Reaction of Re2(μ-O2CCH3)4Cl2 with Bis(dicyclohexylphosphino)methane (dcpm): Isolation of the Mixed-Valent Complex O3ReReCl(η2-dcpm)2 Containing an Unsupported Re-Re Bond
Jitendra K. Bera; Phillip E. Fanwick; Richard A. Walton; Inorganic Chemistry 40 (2001) 2914–2917; doi:10.1021/ic0100471

data_4319799
_publ_contact_author_address
;    Department of Chemistry
      Purdue University
      W. Lafayette
      IN 47907
      USA
;
_publ_contact_author_email       rawalton@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Richard A. Walton'
_publ_contact_author_phone       1(765)4945464
_publ_section_title
;
 Reaction of Re2(\m-O2CCH3)4Cl2 with Bis(dicyclohexylphosphino)methane
 (dcpm): Isolation of the Mixed-Valent Complex O3ReReCl(\h2-dcpm)2
 Containing an Unsupported Re-Re Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2914
_journal_page_last               2917
_journal_paper_doi               10.1021/ic0100471
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C51 H94 Cl3 O3 P4 Re2'
_chemical_formula_weight         1357.97
_chemical_name_systematic        ' ?'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             4-08-00
_audit_creation_method           from_MolEN_and_SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0179(4)
_cell_length_b                   22.8589(5)
_cell_length_c                   13.5102(7)
_cell_measurement_reflns_used    34524
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5564.4(3)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
     ORTEP (Johnson, 1976)
     Xtal_GX (Hall, 1995)
     PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    Direct_methods_(Shelxs97,_Sheldrick,_1997)
_diffrn_ambient_temperature      150
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34524
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    4.703
_exptl_absorpt_correction_T_max  0.3904
_exptl_absorpt_correction_T_min  0.3299
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.62
_exptl_crystal_description       needle
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.38
_refine_diff_density_min         -1.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6464
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+27.3572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.106
_reflns_number_gt                10031
_reflns_number_total             12622
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic0100471.cif
_cod_data_source_block           SDC25R
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5564.4(5)
_cod_original_sg_symbol_H-M      'p n m a'
_cod_database_code               4319799