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_7709346
_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         'C30 H33 Co N4 O3, C24 H20 B'
_chemical_formula_sum            'C54 H53 B Co N4 O3'
_chemical_formula_weight         875.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-12-07
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.10.14 svn.r9718050b for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-12-13 deposited with the CCDC.	2021-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                86.897(4)
_cell_angle_beta                 88.338(4)
_cell_angle_gamma                70.768(4)
_cell_formula_units_Z            2
_cell_length_a                   11.211(2)
_cell_length_b                   14.094(3)
_cell_length_c                   14.988(3)
_cell_measurement_reflns_used    8656
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.34
_cell_volume                     2232.6(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.995
_diffrn_reflns_theta_min         1.361
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0838 before and 0.0416 after correction.
The Ratio of minimum to maximum transmission is 0.8695.
The \l/2 correction factor is 0.0015.
;
_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    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         10418
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.5918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8090
_reflns_number_total             10418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02235k2.cif
_cod_data_source_block           bc214_0m
_cod_database_code               7709346
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 C23B, O2, C22, O1, C24, O4, C29, C6, C25, C55, C26, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C23C, O1A, C22A, O2A, C24A, O4A, C29A, C6A, C25A, C55A, C26A, C56A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: O2(0.5) O1(0.5) C24(0.5) C22(0.5) C29(0.5) H29(0.5) C23B(0.5)
 H23B(0.5) O4(0.5) C6(0.5) H6(0.5) C56(0.5) H56(0.5) C26(0.5) H26(0.5) C55(0.5)
 H55(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) O1A(0.5) C22A(0.5) C24A(0.5)
 C29A(0.5) H29A(0.5) C23C(0.5) H23C(0.5) O4A(0.5) C55A(0.5) H55A(0.5) C25A(0.5)
 H25D(0.5) H25E(0.5) C6A(0.5) H6A(0.5) C56A(0.5) H56A(0.5) C26A(0.5) H26A(0.5)
 H25F(0.5) O2A(0.5)
4.a Ternary CH refined with riding coordinates:
 C23B(H23B), C23C(H23C)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C29(H29), C6(H6), C56(H56), C26(H26), C55(H55), C29A(H29A),
 C55A(H55A), C6A(H6A), C56A(H56A), C26A(H26A)
;
_shelx_res_checksum              60734
_shelx_hkl_checksum              74661
_olex2_submission_special_instructions 'No special instructions were received'