#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:03:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178766 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102081.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_4102081
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         425.15
_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                 94.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.302(13)
_cell_length_b                   18.15(3)
_cell_length_c                   10.267(18)
_cell_measurement_reflns_used    7803
_cell_measurement_temperature    340(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      3.0
_cell_volume                     1357(4)
_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      293(2)
_diffrn_detector_area_resol_mean -
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7803
_diffrn_reflns_theta_full        28.68
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    3.343
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.125
_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         2.927
_refine_diff_density_min         -4.081
_refine_diff_density_rms         0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.958
_refine_ls_R_factor_all          0.2036
_refine_ls_R_factor_gt           0.1235
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.003
_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          0.3049
_refine_ls_wR_factor_ref         0.3754
_reflns_number_gt                1672
_reflns_number_total             3265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910600b_340K.cif
_cod_data_source_block           als47_8_9
_cod_database_code               4102081
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 0.1359(3) 0.09474(8) 0.7850(2) 0.0445(6) Uani 1 1 d . . .
Cu2 Cu -0.0375(3) 0.06834(8) 1.0708(2) 0.0487(7) Uani 1 1 d . . .
S3 S 0.1267(5) 0.43500(18) 1.3093(5) 0.0472(11) Uani 1 1 d . . .
O1 O 0.0590(16) 0.1682(5) 1.0844(12) 0.055(3) Uani 1 1 d . . .
O2 O 0.1297(12) 0.0343(4) 0.9446(11) 0.036(2) Uani 1 1 d . . .
O3 O 0.1552(16) 0.0145(5) 0.6602(15) 0.063(4) Uani 1 1 d . . .
O4 O 0.1216(17) 0.1866(5) 0.8742(11) 0.050(3) Uani 1 1 d . . .
O5 O 0.148(3) 0.5128(6) 1.2988(18) 0.112(7) Uani 1 1 d . . .
O6 O -0.173(2) 0.0896(5) 1.2225(16) 0.074(4) Uani 1 1 d . . .
O7 O -0.2257(18) 0.0990(7) 0.8906(17) 0.079(5) Uani 1 1 d . . .
O8 O -0.0467(17) 0.4100(10) 1.356(2) 0.105(7) Uani 1 1 d . . .
C1 C 0.145(2) 0.3964(7) 1.1486(15) 0.039(3) Uani 1 1 d . . .
C2 C 0.235(2) 0.4055(7) 0.933(2) 0.062(6) Uani 1 1 d . . .
C3 C 0.201(2) 0.3310(6) 0.912(2) 0.055(5) Uani 1 1 d . . .
H3 H 0.2192 0.3096 0.8320 0.066 Uiso 1 1 calc R . .
C4 C 0.139(2) 0.2885(6) 1.0149(17) 0.043(4) Uani 1 1 d . . .
C5 C 0.104(2) 0.2070(6) 0.9954(17) 0.042(4) Uani 1 1 d . . .
C6 C 0.107(2) 0.3208(7) 1.1308(19) 0.049(4) Uani 1 1 d . . .
H6 H 0.0598 0.2934 1.1973 0.058 Uiso 1 1 calc R . .
C7 C 0.205(2) 0.4388(7) 1.044(2) 0.052(5) Uani 1 1 d . . .
H7 H 0.2230 0.4893 1.0537 0.062 Uiso 1 1 calc R . .
C8 C 0.195(2) -0.0533(7) 0.685(2) 0.051(5) Uani 1 1 d . . .
O9W O 0.1228(18) 0.1556(6) 0.6166(12) 0.057(3) Uani 1 1 d . . .
O10W O 0.047(3) 0.2998(10) 0.5799(19) 0.109(10) Uani 0.93(5) 1 d P . .
O11W O 0.206(6) 0.134(3) 0.362(3) 0.13(2) Uani 0.50(5) 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 167.4(5) . . ?
O4 Cu1 O2 94.7(4) . . ?
O3 Cu1 O2 97.9(5) . . ?
O4 Cu1 O9W 86.1(5) . . ?
O3 Cu1 O9W 81.3(5) . . ?
O2 Cu1 O9W 175.9(5) . . ?
O4 Cu1 O8 88.3(6) . 4_665 ?
O3 Cu1 O8 93.4(6) . 4_665 ?
O2 Cu1 O8 78.8(5) . 4_665 ?
