A Highly Reactive Chromium(V)–Oxo TAML Cation Radical Complex in Electron Transfer and Oxygen Atom Transfer Reactions
Hong, Young Hyun; Jang, Yuri; Ezhov, Roman; Seo, Mi Sook; Lee, Yong-Min; Pandey, Bhawana; Hong, Seungwoo; Pushkar, Yulia; Fukuzumi, Shunichi; Nam, Wonwoo; ACS Catalysis  (2021) 2889–2901; doi:10.1021/acscatal.1c00079

data_4518521
_publ_section_title
;
 A Highly Reactive Chromium(V)--Oxo TAML Cation Radical Complex in
 Electron Transfer and Oxygen Atom Transfer Reactions
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              2889
_journal_page_last               2901
_journal_paper_doi               10.1021/acscatal.1c00079
_journal_year                    2021
_chemical_formula_moiety         'C19 H22 Cr N4 O5, C24 H20 P'
_chemical_formula_sum            'C43 H42 Cr N4 O5 P'
_chemical_formula_weight         777.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2018-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.728(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2209(13)
_cell_length_b                   31.649(5)
_cell_length_c                   15.344(2)
_cell_measurement_reflns_used    5673
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      2.36
_cell_volume                     3894.2(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_unetI/netI     0.1250
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27494
_diffrn_reflns_theta_full        25.0142
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0710 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.8257.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.3266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1630.3870
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.2446
_refine_diff_density_min         -1.0458
_refine_diff_density_rms         0.1983
_refine_ls_d_res_high            0.8404
_refine_ls_d_res_low             15.8245
_refine_ls_goodness_of_fit_ref   0.8235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8235
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.0057
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1401P)^2^+7.0040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.2092
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -9
_reflns_limit_k_max              37
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -6
_reflns_number_gt                3991
_reflns_number_total             6860
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            cs1c00079_si_002.cif
_cod_data_source_block           pre1
_cod_depositor_comments
;

2025-09-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C21.5 H21 Cr0.5 N2 O2.5 P0.5'
_cod_original_formula_weight         388.90
_cod_original_formula_moiety         '0.5(C19 H22 Cr N4 O5), 0.5(C24 H20 P)'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        3894.2(11)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4518521
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C28(H28), C20(H20), C7(H7), C14(H14), C24(H24), C42(H42), C37(H37),
 C4(H4), C31(H31), C36(H36), C22(H22), C9(H9), C15(H15), C30(H30), C27(H27),
 C29(H29), C38(H38), C2(H2), C16(H16), C39(H39), C34(H34), C40(H40), C13(H13)
2.b Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C25(H25a,H25b,H25c), C32(H32a,H32b,H32c), C35(H35a,H35b,
 H35c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c)
;
_olex2_submission_special_instructions 'No special instructions were received'