Preparation, Structure, and Reactivity of Heterometallic Sn-Containing Single- and Double-Cube Derivatives of [Mo3Se4(H2O)9]4+ and [W3Se4(H2O)9]4+
Rita Hernandez-Molina; Danil N. Dybtsev; Vladimir P. Fedin; Mark R. J. Elsegood; William Clegg; A. Geoffrey Sykes; Inorganic Chemistry 37 (1998) 2995–3001; doi:10.1021/ic980047+

data_4327688
_publ_section_title
;
 Preparation, Structure, and Reactivity of Heterometallic Sn-Containing
 Single- and Double-Cube Derivatives of [Mo3Se4(H2O)9]4+ and
 [W3Se4(H2O)9]4+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2995
_journal_page_last               3001
_journal_paper_doi               10.1021/ic980047+
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C21 H49 Cl3 Mo3 N15 O0.5 S9 Se4 Sn'
_chemical_formula_weight         1636.99
_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                 95.028(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.602(2)
_cell_length_b                   11.9783(6)
_cell_length_c                   21.7785(12)
_cell_measurement_reflns_used    22903
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.20
_cell_volume                     11070.8(10)
_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_measured_fraction_theta_full 0.473
_diffrn_measured_fraction_theta_max 0.428
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34805
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.260
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.372
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_description       plate
_exptl_crystal_F_000             6328
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.360
_refine_diff_density_min         -1.508
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         13135
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                9626
_reflns_number_total             13135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9800472B_2.cif
_cod_data_source_block           ags24
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0731P)^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^)+(0.0731P)^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        11070.9(10)
_cod_original_formula_sum        'C21 H49 Cl3 Mo3 N15 O0.50 S9 Se4 Sn'
_cod_database_code               4327688