#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:03:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178766 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102077.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_4102077
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         428.83
_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
;
2009-10-29 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.307(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.301(8)
_cell_length_b                   18.032(19)
_cell_length_c                   10.133(11)
_cell_measurement_reflns_used    8055
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      3.3
_cell_volume                     1330(2)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'ApexII (Brucker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'Diamond 2.1a (Brandenberg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare  et. al. , 1999)'
_diffrn_ambient_temperature      320(2)
_diffrn_detector_area_resol_mean -
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8055
_diffrn_reflns_theta_full        31.46
_diffrn_reflns_theta_max         31.46
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    3.411
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.168
_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         1.374
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0605
_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          0.1652
_refine_ls_wR_factor_ref         0.1896
_reflns_number_gt                2226
_reflns_number_total             3232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910600b_320K.cif
_cod_data_source_block           als47_4_5
_cod_database_code               4102077
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 0.13493(11) 0.09464(4) 0.78361(7) 0.0289(2) Uani 1 1 d . . .
Cu2 Cu -0.04131(12) 0.06848(4) 1.06952(7) 0.0295(2) Uani 1 1 d . . .
S3 S 0.1223(2) 0.43484(9) 1.30927(15) 0.0313(4) Uani 1 1 d . . .
O1 O 0.0538(8) 0.1684(2) 1.0852(4) 0.0390(12) Uani 1 1 d . . .
O2 O 0.1291(6) 0.0350(2) 0.9434(4) 0.0270(9) Uani 1 1 d . . .
O3 O 0.1587(8) 0.0137(3) 0.6632(5) 0.0418(12) Uani 1 1 d . . .
O4 O 0.1199(7) 0.1862(2) 0.8752(4) 0.0378(12) Uani 1 1 d . . .
O5 O 0.1340(12) 0.5124(3) 1.3002(6) 0.083(3) Uani 1 1 d . . .
O6 O -0.1823(9) 0.0895(3) 1.2164(5) 0.0455(13) Uani 1 1 d . . .
O7 O -0.2270(9) 0.0980(3) 0.8887(6) 0.0587(17) Uani 1 1 d . . .
O8 O -0.0479(8) 0.4082(4) 1.3533(6) 0.0578(16) Uani 1 1 d . . .
C1 C 0.1409(9) 0.3963(3) 1.1496(6) 0.0289(13) Uani 1 1 d . . .
C2 C 0.2299(9) 0.4046(3) 0.9303(6) 0.0292(13) Uani 1 1 d . . .
C3 C 0.1971(10) 0.3304(3) 0.9145(6) 0.0316(14) Uani 1 1 d . . .
H3 H 0.2173 0.3080 0.8342 0.038 Uiso 1 1 calc R . .
C4 C 0.1349(10) 0.2879(3) 1.0151(6) 0.0330(14) Uani 1 1 d . . .
C5 C 0.0989(10) 0.2070(3) 0.9911(6) 0.0315(14) Uani 1 1 d . . .
C6 C 0.1037(10) 0.3205(3) 1.1344(6) 0.0327(14) Uani 1 1 d . . .
H6 H 0.0592 0.2930 1.2028 0.039 Uiso 1 1 calc R . .
C7 C 0.2024(10) 0.4383(3) 1.0515(6) 0.0311(14) Uani 1 1 d . . .
H7 H 0.2259 0.4886 1.0644 0.037 Uiso 1 1 calc R . .
C8 C 0.1975(10) -0.0527(3) 0.6803(7) 0.0329(14) Uani 1 1 d . . .
O9W O 0.1193(9) 0.1562(3) 0.6237(5) 0.0480(14) Uani 1 1 d . . .
O10W O 0.0385(13) 0.3011(4) 0.5874(8) 0.092(4) Uani 0.98(2) 1 d P . .
O11W O 0.2156(18) 0.1336(8) 0.3670(10) 0.095(6) Uani 0.68(2) 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 169.2(2) . . ?
O4 Cu1 O2 93.91(19) . . ?
O3 Cu1 O2 96.7(2) . . ?
O4 Cu1 O9W 84.8(2) . . ?
O3 Cu1 O9W 84.7(2) . . ?
O2 Cu1 O9W 175.3(2) . . ?
O4 Cu1 O8 88.0(2) . 4_665 ?
O3 Cu1 O8 92.3(2) . 4_665 ?
