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_4313850
_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_formula_moiety
'C44 H39 N3 P3 Re, C8 H10 N, C2 H5 O, C2 H5, 2(C2 H3 N)'
_chemical_formula_sum            'C60 H65 N6 O P3 Re'
_chemical_formula_weight         1165.29
_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                 94.375(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.587(6)
_cell_length_b                   14.115(5)
_cell_length_c                   21.662(8)
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.102
_cell_measurement_theta_min      2.197
_cell_volume                     5667(3)
_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 0.950
_diffrn_measured_fraction_theta_max 0.950
_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  0.0860
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35519
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.052
_refine_diff_density_max         2.160
_refine_diff_density_min         -1.861
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       0.00011(9)
_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   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         13537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          4.924
_refine_ls_shift/su_mean         0.254
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020661s_s1_1.cif
_cod_data_source_block           compound_3
_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               4313850