Bis-cycloheptyl-fused bis(imino)pyridine-cobalt catalysts for PE wax formation: positive effects of fluoride substitution on catalytic performance and thermal stability.
Zhang, Qiuyue; Wu, Ningning; Xiang, Junfeng; Solan, Gregory A.; Suo, Hongyi; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9425–9437; doi:10.1039/d0dt01876g

data_7704717
_publ_section_title
;
 Bis-cycloheptyl-fused bis(imino)pyridine-cobalt catalysts for PE wax
 formation: positive effects of fluoride substitution on catalytic
 performance and thermal stability.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9425
_journal_page_last               9437
_journal_paper_doi               10.1039/d0dt01876g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C79 H65 Cl2 Co F2 N3, C H2 Cl2, C4 H8 O'
_chemical_formula_sum            'C84 H75 Cl4 Co F2 N3 O'
_chemical_formula_weight         1381.20
_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             2020-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-21 deposited with the CCDC.	2020-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                65.813(4)
_cell_angle_beta                 76.760(4)
_cell_angle_gamma                81.879(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4294(4)
_cell_length_b                   18.2182(7)
_cell_length_c                   20.3353(7)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    169.99(12)
_cell_measurement_theta_max      71.5510
_cell_measurement_theta_min      2.4400
_cell_volume                     3426.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.946
_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    -77.00  20.00   0.50    0.14    --  -46.95  93.00 158.00  194
  2  \w    -61.00 -32.00   0.50    1.50    --  -99.00 125.00 150.00   58
  3  \w    -70.00 -44.00   0.50    1.50    --  -99.00 125.00  60.00   52
  4  \w    -68.00 -30.00   0.50    1.50    --  -99.00  61.00 150.00   76
  5  \w   -105.00 -72.00   0.50    1.50    --  -99.00  93.00 158.00   66
  6  \w   -111.00 -85.00   0.50    1.50    --  -99.00 125.00 150.00   52
  7  \w   -112.00 -84.00   0.50    1.50    --  -99.00 125.00 120.00   56
  8  \w   -101.00 -28.00   0.50    1.50    --  -99.00  77.00  60.00  146
  9  \w    -67.00 -38.00   0.50    1.50    --  -99.00  61.00   0.00   58
 10  \w    -65.00 -40.00   0.50    1.50    --  -99.00  61.00 -30.00   50
 11  \w    -63.00 -37.00   0.50    1.50    --  -99.00 125.00 -60.00   52
 12  \w    -56.00 -30.00   0.50    1.50    --  -99.00 142.00-119.81   52
 13  \w   -109.00 -60.00   0.50    1.50    --  -99.00 125.00  30.00   98
 14  \w   -110.00 -70.00   0.50    1.50    --  -99.00 125.00 -60.00   80
 15  \w   -108.00 -68.00   0.50    1.50    --  -99.00 111.00  15.35   80
 16  \w   -124.00 -69.00   0.50    1.50    --  -99.00 142.00-119.81  110
 17  \w    -27.00  23.00   0.50    0.14    --   46.95 -19.00 150.00  100
 18  \w    -23.00  74.00   0.50    0.14    --   46.95 -93.00  46.00  194
 19  \w     68.00  95.00   0.50    1.50    --  103.25 -93.00  46.00   54
 20  \w     81.00 106.00   0.50    1.50    --  103.25 -94.00   0.00   50
 21  \w     81.00 106.00   0.50    1.50    --  103.25 -94.00 -90.00   50
 22  \w     50.00 106.00   0.50    1.50    --  103.25 -94.00-150.00  112
 23  \w     40.00  66.00   0.50    1.50    --  103.25 -61.00-120.00   52
 24  \w     34.00  60.00   0.50    1.50    --  103.25 -61.00 -90.00   52
 25  \w     32.00  75.00   0.50    1.50    --  103.25 -61.00-150.00   86
 26  \w     39.00 106.00   0.50    1.50    --  103.25-125.00-150.00  134
 27  \w     32.00  87.00   0.50    1.50    --  103.25-125.00-180.00  110
 28  \w     32.00  62.00   0.50    1.50    --  103.25 -94.00   0.00   60
 29  \w     73.00 103.00   0.50    1.50    --  103.25 -77.00 150.00   60
