#------------------------------------------------------------------------------
#$Date: 2016-01-09 12:37:09 +0200 (Sat, 09 Jan 2016) $
#$Revision: 173764 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/30/7223093.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_7223093
loop_
_publ_author_name
'Fujita, Wataru'
_publ_section_title
;
 Convenient crystal growth, structural determination and magnetic studies
 of layered copper hydroxides containing aromatic sulfonates
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              9193
_journal_paper_doi               10.1039/C5CE01731A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C10 H26 Cu5 O20 S2'
_chemical_formula_sum            'C10 H26 Cu5 O20 S2'
_chemical_formula_weight         848.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-10-05 deposited with the CCDC.
2015-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                95.208(10)
_cell_angle_beta                 98.408(9)
_cell_angle_gamma                107.430(7)
_cell_formula_units_Z            1
_cell_length_a                   5.4530(5)
_cell_length_b                   8.0998(9)
_cell_length_c                   14.4067(17)
_cell_measurement_reflns_used    2398
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.20
_cell_volume                     594.44(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5801
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.206
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.668
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             423.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0552P)²+0.2035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2180
_reflns_number_total             2616
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c5ce01731a2.cif
_cod_data_source_block           140510f13
_cod_depositor_comments
'Adding full bibliography for 7223093--7223096.cif.'
_cod_original_cell_volume        594.44(11)
_cod_database_code               7223093
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.5000 0.5000 0.01019(15) Uani 1 2 d S . P
Cu2 Cu 0.92119(6) 0.30231(4) 0.50188(2) 0.00976(13) Uani 1 1 d . . .
Cu3 Cu 0.30101(6) 0.09474(4) 0.49468(2) 0.00996(13) Uani 1 1 d . . .
S1 S 0.30209(14) 0.43899(11) 0.81332(5) 0.0177(2) Uani 1 1 d . . .
O1 O 0.2950(4) 0.2709(3) 0.76243(16) 0.0245(5) Uani 1 1 d . . .
O2 O 0.5628(4) 0.5451(3) 0.85810(16) 0.0258(5) Uani 1 1 d . . .
O3 O 0.1701(4) 0.5318(3) 0.75014(15) 0.0211(5) Uani 1 1 d . . .
O4 O 0.7920(4) 0.4742(3) 0.43946(17) 0.0109(4) Uani 1 1 d . . .
H4A H 0.767(7) 0.459(5) 0.385(3) 0.013 Uiso 1 1 d . U .
O5 O 0.2516(4) 0.2847(3) 0.43102(16) 0.0122(5) Uani 1 1 d . . .
H5A H 0.253(7) 0.268(5) 0.379(3) 0.015 Uiso 1 1 d . U .
O6 O 1.0481(4) 0.1397(3) 0.57163(16) 0.0114(4) Uani 1 1 d . . .
H6A H 1.091(7) 0.173(5) 0.627(3) 0.014 Uiso 1 1 d . U .
O7 O 0.3806(4) -0.0938(3) 0.55818(16) 0.0112(4) Uani 1 1 d . . .
H7A H 0.390(6) -0.077(5) 0.618(3) 0.013 Uiso 1 1 d . U .
O8 O 0.6696(5) 0.3568(3) 0.63747(18) 0.0212(5) Uani 1 1 d . . .
H8A H 0.571(8) 0.327(5) 0.669(3) 0.025 Uiso 1 1 d . U .
H8B H 0.808(8) 0.412(5) 0.671(3) 0.025 Uiso 1 1 d . U .
O9 O 0.8175(5) 0.8098(4) 0.76314(19) 0.0288(6) Uani 1 1 d . . .
H9A H 0.790(8) 0.741(6) 0.797(3) 0.035 Uiso 1 1 d . U .
H9B H 0.689(8) 0.852(6) 0.761(3) 0.035 Uiso 1 1 d . U .
O10 O 0.3837(6) 0.9434(4) 0.7527(2) 0.0297(6) Uani 1 1 d . . .
H10A H 0.245(8) 0.873(6) 0.759(3) 0.036 Uiso 1 1 d . U .
H10B H 0.402(9) 1.023(6) 0.774(3) 0.036 Uiso 1 1 d . U .
C1 C 0.1135(6) 0.3881(4) 0.9033(2) 0.0173(6) Uani 1 1 d . . .
