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#$Date: 2016-03-21 17:03:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178766 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102076.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_4102076
loop_
_publ_author_name
'Phoebe K. Allan'
'Bo Xiao'
'Simon J. Teat'
'Jason W. Knight'
'Russell E. Morris'
_publ_section_title
;
 In Situ Single-Crystal Diffraction Studies of the Structural Transition
 of Metal-Organic Framework Copper 5-Sulfoisophthalate, Cu-SIP-3
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3605
_journal_page_last               3611
_journal_paper_doi               10.1021/ja910600b
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C8 H3 Cu2 O10.72 S'
_chemical_formula_weight         429.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-09-25 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.337(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3354(19)
_cell_length_b                   18.140(4)
_cell_length_c                   10.179(3)
_cell_measurement_reflns_used    8632
_cell_measurement_temperature    325(2)
_cell_measurement_theta_max      33.1
_cell_measurement_theta_min      3.3
_cell_volume                     1350.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      325(2)
_diffrn_detector_area_resol_mean -
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS APEXII'
_diffrn_measurement_method       -
_diffrn_radiation_monochromator  'Si(111) crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8632
_diffrn_reflns_theta_full        31.32
_diffrn_reflns_theta_max         31.32
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    3.359
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Block, well formed'
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.895
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          8.098
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                2723
_reflns_number_total             3412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910600b_315K.cif
_cod_data_source_block           als47_2_3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4102076
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.13457(8) 0.09449(3) 0.78304(5) 0.02738(18) Uani 1 1 d . . .
Cu2 Cu -0.04321(7) 0.06850(3) 1.06845(5) 0.02700(18) Uani 1 1 d . . .
S3 S 0.12060(15) 0.43463(7) 1.30905(11) 0.0290(3) Uani 1 1 d . . .
O1 O 0.0526(5) 0.16804(18) 1.0856(3) 0.0361(8) Uani 1 1 d . . .
O2 O 0.1294(4) 0.03479(17) 0.9426(3) 0.0245(6) Uani 1 1 d . . .
O3 O 0.1588(5) 0.01353(19) 0.6633(3) 0.0386(8) Uani 1 1 d . . .
O4 O 0.1188(5) 0.18607(18) 0.8748(3) 0.0370(8) Uani 1 1 d . . .
O5 O 0.1297(8) 0.5128(3) 1.2981(4) 0.0720(16) Uani 1 1 d . . .
O6 O -0.1856(6) 0.0896(2) 1.2141(4) 0.0426(9) Uani 1 1 d . . .
O7 O -0.2263(6) 0.0973(3) 0.8879(4) 0.0551(12) Uani 1 1 d . . .
O8 O -0.0492(5) 0.4073(3) 1.3549(4) 0.0538(12) Uani 1 1 d . . .
C1 C 0.1385(6) 0.3959(2) 1.1504(4) 0.0275(9) Uani 1 1 d . . .
C2 C 0.2290(6) 0.4050(2) 0.9309(5) 0.0287(9) Uani 1 1 d . . .
C3 C 0.1964(6) 0.3300(2) 0.9139(4) 0.0314(10) Uani 1 1 d . . .
H3 H 0.2176 0.3077 0.8341 0.038 Uiso 1 1 calc R . .
C4 C 0.1321(6) 0.2876(2) 1.0152(4) 0.0281(9) Uani 1 1 d . . .
C5 C 0.0980(6) 0.2071(2) 0.9909(4) 0.0286(9) Uani 1 1 d . . .
C6 C 0.1040(6) 0.3208(3) 1.1349(4) 0.0302(9) Uani 1 1 d . . .
H6 H 0.0627 0.2932 1.2038 0.036 Uiso 1 1 calc R . .
C7 C 0.1991(6) 0.4387(2) 1.0496(4) 0.0292(9) Uani 1 1 d . . .
H7 H 0.2194 0.4889 1.0614 0.035 Uiso 1 1 calc R . .
C8 C 0.1987(6) -0.0534(3) 0.6821(5) 0.0302(9) Uani 1 1 d . . .
O9W O 0.1181(7) 0.1556(2) 0.6226(4) 0.0592(17) Uani 1.000(15) 1 d . . .
O10W O 0.0392(9) 0.3010(3) 0.5870(6) 0.089(3) Uani 0.985(18) 1 d P . .
O11W O 0.2147(11) 0.1337(5) 0.3639(7) 0.082(3) Uani 0.732(18) 1 d P . .
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'
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'
Cu Cu 0.3201 1.2651 '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
_geom_angle_publ_flag
O4 Cu1 O3 169.46(15) . . ?
O4 Cu1 O2 93.99(13) . . ?
O3 Cu1 O2 96.42(14) . . ?
