A general and expedient amination of alcohols catalysed by a single-site (NN)Co(ii)-bidentate complex under solventless conditions
Kumar, Rohit; Srivastava, Ankit Kumar; Nagarasu, Palaniyappan; Madhu, Vedichi; Balaraman, Ekambaram; Catalysis Science & Technology 14 (2024) 98–109; doi:10.1039/D3CY00809F

data_1570363
_publ_section_title
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 A general and expedient amination of alcohols catalysed by a single-site
 (NN)Co(ii)-bidentate complex under solventless conditions
;
_journal_issue                   1
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              98
_journal_page_last               109
_journal_paper_doi               10.1039/D3CY00809F
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C10 H11 Br2 Co N3'
_chemical_formula_sum            'C10 H11 Br2 Co N3'
_chemical_formula_weight         391.97
_chemical_name_systematic        Cobaltbromide_Pyridine3_methylpyrazole
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-19 deposited with the CCDC.	2023-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                75.188(8)
_cell_angle_beta                 78.772(8)
_cell_angle_gamma                73.732(8)
_cell_formula_units_Z            2
_cell_length_a                   7.948(2)
_cell_length_b                   8.256(2)
_cell_length_c                   10.775(3)
_cell_measurement_reflns_used    8737
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      31.420
_cell_measurement_theta_min      2.693
_cell_volume                     650.4(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            71153
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.496
_diffrn_reflns_theta_min         2.631
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.440
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1130 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.6697.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       block
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0223P)^2^+0.5301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2576
_reflns_number_total             2685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy00809f2.cif
_cod_data_source_block           mo_pc_3p_cobr2_3_0m_a
_cod_depositor_comments          'Adding full bibliography for 1570363.cif.'
_cod_original_cell_volume        650.3(3)
_cod_database_code               1570363
_shelx_shelxl_version_number     2019/1
_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:
 C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C4(H4), C7(H7), C3(H3), C2(H2), C5(H5)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              1484
_olex2_submission_original_sample_id CC_3P_COBr2
_olex2_submission_special_instructions 'No special instructions were received'