O2 Cu1 O8 79.75(19) . 4_665 ?
O9W Cu1 O8 104.7(2) . 4_665 ?
O6 Cu2 O1 87.8(2) . . ?
O6 Cu2 O2 169.2(2) . . ?
O1 Cu2 O2 95.7(2) . . ?
O6 Cu2 O2 92.76(19) . 3_557 ?
O1 Cu2 O2 177.7(2) . 3_557 ?
O2 Cu2 O2 83.31(18) . 3_557 ?
O6 Cu2 O7 105.0(3) . . ?
O1 Cu2 O7 92.1(2) . . ?
O2 Cu2 O7 85.1(2) . . ?
O2 Cu2 O7 89.83(19) 3_557 . ?
O6 Cu2 Cu2 133.23(15) . 3_557 ?
O1 Cu2 Cu2 137.73(16) . 3_557 ?
O2 Cu2 Cu2 42.02(12) . 3_557 ?
O2 Cu2 Cu2 41.28(13) 3_557 3_557 ?
O7 Cu2 Cu2 86.63(19) . 3_557 ?
O5 S3 O8 114.3(4) . . ?
O5 S3 O7 113.5(4) . 4_666 ?
O8 S3 O7 109.4(4) . 4_666 ?
O5 S3 C1 108.7(3) . . ?
O8 S3 C1 106.3(3) . . ?
O7 S3 C1 103.9(3) 4_666 . ?
C5 O1 Cu2 124.9(4) . . ?
Cu2 O2 Cu1 115.5(2) . . ?
Cu2 O2 Cu2 96.69(18) . 3_557 ?
Cu1 O2 Cu2 119.6(2) . 3_557 ?
C8 O3 Cu1 132.6(5) . . ?
C5 O4 Cu1 137.1(4) . . ?
C8 O6 Cu2 129.3(5) 3_557 . ?
S3 O7 Cu2 138.0(3) 4_565 . ?
S3 O8 Cu1 139.8(4) . 4_566 ?
C7 C1 C6 122.6(6) . . ?
C7 C1 S3 120.2(5) . . ?
C6 C1 S3 117.0(5) . . ?
C3 C2 C7 119.5(5) . . ?
C3 C2 C8 119.1(5) . 2_556 ?
C7 C2 C8 121.3(6) . 2_556 ?
C2 C3 C4 121.5(6) . . ?
C6 C4 C3 119.7(6) . . ?
C6 C4 C5 121.3(5) . . ?
C3 C4 C5 119.0(5) . . ?
O1 C5 O4 127.6(6) . . ?
O1 C5 C4 118.2(5) . . ?
O4 C5 C4 114.2(5) . . ?
C4 C6 C1 118.0(6) . . ?
C1 C7 C2 118.7(6) . . ?
O3 C8 O6 126.6(6) . 3_557 ?
O3 C8 C2 119.0(6) . 2_546 ?
O6 C8 C2 114.5(6) 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 1.902(5) . ?
Cu1 O3 1.919(5) . ?
Cu1 O2 1.947(4) . ?
Cu1 O9W 1.960(5) . ?
Cu1 O8 2.370(6) 4_665 ?
Cu2 O6 1.910(5) . ?
Cu2 O1 1.933(5) . ?
Cu2 O2 1.945(4) . ?
Cu2 O2 1.974(4) 3_557 ?
Cu2 O7 2.260(6) . ?
Cu2 Cu2 2.928(3) 3_557 ?
S3 O5 1.405(6) . ?
S3 O8 1.434(6) . ?
S3 O7 1.441(6) 4_666 ?
S3 C1 1.776(6) . ?
O1 C5 1.245(7) . ?
O2 Cu2 1.974(4) 3_557 ?
O3 C8 1.239(8) . ?
O4 C5 1.252(8) . ?
O6 C8 1.251(8) 3_557 ?
O7 S3 1.441(6) 4_565 ?
O8 Cu1 2.370(6) 4_566 ?
C1 C7 1.353(8) . ?
C1 C6 1.399(8) . ?
C2 C3 1.367(8) . ?
C2 C7 1.398(8) . ?
C2 C8 1.489(8) 2_556 ?
C3 C4 1.379(8) . ?
C4 C6 1.380(9) . ?
C4 C5 1.499(9) . ?
C8 O6 1.251(8) 3_557 ?
C8 C2 1.489(8) 2_546 ?
