Hexakis(dimethyl sulfoxide-κ<i>O</i>)zinc <i>mer</i>-aquatris(dimethyl sulfoxide-κ<i>O</i>)(ethanol-κ<i>O</i>)[octadecatungstodiphosphato(V)-κ<i>O</i>]zincate(II)‒dimethyl sulfoxide‒ethanol‒water (2/4/2/3)
Hammami, Imen; Ghandour, Yassine; Belkhiria, Mohamed Salah; IUCrData 1 (2016) x160406–; doi:10.1107/S2414314616004065

data_1542903
_publ_section_title
;
 Hexakis(dimethyl sulfoxide-\k<i>O</i>)zinc <i>mer</i>-aquatris(dimethyl
 sulfoxide-\k<i>O</i>)(ethanol-\k<i>O</i>)[octadecatungstodiphosphato(V)-\k<i>O</i>]zincate(II)--dimethyl
 sulfoxide--ethanol--water (2/4/2/3)
;
_journal_coeditor_code           XU4002
_journal_issue                   3
_journal_name_full               IUCrData
_journal_page_first              x160406
_journal_paper_doi               10.1107/S2414314616004065
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac
;
[Zn (C2 H6 O1 S1)6]2 [Zn (P2 W18 O62) (C2 H6 O1 S1)3 (C2 H6 O1) (H2 O1)],
2C2 H6 O S, C2 H6 O1, 1.5H2 O1
;
_chemical_formula_moiety
;
2(C12 H36 O6 S6 Zn 2+), C8 H26 O67 P2 S3 W18 Zn 4-, 2(C2 H6 O S),
C2 H6 O1, 1.5(H2 O1)
;
_chemical_formula_sum            'C38 H119 O83.5 P2 S17 W18 Zn3'
_chemical_formula_weight         6024.70
_chemical_name_systematic
;Hexakis(dimethyl sulfoxide-\k<i>O</i>)zinc(II)
<i>mer</i>-aquatris(dimethyl
sulfoxide-\k<i>O</i>)(ethanol-\k<i>O</i>)[octadecatungstodiphosphato(V)-\k<i>O</i>]zincate(II)--dimethyl sulfoxide--ethanol--water (2/4/2/3)
;
_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_creation_method           SHELXL-2014/7
_cell_angle_alpha                94.766(2)
_cell_angle_beta                 90.035(3)
_cell_angle_gamma                104.681(2)
_cell_formula_units_Z            2
_cell_length_a                   17.3770(10)
_cell_length_b                   18.889(8)
_cell_length_c                   19.705(6)
_cell_measurement_reflns_used    117368
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.075
_cell_measurement_theta_min      1.037
_cell_volume                     6233(3)
_computing_cell_refinement
;
DENZO/SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 2002)
;
_computing_data_reduction
;
<i>SORTAV</i> (Blessing, 1995),
CALC-OH (Nardelli (1999)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            117368
_diffrn_reflns_theta_full        27.103
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.057
_exptl_absorpt_coefficient_mu    17.501
_exptl_absorpt_correction_T_max  0.237
_exptl_absorpt_correction_T_min  0.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.210
_exptl_crystal_description       prism
_exptl_crystal_F_000             5478
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.216
_refine_diff_density_min         -3.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1459
_refine_ls_number_reflns         27441
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                19368
_reflns_number_total             27441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xu4002sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C38 H119 O83.50 P2 S17 W18 Zn3'
_cod_database_code               1542903
_shelx_estimated_absorpt_t_min   0.128
_shelx_estimated_absorpt_t_max   0.622
_shelx_hkl_checksum              655
_shelx_res_checksum              70974
_cod_database_fobs_code 1542903