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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/4/10/63/4106366.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_4106366
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           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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            4
_cell_length_a                   16.510(3)
_cell_length_b                   14.417(3)
_cell_length_c                   14.910(3)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     3548.9(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.973
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18472
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        20
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
R values before squeeze:
 R1 =  0.1091 for   2544 Fo > 4sig(Fo)  and  0.1560 for all   4143 data
 wR2 =  0.3581,  GooF = S =   1.122,  Restrained GooF =    1.130  for all data
   208 parameters refined using     24 restraints
;
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4143
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_obs          0.0704
_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)+(0.1082P)²+2.9881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2133
_refine_ls_wR_factor_obs         0.1965
_reflns_number_observed          2501
_reflns_number_total             4143
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja201170c_si_002.cif
_cod_data_source_block           4
_cod_database_code               4106366
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'
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 0.93200(3) -0.2500 0.2500 0.0260(2) Uani 1 2 d S . .
N1 N 1.01818(18) -0.2456(2) 0.3460(2) 0.0269(7) Uani 1 1 d . . .
N2 N 0.84360(19) -0.2497(2) 0.1553(2) 0.0273(7) Uani 1 1 d . . .
C1 C 1.0802(2) -0.1854(3) 0.3394(3) 0.0350(10) Uani 1 1 d . . .
H1 H 1.0805 -0.1435 0.2920 0.042 Uiso 1 1 calc R . .
C2 C 1.1440(2) -0.1833(3) 0.4004(3) 0.0376(10) Uani 1 1 d . . .
H2 H 1.1858 -0.1407 0.3933 0.045 Uiso 1 1 calc R . .
C3 C 1.1452(2) -0.2440(3) 0.4712(3) 0.0297(9) Uani 1 1 d . . .
C4 C 1.0805(3) -0.3062(4) 0.4793(3) 0.0416(12) Uani 1 1 d . . .
H4 H 1.0786 -0.3484 0.5264 0.050 Uiso 1 1 calc R . .
C5 C 1.0189(2) -0.3037(3) 0.4155(3) 0.0368(11) Uani 1 1 d . . .
H5 H 0.9759 -0.3449 0.4218 0.044 Uiso 1 1 calc R . .
C6 C 0.8356(3) -0.3181(3) 0.0952(3) 0.0400(11) Uani 1 1 d . . .
H6 H 0.8744 -0.3649 0.0940 0.048 Uiso 1 1 calc R . .
C7 C 0.7732(3) -0.3222(3) 0.0358(3) 0.0418(11) Uani 1 1 d . . .
H7 H 0.7700 -0.3712 -0.0046 0.050 Uiso 1 1 calc R . .
C8 C 0.7143(2) -0.2536(3) 0.0354(3) 0.0306(9) Uani 1 1 d . . .
C9 C 0.7228(2) -0.1833(3) 0.0976(3) 0.0400(11) Uani 1 1 d . . .
H9 H 0.6844 -0.1361 0.1005 0.048 Uiso 1 1 calc R . .
C10 C 0.7879(3) -0.1830(3) 0.1555(3) 0.0380(11) Uani 1 1 d . . .
H10 H 0.7930 -0.1344 0.1961 0.046 Uiso 1 1 calc R . .
F2 F 0.9302(4) 0.1663(3) 0.3065(5) 0.201(4) Uani 1 1 d D . .
F3 F 0.9263(4) 0.0528(4) 0.3987(3) 0.157(3) Uani 1 1 d D . .
O1 O 0.93512(17) -0.0825(2) 0.25288(19) 0.0404(7) Uani 1 1 d D . .
O3 O 0.9320(3) 0.0423(4) 0.1485(3) 0.117(2) Uani 1 1 d D . .
C11A C 0.9110(6) 0.0775(5) 0.3137(6) 0.118(6) Uani 0.704(6) 1 d PD A 1
S1A S 0.9598(2) 0.00634(14) 0.22829(14) 0.0515(7) Uani 0.704(6) 1 d PD A 1
F1A F 0.8309(4) 0.0681(5) 0.3020(4) 0.119(3) Uani 0.704(6) 1 d PD A 1
O2A O 1.0442(3) 0.0223(5) 0.2409(6) 0.122(4) Uani 0.704(6) 1 d PD A 1
S1B S 0.9132(4) 0.0131(3) 0.2382(3) 0.0438(15) Uani 0.296(6) 1 d PD A 2
F1B F 1.0368(6) 0.0784(12) 0.3295(12) 0.142(7) Uiso 0.296(6) 1 d PD A 2
O2B O 0.8285(5) 0.0242(8) 0.2495(10) 0.063(4) Uiso 0.296(6) 1 d PD A 2
C11B C 0.9579(7) 0.0832(7) 0.3247(7) 0.105(12) Uiso 0.296(6) 1 d PD A 2
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
N1 Cu1 N1 90.41(17) 4_545 .
N1 Cu1 N2 90.77(12) 4_545 .
N1 Cu1 N2 177.79(13) . .
