#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/05/7000515.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_7000515
loop_
_publ_author_name
'Huang, Yu-Jian'
'Song, Ying-Lin'
'Chen, Yang'
'Li, Hong-Xi'
'Zhang, Yong'
'Lang, Jian-Ping'
_publ_section_title
;
 Formation of dimeric and polymeric W/Cu/S clusters via degradation or
 expansion of the cluster core in [Et4N]4[WS4Cu4I6]
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1411
_journal_paper_doi               10.1039/b816312j
_journal_year                    2009
_chemical_formula_moiety         '2(C21 H24 Cu2 N6 S4 W), H2 O'
_chemical_formula_sum            'C42 H50 Cu4 N12 O S8 W2'
_chemical_formula_weight         1617.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           152
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.9875(17)
_cell_length_b                   11.9875(17)
_cell_length_c                   32.248(6)
_cell_measurement_reflns_used    11222
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.15
_cell_volume                     4013.2(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'Shelxl-97 (Sheldrick, 1997)'
_computing_publication_material  'Shelxl-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            29323
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.201
_exptl_absorpt_correction_T_max  0.176
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2358
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.779
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details '2034 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.013(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0372P)²+9.8798P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                4315
_reflns_number_total             4857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816312j.txt
_cod_data_source_block           3
_cod_original_sg_symbol_Hall     'P 31 2'
_cod_database_code               7000515
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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
W1 W 0.29454(4) 1.11494(5) 1.218339(14) 0.03497(14) Uani 1 1 d . . .
Cu1 Cu 0.45566(14) 1.25222(15) 1.15761(5) 0.0434(4) Uani 1 1 d . . .
Cu2 Cu 0.10567(16) 0.96560(18) 1.26702(6) 0.0615(5) Uani 1 1 d . . .
S1 S 0.3332(3) 1.0336(3) 1.16211(10) 0.0485(8) Uani 1 1 d . . .
S2 S 0.4362(3) 1.3226(3) 1.22195(10) 0.0472(8) Uani 1 1 d . . .
S3 S 0.0969(3) 1.0840(5) 1.21560(12) 0.0687(11) Uani 1 1 d . . .
S4 S 0.3085(3) 1.0128(3) 1.27424(9) 0.0446(7) Uani 1 1 d . . .
O1 O 1.0000 1.7847(19) 1.1667 0.124 Uiso 1 2 d S . .
H1O1 H 1.0553 1.7782 1.1802 0.186 Uiso 0.50 1 d PR . .
H2O1 H 1.0162 1.8604 1.1686 0.186 Uiso 0.50 1 d PR . .
N1 N 0.8164(9) 1.4506(9) 1.1067(3) 0.041(2) Uani 1 1 d . . .
N2 N 0.6292(10) 1.3188(9) 1.1327(3) 0.039(2) Uani 1 1 d . . .
N3 N 1.3054(9) 1.4373(9) 1.0808(3) 0.045(2) Uani 1 1 d . . .
N4 N 1.3582(9) 1.3182(10) 1.1187(3) 0.045(3) Uani 1 1 d . . .
N5 N 0.9093(11) 1.2389(9) 0.9670(3) 0.046(2) Uani 1 1 d . . .
N6 N 0.8749(12) 1.0451(11) 0.9594(3) 0.059(3) Uani 1 1 d . . .
C1 C 1.0064(10) 1.5490(10) 1.0598(3) 0.032(2) Uani 1 1 d . . .
C2 C 1.1306(11) 1.5691(10) 1.0714(3) 0.035(3) Uani 1 1 d . . .
C3 C 1.1986(10) 1.5376(10) 1.0430(4) 0.037(3) Uani 1 1 d . . .
C4 C 1.1428(12) 1.4800(11) 1.0049(4) 0.041(3) Uani 1 1 d . . .
C5 C 1.0214(10) 1.4566(9) 0.9954(3) 0.032(2) Uani 1 1 d . . .
C6 C 0.9570(9) 1.4974(9) 1.0214(3) 0.030(3) Uani 1 1 d . . .
