Mononuclear Molybdenum(IV) Complexes with Two Multiply Bonded Chalcogen Ligands in Trans Configuration and Chelating Biphosphine Ligands
F. Albert Cotton; Günter Schmid; Inorganic Chemistry 36 (1997) 2267–2278; doi:10.1021/ic961071v

data_4323440
_publ_section_title
;
 Mononuclear Molybdenum(IV) Complexes with Two Multiply Bonded Chalcogen
 Ligands in Trans Configuration and Chelating Biphosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2267
_journal_page_last               2278
_journal_paper_doi               10.1021/ic961071v
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'data were measured by Sanjay K. Mandel'
_chemical_formula_moiety         'C52 H44 Mo O P4 S'
_chemical_formula_sum            'C52 H44 Mo O P4 S'
_chemical_formula_weight         936.75
_chemical_name_common            trans-Mo(O)(S)(dppee)~2~
_chemical_name_systematic
; 
 trans-bis(cis-1,2-bis(diphenylphosphino)ethylene-P,P')-oxo-sulfido-
 molybdenum (IV) 
;
_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                75.300(10)
_cell_angle_beta                 85.930(10)
_cell_angle_gamma                63.210(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0400(10)
_cell_length_b                   10.5630(10)
_cell_length_c                   12.162(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.5
_cell_measurement_theta_min      29
_cell_volume                     1112.3(3)
_computing_cell_refinement       'TEXSAN-TEXRAY, MSC 1985'
_computing_data_collection       'TEXSAN-TEXRAY, MSC 1985'
_computing_data_reduction        'TEXSAN-TEXRAY, MSC 1985'
_computing_molecular_graphics    'ORTEP, ULM 1992'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'MSC-Rigaku AFC5R'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3313
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         3.76
_diffrn_standards_decay_%        unknown
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  'based on count'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.504
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   'empirical \Y-scan corrections'
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not done'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.102
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    'AFIX 43, common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_obs          0.0299
_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^)+(0.0000P)^2^+0.7276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0981
_refine_ls_wR_factor_obs         0.0980
_reflns_number_observed          3293
_reflns_number_total             3313
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_7.cif
_cod_data_source_block           MoOSdppee2_7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (11 times).

'_geom_bond_publ_flag' value 'N'
changed to 'n' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (24
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (19 times).

'_geom_angle_publ_flag'
value 'N' changed to 'n' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(38 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not done' 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^)+(0.0000P)^2^+0.7276P] 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^)+(0.0000P)^2^+0.7276P] 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        1112.3(2)
_cod_database_code               4323440