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#$Date: 2016-03-21 18:20:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178809 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/63/4106368.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_4106368
loop_
_publ_author_name
'Atsushi Kondo'
'Hiroshi Kajiro'
'Hiroshi Noguchi'
'Lucia Carlucci'
'Davide M. Proserpio'
'Gianfranco Ciani'
'Kenichi Kato'
'Masaki Takata'
'Hiroko Seki'
'Masami Sakamoto'
'Yoshiyuki Hattori'
'Fujio Okino'
'Kazuyuki Maeda'
'Tomonori Ohba'
'Katsumi Kaneko'
'Hirofumi Kanoh'
_publ_section_title
;
 Super Flexibility of a 2D Cu-Based Porous Coordination Framework on Gas
 Adsorption in Comparison with a 3D Framework of Identical Composition:
 Framework Dimensionality-Dependent Gas Adsorptivities
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10512
_journal_page_last               10522
_journal_paper_doi               10.1021/ja201170c
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C22 H16 Cu F6 N4 O6 S2'
_chemical_formula_weight         674.05
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   28.564(2)
_cell_length_b                   28.564(2)
_cell_length_c                   18.2725(13)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     14908.6(18)
_computing_molecular_graphics    TOPOS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79208
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        8
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       column
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;

R values before squeeze:
 R1 =  0.1236 for   3606 Fo > 4sig(Fo)  and  0.1323 for all   4144 data
 wR2 =  0.3658,  GooF = S =   1.343,  Restrained GooF =    1.346  for all data
  186 parameters refined using      6 restraints

;
_refine_diff_density_max         0.656
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4144
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_obs          0.0899
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1515P)²+95.9299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2636
_refine_ls_wR_factor_obs         0.2572
_reflns_number_observed          3674
_reflns_number_total             4144
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja201170c_si_004.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4106368
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
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
Cu1 Cu 0.7500 0.25885(2) 1.0000 0.0318(3) Uani 1 2 d S
S1 S 0.68315(13) 0.27246(12) 0.82152(12) 0.1190(10) Uani 1 1 d D
F1 F 0.6084(6) 0.2786(5) 0.7541(9) 0.342(10) Uani 1 1 d D
F2 F 0.6036(3) 0.2805(5) 0.8808(9) 0.254(6) Uani 1 1 d D
F3 F 0.6234(7) 0.2123(4) 0.8289(6) 0.302(9) Uani 1 1 d D
O1 O 0.70029(13) 0.25946(14) 0.89167(19) 0.0514(9) Uani 1 1 d D
O2 O 0.6888(6) 0.3242(3) 0.8125(7) 0.231(8) Uani 1 1 d D
O3 O 0.7011(7) 0.2519(6) 0.7585(5) 0.276(9) Uani 1 1 d D
N1 N 0.79169(12) 0.20820(11) 0.9566(2) 0.0341(8) Uani 1 1 d .
N2 N 0.70799(12) 0.30752(11) 1.0463(2) 0.0327(8) Uani 1 1 d .
C1 C 0.83758(16) 0.20679(16) 0.9730(3) 0.0418(11) Uani 1 1 d .
H1 H 0.8496 0.2287 1.0056 0.050 Uiso 1 1 calc R
C2 C 0.86748(16) 0.17393(17) 0.9430(3) 0.0429(11) Uani 1 1 d .
H2 H 0.8990 0.1735 0.9559 0.051 Uiso 1 1 calc R
C3 C 0.84967(15) 0.14130(15) 0.8930(3) 0.0379(10) Uani 1 1 d .
C4 C 0.80315(17) 0.14328(19) 0.8770(4) 0.0593(17) Uani 1 1 d .
H4 H 0.7903 0.1218 0.8444 0.071 Uiso 1 1 calc R
C5 C 0.77472(16) 0.17689(17) 0.9086(4) 0.0519(14) Uani 1 1 d .
H5 H 0.7431 0.1778 0.8964 0.062 Uiso 1 1 calc R
C6 C 0.68949(18) 0.34270(16) 1.0075(3) 0.0440(12) Uani 1 1 d .
H6 H 0.6986 0.3465 0.9590 0.053 Uiso 1 1 calc R
C7 C 0.65737(18) 0.37352(16) 1.0370(3) 0.0475(12) Uani 1 1 d .
H7 H 0.6449 0.3974 1.0085 0.057 Uiso 1 1 calc R
C8 C 0.64394(16) 0.36846(14) 1.1094(3) 0.0376(10) Uani 1 1 d .
C9 C 0.66364(19) 0.33300(17) 1.1487(3) 0.0463(12) Uani 1 1 d .
H9 H 0.6552 0.3287 1.1974 0.056 Uiso 1 1 calc R
C10 C 0.69595(18) 0.30356(17) 1.1168(3) 0.0448(12) Uani 1 1 d .
