A 1:2 Adduct of Tetrakis(μ-thiobenzoato-<i>O</i>,<i>S</i>)dimolybdenum(II)(<i>Mo{—</i>Mo}) with Triphenylphosphine Oxide, [Mo~2~(C~7~H~5~OS)~4~].2[(C~6~H~5~)~3~OP]
Cindrić, M.; Vrdoljak, V.; Matković-Čalogović, D.; Kamenar, B.; Acta Crystallographica Section C 52 (1996) 3016–3018; doi:10.1107/S0108270196010293

data_2005803
_publ_contact_author
;
      Professor Boris Kamenar
      Laboratory of General and Inorganic Chemistry
      Faculty of Science, University of Zagreb
      Ul. kralja Zvonimira 8
      10000 Zagreb, Croatia
;
_publ_section_title
;A 1:2 Adduct of
 Tetrakis(\m-thiobenzoato-<i>O</i>,<i>S</i>)dimolybdenum(II)(<i>Mo{---</i>Mo})
 with Triphenylphosphine Oxide, [Mo~2~(C~7~H~5~OS)~4~].2[(C~6~H~5~)~3~OP]
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              3016
_journal_page_last               3018
_journal_paper_doi               10.1107/S0108270196010293
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Mo2 (C7 H5 O S)4] , 2C18 H15 O P'
_chemical_formula_moiety         '[Mo2 (C6 H5 C O S)4] , 2[(C6 H5)3 O P]'
_chemical_formula_structural     '(Mo2 (C6 H5 C O S)4 ((C6 H5)3 P O)2'
_chemical_formula_sum            'C64 H50 Mo2 O6 P2 S4'
_chemical_formula_weight         1297.1
_chemical_name_systematic
;
Tetrakis(\m-thiobenzoato-O,S)bis(triphenylphosphineoxide-O)dimolybdenum(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.936(2)
_cell_length_b                   20.053(3)
_cell_length_c                   12.306(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      7.6
_cell_volume                     2940.0(10)
_computing_cell_refinement       STADI-4
_computing_data_collection       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_reduction        'XRED (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'ORTEX5 (McArdle, 1996)'
_computing_publication_material  SHELXL96
_computing_structure_refinement  'SHELXL96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device
'Philips PW1100 diffractometer updated by Stoe'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  'Planar Graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6043
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        4.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         '1.01 (close to Mo)'
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.974
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_obs          0.0494
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0494P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1144
_refine_ls_wR_factor_obs         0.0933
_reflns_number_observed          3213
_reflns_number_total             5731
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1284.cif
_cod_data_source_block           text
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0494P)^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^)+(0.0494P)^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_sg_symbol_H-M      'P 21/c'
_cod_database_code               2005803