#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:03:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178766 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/20/4102085.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_4102085
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            'C16 H6 Cu4 O16 S2'
_chemical_formula_weight         306.70
_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
;
2010-01-26 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 139.21(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.814(5)
_cell_length_b                   19.437(10)
_cell_length_c                   12.067(6)
_cell_measurement_reflns_used    7694
_cell_measurement_temperature    435(2)
_cell_measurement_theta_max      22.7
_cell_measurement_theta_min      3.1
_cell_volume                     2116.7(19)
_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  '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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7694
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    2.280
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Block, well formed'
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1097P)²+5.3801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1569
_reflns_number_gt                1803
_reflns_number_total             2810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910600b_435K.cif
_cod_data_source_block           new
_cod_original_cell_volume        2116.6(17)
_cod_database_code               4102085
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 1.18379(15) 0.06506(5) 0.22365(19) 0.0468(4) Uani 1 1 d . . .
Cu2 Cu 0.78694(16) -0.04884(5) 0.2313(2) 0.0493(4) Uani 1 1 d . . .
Cu3 Cu 0.94587(16) 0.08250(5) 0.2314(2) 0.0500(5) Uani 1 1 d . . .
Cu4 Cu 1.07133(16) -0.05835(5) 0.3034(2) 0.0532(5) Uani 1 1 d . . .
S1 S 0.8006(3) 0.41557(11) 0.1096(4) 0.0444(7) Uani 1 1 d . . .
S2 S 0.2785(3) 0.10659(13) 0.0831(4) 0.0493(8) Uani 1 1 d . . .
O1 O 0.3358(8) 0.0947(3) 0.2445(10) 0.0458(18) Uani 1 1 d . . .
O2 O 1.1499(8) 0.1596(3) 0.2270(10) 0.052(2) Uani 1 1 d . . .
O3 O 0.8543(8) -0.1417(3) 0.2802(10) 0.0473(19) Uani 1 1 d . . .
O4 O 1.0827(8) -0.1378(3) 0.4048(10) 0.0471(19) Uani 1 1 d . . .
O5 O 0.7896(8) 0.4823(3) 0.0470(11) 0.063(2) Uani 1 1 d . . .
O6 O 0.8539(8) 0.4195(3) 0.2706(10) 0.053(2) Uani 1 1 d . . .
O7 O 0.6654(7) 0.3753(3) -0.0147(10) 0.0513(19) Uani 1 1 d . . .
O8 O 0.8224(9) 0.1290(3) 0.2299(12) 0.067(3) Uani 1 1 d . . .
O9 O 0.9276(8) 0.1606(3) 0.1190(10) 0.052(2) Uani 1 1 d . . .
O10 O 1.1911(9) -0.1066(3) 0.3003(11) 0.060(2) Uani 1 1 d . . .
O11 O 0.2596(10) 0.0430(4) 0.0060(12) 0.075(3) Uani 1 1 d . . .
C1 C 0.4175(12) 0.1504(5) 0.1281(14) 0.044(3) Uani 1 1 d . . .
O12 O 0.9746(7) -0.0047(3) 0.3399(9) 0.0438(18) Uani 1 1 d . . .
C2 C 0.5240(11) 0.2534(4) 0.1500(14) 0.040(3) Uani 1 1 d . . .
C3 C 1.1430(12) 0.3028(4) 0.1998(15) 0.050(3) Uani 1 1 d . . .
H021 H 1.2117 0.2801 0.2150 0.060 Uiso 1 1 calc R . .
O13 O 0.1454(9) 0.1477(5) -0.0297(12) 0.076(3) Uani 1 1 d . . .
C4 C 1.0417(12) 0.4082(4) 0.1838(15) 0.047(3) Uani 1 1 d . . .
H023 H 1.0424 0.4559 0.1891 0.057 Uiso 1 1 calc R . .
O14 O 1.0236(8) 0.0261(3) 0.1755(10) 0.0441(18) Uani 1 1 d . . .
C5 C 0.6257(12) 0.2157(4) 0.1767(14) 0.044(3) Uani 1 1 d . . .
H025 H 0.6975 0.2375 0.1961 0.053 Uiso 1 1 calc R . .
C6 C 1.0383(11) 0.2659(4) 0.1697(14) 0.038(3) Uani 1 1 d . . .
C7 C 0.5177(12) 0.1121(5) 0.1560(15) 0.047(3) Uani 1 1 d . . .
H027 H 0.5187 0.0644 0.1631 0.057 Uiso 1 1 calc R . .
O15 O 0.6969(10) 0.0379(3) 0.1784(15) 0.091(4) Uani 1 1 d . . .
O16 O 1.2171(11) -0.0258(3) 0.1951(14) 0.083(3) Uani 1 1 d . . .
C8 C 0.4198(11) 0.2215(4) 0.1247(14) 0.042(3) Uani 1 1 d . . .
