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_4323434
_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        'Reac. of MoOCl(dppee)2/Li2S methanol/air'
_chemical_formula_analytical     'FAB (M+H)+ at 923u'
_chemical_formula_moiety         'C52 H44 Mo1 O2 P4, 2 (C H4 O)'
_chemical_formula_structural
;
 Mo (O)2 ( (C6 H5)2 P C H C H P (C6 H5)2 )2, 2 (C H3 O H)
;
_chemical_formula_sum            'C54 H52 Mo O4 P4'
_chemical_formula_weight         984.84
_chemical_name_common            'trans-Mo(O)~2~(dppee)~2~, 2 CH~3~OH'
_chemical_name_systematic
;
trans-bis(cis-1,2-bis(diphenylphosphino)ethylene-P,P')-di-oxo-molybdenum(IV) 
methanol solvate
;
_chemical_temperature_decomposition 433
_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'
_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                 110.999(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1340(15)
_cell_length_b                   18.435(2)
_cell_length_c                   12.515(2)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      13.0
_cell_volume                     2398.2(6)
_computing_cell_refinement       'LCR out of package ULM'
_computing_data_collection       'Enraf Nonius CAD4 software'
_computing_data_reduction        STP
_computing_molecular_graphics    'ORETP out package ULM'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'Mo in position 0.0 0.0 0.0'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3949
_diffrn_reflns_theta_max         23.94
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.9677
_exptl_absorpt_correction_type   \Y-Scans
_exptl_crystal_colour            'light yellow-orange'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not done'
_exptl_crystal_description       'thick plate with brownish inclusions'
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_obs          0.0323
_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^)+(0.0367P)^2^+2.1818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0872
_refine_ls_wR_factor_obs         0.0796
_reflns_number_observed          3045
_reflns_number_total             3759
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_1.cif
_cod_data_source_block           MoO2dppee2_1
_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 (10 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 (26
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 (14 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^)+(0.0367P)^2^+2.1818P] 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^)+(0.0367P)^2^+2.1818P] 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        2398.3(5)
_cod_database_code               4323434