A Trinuclear Cluster of Molybdenum(IV), Mo~3~(μ~3~-S)(μ~2~-S)~3~(HC~2~O~4~)~2~(C~2~O~4~)(H~2~O)~3~
Cotton, F. A.; Daniels, L. M.; Shang, M.; Llusar, R.; Schwotzer, W.; Acta Crystallographica Section C 52 (1996) 835–838; doi:10.1107/S0108270195013928

data_2004725
_publ_contact_author
;
 Prof. F.A. Cotton
 Department of Chemistry
 Mail Stop 3255
 Texas A&M University
 College Station, TX 77843
 USA
;
_publ_section_title
;
 A Trinuclear Cluster of Molybdenum(IV),
 Mo~3~(\m~3~-S)(\m~2~-S)~3~(HC~2~O~4~)~2~(C~2~O~4~)(H~2~O)~3~
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              835
_journal_page_last               838
_journal_paper_doi               10.1107/S0108270195013928
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac
'[Mo3 S4 (C2 H O4)2 (C2 O4) (H2 O)3] , 2C2 H6 O'
_chemical_formula_moiety         'C6 H8 Mo3 O15 S4, 2(C2 H6 O)'
_chemical_formula_sum            'C10 H20 Mo3 O17 S4'
_chemical_formula_weight         828.32
_chemical_name_systematic
;
triaquabis(O,O'-hydrogenoxalate)
(O,O'-oxalate)(\m^3^-sulfide)tris(\m^2^-sulfide)trimolybdenum(IV)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.38(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.403(5)
_cell_length_b                   6.5550(10)
_cell_length_c                   19.512(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      6.0
_cell_volume                     2461.1(11)
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P3 equivalent'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_sigmaI/netI    0.3068
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3294
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.919
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_description       platey
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.80(10)
_refine_diff_density_min         -0.70(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.825
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.845
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.1637
_refine_ls_R_factor_obs          0.0514
_refine_ls_shift/esd_max         -0.011
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1027
_refine_ls_wR_factor_obs         0.0931
_reflns_number_observed          1712
_reflns_number_total             3194
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1088.cif
_cod_data_source_block           mo3sulfoxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0356P)^2^] 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^)+(0.0356P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2461.0(10)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2004725