Preparation, structure and properties of three [MoxW4−xS4(H2O)12]5+ (x = 1‒3) and [MoW3Se4(H2O)12]5+ cuboidal complexes alongside [Mo4S4(H2O)12]5+ and [Mo4Se4(H2O)12]5+
McLean, Iain J.; Hernandez-Molina, Rita; Sokolov, Maxim N.; Seo, Mi-Sook; Virovets, Alexander V.; Elsegood, Mark R. J.; Clegg, William; Sykes, A. Geoffrey; Journal of the Chemical Society, Dalton Transactions  (1998) 2557–; doi:10.1039/a803396j

data_7028185
_publ_section_title
;
 Preparation, structure and properties of three
 [MoxW4&#x2212;xS4(H2O)12]5+ (x&#x2005;=&#x2005;1--3) and
 [MoW3Se4(H2O)12]5+ cuboidal complexes alongside [Mo4S4(H2O)12]5+ and
 [Mo4Se4(H2O)12]5+
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2557
_journal_paper_doi               10.1039/a803396j
_journal_year                    1998
_chemical_formula_sum            'C42 H103 Mo O46 S10 W3'
_chemical_formula_weight         2312.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 110.311(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8310(7)
_cell_length_b                   31.0531(17)
_cell_length_c                   19.7278(10)
_cell_measurement_reflns_used    16553
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.20
_cell_volume                     7946.2(7)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29322
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.841
_exptl_absorpt_correction_T_max  0.263
_exptl_absorpt_correction_T_min  0.209
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4588
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.522
_refine_diff_density_min         -1.636
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       0.000037(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9508
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                7366
_reflns_number_total             9508
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            j803396sup1.cif
_cod_data_source_block           ags25
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7028185