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_4301099
_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_formula_moiety         C52H32Mn2N2O6,C18H36KN2O6,C4H8O
_chemical_formula_sum            'C74 H76 K Mn2 N4 O13'
_chemical_formula_weight         1378.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.8240(10)
_cell_angle_beta                 84.8320(10)
_cell_angle_gamma                75.6350(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6590(10)
_cell_length_b                   15.8380(10)
_cell_length_c                   17.6010(10)
_cell_measurement_reflns_used    10450
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     3364.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega 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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39225
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.9236
_exptl_absorpt_correction_T_min  0.8971
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1442
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0007(6)
_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   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         19599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                14843
_reflns_number_total             19599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801434h_si_001_5.cif
_cod_data_source_block           '[K(222)][3a]_thf'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4301099