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_7042851
_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_formula_moiety         'C54 H43 Br2 N3 Ni O2, C4 H10 O'
_chemical_formula_sum            'C58 H53 Br2 N3 Ni O3'
_chemical_formula_weight         1058.52
_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'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-04-09 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.51(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.378(3)
_cell_length_b                   11.187(2)
_cell_length_c                   30.360(6)
_cell_measurement_reflns_used    14994
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4853
_cell_measurement_theta_min      1.6191
_cell_volume                     4868.2(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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9960
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9308
              2theta: -19.7950
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9308
              2theta: -19.7950
scan:
    Number of images: 282
               Slice: -94.0000 - 47.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9308
              2theta: -19.7950
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0144
_diffrn_orient_matrix_UB_12      -0.0075
_diffrn_orient_matrix_UB_13      -0.0678
_diffrn_orient_matrix_UB_21      0.0831
_diffrn_orient_matrix_UB_22      0.0257
_diffrn_orient_matrix_UB_23      -0.0206
_diffrn_orient_matrix_UB_31      0.0095
_diffrn_orient_matrix_UB_32      -0.0316
_diffrn_orient_matrix_UB_33      -0.0012
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            52064
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.089
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5613
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.4442
_exptl_crystal_description       needle
_exptl_crystal_F_000             2175.9575
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.3707
_refine_diff_density_min         -0.7114
_refine_diff_density_rms         0.1027
_refine_ls_d_res_high            0.7701
_refine_ls_d_res_low             10.4928
_refine_ls_goodness_of_fit_ref   1.0618
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    94
_refine_ls_number_parameters     607
_refine_ls_number_reflns         11117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0618
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+11.4340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                10593
_reflns_number_total             11117
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt01295k1.cif
_cod_data_source_block           Ni2
_cod_original_cell_volume        4868.1(17)
_cod_database_code               7042851
_diffrn_number_total             11724
_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:
 C19(H19), C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C47(H47a,H47b), C52(H52a,H52b), C56(H56a,H56b), C57(H57a,H57b)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C34(H34), C15(H15), C28(H28), C3(H3), C48(H48), C8(H8), C40(H40),
 C10(H10), C4(H4), C50(H50), C38(H38), C27(H27), C31(H31), C35(H35), C25(H25),
 C21(H21), C41(H41), C43(H43), C23(H23), C29(H29), C37(H37), C44(H44), C9(H9),
 C24(H24), C36(H36), C30(H30), C49(H49), C5(H5), C42(H42), C22(H22)
2.d Idealised Me refined as rotating group:
 C53(H53a,H53b,H53c), C54(H54a,H54b,H54c), C55(H55a,H55b,H55c), C58(H58a,H58b,
 H58c)
;
_olex2_submission_special_instructions 'No special instructions were received'