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_4321574
_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 Mo~3~(SnCl~3~)OS~3~(S~2~P(OC~2~H~5~)~3~(C~5~H~5~N)~3~ was
synthesized from the reaction of molybdenum cluster
Mo~3~OS~3~(S~2~P(OC~2~H~5~)~4~H~2~O with SnCl~2~(H~2~O)~2~,
(C~6~H~5~)~3~PNP(C~6~H~5~)~3~Cl and pyridine.
;
_chemical_formula_moiety         'C27 H45 Cl3 Mo3 N3 O7 P3 S9 Sn'
_chemical_formula_structural     Mo3OS3(SnCl3)(S2P(OC2H5)2)3(C5H5N)3
_chemical_formula_sum            'C27 H45 Cl3 Mo3 N3 O7 P3 S9 Sn'
_chemical_formula_weight         1417.97
_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                84.0540(10)
_cell_angle_beta                 87.0950(10)
_cell_angle_gamma                84.5170(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7423(2)
_cell_length_b                   14.03570(10)
_cell_length_c                   16.9346(2)
_cell_measurement_reflns_used    7403
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2
_cell_volume                     2525.82(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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10270
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.883
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  .716
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_obs          0.0377
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+5.0408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1034
_refine_ls_wR_factor_obs         0.0932
_reflns_number_observed          5584
_reflns_number_total             6916
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990750d_1.cif
_cod_data_source_block           Mo3(SnCl3)OS3(dtp)3(py)3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+5.0408P] 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^)+(0.0466P)^2^+5.0408P] where P=(Fo^2^+2Fc^2^)/3'.

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

2020-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C54 H90 Cl6 Mo6 N6 O14 P6 S18 Sn2'
_cod_original_formula_weight         2835.94
_cod_original_formula_moiety         'C54 H90 Cl6 Mo6 N6 O14 P6 S18 Sn2'
_cod_original_formula_units_Z            1
_cod_database_code               4321574