A passage from pincer complexes to rationally designed phosphine-free Co(iii) catalysts supported by a pentadentate ligand for activation of alcohols: studies on sp3 C–H alkylation of 9H-fluorene and quinoline synthesis
Kukreti, Prashant; Chauhan, Rahul; Ghosh, Kaushik; Catalysis Science & Technology 15 (2025) 3816–3826; doi:10.1039/D5CY00422E

data_1574636
_publ_section_title
;
 A passage from pincer complexes to rationally designed phosphine-free
 Co(iii) catalysts supported by a pentadentate ligand for activation of
 alcohols: studies on sp3 C--H alkylation of 9H-fluorene and quinoline
 synthesis
;
_journal_issue                   13
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3816
_journal_page_last               3826
_journal_paper_doi               10.1039/D5CY00422E
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C25 H23 Br Co N6 O, Cl O4, C2 H3 N'
_chemical_formula_sum            'C27 H26 Br Cl Co N7 O5'
_chemical_formula_weight         702.84
_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   geom
_audit_creation_date             2023-07-05
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2024-05-18 deposited with the CCDC.	2025-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                111.807(2)
_cell_angle_beta                 96.893(2)
_cell_angle_gamma                100.568(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1862(4)
_cell_length_b                   12.1495(5)
_cell_length_c                   14.5113(7)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      27.668
_cell_measurement_theta_min      2.305
_cell_volume                     1446.42(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      109.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54627
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.369
_diffrn_reflns_theta_min         2.305
_exptl_absorpt_coefficient_mu    2.118
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0899 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.8747. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0510P)^2^+1.1075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6009
_reflns_number_total             7216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy00422e2.cif
_cod_data_source_block           kg_pk_meoh298_0298_0ma_a
_cod_depositor_comments
'Adding full bibliography for 1574636--1574637.cif.'
_cod_original_cell_volume        1446.42(11)
_cod_database_code               1574636
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.759
_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:
 C11(H11A,H11B), C18(H18A,H18B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              24512
_shelx_hkl_checksum              7605
_olex2_submission_special_instructions 'No special instructions were received'