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_4327687
_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            'C70 H112 Mo6 O76 S10 Se8 Sn'
_chemical_formula_weight         3816.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                63.032(2)
_cell_angle_beta                 76.024(2)
_cell_angle_gamma                86.799(2)
_cell_formula_units_Z            1
_cell_length_a                   12.1069(7)
_cell_length_b                   17.9192(10)
_cell_length_c                   18.3662(10)
_cell_measurement_reflns_used    12941
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.77
_cell_measurement_theta_min      2.18
_cell_volume                     3439.4(3)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.865
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26023
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.072
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_description       plate
_exptl_crystal_F_000             1874
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.512
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         15651
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                10738
_reflns_number_total             15651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9800472B_1.cif
_cod_data_source_block           ags22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0587P)^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^)+(0.0587P)^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 
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_cod_database_code               4327687