#------------------------------------------------------------------------------
#$Date: 2017-01-09 05:08:22 +0200 (Mon, 09 Jan 2017) $
#$Revision: 190085 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/67/7226739.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_7226739
loop_
_publ_author_name
'Fujita, Wataru'
'Tokumitu, Akio'
'Fujii, Yutaka'
'Kikuchi, Hikomitsu'
_publ_section_title
;
 Crystal growth, structures and magnetic properties of copper hydroxide
 compounds with distorted diamond chain magnetic networks
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8614
_journal_paper_doi               10.1039/C6CE01631F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C20 H50 Cu3 O16 S2'
_chemical_formula_sum            'C20 H50 Cu3 O16 S2'
_chemical_formula_weight         801.36
_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
;
2016-07-14 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                88.075(5)
_cell_angle_beta                 89.276(5)
_cell_angle_gamma                77.558(5)
_cell_formula_units_Z            1
_cell_length_a                   5.6080(4)
_cell_length_b                   8.6585(7)
_cell_length_c                   17.5909(19)
_cell_measurement_reflns_used    3632
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.30
_cell_volume                     833.62(13)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.914
_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  0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7969
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         3.291
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             417.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3490
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0375P)²+0.4449P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3184
_reflns_number_total             3490
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c6ce01631f2.cif
_cod_data_source_block           141221f53
_cod_depositor_comments
'Adding full bibliography for 7226738--7226744.cif.'
_cod_database_code               7226739
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 1.0000 0.01249(10) Uani 1 2 d S . P
Cu2 Cu 1.00096(4) 0.41417(3) 0.92726(2) 0.01377(9) Uani 1 1 d . . .
S3 S 0.78846(9) 0.95283(6) 0.85625(3) 0.01534(13) Uani 1 1 d . . .
O4 O 0.7950(3) 0.58740(18) 0.98309(9) 0.0140(3) Uani 1 1 d D . .
H4 H 0.756(4) 0.662(3) 0.9568(14) 0.017 Uiso 1 1 d D U .
O5 O 0.4291(3) 0.49549(19) 0.89152(9) 0.0172(3) Uani 1 1 d . . .
O6 O 0.8003(3) 0.46288(19) 0.83664(9) 0.0189(3) Uani 1 1 d . . .
O7 O 0.7650(3) 0.25439(19) 0.99300(10) 0.0168(3) Uani 1 1 d D . .
H7A H 0.809(5) 0.201(3) 1.0289(12) 0.020 Uiso 1 1 d D U .
H7B H 0.729(5) 0.206(3) 0.9616(13) 0.020 Uiso 1 1 d D U .
O8 O 0.6515(3) 0.8544(2) 0.89832(10) 0.0249(4) Uani 1 1 d . . .
O9 O 1.1853(3) 0.2225(2) 0.88008(11) 0.0244(4) Uani 1 1 d D . .
H9A H 1.326(3) 0.198(3) 0.8769(17) 0.029 Uiso 1 1 d D U .
H9B H 1.140(5) 0.142(3) 0.8832(17) 0.029 Uiso 1 1 d D U .
O10 O 1.0409(3) 0.93322(19) 0.88159(10) 0.0225(4) Uani 1 1 d . . .
O11 O 0.6653(3) 1.11999(18) 0.85487(10) 0.0213(4) Uani 1 1 d . . .
C12 C 0.5709(4) 0.4821(3) 0.83464(13) 0.0171(5) Uani 1 1 d . . .
C13 C 0.5591(5) 0.9040(3) 0.72383(15) 0.0284(6) Uani 1 1 d . . .
H13A H 0.4694 1.0158 0.7222 0.034 Uiso 1 1 calc R U .
H13B H 0.4618 0.8416 0.7545 0.034 Uiso 1 1 calc R U .
C14 C 0.4546(4) 0.4838(3) 0.75830(14) 0.0267(5) Uani 1 1 d . . .
H14A H 0.2772 0.4995 0.7646 0.032 Uiso 1 1 calc R U .
H14B H 0.4928 0.5703 0.7263 0.032 Uiso 1 1 calc R U .
H14C H 0.5178 0.3828 0.7340 0.032 Uiso 1 1 calc R U .
C15 C 0.3514(5) 0.8336(4) 0.60521(15) 0.0326(6) Uani 1 1 d . . .
H15A H 0.2417 0.9398 0.6044 0.039 Uiso 1 1 calc R U .
H15B H 0.2709 0.7613 0.6359 0.039 Uiso 1 1 calc R U .
C16 C 0.3864(5) 0.7756(4) 0.52434(15) 0.0353(6) Uani 1 1 d . . .
H16A H 0.4559 0.8526 0.4931 0.042 Uiso 1 1 calc R U .
H16B H 0.5072 0.6737 0.5250 0.042 Uiso 1 1 calc R U .
C17 C 0.5901(5) 0.8426(4) 0.64298(15) 0.0322(6) Uani 1 1 d . . .
