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_1518155
_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            'C21 H20 B2 Cr F8 N5 O2'
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_space_group_name_Hall           '-P 2ybc'
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.683(4)
_cell_length_b                   22.830(8)
_cell_length_c                   11.317(4)
_cell_measurement_temperature    120(2)
_cell_volume                     2419.7(16)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.918
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
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_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.429
_diffrn_reflns_theta_min         1.784
_exptl_absorpt_coefficient_mu    0.566
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             1212
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_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0732
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+4.0629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_total             5584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc02285h2.cif
_cod_data_source_block           Kotani2
_cod_depositor_comments
'Adding full bibliography for 1518154--1518155.cif.'
_cod_original_cell_volume        2419.7(15)
_cod_database_code               1518155
_shelx_estimated_absorpt_t_min   0.844
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2013-4
_shelx_res_checksum              26455