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_1574637
_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         '2(C25 H23 Cl Co N6 O), 2(Cl O4)'
_chemical_formula_sum            'C50 H46 Cl4 Co2 N12 O10'
_chemical_formula_weight         1234.65
_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             2023-10-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-03-06 deposited with the CCDC.	2025-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                85.258(2)
_cell_angle_beta                 76.904(2)
_cell_angle_gamma                86.461(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6873(4)
_cell_length_b                   16.7926(8)
_cell_length_c                   18.9662(10)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      28.256
_cell_measurement_theta_min      2.409
_cell_volume                     2683.0(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      104.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            102746
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0960 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.9387. 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    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.678
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0626P)^2^+5.4666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11554
_reflns_number_total             13389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy00422e2.cif
_cod_data_source_block           kg_pk_112_meoh_0359_0m_a
_cod_depositor_comments
'Adding full bibliography for 1574636--1574637.cif.'
_cod_database_code               1574637
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.841
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C26(H26A,H26B), C39(H39A,H39B), C46(H46A,
 H46B), C52(H52A,H52B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
 C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C48(H48), C49(H49),
  C50(H50), C51(H51)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38187
_shelx_hkl_checksum              84457
_shelx_fab_checksum              95328
_olex2_submission_special_instructions 'No special instructions were received'