Direct Synthesis of Ligand-Based Radicals by the Addition of Bipyridine to Chromium(II) Compounds
Wen Zhou; Addison N. Desnoyer; James A. Bailey; Brian O. Patrick; Kevin M. Smith; Inorganic Chemistry 52 (2013) 2271–2273; doi:10.1021/ic302590g

data_4334025
_publ_section_title
;
 Direct Synthesis of Ligand-Based Radicals by the Addition of Bipyridine
 to Chromium(II) Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2271
_journal_page_last               2273
_journal_paper_doi               10.1021/ic302590g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C40 H62 Cr N2 O4'
_chemical_formula_weight         686.92
_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                90.00
_cell_angle_beta                 98.6660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1700(4)
_cell_length_b                   25.4150(12)
_cell_length_c                   18.1110(8)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5475
_cell_measurement_theta_min      2.784
_cell_volume                     4627.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36932
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.986
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         10684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.1432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                7621
_reflns_number_total             10684
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302590g_si_002_2.cif
_cod_data_source_block           1a_tBuAcac2_tBuBpy
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334025