Ligand Exchange or Reduction at Multiply Bonded Dimetal Units of Molybdenum and Rhenium by 2,6-Bis(diphenylphosphino)pyridine
F. Albert Cotton; Evgeny V. Dikarev; Glenn T. Jordan; Carlos A. Murillo; Marina A. Petrukhina; Inorganic Chemistry 37 (1998) 4611–4616; doi:10.1021/ic980455d

data_4323005
_publ_section_title
;
 Ligand Exchange or Reduction at Multiply Bonded Dimetal Units of
 Molybdenum and Rhenium by 2,6-Bis(diphenylphosphino)pyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4611
_journal_page_last               4616
_journal_paper_doi               10.1021/ic980455d
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
; 
 Compound was obtained by reflux of K4Mo2Cl8 with (Ph2P)2Py ligand 
 in methanol. Green solid precipitated after 10 hours of reflux. Crystals 
 were grown from CH2Cl2 solution layered with hexanes. 
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 Mo2 Cl4 (((C6 H5)2 P)2 N1 C5 H3)2, 2(C1 H2 Cl2)
;
_chemical_formula_structural     'Mo2Cl4((Ph2P)2Py)2, 2CH2Cl2'
_chemical_formula_sum            'C60 H50 Cl8 Mo2 N2 P4'
_chemical_formula_weight         1398.38
_chemical_melting_point          ?
_chemical_name_systematic
; 
 bis(/m-2,6-bis(Diphenylphosphino)-pyridine-N,P)-tetrachloro-di-molybdenum (II),
 dichloromethane solvate 
;
_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                 98.178(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.475(2)
_cell_length_b                   11.5958(7)
_cell_length_c                   16.7637(6)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    242(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     2977.6(4)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_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      242(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_sigmaI/netI    0.1053
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3551
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.14
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_obs   1.213
_refine_ls_hydrogen_treatment    allref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         3426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.213
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_obs          0.0518
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1479
_refine_ls_wR_factor_obs         0.1341
_reflns_number_observed          2489
_reflns_number_total             3551
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980455d_2.cif
_cod_data_source_block           Mo2Cl4(bdppp)2,2(CH2Cl2)
_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^)+(0.0652P)^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^)+(0.0652P)^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_database_code               4323005