Ultra-low-molecular-weight PE wax using a cyclohexyl-fused bis(imino)pyridine-cobalt catalyst functionalized with a remote para-phenyl group
Wang, Yizhou; Wang, Zheng; Zhang, Qiuyue; Wang, Quanchao; Solan, Gregory A.; Duan, Xuelei; Ma, Yanping; Gao, Jiahao; Zhou, Zhe; Sun, Wen-Hua; Polymer Chemistry 16 (2025) 2718–2731; doi:10.1039/D5PY00358J

data_1574627
_publ_section_title
;
 Ultra-low-molecular-weight PE wax using a cyclohexyl-fused
 bis(imino)pyridine-cobalt catalyst functionalized with a remote
 para-phenyl group
;
_journal_issue                   23
_journal_name_full               'Polymer Chemistry'
_journal_page_first              2718
_journal_page_last               2731
_journal_paper_doi               10.1039/D5PY00358J
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C43 H51 Cl2 Co N3'
_chemical_formula_sum            'C43 H51 Cl2 Co N3'
_chemical_formula_weight         739.69
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-04-04 deposited with the CCDC.	2025-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7671(8)
_cell_length_b                   22.7671(8)
_cell_length_c                   14.8686(7)
_cell_measurement_reflns_used    3801
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      69.4110
_cell_measurement_theta_min      3.5060
_cell_volume                     7707.0(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.964
_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   -113.00 -88.00   0.50    4.00    --  -46.70-163.00 102.00   50
  2  \w     43.00 127.00   0.50    6.00    --  103.25-163.00 102.00  168
  3  \w   -164.00 -97.00   0.50    6.00    -- -104.50 -34.00 108.00  134
  4  \w    -22.00  16.00   0.50    4.00    --  -46.70  19.00  30.00   76
  5  \w    -19.00  23.00   0.50    4.00    --  -46.70  19.00  90.00   84
  6  \w    -18.00  21.00   0.50    4.00    --  -46.70  19.00 -30.00   78
  7  \w     41.00  68.00   0.50    6.00    --  103.25 -61.00 -90.00   54
  8  \w     32.00  71.00   0.50    6.00    --  103.25 -61.00  30.00   78
  9  \w    -66.00 -38.00   0.50    6.00    -- -104.50  61.00  30.00   56
 10  \w    -64.00 -36.00   0.50    6.00    -- -104.50  61.00-180.00   56
 11  \w    -66.00 -32.00   0.50    6.00    -- -104.50  61.00 -60.00   68
 12  \w    -67.00 -41.00   0.50    6.00    -- -104.50  61.00 -90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0543018000
_diffrn_orient_matrix_UB_12      -0.0271797000
_diffrn_orient_matrix_UB_13      0.0455964000
_diffrn_orient_matrix_UB_21      0.0290783000
_diffrn_orient_matrix_UB_22      0.0610610000
_diffrn_orient_matrix_UB_23      0.0050274000
_diffrn_orient_matrix_UB_31      -0.0281471000
_diffrn_orient_matrix_UB_32      0.0100627000
_diffrn_orient_matrix_UB_33      0.0929374000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            11391
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.315
_diffrn_reflns_theta_min         3.550
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.013
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             3128
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 961 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.797
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.797
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1914P)^2^+8.3362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.2072
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.851
_reflns_number_gt                2966
_reflns_number_total             3703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py00358j2.cif
_cod_data_source_block           Co3
_cod_depositor_comments
'Adding full bibliography for 1574627--1574628.cif.'
_cod_original_cell_volume        7707.0(7)
_cod_database_code               1574627
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N Co Cl'
_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:
 C18(H18), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C16(H16), C11(H11), C15(H15), C14(H14)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              37567
_shelx_hkl_checksum              5694
_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 1.379
_oxdiff_exptl_absorpt_empirical_full_min 0.642