Advancing polyethylene properties by incorporating ‒NO2 moiety in 1,2-bis(arylimino)acenaphthylylnickel precatalysts: Synthesis, characterization and ethylene polymerization
Mahmood, Qaiser; Zemg, Yanning; Wang, Xinxin; Sun, Yang; Sun, Wen Hua; Dalton Trans.  (2017) –; doi:10.1039/C7DT01295K

data_7042850
_publ_section_title
;
 Advancing polyethylene properties by incorporating --NO2 moiety in
 1,2-bis(arylimino)acenaphthylylnickel precatalysts: Synthesis,
 characterization and ethylene polymerization
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01295K
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C52 H39 Br2 N3 Ni O2'
_chemical_formula_sum            'C52 H39 Br2 N3 Ni O2'
_chemical_formula_weight         956.35
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-09 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                72.25(3)
_cell_angle_beta                 88.46(3)
_cell_angle_gamma                60.83(3)
_cell_formula_units_Z            1
_cell_length_a                   10.577(2)
_cell_length_b                   10.776(2)
_cell_length_c                   13.294(3)
_cell_measurement_reflns_used    4440
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1246.5(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 44.9715
              2theta: -19.6886
scan:
    Number of images: 292
               Slice: -110.0000 - 36.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9715
              2theta: -19.6886
scan:
    Number of images: 160
               Slice: -20.0000 - 60.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9715
              2theta: -19.6886
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.103615
_diffrn_orient_matrix_UB_12      0.033316
_diffrn_orient_matrix_UB_13      -0.011489
_diffrn_orient_matrix_UB_21      -0.063472
_diffrn_orient_matrix_UB_22      -0.020379
_diffrn_orient_matrix_UB_23      -0.090943
_diffrn_orient_matrix_UB_31      -0.009559
_diffrn_orient_matrix_UB_32      0.075931
_diffrn_orient_matrix_UB_33      0.022735
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10445
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.031
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.117
_platon_squeeze_details
;
;
_refine_diff_density_max         0.983
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.028(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7312
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.2461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                7197
_reflns_number_total             7312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01295k1.cif
_cod_data_source_block           Ni1
_cod_original_cell_volume        1246.6(4)
_cod_database_code               7042850
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C32(H32), C19(H19)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C27(H27), C38(H38), C40(H40), C25(H25), C34(H34), C17(H17),
 C49(H49), C9(H9), C44(H44), C43(H43), C4AA(H4AA), C29(H29), C28(H28), C36(H36),
  C35(H35), C50(H50), C41(H41), C22(H22), C4(H4), C8(H8), C48(H48), C37(H37),
 C23(H23), C3(H3), C30(H30), C10(H10), C5(H5), C24(H24), C21(H21), C42(H42)
2.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C52(H52A,H52B,H52C)
;
_olex2_submission_special_instructions 'No special instructions were received'