O9W Cu1 O8 105.3(6) . 4_665 ?
O2 Cu2 O6 167.9(5) . . ?
O2 Cu2 O1 95.9(5) . . ?
O6 Cu2 O1 87.7(5) . . ?
O2 Cu2 O2 82.8(4) . 3_557 ?
O6 Cu2 O2 93.5(4) . 3_557 ?
O1 Cu2 O2 178.5(4) . 3_557 ?
O2 Cu2 O7 84.7(5) . . ?
O6 Cu2 O7 106.8(6) . . ?
O1 Cu2 O7 91.5(5) . . ?
O2 Cu2 O7 89.0(4) 3_557 . ?
O2 Cu2 Cu2 41.9(2) . 3_557 ?
O6 Cu2 Cu2 133.3(3) . 3_557 ?
O1 Cu2 Cu2 137.8(4) . 3_557 ?
O2 Cu2 Cu2 40.8(3) 3_557 3_557 ?
O7 Cu2 Cu2 85.9(4) . 3_557 ?
O5 S3 O7 112.4(10) . 4_666 ?
O5 S3 O8 115.9(10) . . ?
O7 S3 O8 107.9(11) 4_666 . ?
O5 S3 C1 107.4(9) . . ?
O7 S3 C1 105.1(9) 4_666 . ?
O8 S3 C1 107.5(10) . . ?
C5 O1 Cu2 126.9(11) . . ?
Cu2 O2 Cu1 115.4(4) . . ?
Cu2 O2 Cu2 97.2(4) . 3_557 ?
Cu1 O2 Cu2 118.9(5) . 3_557 ?
C8 O3 Cu1 127.6(14) . . ?
C5 O4 Cu1 135.5(8) . . ?
C8 O6 Cu2 130.0(10) 3_557 . ?
S3 O7 Cu2 137.6(8) 4_565 . ?
S3 O8 Cu1 139.6(14) . 4_566 ?
C7 C1 C6 120.1(15) . . ?
C7 C1 S3 121.8(11) . . ?
C6 C1 S3 118.0(12) . . ?
C7 C2 C3 122.7(18) . . ?
C7 C2 C8 122.7(12) . 2_556 ?
C3 C2 C8 114.6(19) . 2_556 ?
C2 C3 C4 118.8(18) . . ?
C6 C4 C3 120.2(12) . . ?
C6 C4 C5 119.9(14) . . ?
C3 C4 C5 119.9(14) . . ?
O1 C5 O4 126.8(12) . . ?
O1 C5 C4 121.2(15) . . ?
O4 C5 C4 112.0(12) . . ?
C4 C6 C1 119.1(15) . . ?
C2 C7 C1 118.8(13) . . ?
O6 C8 O3 130.8(17) 3_557 . ?
O6 C8 C2 115.8(13) 3_557 2_546 ?
O3 C8 C2 113.1(17) . 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 1.909(10) . ?
Cu1 O3 1.952(12) . ?
Cu1 O2 1.975(10) . ?
Cu1 O9W 2.048(12) . ?
Cu1 O8 2.381(15) 4_665 ?
Cu2 O2 1.942(10) . ?
Cu2 O6 1.940(14) . ?
Cu2 O1 1.947(9) . ?
Cu2 O2 1.984(9) 3_557 ?
Cu2 O7 2.294(16) . ?
Cu2 Cu2 2.946(5) 3_557 ?
S3 O5 1.425(12) . ?
S3 O7 1.454(14) 4_666 ?
S3 O8 1.456(15) . ?
S3 C1 1.806(15) . ?
O1 C5 1.217(18) . ?
O2 Cu2 1.984(9) 3_557 ?
O3 C8 1.285(16) . ?
O4 C5 1.313(19) . ?
O6 C8 1.18(2) 3_557 ?
O7 S3 1.454(14) 4_565 ?
O8 Cu1 2.381(15) 4_566 ?
C1 C7 1.41(2) . ?
C1 C6 1.410(17) . ?
C2 C7 1.32(3) . ?
C2 C3 1.388(17) . ?
C2 C8 1.54(3) 2_556 ?
C3 C4 1.40(2) . ?
C4 C6 1.36(2) . ?
C4 C5 1.513(16) . ?
C8 O6 1.18(2) 3_557 ?
C8 C2 1.54(3) 2_546 ?
