New Paramagnetic Re(II) Compounds with Nitrile and Cyanide Ligands Prepared by Homolytic Scission of Dirhenium Complexes
Eric J. Schelter; Jitendra K. Bera; John Bacsa; José Ramón Galán-Mascarós; Kim R. Dunbar; Inorganic Chemistry 42 (2003) 4256–4258; doi:10.1021/ic020661s

data_4313852
_publ_contact_author_address
;   Department of Chemistry
     Texas A&M University
     P.O. Box 30012
     College Station
     tx 77842-3012
     USA
;
_publ_contact_author_email       dunbar@mail.chem.tamu.edu
_publ_contact_author_fax         '+1 979 8457177'
_publ_contact_author_name        '   Kim R. Dunbar'
_publ_contact_author_phone       '+1 979 8455235'
_publ_section_title
;
 New Paramagnetic Re(II) Compounds with Nitrile and Cyanide Ligands
 Prepared by Homolytic Scission of Dirhenium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4256
_journal_page_last               4258
_journal_paper_doi               10.1021/ic020661s
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C47 H48 N3 P3 Re, 2(F6 P)'
_chemical_formula_sum            'C47 H48 N3 P5 Re'
_chemical_formula_weight         1223.93
_chemical_name_systematic
;
  ?
;
_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-97
_cell_angle_alpha                90
_cell_angle_beta                 106.67(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.429(3)
_cell_length_b                   18.750(4)
_cell_length_c                   19.823(4)
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      21.463
_cell_measurement_theta_min      2.171
_cell_volume                     4781.5(19)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0749
_diffrn_reflns_av_sigmaI/netI    0.1064
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27516
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    2.794
_exptl_absorpt_correction_T_max  0.8393
_exptl_absorpt_correction_T_min  0.5759
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.795
_refine_diff_density_min         -2.530
_refine_diff_density_rms         0.229
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       0.00035(14)
_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_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         10783
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.135
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2178
_reflns_number_gt                7398
_reflns_number_total             10783
_reflns_threshold_expression     I>2\\s(I)
_cod_data_source_file            ic020661s_s1_3.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/c'
_cod_database_code               4313852