O4 Cu1 O9W 85.06(16) . . ?
O3 Cu1 O9W 84.70(17) . . ?
O2 Cu1 O9W 175.33(17) . . ?
O4 Cu1 O8 87.41(17) . 4_665 ?
O3 Cu1 O8 92.86(17) . 4_665 ?
O2 Cu1 O8 79.45(13) . 4_665 ?
O9W Cu1 O8 105.05(18) . 4_665 ?
O6 Cu2 O1 87.65(15) . . ?
O6 Cu2 O2 169.23(16) . . ?
O1 Cu2 O2 95.84(14) . . ?
O6 Cu2 O2 92.46(14) . 3_557 ?
O1 Cu2 O2 176.87(14) . 3_557 ?
O2 Cu2 O2 83.51(12) . 3_557 ?
O6 Cu2 O7 105.00(19) . . ?
O1 Cu2 O7 92.71(16) . . ?
O2 Cu2 O7 85.06(16) . . ?
O2 Cu2 O7 90.28(14) 3_557 . ?
O6 Cu2 Cu2 133.25(11) . 3_557 ?
O1 Cu2 Cu2 137.67(11) . 3_557 ?
O2 Cu2 Cu2 41.92(9) . 3_557 ?
O2 Cu2 Cu2 41.60(8) 3_557 3_557 ?
O7 Cu2 Cu2 86.89(14) . 3_557 ?
O5 S3 O8 114.3(3) . . ?
O5 S3 O7 113.7(3) . 4_666 ?
O8 S3 O7 109.5(3) . 4_666 ?
O5 S3 C1 108.4(2) . . ?
O8 S3 C1 106.4(2) . . ?
O7 S3 C1 103.8(2) 4_666 . ?
C5 O1 Cu2 124.7(3) . . ?
Cu1 O2 Cu2 115.04(15) . . ?
Cu1 O2 Cu2 120.25(15) . 3_557 ?
Cu2 O2 Cu2 96.49(12) . 3_557 ?
C8 O3 Cu1 132.1(3) . . ?
C5 O4 Cu1 137.4(3) . . ?
C8 O6 Cu2 128.9(3) 3_557 . ?
S3 O7 Cu2 138.4(3) 4_565 . ?
S3 O8 Cu1 138.3(3) . 4_566 ?
C7 C1 C6 122.0(4) . . ?
C7 C1 S3 120.1(3) . . ?
C6 C1 S3 117.7(3) . . ?
C7 C2 C3 120.2(4) . . ?
C7 C2 C8 122.3(4) . 2_556 ?
C3 C2 C8 117.5(4) . 2_556 ?
C2 C3 C4 120.8(4) . . ?
C6 C4 C3 119.3(4) . . ?
C6 C4 C5 122.2(4) . . ?
C3 C4 C5 118.4(4) . . ?
O4 C5 O1 127.1(4) . . ?
O4 C5 C4 114.8(4) . . ?
O1 C5 C4 118.1(4) . . ?
C4 C6 C1 119.1(4) . . ?
C1 C7 C2 118.6(4) . . ?
O6 C8 O3 126.9(4) 3_557 . ?
O6 C8 C2 115.8(4) 3_557 2_546 ?
O3 C8 C2 117.3(4) . 2_546 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O4 1.914(3) . ?
Cu1 O3 1.925(3) . ?
Cu1 O2 1.955(3) . ?
Cu1 O9W 1.970(4) . ?
Cu1 O8 2.379(4) 4_665 ?
Cu2 O6 1.916(3) . ?
Cu2 O1 1.941(3) . ?
Cu2 O2 1.966(3) . ?
Cu2 O2 1.978(3) 3_557 ?
Cu2 O7 2.254(4) . ?
Cu2 Cu2 2.9417(12) 3_557 ?
S3 O5 1.425(5) . ?
S3 O8 1.450(4) . ?
S3 O7 1.451(4) 4_666 ?
S3 C1 1.775(4) . ?
O1 C5 1.262(5) . ?
O2 Cu2 1.978(3) 3_557 ?
O3 C8 1.260(6) . ?
O4 C5 1.262(5) . ?
O6 C8 1.253(6) 3_557 ?
O7 S3 1.451(4) 4_565 ?
O8 Cu1 2.379(4) 4_566 ?
C1 C7 1.386(6) . ?
C1 C6 1.392(6) . ?
C2 C7 1.386(6) . ?
C2 C3 1.391(6) . ?
C2 C8 1.505(6) 2_556 ?
C3 C4 1.396(6) . ?
C4 C6 1.389(6) . ?
C4 C5 1.498(6) . ?
C8 O6 1.253(6) 3_557 ?
C8 C2 1.505(6) 2_546 ?
