Synthesis and Characterization of Three Tetranuclear Clusters Containing a [Mo3OS3Sn]6+ Cubane-like Core
Rong-Min Yu; Shao-Fang Lu; Jian-Quan Huang; Xiao-Ying Huang; Qiang-Jin Wu; Da-Xu Wu; Inorganic Chemistry 39 (2000) 5348–5353; doi:10.1021/ic990750d

data_4321575
_publ_section_title
;
 Synthesis and Characterization of Three Tetranuclear Clusters Containing
 a [Mo3OS3Sn]6+ Cubane-like Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5348
_journal_page_last               5353
_journal_paper_doi               10.1021/ic990750d
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source
;         
The compound (C~6~H~5~)~3~PNP(C~6~H~5~)~3~[Mo~3~(SnCl~3~)OS~3~(dtp)~3~(OAc)(py)]
was synthesized from the reaction of trinuclear cluster 
[Mo~3~OS~3~(dtp)~3~(OAc)(py)] with SnCl~2~ (H~2~O)~2~, 
(C~6~H~5~)~3~PNP(C~6~H~5~)~3~Cl and pyridine.
;
_chemical_formula_moiety         'C55 H67 Cl3 Mo3 N2 O9 P5 S9 Sn'
_chemical_formula_structural     ((C6H5)3P)2N[Mo3(SnCl3)OS3(dtp)3(OAc)(py)]
_chemical_formula_sum            'C55 H67 Cl3 Mo3 N2 O9 P5 S9 Sn'
_chemical_formula_weight         1856.36
_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
_cell_angle_alpha                92.0830(10)
_cell_angle_beta                 97.9080(10)
_cell_angle_gamma                110.3370(10)
_cell_formula_units_Z            2
_cell_length_a                   12.95290(10)
_cell_length_b                   15.6324(2)
_cell_length_c                   19.63550(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2
_cell_volume                     3677.41(6)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14426
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .835
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1858
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         10254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_obs          0.0339
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+7.0773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0831
_refine_ls_wR_factor_obs         0.0770
_reflns_number_observed          8665
_reflns_number_total             10254
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990750d_2.cif
_cod_data_source_block           (PPN)[Mo3(SnCl3)OS3(dtp)3(OAc)(py)]
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+7.0773P] 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^)+(0.0296P)^2^+7.0773P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321575