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_7028186
_publ_section_title
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 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+
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_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            'C24 H49 Mo N18 O0.5 S16 W3'
_chemical_formula_weight         1758.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.759(6)
_cell_length_b                   22.759(6)
_cell_length_c                   22.759(6)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.1
_cell_measurement_theta_min      9.7
_cell_volume                     11789(5)
_computing_cell_refinement       CD4CA0
_computing_data_collection       CD4CA0
_computing_data_reduction        CADDAT
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXL-93 and local programs'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_sigmaI/netI    0.4713
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5312
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.650
_exptl_absorpt_correction_T_max  1.109
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_description       prism
_exptl_crystal_F_000             6744
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.000036(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.606
_refine_ls_goodness_of_fit_obs   0.963
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2454
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.606
_refine_ls_restrained_S_obs      0.962
_refine_ls_R_factor_all          0.1810
_refine_ls_R_factor_obs          0.0351
_refine_ls_shift/esd_max         1.850
_refine_ls_shift/esd_mean        0.370
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0093P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0646
_refine_ls_wR_factor_obs         0.0523
_reflns_number_observed          781
_reflns_number_total             2454
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            j803396sup1.cif
_cod_data_source_block           mow3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0093P)^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^)+( 0.0093P)^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_cell_volume        11788.5(54)
_cod_original_formula_sum        'C24 H49 Mo N18 O0.50 S16 W3'
_cod_database_code               7028186