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_7704718
_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 H57 Cl2 Co F10 N3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C81 H62 Cl2 Co F10 N3 O0.5'
_chemical_formula_weight         1405.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-30
_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                90
_cell_angle_beta                 92.5730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6079(2)
_cell_length_b                   28.3387(4)
_cell_length_c                   33.8316(5)
_cell_measurement_reflns_used    25668
_cell_measurement_temperature    169.99(12)
_cell_measurement_theta_max      73.2370
_cell_measurement_theta_min      2.5650
_cell_volume                     14948.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.952
_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      0.00  59.00   0.50    2.06    --   46.70 -38.00   0.00  118
  2  \w     39.00 119.00   0.50    2.06    --   46.70  38.00 -30.00  160
  3  \w     84.00 169.00   0.50    8.25    --  103.25  90.00-118.00  170
  4  \w    134.00 163.00   0.50    8.25    --  103.25  45.00  30.00   58
  5  \w    137.00 166.00   0.50    8.25    --  103.25  77.00  30.00   58
  6  \w     97.00 122.00   0.50    8.25    --  103.25  45.00  30.00   50
  7  \w     85.00 132.00   0.50    8.25    --  103.25  77.00  30.00   94
  8  \w     31.00 120.00   0.50    8.25    --  103.25 -61.00 120.00  178
  9  \w     54.00 115.00   0.50    8.25    --  103.25 -90.00 126.00  122
 10  \w     18.00  52.00   0.50    2.06    --   46.70 -90.00 126.00   68
 11  \w    -22.00  13.00   0.50    2.06    --   46.70 -90.00 126.00   70
 12  \w    -73.00  26.00   0.50    2.06    --  -46.70  90.00-118.00  198
 13  \w   -117.00 -27.00   0.50    8.25    --  -99.00  90.00-118.00  180
 14  \w   -121.00 -91.00   0.50    8.25    --  -99.00 -30.00  30.00   60
 15  \w   -153.00-128.00   0.50    8.25    --  -99.00 -30.00  30.00   50
 16  \w   -165.00-139.00   0.50    8.25    --  -99.00 -90.00 126.00   52
 17  \w   -162.00 -94.00   0.50    8.25    --  -99.00 -45.00 150.00  136
 18  \w   -168.00 -88.00   0.50    8.25    --  -99.00 -45.00-150.00  160
 19  \w   -168.00 -95.00   0.50    8.25    --  -99.00 -45.00-180.00  146
;
_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      -0.0216769000
_diffrn_orient_matrix_UB_12      0.0494551000
_diffrn_orient_matrix_UB_13      -0.0164592000
_diffrn_orient_matrix_UB_21      -0.0760324000
_diffrn_orient_matrix_UB_22      0.0033508000
_diffrn_orient_matrix_UB_23      0.0273851000
_diffrn_orient_matrix_UB_31      0.0591874000
_diffrn_orient_matrix_UB_32      0.0223957000
_diffrn_orient_matrix_UB_33      0.0324983000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            109151
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.636
_diffrn_reflns_theta_min         2.615
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
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    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             5792
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1758
_refine_ls_number_reflns         29571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0919
_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^)+(0.1149P)^2^+48.1473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2534
_refine_ls_wR_factor_ref         0.2680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22224
_reflns_number_total             29571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01876g2.cif
_cod_data_source_block           Co5
_cod_depositor_comments
;
Adding full bibliography for 7704715--7704718.cif.

2024-11-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C162 H124 Cl4 Co2 F20 N6 O'
_cod_original_formula_weight         2810.32
_cod_original_formula_moiety         '2(C79 H57 Cl2 Co F10 N3), C4 H10 O'
_cod_original_formula_units_Z            4
_cod_database_code               7704718
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H N Co Cl'
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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), C133(H133), C67(H67), C146(H146), C101(H101), C23(H23), C36(H36),
 C114(H114)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C4(H4A,H4B), C81(H81A,H81B), C2(H2A,H2B), C3(H3A,H3B),
 C82(H82A,H82B), C5(H5A,H5B), C83(H83A,H83B), C84(H84A,H84B), C91(H91A,H91B),
 C11(H11A,H11B), C9(H9A,H9B), C10(H10A,H10B), C90(H90A,H90B), C88(H88A,H88B),
 C89(H89A,H89B), C161(H16A,H16B), C160(H16C,H16D)
2.c Aromatic/amide H refined with riding coordinates:
 C73(H73), C52(H52), C129(H129), C50(H50), C99(H99), C19(H19), C131(H131),
 C97(H97), C104(H104), C72(H72), C21(H21), C158(H158), C145(H145), C7(H7),
 C47(H47), C75(H75), C62(H62), C103(H103), C113(H113), C79(H79), C157(H157),
 C126(H126), C152(H152), C48(H48), C141(H141), C69(H69), C109(H109), C66(H66),
 C139(H139), C107(H107), C125(H125), C86(H86), C112(H112), C116(H116),
 C142(H142), C123(H123), C149(H149), C135(H135), C70(H70), C122(H122), C44(H44),
  C56(H56), C63(H63), C29(H29), C28(H28), C120(H120), C76(H76), C25(H25),
 C106(H106), C65(H65), C117(H117), C151(H151), C60(H60), C42(H42), C31(H31),
 C38(H38), C78(H78), C119(H119), C148(H148), C35(H35), C45(H45), C138(H138),
 C39(H39), C59(H59), C110(H110), C144(H144), C41(H41), C26(H26), C32(H32),
 C57(H57), C136(H136), C34(H34), C154(H154), C155(H155)
2.d Idealised Me refined as rotating group:
 C159(H15A,H15B,H15C), C162(H16E,H16F,H16G)
;
_shelx_res_checksum              99828
_shelx_fab_checksum              42062
_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 1.636
_oxdiff_exptl_absorpt_empirical_full_min 0.603