H17A H 0.6722 0.9128 0.6114 0.039 Uiso 1 1 calc R U .
H17B H 0.6981 0.7358 0.6445 0.039 Uiso 1 1 calc R U .
C18 C 0.1551(5) 0.7527(4) 0.48644(16) 0.0352(6) Uani 1 1 d . . .
H18A H 0.0904 0.6711 0.5158 0.042 Uiso 1 1 calc R U .
H18B H 0.0308 0.8530 0.4880 0.042 Uiso 1 1 calc R U .
C19 C 0.8067(4) 0.8914(3) 0.76111(14) 0.0271(6) Uani 1 1 d . . .
H19A H 0.9005 0.9567 0.7308 0.032 Uiso 1 1 calc R U .
H19B H 0.8982 0.7801 0.7599 0.032 Uiso 1 1 calc R U .
C20 C 0.1941(6) 0.7036(4) 0.40471(17) 0.0433(8) Uani 1 1 d . . .
H20A H 0.3242 0.6062 0.4032 0.052 Uiso 1 1 calc R U .
H20B H 0.2529 0.7875 0.3752 0.052 Uiso 1 1 calc R U .
C21 C -0.0314(6) 0.6729(4) 0.36584(19) 0.0499(9) Uani 1 1 d . . .
H21A H 0.0098 0.6419 0.3134 0.060 Uiso 1 1 calc R U .
H21B H -0.0889 0.5877 0.3936 0.060 Uiso 1 1 calc R U .
H21C H -0.1602 0.7695 0.3655 0.060 Uiso 1 1 calc R U .
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 180.00(9) 2_667 .
O5 Cu1 O4 85.77(6) 2_667 .
O5 Cu1 O4 94.23(6) . .
O5 Cu1 O4 94.22(6) 2_667 2_667
O5 Cu1 O4 85.78(6) . 2_667
O4 Cu1 O4 180.0 . 2_667
O5 Cu1 O7 90.03(6) 2_667 2_667
O5 Cu1 O7 89.97(6) . 2_667
O4 Cu1 O7 94.74(6) . 2_667
O4 Cu1 O7 85.26(6) 2_667 2_667
O5 Cu1 O7 89.97(6) 2_667 .
O5 Cu1 O7 90.03(6) . .
O4 Cu1 O7 85.26(6) . .
O4 Cu1 O7 94.74(6) 2_667 .
O7 Cu1 O7 180.0 2_667 .
O5 Cu1 Cu2 76.52(4) 2_667 2_667
O5 Cu1 Cu2 103.48(4) . 2_667
O4 Cu1 Cu2 140.20(4) . 2_667
O4 Cu1 Cu2 39.80(4) 2_667 2_667
O7 Cu1 Cu2 50.69(4) 2_667 2_667
O7 Cu1 Cu2 129.31(4) . 2_667
O5 Cu1 Cu2 103.48(4) 2_667 .
O5 Cu1 Cu2 76.51(4) . .
O4 Cu1 Cu2 39.80(4) . .
O4 Cu1 Cu2 140.20(4) 2_667 .
O7 Cu1 Cu2 129.31(4) 2_667 .
O7 Cu1 Cu2 50.69(4) . .
Cu2 Cu1 Cu2 180.0 2_667 .
O6 Cu2 O4 167.87(7) . 2_767
O6 Cu2 O9 89.64(7) . .
O4 Cu2 O9 98.90(7) 2_767 .
O6 Cu2 O4 92.38(7) . .
O4 Cu2 O4 80.29(7) 2_767 .
O9 Cu2 O4 172.30(7) . .
O6 Cu2 O7 97.74(6) . .
O4 Cu2 O7 91.14(6) 2_767 .
O9 Cu2 O7 88.33(7) . .
O4 Cu2 O7 84.04(6) . .
O6 Cu2 Cu2 131.69(5) . 2_767
O4 Cu2 Cu2 40.26(4) 2_767 2_767
O9 Cu2 Cu2 138.66(6) . 2_767
O4 Cu2 Cu2 40.03(4) . 2_767
O7 Cu2 Cu2 86.84(4) . 2_767
O6 Cu2 Cu1 80.05(5) . .
O4 Cu2 Cu1 99.86(4) 2_767 .
O9 Cu2 Cu1 133.40(5) . .
O4 Cu2 Cu1 40.03(4) . .
O7 Cu2 Cu1 49.15(4) . .
Cu2 Cu2 Cu1 67.023(10) 2_767 .
O8 S3 O11 112.32(10) . .
O8 S3 O10 113.79(10) . .
O11 S3 O10 110.52(9) . .
O8 S3 C19 106.92(12) . .
O11 S3 C19 106.98(12) . .
O10 S3 C19 105.81(11) . .
Cu2 O4 Cu2 99.71(7) 2_767 .
Cu2 O4 Cu1 115.46(8) 2_767 .
Cu2 O4 Cu1 100.17(7) . .
Cu2 O4 H4 122(2) 2_767 .
Cu2 O4 H4 111(2) . .