C2 C -0.0075(6) 0.2162(4) 0.9087(2) 0.0240(7) Uani 1 1 d . . .
H2 H 0.0165 0.1276 0.8665 0.029 Uiso 1 1 calc R U .
C3 C -0.1669(7) 0.1698(5) 0.9762(2) 0.0262(8) Uani 1 1 d . . .
H3 H -0.2491 0.0498 0.9797 0.031 Uiso 1 1 calc R U .
C4 C -0.2052(6) 0.2950(4) 1.0370(2) 0.0219(7) Uani 1 1 d . . .
H4 H -0.3158 0.2612 1.0818 0.026 Uiso 1 1 calc R U .
C5 C 0.0817(6) 0.5245(4) 0.9659(2) 0.0153(6) 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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cu Cu 0.3201 1.2651
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(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
O5 Cu1 O5 180.0 . 2_666
O5 Cu1 O4 94.14(9) . .
O5 Cu1 O4 85.86(10) 2_666 .
O5 Cu1 O4 85.86(10) . 2_666
O5 Cu1 O4 94.14(9) 2_666 2_666
O4 Cu1 O4 180.0 . 2_666
O6 Cu2 O4 176.29(8) . .
O6 Cu2 O7 85.61(9) . 2_656
O4 Cu2 O7 96.12(9) . 2_656
O6 Cu2 O4 98.63(9) . 2_766
O4 Cu2 O4 79.53(10) . 2_766
O7 Cu2 O4 175.30(8) 2_656 2_766
O6 Cu2 O5 78.34(9) . 1_655
O4 Cu2 O5 104.28(9) . 1_655
O7 Cu2 O5 105.48(9) 2_656 1_655
O4 Cu2 O5 77.49(9) 2_766 1_655
O6 Cu2 Cu3 39.82(6) . 1_655
O4 Cu2 Cu3 143.14(7) . 1_655
O7 Cu2 Cu3 91.62(6) 2_656 1_655
O4 Cu2 Cu3 92.94(6) 2_766 1_655
O5 Cu2 Cu3 39.22(6) 1_655 1_655
O5 Cu3 O7 175.42(8) . .
O5 Cu3 O6 85.30(9) . 1_455
O7 Cu3 O6 98.53(9) . 1_455
O5 Cu3 O7 94.07(9) . 2_656
O7 Cu3 O7 81.60(9) . 2_656
O6 Cu3 O7 165.87(9) 1_455 2_656
O5 Cu3 O6 104.97(8) . 2_656
O7 Cu3 O6 78.16(8) . 2_656
O6 Cu3 O6 81.83(9) 1_455 2_656
O7 Cu3 O6 111.85(9) 2_656 2_656
O5 Cu3 Cu3 134.55(7) . 2_656
O7 Cu3 Cu3 41.10(6) . 2_656
O6 Cu3 Cu3 137.89(7) 1_455 2_656
O7 Cu3 Cu3 40.50(6) 2_656 2_656
O6 Cu3 Cu3 96.47(5) 2_656 2_656
O5 Cu3 Cu2 47.06(7) . 1_455
O7 Cu3 Cu2 137.08(6) . 1_455
O6 Cu3 Cu2 39.03(6) 1_455 1_455
O7 Cu3 Cu2 140.83(6) 2_656 1_455
O6 Cu3 Cu2 87.20(5) 2_656 1_455
Cu3 Cu3 Cu2 174.88(2) 2_656 1_455
O2 S1 O3 112.59(15) . .
O2 S1 O1 112.60(14) . .
O3 S1 O1 110.44(14) . .
O2 S1 C1 107.99(14) . .
O3 S1 C1 106.23(14) . .
O1 S1 C1 106.56(15) . .
Cu2 O4 Cu1 106.78(11) . .
Cu2 O4 Cu2 100.47(10) . 2_766
Cu1 O4 Cu2 101.13(10) . 2_766
Cu2 O4 H4A 116(3) . .
Cu1 O4 H4A 117(3) . .
Cu2 O4 H4A 114(3) 2_766 .
Cu3 O5 Cu1 107.99(11) . .
Cu3 O5 Cu2 93.72(9) . 1_455
Cu1 O5 Cu2 95.42(9) . 1_455
Cu3 O5 H5A 111(3) . .
Cu1 O5 H5A 116(3) . .
