Fluorinated cobalt catalysts and their use in forming narrowly dispersed polyethylene waxes of high linearity and incorporating vinyl functionality
Zhang, Qiuyue; Li, Zilong; Han, Mingyang; Xiang, Junfeng; Solan, Gregory A.; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; Catalysis Science & Technology 11 (2021) 656–670; doi:10.1039/D0CY01917H

data_1559568
_publ_section_title
;
 Fluorinated cobalt catalysts and their use in forming narrowly dispersed
 polyethylene waxes of high linearity and incorporating vinyl
 functionality
;
_journal_issue                   2
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              656
_journal_page_last               670
_journal_paper_doi               10.1039/D0CY01917H
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         '5(C52 H44 Cl2 Co F5 N3)'
_chemical_formula_sum            'C260 H220 Cl10 Co5 F25 N15'
_chemical_formula_weight         4678.65
_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     iterative
_audit_creation_date             2020-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-18 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                94.0520(10)
_cell_angle_beta                 105.3480(10)
_cell_angle_gamma                102.8980(10)
_cell_formula_units_Z            2
_cell_length_a                   20.2887(2)
_cell_length_b                   22.5854(2)
_cell_length_c                   30.0093(2)
_cell_measurement_reflns_used    38822
_cell_measurement_temperature    169.99(14)
_cell_measurement_theta_max      74.8580
_cell_measurement_theta_min      2.4030
_cell_volume                     12802.4(2)
_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(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.955
_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     31.00 117.00   0.50    1.00    --   47.20  73.00  14.00  172
  2  \w     84.00 164.00   0.50   13.00    --  103.25  73.00  14.00  160
  3  \w    115.00 153.00   0.50   13.00    --  103.25  45.00   0.00   76
  4  \w     92.00 169.00   0.50   13.00    --  103.25  30.00 -60.00  154
  5  \w     92.00 168.00   0.50   13.00    --  103.25  30.00 -30.00  152
  6  \w     75.00 108.00   0.50   13.00    --  103.25 -94.00  60.00   66
  7  \w     92.00 117.00   0.50   13.00    --  103.25-125.00 -30.00   50
  8  \w     49.00  75.00   0.50   13.00    --  103.25 -94.00-120.00   52
  9  \w     46.00 110.00   0.50   13.00    --  103.25-125.00-150.00  128
 10  \w     32.00  84.00   0.50   13.00    --  103.25 -73.00-115.00  104
 11  \w     36.00  62.00   0.50   13.00    --  103.25-125.00 -30.00   52
 12  \w     33.00 102.00   0.50   13.00    --  103.25 -94.00   0.00  138
 13  \w     35.00  66.00   0.50   13.00    --  103.25 -94.00  60.00   62
 14  \w     31.00 125.00   0.50   13.00    --  103.25 -77.00  60.00  188
 15  \w     19.00  95.00   0.50    1.00    --   47.20-125.00 120.00  152
 16  \w     -3.00  64.00   0.50    1.00    --   47.20 -73.00-115.00  134
 17  \w     16.00  94.00   0.50    1.00    --   47.20-125.00-120.00  156
 18  \w     32.00 114.00   0.50   13.00    --  103.25 -77.00-180.00  164
 19  \w    -68.00  10.00   0.50    1.00    --  -47.20  73.00  14.00  156
 20  \w    -51.00 -26.00   0.50   13.00    --  -99.00 125.00  30.00   50
 21  \w    -58.00 -26.00   0.50   13.00    --  -99.00  77.00  60.00   64
 22  \w    -90.00 -37.00   0.50   13.00    --  -99.00  73.00  14.00  106
 23  \w   -117.00 -86.00   0.50   13.00    --  -99.00  77.00  60.00   62
 24  \w   -117.00 -90.00   0.50   13.00    --  -99.00 125.00  30.00   54
 25  \w   -117.00 -76.00   0.50   13.00    --  -99.00 125.00 150.00   82
 26  \w   -117.00 -44.00   0.50   13.00    --  -99.00 125.00 -90.00  146
 27  \w   -108.00 -28.00   0.50   13.00    --  -99.00  45.00-150.00  160
 28  \w   -115.00 -46.00   0.50    1.00    --  -47.20 -73.00-115.00  138
 29  \w   -110.00 -72.00   0.50    1.00    --  -47.20-125.00  30.00   76
 30  \w   -141.00 -80.00   0.50   13.00    --  -99.00 -77.00 120.00  122
 31  \w   -167.00 -91.00   0.50   13.00    --  -99.00 -30.00  90.00  152
 32  \w   -163.00 -80.00   0.50   13.00    --  -99.00 -73.00-115.00  166
 33  \w   -168.00 -98.00   0.50   13.00    --  -99.00 -30.00-180.00  140
;
_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      0.0349110000
_diffrn_orient_matrix_UB_12      0.0460798000
_diffrn_orient_matrix_UB_13      -0.0275883000
_diffrn_orient_matrix_UB_21      -0.0028921000
_diffrn_orient_matrix_UB_22      0.0535575000
_diffrn_orient_matrix_UB_23      0.0335892000
_diffrn_orient_matrix_UB_31      0.0734268000
_diffrn_orient_matrix_UB_32      -0.0001119000
_diffrn_orient_matrix_UB_33      0.0316169000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            172540
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.617
_diffrn_reflns_theta_min         2.371
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69318
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       plate
_exptl_crystal_F_000             4830
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2881
_refine_ls_number_reflns         50851
_refine_ls_number_restraints     6911
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0862
_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^)+(0.0926P)^2^+23.5464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29988
_reflns_number_total             50851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy01917h2.cif
_cod_data_source_block           Co5
_cod_depositor_comments
'Adding full bibliography for 1559567--1559568.cif.'