H030 H 0.3516 0.2474 0.1055 0.051 Uiso 1 1 calc R . .
C9 C 0.9392(11) 0.3712(4) 0.1531(14) 0.040(3) Uani 1 1 d . . .
C10 C 0.9367(12) 0.2999(4) 0.1476(14) 0.045(3) Uani 1 1 d . . .
H032 H 0.8677 0.2754 0.1293 0.054 Uiso 1 1 calc R . .
C11 C 0.6166(12) 0.1449(4) 0.1734(15) 0.046(3) Uani 1 1 d . . .
C12 C 1.1427(12) 0.3753(4) 0.2066(15) 0.048(3) Uani 1 1 d . . .
C13 C 0.7225(12) 0.1008(4) 0.1978(15) 0.046(3) Uani 1 1 d . . .
C14 C 1.0406(11) 0.1887(4) 0.1725(14) 0.039(3) Uani 1 1 d . . .
C15 C 0.9700(12) -0.1684(4) 0.3448(15) 0.045(3) Uani 1 1 d . . .
C16 C 1.2492(13) -0.0835(4) 0.2657(15) 0.046(3) 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
O2 Cu1 O16 170.8(3) . . ?
O2 Cu1 O14 98.0(2) . . ?
O16 Cu1 O14 87.8(3) . . ?
O2 Cu1 O1 88.4(3) . 1_655 ?
O16 Cu1 O1 85.2(3) . 1_655 ?
O14 Cu1 O1 171.0(3) . 1_655 ?
O15 Cu2 O3 170.9(3) . . ?
O15 Cu2 O12 91.9(3) . . ?
O3 Cu2 O12 96.7(3) . . ?
O15 Cu2 O6 83.5(3) . 2_645 ?
O3 Cu2 O6 87.4(3) . 2_645 ?
O12 Cu2 O6 153.2(3) . 2_645 ?
O15 Cu2 O11 92.4(4) . 3_655 ?
O3 Cu2 O11 92.4(3) . 3_655 ?
O12 Cu2 O11 78.9(3) . 3_655 ?
O6 Cu2 O11 127.6(3) 2_645 3_655 ?
O8 Cu3 O9 88.9(3) . . ?
O8 Cu3 O14 165.2(4) . . ?
O9 Cu3 O14 90.7(3) . . ?
O8 Cu3 O12 98.0(3) . . ?
O9 Cu3 O12 172.8(3) . . ?
O14 Cu3 O12 82.1(2) . . ?
O8 Cu3 O7 96.4(3) . 4_666 ?
O9 Cu3 O7 89.7(3) . 4_666 ?
O14 Cu3 O7 98.3(3) . 4_666 ?
O12 Cu3 O7 91.3(3) . 4_666 ?
O8 Cu3 Cu4 138.4(2) . . ?
O9 Cu3 Cu4 131.7(2) . . ?
O14 Cu3 Cu4 41.17(18) . . ?
O12 Cu3 Cu4 41.20(17) . . ?
O7 Cu3 Cu4 92.89(17) 4_666 . ?
O4 Cu4 O10 87.9(3) . . ?
O4 Cu4 O12 91.4(3) . . ?
O10 Cu4 O12 171.9(3) . . ?
O4 Cu4 O14 170.1(3) . . ?
O10 Cu4 O14 99.9(3) . . ?
O12 Cu4 O14 81.7(3) . . ?
O4 Cu4 Cu3 132.5(2) . . ?
O10 Cu4 Cu3 139.2(2) . . ?
O12 Cu4 Cu3 41.15(17) . . ?
O14 Cu4 Cu3 40.81(18) . . ?
O7 S1 O5 113.5(5) . . ?
O7 S1 O6 111.0(4) . . ?
O5 S1 O6 113.1(5) . . ?
O7 S1 C9 107.4(4) . . ?
O5 S1 C9 104.6(4) . . ?
O6 S1 C9 106.6(5) . . ?
O13 S2 O11 112.7(6) . . ?
O13 S2 O1 111.3(5) . . ?
O11 S2 O1 111.9(5) . . ?
O13 S2 C1 109.6(5) . . ?
O11 S2 C1 103.5(4) . . ?
O1 S2 C1 107.5(5) . . ?
S2 O1 Cu1 114.8(4) . 1_455 ?
C14 O2 Cu1 130.6(6) . . ?
C15 O3 Cu2 133.1(6) . . ?
C15 O4 Cu4 123.2(7) . . ?
S1 O6 Cu2 119.1(5) . 2_655 ?
S1 O7 Cu3 123.8(4) . 4_565 ?
C13 O8 Cu3 124.4(6) . . ?
C14 O9 Cu3 121.7(7) . . ?
C16 O10 Cu4 128.0(6) . . ?
S2 O11 Cu2 118.5(5) . 3_655 ?
C7 C1 C8 120.6(9) . . ?