C7 C 0.9283(13) 1.5742(12) 1.0905(4) 0.050(3) Uani 1 1 d . . .
H7A H 0.8960 1.6254 1.0775 0.061 Uiso 1 1 calc R . .
H7B H 0.9828 1.6234 1.1135 0.061 Uiso 1 1 calc R . .
C8 C 1.1831(15) 1.6253(16) 1.1139(4) 0.073(5) Uani 1 1 d . . .
H8A H 1.2541 1.6126 1.1204 0.110 Uiso 1 1 calc R . .
H8B H 1.1166 1.5831 1.1343 0.110 Uiso 1 1 calc R . .
H8C H 1.2120 1.7158 1.1137 0.110 Uiso 1 1 calc R . .
C9 C 1.3239(12) 1.5519(12) 1.0576(4) 0.050(3) Uani 1 1 d . . .
H9A H 1.3788 1.5655 1.0338 0.060 Uiso 1 1 calc R . .
H9B H 1.3670 1.6272 1.0753 0.060 Uiso 1 1 calc R . .
C10 C 1.2150(16) 1.4367(16) 0.9765(5) 0.080(5) Uani 1 1 d . . .
H10A H 1.1548 1.3578 0.9630 0.119 Uiso 1 1 calc R . .
H10B H 1.2746 1.4232 0.9925 0.119 Uiso 1 1 calc R . .
H10C H 1.2612 1.5019 0.9560 0.119 Uiso 1 1 calc R . .
C11 C 0.9556(16) 1.3760(12) 0.9572(4) 0.066(5) Uani 1 1 d . . .
H11A H 0.8836 1.3870 0.9493 0.079 Uiso 1 1 calc R . .
H11B H 1.0159 1.4035 0.9342 0.079 Uiso 1 1 calc R . .
C12 C 0.8241(13) 1.4745(14) 1.0097(4) 0.059(4) Uani 1 1 d . . .
H12A H 0.7939 1.5092 1.0309 0.088 Uiso 1 1 calc R . .
H12B H 0.7655 1.3837 1.0071 0.088 Uiso 1 1 calc R . .
H12C H 0.8292 1.5162 0.9838 0.088 Uiso 1 1 calc R . .
C13 C 0.7072(11) 1.4394(12) 1.1201(4) 0.041(3) Uani 1 1 d . . .
H13A H 0.6877 1.5054 1.1207 0.050 Uiso 1 1 calc R . .
C14 C 0.6968(14) 1.2539(14) 1.1269(4) 0.052(3) Uani 1 1 d . . .
H14A H 0.6663 1.1677 1.1331 0.062 Uiso 1 1 calc R . .
C15 C 0.8134(12) 1.3357(12) 1.1109(4) 0.052(3) Uani 1 1 d . . .
H15A H 0.8782 1.3178 1.1041 0.062 Uiso 1 1 calc R . .
C16 C 1.3981(12) 1.4277(12) 1.1009(4) 0.050(3) Uani 1 1 d . . .
H16A H 1.4833 1.4941 1.1019 0.060 Uiso 1 1 calc R . .
C17 C 1.2290(12) 1.2500(13) 1.1084(5) 0.063(4) Uani 1 1 d . . .
H17A H 1.1716 1.1666 1.1171 0.075 Uiso 1 1 calc R . .
C18 C 1.1987(12) 1.3194(14) 1.0846(5) 0.073(5) Uani 1 1 d . . .
H18A H 1.1189 1.2927 1.0725 0.088 Uiso 1 1 calc R . .
C19 C 0.9221(15) 1.1572(14) 0.9427(4) 0.060(4) Uani 1 1 d . . .
H19A H 0.9606 1.1782 0.9167 0.073 Uiso 1 1 calc R . .
C20 C 0.8274(15) 1.0556(12) 0.9972(4) 0.059(4) Uani 1 1 d . . .
H20A H 0.7875 0.9899 1.0166 0.070 Uiso 1 1 calc R . .