_cod_database_code               1559568
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNOCoCl
_chemical_oxdiff_usercomment     'C H N Co Cl F'
_reflns_odcompleteness_completeness 99.54
_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. Restrained distances
 C70A-C67 = C71A-C70A = C70-C67 = C71-C70
 1.54 with sigma of 0.01
 C71-C67
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C71 \\sim C70 \\sim C70A \\sim C71A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
C230 \\sim C215 \\sim C248 \\sim C216 \\sim C249 \\sim C234 \\sim C231 \\sim C3
\\sim C229 \\sim C254 \\sim C114 \\sim C236 \\sim C232 \\sim C233 \\sim C7
\\sim C4 \\sim C8 \\sim C5 \\sim C159 \\sim C125 \\sim C107 \\sim C214 \\sim
C235 \\sim C21 \\sim C2 \\sim C260 \\sim C188 \\sim C119 \\sim C218 \\sim C211
\\sim C110 \\sim C242 \\sim C111 \\sim C175 \\sim C180 \\sim C250 \\sim C130
\\sim C6 \\sim C219 \\sim C255 \\sim C210 \\sim C99 \\sim C44 \\sim C178 \\sim
C76 \\sim C19 \\sim C158 \\sim C217 \\sim C60 \\sim C207 \\sim C18 \\sim C23
\\sim C247 \\sim C176 \\sim C253 \\sim C223 \\sim C117 \\sim C256 \\sim C20
\\sim C237 \\sim C251 \\sim C24 \\sim C56 \\sim C213 \\sim C115 \\sim C37 \\sim
C58 \\sim C106 \\sim C31 \\sim C75 \\sim C120 \\sim C177 \\sim C73 \\sim C179
\\sim C92 \\sim C22 \\sim C10 \\sim C212 \\sim C109 \\sim C112 \\sim C118 \\sim
C241 \\sim C194 \\sim C259 \\sim C160 \\sim C55 \\sim C45 \\sim C74 \\sim C108
\\sim C57 \\sim C222 \\sim C126 \\sim C77 \\sim C116 \\sim C11 \\sim C238 \\sim
C252 \\sim C163 \\sim C189 \\sim C239 \\sim C42 \\sim C61 \\sim C129 \\sim C240
\\sim C220 \\sim C9 \\sim C48 \\sim C181 \\sim C201 \\sim C164 \\sim C151 \\sim
C128 \\sim C59 \\sim C1 \\sim C193 \\sim C121 \\sim C127 \\sim C226 \\sim C138
\\sim C195 \\sim C25 \\sim C36 \\sim C104 \\sim C15 \\sim C162 \\sim C49 \\sim
C78 \\sim C32 \\sim C47 \\sim C43 \\sim C144 \\sim C209 \\sim C38 \\sim C46
\\sim C221 \\sim C208 \\sim C191 \\sim C41 \\sim C192 \\sim C105 \\sim C145
\\sim C157 \\sim C227 \\sim C246 \\sim C202 \\sim C113 \\sim C257 \\sim C12
\\sim C131 \\sim C80 \\sim C182 \\sim C30 \\sim C103 \\sim C26 \\sim C258 \\sim
C79 \\sim C152 \\sim C206 \\sim C14 \\sim C161 \\sim C54 \\sim C13 \\sim C245
\\sim C86 \\sim C139 \\sim C132 \\sim C165 \\sim C224 \\sim C190 \\sim C100
\\sim C40 \\sim C169 \\sim C243 \\sim C205 \\sim C102 \\sim C141 \\sim C16
\\sim C101 \\sim C39 \\sim C93 \\sim C17 \\sim C62 \\sim C204 \\sim C34 \\sim
C153 \\sim C156 \\sim C28 \\sim C244 \\sim C35 \\sim C137 \\sim C122 \\sim C33
\\sim C124 \\sim C172 \\sim C166 \\sim C52 \\sim C167 \\sim C27 \\sim C154
\\sim C140 \\sim C203 \\sim C29 \\sim C183 \\sim C168 \\sim C200 \\sim C196
\\sim C155 \\sim C81 \\sim C53 \\sim C143 \\sim C228 \\sim C51 \\sim C142 \\sim
C63 \\sim C136 \\sim C146 \\sim C170 \\sim C133 \\sim C184 \\sim C187 \\sim C87
\\sim C123 \\sim C91 \\sim C148 \\sim C199 \\sim C150 \\sim C135 \\sim C185
\\sim C147 \\sim C197 \\sim C67 \\sim C174 \\sim C85 \\sim C173 \\sim C82 \\sim
C171 \\sim C83 \\sim C98 \\sim C186 \\sim C149 \\sim C50 \\sim C134 \\sim C88
