Stable and Highly Persistent Quinoxaline-Centered Metalloorganic Radical Anions: Preparation, Structural, Spectroscopic, and Computational Investigations
Sylvie Choua; Jean-Pierre Djukic; Jérôme Dalléry; André Bieber; Richard Welter; Jean-Paul Gisselbrecht; Philippe Turek; Louis Ricard; Inorganic Chemistry 48 (2009) 149–163; doi:10.1021/ic801434h

data_4301096
_publ_contact_author_address
;Institut de Chimie de Strasbourg 
CNRS
Universite Louis Pasteur
4 rue Blaise Pascal 
67000 Strasbourg 
France
;
_publ_contact_author_email       choua@chimie.u-strasbg.fr
_publ_contact_author_name        'Sylvie CHOUA'
_publ_section_title
;
Stable and Highly Persistent Quinoxaline-Centered Metalloorganic Radical
Anions: Preparation, Structural, Spectroscopic, and Computational
Investigations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              149
_journal_page_last               163
_journal_paper_doi               10.1021/ic801434h
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C28 H12 N2 O8 Re2'
_chemical_formula_sum            'C28 H12 N2 O8 Re2'
_chemical_formula_weight         876.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.00
_cell_angle_beta                 90.930(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.693(3)
_cell_length_b                   13.087(3)
_cell_length_c                   13.326(4)
_cell_measurement_reflns_used    6481
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2562.1(11)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7480
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.39
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.497
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
_exptl_crystal_recrystallization_method diffusion
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.158
_refine_diff_density_min         -2.852
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                5743
_reflns_number_total             7480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801434h_si_001_2.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301096