#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:03:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178766 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102068.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_4102068
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 H4 Cu2 O11 S'
_chemical_formula_weight         434.27
_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
;
2009-11-02 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.502(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.355(4)
_cell_length_b                   18.215(9)
_cell_length_c                   10.152(5)
_cell_measurement_reflns_used    13672
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      33.7
_cell_measurement_theta_min      3.6
_cell_volume                     1355.9(12)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEXII (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'Diamond 2.1a (Brandenberg, 1999)'
_computing_publication_material  'SHELX97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare  et. al. , 1999)'
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean -
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker AXS APEXII'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  'Si(111) Crystal'
_diffrn_radiation_source         '11.3.1 ALS, LBNL. CA'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13672
_diffrn_reflns_theta_full        33.70
_diffrn_reflns_theta_max         33.70
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    3.346
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.127
_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          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_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          0.1487
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                3578
_reflns_number_total             4101
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4102067
_cod_data_source_file            ja910600b_240K.cif
_cod_data_source_block           test
_cod_original_cell_volume        1356.0(12)
_cod_database_code               4102068
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 0.13343(5) 0.093357(19) 0.78233(3) 0.01738(13) Uani 1 1 d . . .
Cu2 Cu -0.04923(5) 0.068478(18) 1.06565(3) 0.01539(13) Uani 1 1 d . . .
S3 S 0.11542(10) 0.43386(4) 1.30646(7) 0.01795(17) Uani 1 1 d . . .
O1 O 0.0466(3) 0.16771(11) 1.0844(2) 0.0224(4) Uani 1 1 d . . .
O2 O 0.1312(3) 0.03516(11) 0.94523(19) 0.0150(4) Uani 1 1 d . . .
O3 O 0.1610(3) 0.01109(12) 0.6649(2) 0.0256(5) Uani 1 1 d . . .
O4 O 0.1153(3) 0.18521(12) 0.8738(2) 0.0239(5) Uani 1 1 d . . .
O5 O 0.1128(4) 0.51284(15) 1.2943(3) 0.0397(7) Uani 1 1 d . . .
O6 O -0.1992(4) 0.09033(12) 1.2069(2) 0.0238(5) Uani 1 1 d . . .
O7 O -0.2222(4) 0.09414(16) 0.8811(3) 0.0358(6) Uani 1 1 d . . .
O8 O -0.0487(3) 0.40326(15) 1.3576(2) 0.0283(5) Uani 1 1 d . . .
C1 C 0.1312(4) 0.39512(15) 1.1483(3) 0.0177(5) Uani 1 1 d . . .
C2 C 0.2221(4) 0.40357(15) 0.9265(3) 0.0180(5) Uani 1 1 d . . .
C3 C 0.1896(4) 0.32843(15) 0.9111(3) 0.0193(5) Uani 1 1 d . . .
H3 H 0.2108 0.3058 0.8316 0.023 Uiso 1 1 calc R . .
C4 C 0.1259(4) 0.28681(15) 1.0131(3) 0.0179(5) Uani 1 1 d . . .
C5 C 0.0929(4) 0.20663(15) 0.9892(3) 0.0178(5) Uani 1 1 d . . .
C6 C 0.0950(4) 0.32021(15) 1.1325(3) 0.0180(5) Uani 1 1 d . . .
H6 H 0.0510 0.2931 1.2008 0.022 Uiso 1 1 calc R . .
C7 C 0.1924(4) 0.43709(15) 1.0468(3) 0.0199(6) Uani 1 1 d . . .
H7 H 0.2135 0.4871 1.0586 0.024 Uiso 1 1 calc R . .
C8 C 0.2074(4) -0.05491(16) 0.6855(3) 0.0180(5) Uani 1 1 d . . .
O9W O 0.1122(4) 0.15241(13) 0.6201(2) 0.0324(6) Uani 1 1 d . . .
O10W O 0.0385(5) 0.29967(17) 0.5834(3) 0.0539(9) Uani 1 1 d . . .
O11W O 0.2080(5) 0.1276(2) 0.3603(3) 0.0548(9) Uani 1 1 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'
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 170.27(10) . . ?
O4 Cu1 O9W 85.68(10) . . ?
O3 Cu1 O9W 85.00(10) . . ?
O4 Cu1 O2 93.28(9) . . ?
O3 Cu1 O2 96.25(10) . . ?
O9W Cu1 O2 174.91(10) . . ?
O4 Cu1 O8 85.81(10) . 4_665 ?