C21 C 0.8478(13) 1.1759(12) 1.0017(4) 0.053(4) Uani 1 1 d . . .
H21A H 0.8243 1.2087 1.0240 0.064 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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'
W W -0.8490 6.8722 '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'
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
S2 W1 S3 110.32(16) . . ?
S2 W1 S1 109.12(12) . . ?
S3 W1 S1 109.64(15) . . ?
S2 W1 S4 110.49(12) . . ?
S3 W1 S4 107.97(14) . . ?
S1 W1 S4 109.28(12) . . ?
S2 W1 Cu2 131.30(10) . . ?
S3 W1 Cu2 54.28(12) . . ?
S1 W1 Cu2 119.58(10) . . ?
S4 W1 Cu2 53.99(9) . . ?
S2 W1 Cu1 55.28(9) . . ?
S3 W1 Cu1 117.37(11) . . ?
S1 W1 Cu1 54.79(9) . . ?
S4 W1 Cu1 134.64(9) . . ?
Cu2 W1 Cu1 169.54(6) . . ?
N2 Cu1 N4 105.9(4) . 1_455 ?
N2 Cu1 S1 115.5(3) . . ?
N4 Cu1 S1 108.0(3) 1_455 . ?
N2 Cu1 S2 119.7(3) . . ?
N4 Cu1 S2 102.8(3) 1_455 . ?
S1 Cu1 S2 103.86(13) . . ?
N2 Cu1 W1 146.6(3) . . ?
N4 Cu1 W1 107.5(3) 1_455 . ?
S1 Cu1 W1 52.53(9) . . ?
S2 Cu1 W1 52.19(9) . . ?
N6 Cu2 S4 128.4(4) 2_665 . ?
N6 Cu2 S3 122.8(4) 2_665 . ?
S4 Cu2 S3 108.19(14) . . ?
N6 Cu2 W1 167.3(4) 2_665 . ?
S4 Cu2 W1 54.58(8) . . ?
S3 Cu2 W1 53.92(10) . . ?
W1 S1 Cu1 72.69(10) . . ?
W1 S2 Cu1 72.53(10) . . ?
W1 S3 Cu2 71.80(12) . . ?
Cu2 S4 W1 71.43(11) . . ?
H1O1 O1 H2O1 107.7 . . ?
C13 N1 C15 109.9(11) . . ?
C13 N1 C7 124.2(11) . . ?
C15 N1 C7 125.9(11) . . ?
C13 N2 C14 106.1(10) . . ?
C13 N2 Cu1 125.8(8) . . ?
C14 N2 Cu1 128.0(8) . . ?
C16 N3 C18 104.9(10) . . ?
C16 N3 C9 125.4(10) . . ?
C18 N3 C9 129.6(10) . . ?
C16 N4 C17 103.3(10) . . ?
C16 N4 Cu1 130.7(9) . 1_655 ?
C17 N4 Cu1 125.9(8) . 1_655 ?
C19 N5 C21 108.1(11) . . ?
C19 N5 C11 125.4(11) . . ?
C21 N5 C11 126.5(10) . . ?
C19 N6 C20 105.1(11) . . ?
C19 N6 Cu2 126.1(10) . 3_564 ?
C20 N6 Cu2 128.4(9) . 3_564 ?
C6 C1 C2 119.1(10) . . ?
C6 C1 C7 121.0(10) . . ?
C2 C1 C7 119.8(10) . . ?
C3 C2 C1 118.7(10) . . ?
C3 C2 C8 122.9(11) . . ?
C1 C2 C8 118.4(11) . . ?
C2 C3 C4 120.5(10) . . ?
C2 C3 C9 116.7(11) . . ?
C4 C3 C9 122.3(11) . . ?
C5 C4 C3 119.4(10) . . ?
C5 C4 C10 121.7(12) . . ?
C3 C4 C10 118.8(12) . . ?
C4 C5 C6 121.1(9) . . ?
C4 C5 C11 118.0(11) . . ?
C6 C5 C11 120.7(11) . . ?
C1 C6 C5 120.9(9) . . ?
