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_4334024
_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            'C32 H46 Cr N2 O4'
_chemical_formula_weight         574.71
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3695(12)
_cell_length_b                   11.8910(11)
_cell_length_c                   18.1768(15)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.992
_cell_measurement_theta_min      2.240
_cell_volume                     3105.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19664
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.275
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+1.8919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                3900
_reflns_number_total             4531
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302590g_si_002_1.cif
_cod_data_source_block           1_Cr_tBuAcac2_Bpy
_cod_database_code               4334024