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_1574628
_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         'C37 H39 Cl2 Co N3'
_chemical_formula_sum            'C37 H39 Cl2 Co N3'
_chemical_formula_weight         655.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-09-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_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            16
_cell_length_a                   33.7269(6)
_cell_length_b                   32.7780(6)
_cell_length_c                   14.0568(3)
_cell_measurement_reflns_used    7468
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.2050
_cell_measurement_theta_min      3.6520
_cell_volume                     15539.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.953
_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   -103.00 -32.00   0.50    1.80    --  -46.42 -55.00 -76.00  142
  2  \w   -151.00-126.00   0.50    5.00    -- -104.50 -83.00  63.00   50
  3  \w   -166.00-114.00   0.50    5.00    -- -104.50 -55.00 -76.00  104
  4  \w     37.00  65.00   0.50    5.00    --  108.85 -55.00 -76.00   56
  5  \w     38.00 136.00   0.50    5.00    --  108.85 -86.00 171.00  196
  6  \w    -24.00  26.00   0.50    1.80    --   46.42 -19.00 150.00  100
  7  \w     22.00  58.00   0.50    1.80    --   46.42-125.00 150.00   72
  8  \w    -58.00 -31.00   0.50    5.00    -- -104.50  61.00 -90.00   54
  9  \w    -68.00 -42.00   0.50    5.00    -- -104.50  61.00 150.00   52
 10  \w     43.00  68.00   0.50    5.00    --  108.85 -61.00  60.00   50
 11  \w     59.00  97.00   0.50    5.00    --  108.85 -77.00 -90.00   76
 12  \w     98.00 177.00   0.50    5.00    --  108.85  61.00-180.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0261875000
_diffrn_orient_matrix_UB_12      0.0307776000
_diffrn_orient_matrix_UB_13      0.0540450000
_diffrn_orient_matrix_UB_21      -0.0310683000
_diffrn_orient_matrix_UB_22      -0.0021006000
_diffrn_orient_matrix_UB_23      -0.0800922000
_diffrn_orient_matrix_UB_31      -0.0208752000
_diffrn_orient_matrix_UB_32      -0.0354735000
_diffrn_orient_matrix_UB_33      0.0516506000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13794
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.612
_diffrn_reflns_theta_min         3.664
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.916
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.96a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             5488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.062(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6154
_refine_ls_number_restraints     383
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1111P)^2^+55.4265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.1925
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                5538
_reflns_number_total             6154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py00358j2.cif
_cod_data_source_block           Co4
_cod_depositor_comments
'Adding full bibliography for 1574627--1574628.cif.'
_cod_database_code               1574628
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N Co Cl'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.938(7)
 0.062(7)
2. 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
3. Restrained distances
 Co1-Cl1 \\sim Co1-Cl1A
 with sigma of 0.02
 Co1-Cl2 \\sim Co1-Cl2A
 with sigma of 0.02
 C34-C35 \\sim C34-C35A
 with sigma of 0.02
 C23-C28 \\sim C23-C28A
 with sigma of 0.02
4. Rigid bond restraints
 C35, C36, C37, C27, C26, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1A, Cl1, Cl2, Cl2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
Uanis(Cl1A) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2A) \\sim Ueq, Uanis(Cl2)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
6. Others
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Sof(Cl2A)=1-FVAR(2)
 Sof(Cl2)=FVAR(2)
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(3)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(3)
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(4)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C3(H3A,H3B), C9(H9A,H9B), C11(H11A,H11B), C10(H10A,
 H10B)
7.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C15(H15), C18(H18), C16(H16), C24(H24), C33(H33),
 C31(H31), C17(H17)
7.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C28(H28A,H28B,H28C), C35A(H35D,H35E,H35F),
 C28A(H28D,H28E,H28F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20328
_shelx_hkl_checksum              33932
_shelx_fab_checksum              40254
_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 4.635
_oxdiff_exptl_absorpt_empirical_full_min 0.511