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_4334026
_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            'C56 H66 B Cr N2 O4'
_chemical_formula_weight         893.92
_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                81.108(2)
_cell_angle_beta                 84.587(2)
_cell_angle_gamma                73.428(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5280(11)
_cell_length_b                   16.2020(19)
_cell_length_c                   16.970(2)
_cell_measurement_reflns_used    9275
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.0245
_cell_measurement_theta_min      2.233
_cell_volume                     2477.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55607
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       prism
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         14530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0464P)^2^+1.1556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                11776
_reflns_number_total             14530
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302590g_si_002_3.cif
_cod_data_source_block           2_Cr_tBuAcac2_Bpy_BPh4
_cod_database_code               4334026