Cobalt complex with a tetradentate aminopyridine ligand: a single-component and efficient catalytic system for the cycloaddition reactions of CO2 and epoxides
Yu, Ning; Zhang, Bowen; Liang, Shuyan; Shi, Minghui; Han, Feng; Zhang, Congcong; Yang, Qingfeng; Miao, Chengxia; New Journal of Chemistry 49 (2025) 1430–1439; doi:10.1039/D4NJ04346D

data_7063606
_publ_section_title
;
 Cobalt complex with a tetradentate aminopyridine ligand: a
 single-component and efficient catalytic system for the cycloaddition
 reactions of CO2 and epoxides
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1430
_journal_page_last               1439
_journal_paper_doi               10.1039/D4NJ04346D
_journal_volume                  49
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C20 H28 Br2 Co N4'
_chemical_formula_sum            'C20 H28 Br2 Co N4'
_chemical_formula_weight         543.21
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-17 deposited with the CCDC.	2024-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.19310(10)
_cell_length_b                   9.19310(10)
_cell_length_c                   23.9143(4)
_cell_measurement_reflns_used    4972
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1780
_cell_measurement_theta_min      5.1360
_cell_volume                     2021.07(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     87.00 176.00   0.50    0.05    --  104.75  90.00-103.00  178
  2  \w    110.00 177.00   0.50    0.05    --  104.75  50.00  38.00  134
  3  \w     39.00  67.00   0.50    0.05    --  104.75 -61.00-180.00   56
  4  \w    -25.00  74.00   0.50    0.05    --   46.92 -87.00  37.00  198
  5  \w     -7.00  29.00   0.50    0.05    --  -46.92  19.00 150.00   72
  6  \w    -62.00 -30.00   0.50    0.05    -- -102.00  61.00  90.00   64
  7  \w    -56.00 -30.00   0.50    0.05    -- -102.00  61.00-120.00   52
  8  \w   -102.00 -76.00   0.50    0.05    --  -46.92-125.00 -60.00   52
  9  \w   -172.00 -80.00   0.50    0.05    -- -102.00 -87.00  37.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0843783000
_diffrn_orient_matrix_UB_12      -0.0153860000
_diffrn_orient_matrix_UB_13      -0.0553449000
_diffrn_orient_matrix_UB_21      0.0578323000
_diffrn_orient_matrix_UB_22      0.1492306000
_diffrn_orient_matrix_UB_23      -0.0191359000
_diffrn_orient_matrix_UB_31      0.1327815000
_diffrn_orient_matrix_UB_32      -0.0745985000
_diffrn_orient_matrix_UB_33      -0.0268400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6963
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.407
_diffrn_reflns_theta_min         5.154
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 716 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0458P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.600
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                1947
_reflns_number_total             2031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04346d2.cif
_cod_data_source_block           20230913c_auto
_cod_depositor_comments          'Adding full bibliography for 7063606.cif.'
_cod_original_cell_volume        2021.07(6)
_cod_database_code               7063606
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1N1H1Br1Co1
_shelx_estimated_absorpt_t_max   0.209
_shelx_estimated_absorpt_t_min   0.209
_diffrn_oxdiff_digest_frames
;
01d83e5c6dd0481734530842674e57678200154426d
;
_diffrn_oxdiff_digest_hkl
;
0184f5e9d09493042eaf1afa88c1284106f791
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              74608
_shelx_hkl_checksum              19450
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.509
_oxdiff_exptl_absorpt_empirical_full_min 0.783