Cu2 O5 H5A 129(3) 1_455 .
Cu2 O6 Cu3 101.16(10) . 1_655
Cu2 O6 Cu3 93.92(8) . 2_656
Cu3 O6 Cu3 98.16(9) 1_655 2_656
Cu2 O6 H6A 113(3) . .
Cu3 O6 H6A 121(3) 1_655 .
Cu3 O6 H6A 124(3) 2_656 .
Cu3 O7 Cu2 102.28(10) . 2_656
Cu3 O7 Cu3 98.39(9) . 2_656
Cu2 O7 Cu3 110.50(10) 2_656 2_656
Cu3 O7 H7A 113(2) . .
Cu2 O7 H7A 111(2) 2_656 .
Cu3 O7 H7A 120(2) 2_656 .
H8A O8 H8B 107(4) . .
H9A O9 H9B 105(4) . .
H10A O10 H10B 113(5) . .
C2 C1 C5 121.3(3) . .
C2 C1 S1 118.3(2) . .
C5 C1 S1 120.4(2) . .
C1 C2 C3 120.3(3) . .
C1 C2 H2 119.8 . .
C3 C2 H2 119.8 . .
C4 C3 C2 120.7(3) . .
C4 C3 H3 119.7 . .
C2 C3 H3 119.7 . .
C3 C4 C5 120.8(3) . 2_567
C3 C4 H4 119.6 . .
C5 C4 H4 119.6 2_567 .
C4 C5 C5 119.0(4) 2_567 2_567
C4 C5 C1 123.1(3) 2_567 .
C5 C5 C1 117.9(4) 2_567 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5 1.934(2) .
Cu1 O5 1.934(2) 2_666
Cu1 O4 1.978(2) .
Cu1 O4 1.978(2) 2_666
Cu2 O6 1.951(2) .
Cu2 O4 1.968(2) .
Cu2 O7 1.991(2) 2_656
Cu2 O4 2.019(2) 2_766
Cu2 O5 2.231(2) 1_655
Cu2 Cu3 3.0405(5) 1_655
Cu3 O5 1.927(2) .
Cu3 O7 1.973(2) .
Cu3 O6 1.985(2) 1_455
Cu3 O7 1.997(2) 2_656
Cu3 O6 2.262(2) 2_656
Cu3 Cu3 3.0049(6) 2_656
Cu3 Cu2 3.0405(5) 1_455
S1 O2 1.440(2) .
S1 O3 1.473(2) .
S1 O1 1.473(2) .
S1 C1 1.773(3) .
O4 Cu2 2.019(2) 2_766
O4 H4A 0.76(4) .
O5 Cu2 2.231(2) 1_455
O5 H5A 0.75(4) .
O6 Cu3 1.985(2) 1_655
O6 Cu3 2.262(2) 2_656
O6 H6A 0.80(4) .
O7 Cu2 1.991(2) 2_656
O7 Cu3 1.997(2) 2_656
O7 H7A 0.86(4) .
O8 H8A 0.76(4) .
O8 H8B 0.81(4) .
O9 H9A 0.77(5) .
O9 H9B 0.86(4) .
O10 H10A 0.82(4) .
O10 H10B 0.67(5) .
C1 C2 1.366(5) .
C1 C5 1.428(4) .
C2 C3 1.400(5) .
C2 H2 0.9500 .
C3 C4 1.363(5) .
C3 H3 0.9500 .
C4 C5 1.422(5) 2_567
C4 H4 0.9500 .
C5 C4 1.422(5) 2_567
C5 C5 1.427(6) 2_567
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
O2 S1 C1 C2 -123.6(3) .
O3 S1 C1 C2 115.4(3) .
O1 S1 C1 C2 -2.4(3) .
O2 S1 C1 C5 58.8(3) .
O3 S1 C1 C5 -62.2(3) .
O1 S1 C1 C5 180.0(2) .
C5 C1 C2 C3 0.1(5) .
S1 C1 C2 C3 -177.5(3) .
C1 C2 C3 C4 0.5(5) .
C2 C3 C4 C5 -0.8(5) 2_567
C2 C1 C5 C4 179.6(3) 2_567
S1 C1 C5 C4 -2.9(4) 2_567
C2 C1 C5 C5 -0.3(5) 2_567
S1 C1 C5 C5 177.3(3) 2_567