\\sim C94 \\sim C198 \\sim C97 \\sim C225 \\sim C64 \\sim C90 \\sim C89 \\sim
C68 \\sim C96 \\sim C84 \\sim C71 \\sim C95 \\sim C66 \\sim C65 \\sim C72 \\sim
C69 \\sim C70 \\sim C70A \\sim C71A: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C96 \\sim F8 \\sim C97 \\sim C95: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C71A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=1-FVAR(1)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C70)=Sof(H70A)=Sof(H70B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C248(H248), C235(H235), C24(H24), C37(H37), C92(H92), C194(H194), C181(H181),
 C144(H144), C131(H131), C79(H79)
5.b Secondary CH2 refined with riding coordinates:
 C120(H12A,H12B), C226(H22A,H22B), C224(H22F,H22G), C16(H16A,H16B), C17(H17A,
 H17B), C122(H12F,H12G), C172(H17C,H17D), C170(H17E,H17F), C68(H68A,H68B),
 C70(H70A,H70B), C70A(H70C,H70D)
5.c Aromatic/amide H refined with riding coordinates:
 C231(H231), C254(H254), C233(H233), C4(H4), C5(H5), C214(H214), C260(H260),
 C110(H110), C250(H250), C6(H6), C247(H247), C253(H253), C256(H256), C20(H20),
 C237(H237), C251(H251), C56(H56), C213(H213), C58(H58), C75(H75), C177(H177),
 C179(H179), C22(H22), C212(H212), C109(H109), C118(H118), C241(H241),
 C259(H259), C160(H160), C45(H45), C108(H108), C57(H57), C222(H222), C77(H77),
 C116(H116), C238(H238), C189(H189), C42(H42), C129(H129), C240(H240),
 C220(H220), C48(H48), C193(H193), C127(H127), C36(H36), C104(H104), C162(H162),
  C49(H49), C32(H32), C43(H43), C46(H46), C192(H192), C246(H246), C202(H202),
 C257(H257), C12(H12), C30(H30), C103(H103), C26(H26), C152(H152), C206(H206),
 C14(H14), C161(H161), C139(H139), C190(H190), C100(H100), C40(H40), C243(H243),
  C205(H205), C101(H101), C39(H39), C153(H153), C156(H156), C244(H244),
 C35(H35), C137(H137), C33(H33), C166(H166), C27(H27), C140(H140), C203(H203),
 C29(H29), C183(H183), C168(H168), C200(H200), C196(H196), C155(H155), C81(H81),
  C143(H143), C142(H142), C136(H136), C146(H146), C133(H133), C184(H184),
 C187(H187), C87(H87), C91(H91), C199(H199), C150(H150), C147(H147), C197(H197),
  C85(H85), C82(H82), C98(H98), C186(H186), C149(H149), C134(H134), C88(H88),
 C94(H94), C97(H97), C64(H64), C90(H90), C84(H84), C95(H95), C66(H66)
5.d Idealised Me refined as rotating group:
 C217(H21A,H21B,H21C), C61(H61A,H61B,H61C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C),
 C121(H12C,H12D,H12E), C209(H20A,H20B,H20C), C208(H20D,H20E,H20F), C105(H10A,
 H10B,H10C), C157(H15A,H15B,H15C), C227(H22C,H22D,H22E), C113(H11A,H11B,H11C),
 C124(H12H,H12I,H12J), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C228(H22H,H22I,
 H22J), C51(H51A,H51B,H51C), C123(H12K,H12L,H12M), C174(H17G,H17H,H17I),
 C173(H17J,H17K,H17L), C171(H17M,H17N,H17O), C50(H50A,H50B,H50C), C225(H22K,
 H22L,H22M), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C69(H69A,H69B,H69C),
 C71A(H71D,H71E,H71F)
;
_shelx_res_checksum              60027
_shelx_fab_checksum              30315
_platon_squeeze_void_probe_radius 1.20
_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 2.685
_oxdiff_exptl_absorpt_empirical_full_min 0.550