Rigid geometry 8-arylimino-7,7-dimethyl-5,6-dihydroquinolyl nickel bromides: single-site active species towards ethylene polymerization
Huang, Chuanbing; Zhang, Youfu; Liang, Tongling; Zhao, Zhijuan; Hu, Xinquan; Sun, Wen-Hua; New J. Chem. 40 (2016) 9329–; doi:10.1039/C6NJ02464E

data_7055773
_publ_section_title
;
 Rigid geometry 8-arylimino-7,7-dimethyl-5,6-dihydroquinolyl nickel
 bromides: single-site active species towards ethylene polymerization
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              9329
_journal_paper_doi               10.1039/C6NJ02464E
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C40 H48 Br N4 Ni, Br'
_chemical_formula_sum            'C40 H48 Br2 N4 Ni'
_chemical_formula_weight         803.35
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-09-14 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.088(4)
_cell_length_b                   25.088(4)
_cell_length_c                   13.251(3)
_cell_measurement_reflns_used    22890
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4852
_cell_measurement_theta_min      1.1478
_cell_volume                     8340(3)
_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  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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: 0.0000
                 XTD: 45.0346
              2theta: -19.9806
scan:
    Number of images: 240
               Slice: -80.0000 - 40.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.0346
              2theta: -19.9806
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0250
_diffrn_orient_matrix_UB_12      0.0300
_diffrn_orient_matrix_UB_13      0.0078
_diffrn_orient_matrix_UB_21      0.0000
_diffrn_orient_matrix_UB_22      -0.0101
_diffrn_orient_matrix_UB_23      0.0386
_diffrn_orient_matrix_UB_31      0.0588
_diffrn_orient_matrix_UB_32      -0.0458
_diffrn_orient_matrix_UB_33      -0.0120
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56581
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         1.148
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.411
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         9558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0757
_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^)+(0.0405P)^2^+22.4579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8622
_reflns_number_total             9558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj02464e1.cif
_cod_data_source_block           Ni3
_cod_depositor_comments
'Adding full bibliography for 7055772--7055773.cif.'
_cod_database_code               7055773
_diffrn_number_total             9978
_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 Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C25(H25A,H25B), C26(H26A,H26B)
2.b Me refined with riding coordinates:
 C13A(H13A,H13B,H13C)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C14(H14), C16(H16), C18(H18), C19(H19), C20(H20),
 C31(H31), C33(H33)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15A(H15A,H15B,H15C), C17A(H17A,
 H17B,H17C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30A(H30A,H30B,H30C),
 C32A(H32A,H32B,H32C), C34A(H34A,H34B,H34C)
;
_shelx_res_checksum              78033
_shelx_fab_checksum              51461
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'