 30  \w     35.00  62.00   0.50    1.50    --  103.25 -77.00 150.00   54
 31  \w    -25.00  46.00   0.50    0.14    --   46.95 -38.00  90.00  142
 32  \w    -22.00  27.00   0.50    0.14    --   46.95 -19.00  30.00   98
 33  \w     91.00 166.00   0.50    1.50    --  103.25  45.00 -60.00  150
 34  \w    104.00 162.00   0.50    1.50    --  103.25  30.00 -30.00  116
 35  \w    121.00 161.00   0.50    1.50    --  103.25  93.00 158.00   80
 36  \w     92.00 119.00   0.50    1.50    --  103.25  93.00 158.00   54
 37  \w   -112.00 -74.00   0.50    0.14    --  -46.95-125.00 -90.00   76
 38  \w   -118.00 -93.00   0.50    0.14    --  -46.95-125.00-180.00   50
 39  \w   -165.00 -82.00   0.50    1.50    --  -99.00 -64.00-116.47  166
 40  \w   -165.00 -84.00   0.50    1.50    --  -99.00 -93.00  46.00  162
 41  \w   -124.00 -77.00   0.50    1.50    --  -99.00 -75.00 108.88   94
 42  \w   -119.00 -86.00   0.50    1.50    --  -99.00 -50.00  63.88   66
 43  \w   -118.00 -74.00   0.50    0.14    --  -46.95-125.00 120.00   88
 44  \w   -167.00-131.00   0.50    1.50    --  -99.00 -50.00  63.88   72
 45  \w   -160.00-114.00   0.50    1.50    --  -99.00 -45.00  79.92   92
 46  \w   -168.00-106.00   0.50    1.50    --  -99.00 -64.00 128.76  124
 47  \w   -167.00-129.00   0.50    1.50    --  -99.00 -75.00 108.88   76
;
_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      -0.1005928000
_diffrn_orient_matrix_UB_12      0.0727458000
_diffrn_orient_matrix_UB_13      -0.0162120000
_diffrn_orient_matrix_UB_21      -0.0053800000
_diffrn_orient_matrix_UB_22      -0.0005590000
_diffrn_orient_matrix_UB_23      0.0765455000
_diffrn_orient_matrix_UB_31      0.1137764000
_diffrn_orient_matrix_UB_32      0.0576672000
_diffrn_orient_matrix_UB_33      -0.0321249000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47515
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.973
_diffrn_reflns_theta_min         2.426
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.840
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.339
_exptl_crystal_description       needle
_exptl_crystal_F_000             1442
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.163
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         13523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.1134
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3074
_refine_ls_wR_factor_ref         0.3289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9567
_reflns_number_total             13523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01876g2.cif
_cod_data_source_block           Co5-2
_cod_depositor_comments
'Adding full bibliography for 7704715--7704718.cif.'
_cod_database_code               7704717
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C N H Co Cl'
_reflns_odcompleteness_completeness 99.89
_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:
 C54(H54), C36(H36), C67(H67), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C3(H3A,H3B), C2(H2A,H2B), C9(H9A,H9B), C5(H5A,H5B), C11(H11A,
 H11B), C4(H4A,H4B), C10(H10A,H10B), C80(H80A,H80B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C52(H52), C50(H50), C19(H19), C7(H7), C48(H48), C47(H47), C44(H44),
 C59(H59), C60(H60), C62(H62), C79(H79), C58(H58), C46(H46), C45(H45), C31(H31),
  C56(H56), C66(H66), C77(H77), C78(H78), C75(H75), C63(H63), C42(H42),
 C35(H35), C40(H40), C71(H71), C57(H57), C72(H72), C64(H64), C32(H32), C69(H69),
  C76(H76), C38(H38), C65(H65), C73(H73), C33(H33), C70(H70), C29(H29),
 C25(H25), C27(H27), C28(H28), C41(H41), C34(H34), C39(H39), C26(H26), C83(H83),
  C82(H82)
2.d Idealised Me refined as rotating group:
 C81(H81A,H81B,H81C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              88982
_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 2.064
_oxdiff_exptl_absorpt_empirical_full_min 0.476