1 F3B 45.02(3) . 2
F3A Si1 F3B 135.002(9) 3 2
F3A Si1 F3B 45.02(3) 2 2
F2 Si1 F3B 89.5(6) . .
F3A Si1 F3B 135.002(10) 13_565 .
F3A Si1 F3B 45.02(3) . .
F3A Si1 F3B 45.02(3) 3 .
F3A Si1 F3B 135.000(9) 2 .
F3B Si1 F3B 89.997(12) 2 .
F2 Si1 F3B 89.5(6) . 6
F3A Si1 F3B 45.02(3) 13_565 6
F3A Si1 F3B 135.001(10) . 6
F3A Si1 F3B 135.006(9) 3 6
F3A Si1 F3B 45.02(3) 2 6
F3B Si1 F3B 89.992(14) 2 6
F3B Si1 F3B 178.9(12) . 6
F2 Si1 F3B 89.5(6) . 3
F3A Si1 F3B 45.02(3) 13_565 3
F3A Si1 F3B 135.001(10) . 3
F3A Si1 F3B 45.02(3) 3 3
F3A Si1 F3B 135.006(8) 2 3
F3B Si1 F3B 178.9(12) 2 3
F3B Si1 F3B 89.994(14) . 3
F3B Si1 F3B 89.998(12) 6 3
F2 Si1 F3C 90.5(3) . 15_665
F3A Si1 F3C 63.9(4) 13_565 15_665
F3A Si1 F3C 116.0(4) . 15_665
F3A Si1 F3C 153.9(4) 3 15_665
F3A Si1 F3C 26.1(4) 2 15_665
F3B Si1 F3C 71.1(4) 2 15_665
F3B Si1 F3C 161.1(4) . 15_665
F3B Si1 F3C 19.0(4) 6 15_665
F3B Si1 F3C 109.0(4) 3 15_665
F2 Si1 F3C 90.5(3) . 3
F3A Si1 F3C 63.9(4) 13_565 3
F3A Si1 F3C 116.0(4) . 3
F3A Si1 F3C 26.1(4) 3 3
F3A Si1 F3C 153.9(4) 2 3
F3B Si1 F3C 161.1(4) 2 3
F3B Si1 F3C 71.1(4) . 3
F3B Si1 F3C 109.0(4) 6 3
F3B Si1 F3C 19.0(4) 3 3
F3C Si1 F3C 127.9(7) 15_665 3
F2 Si1 F3C 90.5(3) . 16
F3A Si1 F3C 116.0(4) 13_565 16
F3A Si1 F3C 63.9(4) . 16
F3A Si1 F3C 26.1(4) 3 16
F3A Si1 F3C 153.9(4) 2 16
F3B Si1 F3C 108.9(4) 2 16
F3B Si1 F3C 19.0(4) . 16
F3B Si1 F3C 161.1(4) 6 16
F3B Si1 F3C 71.1(4) 3 16
F3C Si1 F3C 179.0(6) 15_665 16
F3C Si1 F3C 52.1(7) 3 16
Si1 F1 Cu1 180.0 . .
Si1 F2 Cu1 180.0 . 1_554
F3C F3A F3C 155(2) 12_655 .
F3C F3A F3B 145.1(15) 12_655 .
F3C F3A F3B 9.8(13) . .
F3C F3A F3B 9.8(13) 12_655 2
F3C F3A F3B 145.1(15) . 2
F3B F3A F3B 135.3(19) . 2
F3C F3A Si1 77.5(10) 12_655 .
F3C F3A Si1 77.5(10) . .
F3B F3A Si1 67.7(10) . .
F3B F3A Si1 67.7(10) 2 .
F3C F3B F3C 160(5) 16 .
F3C F3B F3A 13.5(19) 16 3
F3C F3B F3A 148(4) . 3
F3C F3B F3A 148(4) 16 .
F3C F3B F3A 13.5(19) . .
F3A F3B F3A 134(2) 3 .
F3C F3B Si1 81(3) 16 .
F3C F3B Si1 81(3) . .
F3A F3B Si1 67.3(10) 3 .
F3A F3B Si1 67.3(10) . .
F3B F3C F3A 157(3) . .
F3B F3C F3C 10(3) . 16
F3A F3C F3C 147.5(10) . 16
F3B F3C F3C 144(3) . 12_655
F3A F3C F3C 12.5(10) . 12_655
F3C F3C F3C 135.002(1) 16 12_655
F3B F3C Si1 80(3) . .
F3A F3C Si1 76.4(10) . .
F3C F3C Si1 71.1(4) 16 .
F3C F3C Si1 63.9(4) 12_655 .
C5 N1 C5 49.6(6) 15_665 .
C5 N1 C1 94.9(4) 15_665 .
C5 N1 C1 117.3(4) . .
C5 N1 C1 117.3(4) 15_665 15_665
C5 N1 C1 94.9(4) . 15_665
C1 N1 C1 52.8(5) . 15_665
C5 N1 Cu1 122.4(3) 15_665 .
C5 N1 Cu1 122.4(3) . .
C1 N1 Cu1 120.2(3) . .
C1 N1 Cu1 120.2(3) 15_665 .
C2 C1 N1 122.9(5) . .
C2 C1 H1 118.6 . .
N1 C1 H1 118.6 . .
C1 C2 C3 117.0(5) . .
C1 C2 H2 121.5 . .
C3 C2 H2 121.5 . .
C3 C4 C5 121.8(5) . .
C3 C4 H4 119.1 . .
C5 C4 H4 119.1 . .
N1 C5 C4 123.4(5) . .
N1 C5 H5 118.3 . .
C4 C5 H5 118.3 . .
C4 C3 C6 124.6(3) . .
C4 C3 C2 117.2(4) . .
C6 C3 C2 118.1(3) . .
C6 C6 C3 130.8(6) 9_656 .
C6 C6 H6 114.6 9_656 .
C3 C6 H6 114.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.012(3) 2
Cu1 N1 2.012(3) 6
Cu1 N1 2.012(3) 3
Cu1 N1 2.012(3) .
Cu1 F1 2.258(4) .
Cu1 F2 2.373(5) 1_556
Si1 F2 1.640(5) .
Si1 F3A 1.681(10) 13_565
Si1 F3A 1.681(10) .
Si1 F3A 1.681(10) 3
Si1 F3A 1.681(10) 2
Si1 F3B 1.687(19) 2
Si1 F3B 1.687(19) .
Si1 F3B 1.687(19) 6
Si1 F3B 1.687(19) 3
Si1 F3C 1.689(9) 15_665
Si1 F3C 1.689(9) 3
Si1 F3C 1.689(9) 16
F2 Cu1 2.373(5) 1_554
F3A F3C 0.760(10) 12_655
F3A F3C 0.760(10) .
F3A F3B 1.290(8) .
F3A F3B 1.290(8) 2
F3B F3C 0.556(11) 16
F3B F3C 0.556(11) .
F3B F3A 1.290(8) 3
F3C F3C 1.10(2) 16
F3C F3C 1.48(2) 12_655
N1 C5 1.290(6) 15_665
N1 C5 1.290(6) .
N1 C1 1.376(6) .
N1 C1 1.376(6) 15_665
C1 C2 1.357(9) .
C1 H1 0.9500 .
C2 C3 1.467(6) .
C2 H2 0.9500 .
C4 C3 1.302(6) .
C4 C5 1.380(9) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C3 C6 1.456(5) .
C6 C6 1.253(10) 9_656
C6 H6 0.9500 .
