Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 2. Reactions of Mo2Cl4(NHEt2)4 with Monodentate and Bidentate Phosphines. New Type of Compounds Mo2Cl4(diphosphine)4
F. Albert Cotton; Evgeny V. Dikarev; Santiago Herrero; Inorganic Chemistry 38 (1999) 490–495; doi:10.1021/ic980972w

data_4321772
_publ_section_title
;
 Mixed Chloride/Amine Complexes of Dimolybdenum(II,II). 2. Reactions of
 Mo2Cl4(NHEt2)4 with Monodentate and Bidentate Phosphines. New Type of
 Compounds Mo2Cl4(diphosphine)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              490
_journal_page_last               495
_journal_paper_doi               10.1021/ic980972w
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 Mo2 Cl4 ((C H3)2 P C H2 P (C H3)2)4
;
_chemical_formula_structural     Mo2Cl4(\h1-dmpm)4
_chemical_formula_sum            'C20 H56 Cl4 Mo2 P8'
_chemical_formula_weight         878.09
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Tetrachloro-tetrakis(bis(dimethylphosphino)methane-P)-
 -di-molybdenum(II)
;
_space_group_IT_number           181
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 64 2 (0 0 2)'
_symmetry_space_group_name_H-M   'P 64 2 2'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.396(1)
_cell_length_b                   12.396(1)
_cell_length_c                   21.960(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.62
_cell_measurement_theta_min      29.49
_cell_volume                     2922.3(4)
_computing_cell_refinement       'TEXAN-TEXRAY (1985)'
_computing_data_collection       'TEXAN-TEXRAY (1985)'
_computing_data_reduction        'TEXAN-TEXRAY (1985)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3354
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         4.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.988
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2100
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       0.00054(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_obs          0.0335
_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^)+(0.0546P)^2^+0.2209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0918
_refine_ls_wR_factor_obs         0.0891
_reflns_number_observed          1364
_reflns_number_total             1464
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980972w_2.cif
_cod_data_source_block           Mo2Cl4(\h1-dmpm)4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

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^)+(0.0546P)^2^+0.2209P] 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^)+(0.0546P)^2^+0.2209P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321772