Cu1 O4 H4 106.4(19) . .
C12 O5 Cu1 130.19(14) . .
C12 O6 Cu2 125.75(15) . .
Cu1 O7 Cu2 80.16(5) . .
Cu1 O7 H7A 123(2) . .
Cu2 O7 H7A 124(2) . .
Cu1 O7 H7B 112(2) . .
Cu2 O7 H7B 103(2) . .
H7A O7 H7B 111(3) . .
Cu2 O9 H9A 126(2) . .
Cu2 O9 H9B 121(2) . .
H9A O9 H9B 105(3) . .
O6 C12 O5 126.0(2) . .
O6 C12 C14 117.6(2) . .
O5 C12 C14 116.4(2) . .
C19 C13 C17 110.8(2) . .
C19 C13 H13A 109.5 . .
C17 C13 H13A 109.5 . .
C19 C13 H13B 109.5 . .
C17 C13 H13B 109.5 . .
H13A C13 H13B 108.1 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C17 C15 C16 112.9(2) . .
C17 C15 H15A 109.0 . .
C16 C15 H15A 109.0 . .
C17 C15 H15B 109.0 . .
C16 C15 H15B 109.0 . .
H15A C15 H15B 107.8 . .
C18 C16 C15 114.7(2) . .
C18 C16 H16A 108.6 . .
C15 C16 H16A 108.6 . .
C18 C16 H16B 108.6 . .
C15 C16 H16B 108.6 . .
H16A C16 H16B 107.6 . .
C15 C17 C13 113.9(2) . .
C15 C17 H17A 108.8 . .
C13 C17 H17A 108.8 . .
C15 C17 H17B 108.8 . .
C13 C17 H17B 108.8 . .
H17A C17 H17B 107.7 . .
C20 C18 C16 113.3(2) . .
C20 C18 H18A 108.9 . .
C16 C18 H18A 108.9 . .
C20 C18 H18B 108.9 . .
C16 C18 H18B 108.9 . .
H18A C18 H18B 107.7 . .
C13 C19 S3 113.94(18) . .
C13 C19 H19A 108.8 . .
S3 C19 H19A 108.8 . .
C13 C19 H19B 108.8 . .
S3 C19 H19B 108.8 . .
H19A C19 H19B 107.7 . .
C18 C20 C21 114.8(3) . .
C18 C20 H20A 108.6 . .
C21 C20 H20A 108.6 . .
C18 C20 H20B 108.6 . .
C21 C20 H20B 108.6 . .
H20A C20 H20B 107.5 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5 1.9576(15) 2_667
Cu1 O5 1.9576(15) .
Cu1 O4 1.9773(14) .
Cu1 O4 1.9773(14) 2_667
Cu1 O7 2.3231(16) 2_667
Cu1 O7 2.3231(16) .
Cu1 Cu2 3.0258(3) 2_667
Cu1 Cu2 3.0258(3) .
Cu2 O6 1.9445(16) .
Cu2 O4 1.9582(15) 2_767
Cu2 O9 1.9604(17) .
Cu2 O4 1.9678(15) .
Cu2 O7 2.3760(17) .
Cu2 Cu2 3.0011(6) 2_767
S3 O8 1.4452(17) .
S3 O11 1.4627(16) .
S3 O10 1.4626(16) .
S3 C19 1.768(3) .
O4 Cu2 1.9581(15) 2_767
O4 H4 0.776(17) .
O5 C12 1.263(3) .
O6 C12 1.262(3) .
O7 H7A 0.780(17) .
O7 H7B 0.761(17) .
O9 H9A 0.774(17) .
O9 H9B 0.790(17) .
C12 C14 1.498(3) .
C13 C19 1.524(3) .
C13 C17 1.530(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C17 1.520(4) .
C15 C16 1.521(4) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 C18 1.519(4) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 C20 1.513(4) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C21 1.521(4) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H4 O8 . 2.686(2) 0.78(2) 1.91(2) 176(2) no
O7 H7A O10 2_767 2.784(2) 0.78(2) 2.01(2) 174(3) no
O7 H7B O11 1_545 2.842(3) 0.76(3) 2.10(2) 164(3) no
O9 H9A O11 1_645 2.683(2) 0.774(18) 1.916(18) 171(3) no
O9 H9B O10 1_545 2.793(3) 0.79(3) 2.01(3) 175(3) no
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
Cu2 O6 C12 O5 10.8(3)
Cu2 O6 C12 C14 -166.98(16)
Cu1 O5 C12 O6 2.5(3)
Cu1 O5 C12 C14 -179.71(16)
C17 C15 C16 C18 175.6(3)
C16 C15 C17 C13 178.8(2)
C19 C13 C17 C15 173.4(2)
C15 C16 C18 C20 176.9(3)
C17 C13 C19 S3 -177.71(19)
O8 S3 C19 C13 58.7(2)
O11 S3 C19 C13 -61.8(2)
O10 S3 C19 C13 -179.67(19)
C16 C18 C20 C21 177.6(3)
