Selective oxygenation of C–H and CC bonds with H2O2 by high-spin cobalt(ii)-carboxylate complexes
Ghosh, Ivy; Chakraborty, Biswarup; Bera, Abhijit; Paul, Satadal; Paine, Tapan Kanti; Dalton Transactions  (2022) –; doi:10.1039/D1DT02235K

data_7709344
_publ_section_title
;
 Selective oxygenation of C--H and C&#xE001;C bonds with H2O2 by high-spin
 cobalt(ii)-carboxylate complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02235K
_journal_year                    2022
_chemical_formula_moiety         'C28 H29 Co N4 O2, C24 H20 B'
_chemical_formula_sum            'C52 H49 B Co N4 O2'
_chemical_formula_weight         831.69
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-13 deposited with the CCDC.	2021-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.067(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6102(19)
_cell_length_b                   9.4202(8)
_cell_length_c                   21.831(2)
_cell_measurement_reflns_used    5984
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      22.998
_cell_measurement_theta_min      2.355
_cell_volume                     4433.0(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48560
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.134
_diffrn_reflns_theta_min         1.281
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1091 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.8742.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic pinkish pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       needle
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         9765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0387P)^2^+0.9398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6784
_reflns_number_total             9765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02235k2.cif
_cod_data_source_block           bc116_0ma_a
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C208 H196 B4 Co4 N16 O8'
_cod_original_formula_weight         3326.76
_cod_original_formula_moiety         '4(C28 H29 Co N4 O2), 4(C24 H20 B)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        4433.1(7)
_cod_database_code               7709344
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00E(H00A,H00B), C00G(H00C,H00D), C00J(H00E,H00G)
2.b Aromatic/amide H refined with riding coordinates:
 C00D(H00H), C00F(H00F), C00K(H00K), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C013(H013), C014(H014),
 C015(H015), C016(H016), C018(H018), C019(H019), C01B(H01Q), C01C(H01R),
 C01D(H01D), C01E(H01S), C01F(H01T), C01G(H01G), C01H(H01H), C01I(H01I),
 C01J(H01U), C01M(H01N), C01N(H01O), C01O(H01P)
2.c Idealised Me refined as rotating group:
 C017(H01A,H01B,H01C), C01K(H01E,H01F,H01J), C01L(H01K,H01L,H01M)
;
_shelx_res_checksum              31164
_shelx_hkl_checksum              70931
_olex2_submission_special_instructions 'No special instructions were received'