Formation and characterization of a reactive chromium(v)‒oxo complex: mechanistic insight into hydrogen-atom transfer reactions
Kotani, Hiroaki; Kaida, Suzue; Ishizuka, Tomoya; Sakaguchi, Miyuki; Ogura, Takashi; Shiota, Yoshihito; Yoshizawa, Kazunari; Kojima, Takahiko; Chem. Sci. 6 (2015) 945–; doi:10.1039/C4SC02285H

data_1518154
_publ_section_title
;
 Formation and characterization of a reactive chromium(v)--oxo complex:
 mechanistic insight into hydrogen-atom transfer reactions
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              945
_journal_paper_doi               10.1039/C4SC02285H
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C22 H22.5 B Cl Cr F4 N4.5 O3'
_chemical_formula_weight         572.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_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            8
_cell_length_a                   14.5572(8)
_cell_length_b                   13.9044(8)
_cell_length_c                   24.0822(14)
_cell_measurement_temperature    120(2)
_cell_volume                     4874.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26351
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.9384
_exptl_absorpt_correction_T_min  0.8820
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0608P)^2^+9.4441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                4595
_reflns_number_total             5560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc02285h2.cif
_cod_data_source_block           kaida132
_cod_depositor_comments
'Adding full bibliography for 1518154--1518155.cif.'
_cod_original_formula_sum        'C22 H22.50 B Cl Cr F4 N4.50 O3'
_cod_database_code               1518154