O3 Cu1 O8 93.98(10) . 4_665 ?
O9W Cu1 O8 105.32(11) . 4_665 ?
O2 Cu1 O8 79.55(8) . 4_665 ?
O6 Cu2 O1 87.66(10) . . ?
O6 Cu2 O2 169.43(9) . . ?
O1 Cu2 O2 95.20(9) . . ?
O6 Cu2 O2 92.81(9) . 3_557 ?
O1 Cu2 O2 175.82(9) . 3_557 ?
O2 Cu2 O2 83.60(9) . 3_557 ?
O6 Cu2 O7 105.12(12) . . ?
O1 Cu2 O7 93.77(10) . . ?
O2 Cu2 O7 84.88(11) . . ?
O2 Cu2 O7 90.11(9) 3_557 . ?
O6 Cu2 Cu2 133.65(7) . 3_557 ?
O1 Cu2 Cu2 137.03(7) . 3_557 ?
O2 Cu2 Cu2 41.97(6) . 3_557 ?
O2 Cu2 Cu2 41.64(6) 3_557 3_557 ?
O7 Cu2 Cu2 86.66(9) . 3_557 ?
O5 S3 O7 113.47(18) . 4_666 ?
O5 S3 O8 113.87(17) . . ?
O7 S3 O8 110.38(17) 4_666 . ?
O5 S3 C1 108.77(15) . . ?
O7 S3 C1 102.93(15) 4_666 . ?
O8 S3 C1 106.59(14) . . ?
C5 O1 Cu2 124.26(19) . . ?
Cu1 O2 Cu2 114.00(10) . . ?
Cu1 O2 Cu2 119.30(10) . 3_557 ?
Cu2 O2 Cu2 96.40(8) . 3_557 ?
C8 O3 Cu1 132.5(2) . . ?
C5 O4 Cu1 137.6(2) . . ?
C8 O6 Cu2 127.2(2) 3_557 . ?
S3 O7 Cu2 138.99(16) 4_565 . ?
S3 O8 Cu1 133.43(16) . 4_566 ?
C7 C1 C6 121.6(3) . . ?
C7 C1 S3 120.3(2) . . ?
C6 C1 S3 118.0(2) . . ?
C3 C2 C7 119.3(3) . . ?
C3 C2 C8 118.6(3) . 2_556 ?
C7 C2 C8 122.1(3) . 2_556 ?
C4 C3 C2 121.0(3) . . ?
C6 C4 C3 119.8(3) . . ?
C6 C4 C5 122.2(2) . . ?
C3 C4 C5 118.0(2) . . ?
O4 C5 O1 126.8(3) . . ?
O4 C5 C4 115.0(2) . . ?
O1 C5 C4 118.2(2) . . ?
C4 C6 C1 119.0(2) . . ?
C1 C7 C2 119.4(3) . . ?
O3 C8 O6 126.4(3) . 3_557 ?
O3 C8 C2 117.5(3) . 2_546 ?
O6 C8 C2 116.1(3) 3_557 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 1.923(2) . ?
Cu1 O3 1.935(2) . ?
Cu1 O9W 1.963(2) . ?
Cu1 O2 1.966(2) . ?
Cu1 O8 2.403(3) 4_665 ?
Cu2 O6 1.918(2) . ?
Cu2 O1 1.944(2) . ?
Cu2 O2 1.969(2) . ?
Cu2 O2 1.982(2) 3_557 ?
Cu2 O7 2.230(3) . ?
Cu2 Cu2 2.9456(13) 3_557 ?
S3 O5 1.444(3) . ?
S3 O7 1.456(3) 4_666 ?
S3 O8 1.461(3) . ?
S3 C1 1.766(3) . ?
O1 C5 1.267(3) . ?
O2 Cu2 1.982(2) 3_557 ?
O3 C8 1.263(4) . ?
O4 C5 1.258(3) . ?
O6 C8 1.274(4) 3_557 ?
O7 S3 1.456(3) 4_565 ?
O8 Cu1 2.403(3) 4_566 ?
C1 C7 1.386(4) . ?
C1 C6 1.397(4) . ?
C2 C3 1.396(4) . ?
C2 C7 1.397(4) . ?
C2 C8 1.492(4) 2_556 ?
C3 C4 1.394(4) . ?
C4 C6 1.391(4) . ?
C4 C5 1.497(4) . ?
C8 O6 1.274(4) 3_557 ?
C8 C2 1.492(4) 2_546 ?