H10 H 0.7098 0.2803 1.1451 0.054 Uiso 1 1 calc R
C11 C 0.6217(6) 0.2602(6) 0.8196(8) 0.50(4) Uani 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 Cu1 N2 93.10(19) 7_657 .
N2 Cu1 N1 177.84(14) 7_657 7_657
N2 Cu1 N1 88.78(13) . 7_657
N2 Cu1 N1 88.78(13) 7_657 .
N2 Cu1 N1 177.84(14) . .
N1 Cu1 N1 89.35(19) 7_657 .
N2 Cu1 O1 90.07(15) 7_657 .
N2 Cu1 O1 89.36(15) . .
N1 Cu1 O1 88.89(15) 7_657 .
N1 Cu1 O1 91.70(15) . .
N2 Cu1 O1 89.36(15) 7_657 7_657
N2 Cu1 O1 90.07(15) . 7_657
N1 Cu1 O1 91.70(15) 7_657 7_657
N1 Cu1 O1 88.89(15) . 7_657
O1 Cu1 O1 179.17(19) . 7_657
O3 S1 O1 120.6(8) . .
O3 S1 O2 106.7(9) . .
O1 S1 O2 108.7(5) . .
O3 S1 C11 105.2(10) . .
O1 S1 C11 107.7(5) . .
O2 S1 C11 107.2(9) . .
S1 O1 Cu1 159.3(3) . .
C5 N1 C1 118.5(3) . .
C5 N1 Cu1 121.1(3) . .
C1 N1 Cu1 120.3(3) . .
C10 N2 C6 118.2(4) . .
C10 N2 Cu1 119.8(3) . .
C6 N2 Cu1 122.0(3) . .
N1 C1 C2 122.3(4) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C1 C2 C3 119.1(4) . .
C1 C2 H2 120.5 . .
C3 C2 H2 120.5 . .
C4 C3 C2 117.8(4) . .
C4 C3 C8 122.4(4) . 30_665
C2 C3 C8 119.8(4) . 30_665
C3 C4 C5 120.7(5) . .
C3 C4 H4 119.6 . .
C5 C4 H4 119.6 . .
N1 C5 C4 121.5(4) . .
N1 C5 H5 119.2 . .
C4 C5 H5 119.2 . .
N2 C6 C7 122.3(4) . .
N2 C6 H6 118.9 . .
C7 C6 H6 118.9 . .
C6 C7 C8 119.4(4) . .
C6 C7 H7 120.3 . .
C8 C7 H7 120.3 . .
C9 C8 C7 117.8(4) . .
C9 C8 C3 121.0(4) . 22_676
C7 C8 C3 121.2(4) . 22_676
C8 C9 C10 120.5(4) . .
C8 C9 H9 119.8 . .
C10 C9 H9 119.8 . .
N2 C10 C9 121.8(5) . .
N2 C10 H10 119.1 . .
C9 C10 H10 119.1 . .
F2 C11 F1 116.8(16) . .
F2 C11 F3 109.4(14) . .
F1 C11 F3 120.1(16) . .
F2 C11 S1 105.8(11) . .
F1 C11 S1 102.5(12) . .
F3 C11 S1 99.0(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 2.022(3) 7_657
Cu1 N2 2.022(3) .
Cu1 N1 2.034(3) 7_657
Cu1 N1 2.034(3) .
Cu1 O1 2.436(4) .
Cu1 O1 2.436(4) 7_657
S1 O3 1.392(10) .
S1 O1 1.421(4) .
S1 O2 1.496(8) .
S1 C11 1.789(17) .
F1 C11 1.362(12) .
F2 C11 1.363(13) .
F3 C11 1.379(15) .
N1 C5 1.343(6) .
N1 C1 1.345(6) .
N2 C10 1.340(6) .
N2 C6 1.339(6) .
C1 C2 1.382(6) .
C1 H1 0.9300 .
C2 C3 1.401(6) .
C2 H2 0.9300 .
C3 C4 1.362(7) .
C3 C8 1.490(5) 30_665
C4 C5 1.384(6) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C7 1.381(6) .
C6 H6 0.9300 .
C7 C8 1.384(7) .
C7 H7 0.9300 .
C8 C9 1.364(7) .
C8 C3 1.490(5) 22_676
C9 C10 1.378(6) .
C9 H9 0.9300 .
C10 H10 0.9300 .
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 0.000 0.250 0.346 442 139 ' '
2 0.000 0.750 0.156 442 139 ' '
3 0.250 0.000 0.531 942 247 ' '
4 0.250 0.500 0.141 942 247 ' '
5 0.500 0.250 0.022 442 139 ' '
6 0.500 0.750 0.975 442 139 ' '
7 0.750 0.000 0.969 942 247 ' '
8 0.750 0.500 0.358 942 247 ' '
