Raising the N-aryl fluoride content in unsymmetrical diaryliminoacenaphthylenes as a route to highly active nickel(ii) catalysts in ethylene polymerization.
Wang, Xinxin; Fan, Linlin; Yuan, Yichun; Du, Shizhen; Sun, Yang; Solan, Gregory A.; Guo, Cun-Yue; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18313–18323; doi:10.1039/c6dt03817d

data_7040982
_publ_section_title
;
 Raising the N-aryl fluoride content in unsymmetrical
 diaryliminoacenaphthylenes as a route to highly active nickel(ii)
 catalysts in ethylene polymerization.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18313
_journal_page_last               18323
_journal_paper_doi               10.1039/c6dt03817d
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C54 H39 Br2 F5 N2 Ni, C4 H10 O'
_chemical_formula_sum            'C58 H49 Br2 F5 N2 Ni O'
_chemical_formula_weight         1103.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-16 deposited with the CCDC.
2016-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.625(2)
_cell_length_b                   19.234(4)
_cell_length_c                   24.652(5)
_cell_measurement_reflns_used    6723
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4820
_cell_measurement_theta_min      2.1919
_cell_volume                     5031.6(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.0806
              2theta: -19.8030
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0806
              2theta: -19.8030
scan:
    Number of images: 312
               Slice: -110.0000 - 46.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.0806
              2theta: -19.8030
scan:
    Number of images: 204
               Slice: -42.5000 - 59.5000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0806
              2theta: -19.8030
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0580
_diffrn_orient_matrix_UB_12      -0.0601
_diffrn_orient_matrix_UB_13      -0.0437
_diffrn_orient_matrix_UB_21      -0.0259
_diffrn_orient_matrix_UB_22      0.0400
_diffrn_orient_matrix_UB_23      -0.0208
_diffrn_orient_matrix_UB_31      0.0236
_diffrn_orient_matrix_UB_32      -0.0019
_diffrn_orient_matrix_UB_33      -0.0330
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33529
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.69
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.035
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7631
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         11045
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+5.4653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                9912
_reflns_number_total             11045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03817d2.cif
_cod_data_source_block           Ni2
_cod_depositor_comments
'Adding full bibliography for 7040982--7040983.cif.'
_cod_original_cell_volume        5031.8(17)
_cod_database_code               7040982
_diffrn_number_total             5929
_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:
 C38(H38), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C18A(H18A,H18B), C14A(H14A,H14B), C01R(H01A,H01B), C0AA(H0AA,H0AB)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C9(H9), C36(H36), C31(H31), C40(H40), C28(H28), C21(H21), C43(H43),
 C47(H47), C27(H27), C30(H30), C41(H41), C16(H16), C8(H8), C15(H15), C3(H3),
 C2(H2), C4(H4), C44(H44), C17(H17), C46(H46), C34(H34), C33(H33), C37(H37),
 C50(H50), C7(H7), C49(H49)
2.d Idealised Me refined as rotating group:
 C14B(H14C,H14D,H14E), C01U(H01C,H01D,H01E), C01V(H01F,H01G,H01H), C18B(H18C,
 H18D,H18E)
;
_olex2_submission_special_instructions 'No special instructions were received'