#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:03:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178766 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102078.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_4102078
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         427.71
_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                 94.334(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.301(7)
_cell_length_b                   18.048(16)
_cell_length_c                   10.210(9)
_cell_measurement_reflns_used    8127
_cell_measurement_temperature    325(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      3.3
_cell_volume                     1342(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, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare  et. al. , 1999)'
_diffrn_ambient_temperature      325(2)
_diffrn_detector_area_resol_mean -
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0805
_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            8127
_diffrn_reflns_theta_full        31.22
_diffrn_reflns_theta_max         31.22
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    1.810
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Block, well formed'
_exptl_crystal_F_000             664
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.097
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.006
_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          0.1696
_refine_ls_wR_factor_ref         0.2019
_reflns_number_gt                2070
_reflns_number_total             3191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910600b_325K.cif
_cod_data_source_block           als47_5_6
_cod_original_cell_volume        1341(2)
_cod_database_code               4102078
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 0.13496(13) 0.09466(4) 0.78407(8) 0.0313(3) Uani 1 1 d . . .
Cu2 Cu -0.04000(13) 0.06841(4) 1.06999(8) 0.0321(3) Uani 1 1 d . . .
S3 S 0.1233(3) 0.43481(9) 1.30961(19) 0.0338(4) Uani 1 1 d . . .
O1 O 0.0566(9) 0.1678(2) 1.0849(5) 0.0434(14) Uani 1 1 d . . .
O2 O 0.1288(6) 0.0348(2) 0.9433(4) 0.0259(10) Uani 1 1 d . . .
O3 O 0.1560(9) 0.0138(3) 0.6627(6) 0.0462(14) Uani 1 1 d . . .
O4 O 0.1223(9) 0.1862(2) 0.8757(5) 0.0458(15) Uani 1 1 d . . .
O5 O 0.1386(13) 0.5129(3) 1.2995(7) 0.091(3) Uani 1 1 d . . .
O6 O -0.1802(10) 0.0894(3) 1.2172(6) 0.0533(17) Uani 1 1 d . . .
O7 O -0.2264(10) 0.0985(3) 0.8879(7) 0.0615(19) Uani 1 1 d . . .
O8 O -0.0478(9) 0.4082(4) 1.3524(7) 0.0634(19) Uani 1 1 d . . .
C1 C 0.1437(11) 0.3964(3) 1.1513(7) 0.0334(16) Uani 1 1 d . . .
C2 C 0.2317(11) 0.4051(3) 0.9299(7) 0.0321(16) Uani 1 1 d . . .
C3 C 0.1994(10) 0.3304(3) 0.9149(7) 0.0324(16) Uani 1 1 d . . .
H3 H 0.2215 0.3078 0.8357 0.039 Uiso 1 1 calc R . .
C4 C 0.1354(11) 0.2881(3) 1.0134(8) 0.0366(17) Uani 1 1 d . . .
C5 C 0.1014(11) 0.2070(3) 0.9884(7) 0.0331(16) Uani 1 1 d . . .
C6 C 0.1068(11) 0.3205(3) 1.1335(8) 0.0366(17) Uani 1 1 d . . .
H6 H 0.0640 0.2923 1.2012 0.044 Uiso 1 1 calc R . .
C7 C 0.2047(11) 0.4390(3) 1.0519(7) 0.0343(16) Uani 1 1 d . . .
H7 H 0.2278 0.4893 1.0646 0.041 Uiso 1 1 calc R . .
C8 C 0.1943(11) -0.0529(3) 0.6808(8) 0.0352(17) Uani 1 1 d . . .
O9W O 0.1208(10) 0.1563(3) 0.6237(6) 0.0552(17) Uani 1 1 d . . .
O10W O 0.0371(16) 0.3013(5) 0.5867(10) 0.092(5) Uani 0.90(3) 1 d P . .
O11W O 0.223(2) 0.1359(10) 0.3687(13) 0.115(8) Uani 0.69(3) 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 169.0(2) . . ?
O4 Cu1 O2 93.8(2) . . ?
O3 Cu1 O2 97.1(2) . . ?
O4 Cu1 O9W 85.3(2) . . ?
O3 Cu1 O9W 84.0(2) . . ?
O2 Cu1 O9W 175.6(3) . . ?
O4 Cu1 O8 87.5(3) . 4_665 ?
O3 Cu1 O8 92.8(3) . 4_665 ?