C1 C6 C12 118.5(10) . . ?
C5 C6 C12 120.4(10) . . ?
C1 C7 N1 111.7(9) . . ?
C1 C7 H7A 109.3 . . ?
N1 C7 H7A 109.3 . . ?
C1 C7 H7B 109.3 . . ?
N1 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C3 112.1(10) . . ?
N3 C9 H9A 109.2 . . ?
C3 C9 H9A 109.2 . . ?
N3 C9 H9B 109.2 . . ?
C3 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 C5 108.7(10) . . ?
N5 C11 H11A 110.0 . . ?
C5 C11 H11A 110.0 . . ?
N5 C11 H11B 110.0 . . ?
C5 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
C6 C12 H12A 109.5 . . ?
C6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 N2 109.4(11) . . ?
N1 C13 H13A 125.3 . . ?
N2 C13 H13A 125.3 . . ?
C15 C14 N2 109.2(12) . . ?
C15 C14 H14A 125.4 . . ?
N2 C14 H14A 125.4 . . ?
C14 C15 N1 105.5(12) . . ?
C14 C15 H15A 127.3 . . ?
N1 C15 H15A 127.3 . . ?
N4 C16 N3 113.7(11) . . ?
N4 C16 H16A 123.1 . . ?
N3 C16 H16A 123.1 . . ?
C18 C17 N4 110.5(11) . . ?
C18 C17 H17A 124.7 . . ?
N4 C17 H17A 124.7 . . ?
C17 C18 N3 107.4(11) . . ?
C17 C18 H18A 126.3 . . ?
N3 C18 H18A 126.3 . . ?
N6 C19 N5 112.0(12) . . ?
N6 C19 H19A 124.0 . . ?
N5 C19 H19A 124.0 . . ?
C21 C20 N6 109.3(12) . . ?
C21 C20 H20A 125.4 . . ?
N6 C20 H20A 125.4 . . ?
N5 C21 C20 105.6(12) . . ?
N5 C21 H21A 127.2 . . ?
C20 C21 H21A 127.2 . . ?
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
W1 S2 2.206(3) . ?
W1 S3 2.209(3) . ?
W1 S1 2.214(3) . ?
W1 S4 2.232(3) . ?
W1 Cu2 2.5965(18) . ?
W1 Cu1 2.6637(16) . ?
Cu1 N2 1.987(10) . ?
Cu1 N4 2.118(9) 1_455 ?
Cu1 S1 2.280(4) . ?
Cu1 S2 2.295(4) . ?
Cu2 N6 1.914(11) 2_665 ?
Cu2 S4 2.216(4) . ?
Cu2 S3 2.219(5) . ?
O1 H1O1 0.8301 . ?
O1 H2O1 0.8300 . ?
N1 C13 1.321(15) . ?
N1 C15 1.366(16) . ?
N1 C7 1.510(16) . ?
N2 C13 1.333(15) . ?
N2 C14 1.388(16) . ?
N3 C16 1.341(15) . ?
N3 C18 1.357(16) . ?
N3 C9 1.481(15) . ?
N4 C16 1.287(15) . ?
N4 C17 1.383(16) . ?
N4 Cu1 2.118(9) 1_655 ?
N5 C19 1.321(16) . ?
N5 C21 1.345(15) . ?
N5 C11 1.482(15) . ?
N6 C19 1.286(17) . ?
N6 C20 1.379(17) . ?
N6 Cu2 1.914(11) 3_564 ?
C1 C6 1.380(14) . ?
C1 C2 1.434(15) . ?
C1 C7 1.492(16) . ?
C2 C3 1.398(16) . ?
C2 C8 1.516(17) . ?
C3 C4 1.406(17) . ?
C3 C9 1.499(16) . ?
C4 C5 1.371(16) . ?
C4 C10 1.518(17) . ?
C5 C6 1.383(14) . ?
C5 C11 1.521(15) . ?
C6 C12 1.522(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9300 . ?
C14 C15 1.346(17) . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 C18 1.309(17) . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C21 1.344(17) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