C7 C1 S2 118.3(7) . . ?
C8 C1 S2 121.0(7) . . ?
Cu4 O12 Cu3 97.7(3) . . ?
Cu4 O12 Cu2 112.5(3) . . ?
Cu3 O12 Cu2 114.8(3) . . ?
C8 C2 C5 121.4(8) . . ?
C8 C2 C15 118.4(8) . 2_655 ?
C5 C2 C15 120.2(8) . 2_655 ?
C6 C3 C12 118.7(8) . . ?
C12 C4 C9 120.2(8) . . ?
Cu1 O14 Cu3 117.8(3) . . ?
Cu1 O14 Cu4 116.8(3) . . ?
Cu3 O14 Cu4 98.0(3) . . ?
C11 C5 C2 117.7(8) . . ?
C10 C6 C3 120.3(8) . . ?
C10 C6 C14 119.0(8) . . ?
C3 C6 C14 120.6(8) . . ?
C11 C7 C1 119.2(8) . . ?
C13 O15 Cu2 142.2(7) . . ?
C16 O16 Cu1 134.7(8) . . ?
C2 C8 C1 119.2(8) . . ?
C4 C9 C10 121.5(8) . . ?
C4 C9 S1 119.2(7) . . ?
C10 C9 S1 119.2(7) . . ?
C6 C10 C9 119.0(8) . . ?
C7 C11 C5 121.8(8) . . ?
C7 C11 C13 117.9(8) . . ?
C5 C11 C13 120.2(8) . . ?
C4 C12 C3 120.3(9) . . ?
C4 C12 C16 119.6(8) . 2_755 ?
C3 C12 C16 120.1(9) . 2_755 ?
O8 C13 O15 125.6(9) . . ?
O8 C13 C11 119.4(8) . . ?
O15 C13 C11 115.0(8) . . ?
O2 C14 O9 127.4(8) . . ?
O2 C14 C6 117.8(8) . . ?
O9 C14 C6 114.9(8) . . ?
O3 C15 O4 127.2(8) . . ?
O3 C15 C2 116.5(8) . 2_645 ?
O4 C15 C2 116.2(8) . 2_645 ?
O10 C16 O16 124.1(9) . . ?
O10 C16 C12 121.7(8) . 2_745 ?
O16 C16 C12 114.0(9) . 2_745 ?
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 O2 1.904(6) . ?
Cu1 O16 1.921(7) . ?
Cu1 O14 1.965(6) . ?
Cu1 O1 2.001(6) 1_655 ?
Cu2 O15 1.896(7) . ?
Cu2 O3 1.908(6) . ?
Cu2 O12 2.007(6) . ?
Cu2 O6 2.025(7) 2_645 ?
Cu2 O11 2.416(9) 3_655 ?
Cu3 O8 1.918(6) . ?
Cu3 O9 1.922(6) . ?
Cu3 O14 1.977(6) . ?
Cu3 O12 1.989(6) . ?
Cu3 O7 2.277(8) 4_666 ?
Cu3 Cu4 2.996(2) . ?
Cu4 O4 1.902(6) . ?
Cu4 O10 1.926(7) . ?
Cu4 O12 1.991(6) . ?
Cu4 O14 1.992(6) . ?
S1 O7 1.453(7) . ?
S1 O5 1.450(7) . ?
S1 O6 1.469(8) . ?
S1 C9 1.778(9) . ?
S2 O13 1.443(8) . ?
S2 O11 1.448(8) . ?
S2 O1 1.462(8) . ?
S2 C1 1.769(10) . ?
O1 Cu1 2.001(6) 1_455 ?
O2 C14 1.237(11) . ?
O3 C15 1.243(11) . ?
O4 C15 1.263(11) . ?
O6 Cu2 2.025(7) 2_655 ?
O7 Cu3 2.277(7) 4_565 ?
O8 C13 1.243(11) . ?
O9 C14 1.274(11) . ?
O10 C16 1.238(12) . ?
O11 Cu2 2.416(9) 3_655 ?
C1 C7 1.371(13) . ?
C1 C8 1.385(12) . ?
C2 C8 1.373(12) . ?
C2 C5 1.389(12) . ?
C2 C15 1.522(12) 2_655 ?
C3 C6 1.395(12) . ?
C3 C12 1.413(12) . ?
C4 C12 1.359(13) . ?
C4 C9 1.365(13) . ?
C5 C11 1.380(12) . ?
C6 C10 1.383(12) . ?
C6 C14 1.500(12) . ?
C7 C11 1.372(13) . ?
O15 C13 1.245(11) . ?
O16 C16 1.268(12) . ?
C9 C10 1.386(12) . ?
C11 C13 1.520(13) . ?
C12 C16 1.491(13) 2_755 ?
C15 C2 1.522(12) 2_645 ?
C16 C12 1.491(13) 2_745 ?
