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_4323441
_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: SO2 + Mo(N2)2(dppee)2'
_chemical_formula_analytical     'FAB mass spec: M+ - SO'
_chemical_formula_moiety         'C52 H44 Mo O4 P4 S2'
_chemical_formula_structural
;
  'Mo (S O2)2 ( (C6 H5)2 P C H C H P (C6 H5)2 )2' 
;
_chemical_formula_sum            'C52 H44 Mo O4 P4 S2'
_chemical_formula_weight         1016.81
_chemical_name_common            trans-Mo(\h-SO~2~)~2~(dppee)~2~
_chemical_name_systematic
; 
trans-bis(cis-1,2-bis(diphenylphosphino)ethylene-P,P')
                   -bis-(\h~2~(S,O)-sulfur dioxide)molybdenum (0) 
;
_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                 118.480(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.534(6)
_cell_length_b                   12.4271(13)
_cell_length_c                   19.550(5)
_cell_measurement_reflns_used    '197 (4 times 50, 3 skipped)'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.7
_cell_measurement_theta_min      14.1
_cell_volume                     4598.6(19)
_computing_cell_refinement       'LCR out of ULM package'
_computing_data_collection       'CAD4 - software'
_computing_data_reduction        STP
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2/6\q
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5064
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   'empirical \Y-scan correction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not done'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.663
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment    'CH-free, Ph-H AFIX 43, common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_obs          0.0299
_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^)+(0.0355P)^2^+7.7181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0806
_refine_ls_wR_factor_obs         0.0751
_reflns_number_observed          3418
_reflns_number_total             4036
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_8.cif
_cod_data_source_block           MoSO2_2_dppee2_8
_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 (13 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 (26 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
(39 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^)+(0.0355P)^2^+7.7181P] 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^)+(0.0355P)^2^+7.7181P] 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        4598.4(18)
_cod_database_code               4323441