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_4323439
_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        synthesis
_chemical_formula_sum            'C55.5 H52 Mo P4 Se2'
_chemical_formula_weight         1096.71
_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                 98.541(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   49.566(9)
_cell_length_b                   10.9765(15)
_cell_length_c                   18.282(3)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      13
_cell_volume                     9836(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo Kalpha'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7073
_diffrn_reflns_theta_max         22.92
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.914
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.907
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         6811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_obs          0.0606
_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^)+(0.1055P)^2^+97.4401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1968
_refine_ls_wR_factor_obs         0.1744
_reflns_number_observed          4974
_reflns_number_total             6811
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_6.cif
_cod_data_source_block           MoSe2dppe2_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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^)+(0.1055P)^2^+97.4401P] 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^)+(0.1055P)^2^+97.4401P] 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        9836.0(26)
_cod_original_formula_sum        'C55.50 H52 Mo P4 Se2'
_cod_database_code               4323439