N1 Cu1 N2 177.79(13) 4_545 4_545
N1 Cu1 N2 90.77(12) . 4_545
N2 Cu1 N2 88.11(17) . 4_545
N1 Cu1 O1 86.63(12) 4_545 4_545
N1 Cu1 O1 91.65(12) . 4_545
N2 Cu1 O1 90.29(12) . 4_545
N2 Cu1 O1 91.47(12) 4_545 4_545
N1 Cu1 O1 91.65(12) 4_545 .
N1 Cu1 O1 86.63(12) . .
N2 Cu1 O1 91.47(12) . .
N2 Cu1 O1 90.29(12) 4_545 .
O1 Cu1 O1 177.56(13) 4_545 .
C5 N1 C1 117.1(3) . .
C5 N1 Cu1 122.6(3) . .
C1 N1 Cu1 120.2(3) . .
C10 N2 C6 117.7(3) . .
C10 N2 Cu1 119.8(3) . .
C6 N2 Cu1 122.3(3) . .
N1 C1 C2 122.8(4) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C3 C2 C1 120.0(4) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C2 C3 C4 117.7(4) . .
C2 C3 C8 121.3(4) . 7_656
C4 C3 C8 121.0(4) . 7_656
C5 C4 C3 118.8(4) . .
C5 C4 H4 120.6 . .
C3 C4 H4 120.6 . .
N1 C5 C4 123.6(4) . .
N1 C5 H5 118.2 . .
C4 C5 H5 118.2 . .
N2 C6 C7 122.9(4) . .
N2 C6 H6 118.6 . .
C7 C6 H6 118.6 . .
C6 C7 C8 120.2(4) . .
C6 C7 H7 119.9 . .
C8 C7 H7 119.9 . .
C9 C8 C7 116.7(4) . .
C9 C8 C3 121.8(4) . 7
C7 C8 C3 121.6(4) . 7
C10 C9 C8 120.2(4) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
N2 C10 C9 122.4(4) . .
N2 C10 H10 118.8 . .
C9 C10 H10 118.8 . .
C11B F2 C11A 35.1(7) . .
C11B F3 C11A 35.0(7) . .
S1A O1 S1B 32.3(2) . .
S1A O1 Cu1 157.0(2) . .
S1B O1 Cu1 161.3(3) . .
S1A O3 S1B 32.6(2) . .
F2 C11A F1A 108.9(7) . .
F2 C11A F3 106.7(7) . .
F1A C11A F3 106.4(7) . .
F2 C11A S1A 112.5(6) . .
F1A C11A S1A 106.8(6) . .
F3 C11A S1A 115.3(6) . .
O3 S1A O1 118.4(4) . .
O3 S1A O2A 112.3(4) . .
O1 S1A O2A 113.6(3) . .
O3 S1A C11A 104.1(4) . .
O1 S1A C11A 101.8(3) . .
O2A S1A C11A 104.4(5) . .
O2B S1B O3 107.0(7) . .
O2B S1B O1 109.7(5) . .
O3 S1B O1 111.6(4) . .
O2B S1B C11B 104.8(8) . .
O3 S1B C11B 114.5(5) . .
O1 S1B C11B 109.0(4) . .
F3 C11B F1B 109.6(9) . .
F3 C11B F2 110.2(9) . .
F1B C11B F2 114.1(9) . .
F3 C11B S1B 104.9(7) . .
F1B C11B S1B 114.8(12) . .
F2 C11B S1B 102.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.019(3) 4_545
Cu1 N1 2.019(3) .
Cu1 N2 2.031(3) .
Cu1 N2 2.031(3) 4_545
Cu1 O1 2.416(3) 4_545
Cu1 O1 2.416(3) .
N1 C5 1.332(5) .
N1 C1 1.346(5) .
N2 C10 1.331(5) .
N2 C6 1.339(5) .
C1 C2 1.392(5) .
C1 H1 0.9300 .
C2 C3 1.371(6) .
C2 H2 0.9300 .
C3 C4 1.400(6) .
C3 C8 1.489(5) 7_656
C4 C5 1.392(5) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C7 1.359(6) .
C6 H6 0.9300 .
C7 C8 1.387(6) .
C7 H7 0.9300 .
C8 C9 1.381(6) .
C8 C3 1.489(5) 7
C9 C10 1.378(5) .
C9 H9 0.9300 .
C10 H10 0.9300 .
F2 C11B 1.311(9) .
F2 C11A 1.323(7) .
F3 C11B 1.297(9) .
F3 C11A 1.341(8) .
O1 S1A 1.393(4) .
O1 S1B 1.441(5) .
O3 S1A 1.377(4) .
O3 S1B 1.436(6) .
C11A F1A 1.341(9) .
C11A S1A 1.823(7) .
S1A O2A 1.425(6) .
S1B O2B 1.418(8) .
S1B C11B 1.797(9) .
F1B C11B 1.308(9) .
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 0.250 -0.001 0.250 498 152 ' '
2 0.750 0.001 -0.250 497 152 ' '
