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_4323438
_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
'Reaction: Mo(N2)2(dppe)2, 2 Bz2S3 in toluene'
_chemical_formula_analytical     'FAB mass spectrum: 958u (2NPOE)'
_chemical_formula_moiety         'C52 H48 Mo1 P4 S2, 0.5 (C7H8)'
_chemical_formula_structural
'Mo (S)2 ((C6H5)2P CH2 CH2 P(C6H5)2)2, 0.5 (CH3C6H5)'
_chemical_formula_sum            'C55.5 H52 Mo P4 S2'
_chemical_formula_weight         1002.91
_chemical_melting_point          214
_chemical_name_common            trans-Mo(S)2(dppe)2
_chemical_name_systematic
;
trans-bis(1,2-bis(diphenylphosphino)ethane-P,P')-bis-sulfido-molybdenum (IV), 
toluene solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.306(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   49.515(7)
_cell_length_b                   10.9286(12)
_cell_length_c                   18.203(3)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      13.4
_cell_volume                     9747(2)
_computing_cell_refinement       'LCR out of ULM package'
_computing_data_collection       SDP
_computing_data_reduction        SDP
_computing_molecular_graphics    'ORTEP out of ULM package'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990), Patterson'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8276
_diffrn_reflns_theta_max         23.90
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   'Mode FLAT, CAD4-Diffractometer'
_exptl_crystal_colour            darkgreen
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not determined'
_exptl_crystal_description       'very thin plate'
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    'CH2-H refined, Ph-H: AFIX 43, common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         6507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_obs          0.0395
_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^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1113
_refine_ls_wR_factor_obs         0.0951
_reflns_number_observed          5247
_reflns_number_total             7600
_cod_data_source_file            ic961071v_5.cif
_cod_data_source_block           MoS2dppe2_5
_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 (20 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 (74
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 (31 time).

'_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
(178 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 determined' 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^)+(0.0576P)^2^+0.0000P] 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^)+(0.0576P)^2^+0.0000P] 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        9747.1(26)
_cod_original_formula_sum        'C55.50 H52 Mo P4 S2'
_cod_database_code               4323438