O2 Cu1 O8 80.0(2) . 4_665 ?
O9W Cu1 O8 104.2(3) . 4_665 ?
O6 Cu2 O1 88.2(2) . . ?
O6 Cu2 O2 169.2(2) . . ?
O1 Cu2 O2 95.5(2) . . ?
O6 Cu2 O2 92.7(2) . 3_557 ?
O1 Cu2 O2 177.7(2) . 3_557 ?
O2 Cu2 O2 83.21(19) . 3_557 ?
O6 Cu2 O7 105.7(3) . . ?
O1 Cu2 O7 92.0(2) . . ?
O2 Cu2 O7 84.3(3) . . ?
O2 Cu2 O7 89.8(2) 3_557 . ?
O6 Cu2 Cu2 133.24(16) . 3_557 ?
O1 Cu2 Cu2 137.40(18) . 3_557 ?
O2 Cu2 Cu2 41.92(12) . 3_557 ?
O2 Cu2 Cu2 41.29(13) 3_557 3_557 ?
O7 Cu2 Cu2 86.1(2) . 3_557 ?
O5 S3 O8 115.4(5) . . ?
O5 S3 O7 113.3(5) . 4_666 ?
O8 S3 O7 109.6(5) . 4_666 ?
O5 S3 C1 108.0(4) . . ?
O8 S3 C1 106.3(4) . . ?
O7 S3 C1 103.2(4) 4_666 . ?
C5 O1 Cu2 124.6(4) . . ?
Cu2 O2 Cu1 115.8(2) . . ?
Cu2 O2 Cu2 96.79(19) . 3_557 ?
Cu1 O2 Cu2 119.5(2) . 3_557 ?
C8 O3 Cu1 131.5(5) . . ?
C5 O4 Cu1 137.6(4) . . ?
C8 O6 Cu2 129.4(5) 3_557 . ?
S3 O7 Cu2 137.2(4) 4_565 . ?
S3 O8 Cu1 140.5(5) . 4_566 ?
C7 C1 C6 121.4(7) . . ?
C7 C1 S3 120.5(5) . . ?
C6 C1 S3 118.0(6) . . ?
C3 C2 C7 119.2(6) . . ?
C3 C2 C8 118.8(6) . 2_556 ?
C7 C2 C8 121.9(6) . 2_556 ?
C4 C3 C2 121.9(7) . . ?
C3 C4 C6 119.7(6) . . ?
C3 C4 C5 118.5(6) . . ?
C6 C4 C5 121.8(6) . . ?
O4 C5 O1 127.6(6) . . ?
O4 C5 C4 115.2(6) . . ?
O1 C5 C4 117.2(6) . . ?
C4 C6 C1 119.0(7) . . ?
C1 C7 C2 118.8(6) . . ?
O6 C8 O3 127.2(7) 3_557 . ?
O6 C8 C2 115.0(6) 3_557 2_546 ?
O3 C8 C2 117.8(7) . 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 1.905(5) . ?
Cu1 O3 1.928(5) . ?
Cu1 O2 1.955(5) . ?
Cu1 O9W 1.975(6) . ?
Cu1 O8 2.368(7) 4_665 ?
Cu2 O6 1.918(6) . ?
Cu2 O1 1.930(5) . ?
Cu2 O2 1.950(5) . ?
Cu2 O2 1.974(4) 3_557 ?
Cu2 O7 2.285(6) . ?
Cu2 Cu2 2.934(2) 3_557 ?
S3 O5 1.418(6) . ?
S3 O8 1.437(7) . ?
S3 O7 1.440(6) 4_666 ?
S3 C1 1.776(8) . ?
O1 C5 1.276(8) . ?
O2 Cu2 1.974(4) 3_557 ?
O3 C8 1.246(8) . ?
O4 C5 1.230(9) . ?
O6 C8 1.243(9) 3_557 ?
O7 S3 1.440(6) 4_565 ?
O8 Cu1 2.368(7) 4_566 ?
C1 C7 1.374(10) . ?
C1 C6 1.406(8) . ?
C2 C3 1.376(8) . ?
C2 C7 1.414(10) . ?
C2 C8 1.496(10) 2_556 ?
C3 C4 1.372(10) . ?
C4 C6 1.388(10) . ?
C4 C5 1.502(8) . ?
C8 O6 1.243(9) 3_557 ?
C8 C2 1.496(10) 2_546 ?
