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_4321576
_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 ((C2H5)4N)Mo3(SnCl3)OS3(S2P(OC2H5)2)2(OOCCH3)2(C5H5N) was 
synthesized from the reaction of trimolybdenum cluster 
Mo3OS3(S2P(OC2H5)2)2(OOCCH3)2(C5H5N) with SnCl2 in the presences of Et4NCl and 
pyridine. 
;
_chemical_formula_moiety         'C25 H51 Cl3 Mo3 N2 O9 P2 S7 Sn'
_chemical_formula_structural
((C2H5)4N)Mo3(SnCl3)OS3(S2P(OC2H5)2)2(OOCCH3)2(C5H5N)2
_chemical_formula_sum            'C25 H51 Cl3 Mo3 N2 O9 P2 S7 Sn'
_chemical_formula_weight         1322.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 97.3710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0852(5)
_cell_length_b                   15.1324(5)
_cell_length_c                   23.2691(7)
_cell_measurement_reflns_used    7324
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      1.60
_cell_volume                     4918.7(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_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 P4'
_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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18854
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5808
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.004
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_obs          0.0487
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+4.3539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1362
_refine_ls_wR_factor_obs         0.1199
_reflns_number_observed          4970
_reflns_number_total             7018
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990750d_3.cif
_cod_data_source_block           (Et4N)[Mo3(SnCl3)OS3(OAc)2(dtp)2(py)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+4.3539P] 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^)+(0.0735P)^2^+4.3539P] 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               4321576