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_4323006
_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 [Bu4N]2Re2Cl8 with (Ph2P)2Py in 
 methanol. Green solid was precipitated after 10 hours of reflux. Crystals 
 were obtained from CH2Cl2 solution layered with hexanes.
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Re2 Cl4 (((C6 H5)2 P)2 N1 C5 H3)2'
_chemical_formula_structural     Re2Cl4((Ph2P)2Py)2
_chemical_formula_sum            'C58 H46 Cl4 N2 P4 Re2'
_chemical_formula_weight         1409.05
_chemical_melting_point          ?
_chemical_name_systematic
; 
 bis (/m-2,6-bis(diphenylphosphino)-pyridine-N,P)-tetrachloro-di-rhenium (II) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.17(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.173(2)
_cell_length_b                   11.285(1)
_cell_length_c                   28.771(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      14.36
_cell_measurement_theta_min      10.46
_cell_volume                     5220.6(11)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 V.5 (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_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      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7066
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 600
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.002
_exptl_absorpt_correction_T_max  0.9986
_exptl_absorpt_correction_T_min  0.5471
_exptl_absorpt_correction_type   'empirical, via \y scans'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         6780
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_obs          0.0372
_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^)+(0.0223P)^2^+14.6462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0961
_refine_ls_wR_factor_obs         0.0766
_reflns_number_observed          4071
_reflns_number_total             6780
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980455d_3.cif
_cod_data_source_block           Re2Cl4(bdppp)2
_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^)+(0.0223P)^2^+14.6462P] 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^)+(0.0223P)^2^+14.6462P] 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        5221(1)
_cod_database_code               4323006