Synthesis and Structural Characterizations of New Mononuclear and Dinuclear Molybdenum(V) Anions Containing Trithiocarbonate Ligands
C. Simonnet-Jégat; E. Cadusseau; R. Dessapt; F. Sécheresse; Inorganic Chemistry 38 (1999) 2335–2339; doi:10.1021/ic980907m

data_4321994
_publ_section_title
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 Synthesis and Structural Characterizations of New Mononuclear and
 Dinuclear Molybdenum(V) Anions Containing Trithiocarbonate Ligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2335
_journal_page_last               2339
_journal_paper_doi               10.1021/ic980907m
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H60 Mo N3 S12'
_chemical_formula_weight         919.45
_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                 102.9510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5249(5)
_cell_length_b                   11.8058(4)
_cell_length_c                   20.2942(5)
_cell_measurement_reflns_used    11176
_cell_measurement_temperature    296(2)
_cell_volume                     4325.5(2)
_computing_cell_refinement       'Bruker AXS SMART'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SMART'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device
'three-circle diffractometer with CCD area detector'
_diffrn_measurement_method       '3D profiles from omega 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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29192
_diffrn_reflns_theta_max         29.76
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  59.64
_exptl_absorpt_correction_T_min  3
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          .86
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         11176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_obs          0.0496
_refine_ls_shift/esd_max         -0.271
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+2.1768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1663
_refine_ls_wR_factor_obs         0.1416
_reflns_number_observed          7518
_reflns_number_total             11176
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980907m_1.cif
_cod_data_source_block           (NEt4)3[Mo(CS3)4]_compound1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+2.1768P] 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^)+(0.0906P)^2^+2.1768P] 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               4321994