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_7055772
_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         'C38 H44 Br N4 Ni, C H4 O, Br'
_chemical_formula_sum            'C39 H48 Br2 N4 Ni O'
_chemical_formula_weight         807.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 90.083(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.772(4)
_cell_length_b                   26.504(6)
_cell_length_c                   17.489(4)
_cell_measurement_reflns_used    21677
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4844
_cell_measurement_theta_min      1.3950
_cell_volume                     7311(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 0.997
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 9.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.1739
              2theta: -20.0345
scan:
    Number of images: 240
               Slice: -80.0000 - 40.0000
         Image width: 0.5000
            Exp time: 9.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.1739
              2theta: -20.0345
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0046
_diffrn_orient_matrix_UB_12      -0.0470
_diffrn_orient_matrix_UB_13      0.0423
_diffrn_orient_matrix_UB_21      0.0273
_diffrn_orient_matrix_UB_22      0.0159
_diffrn_orient_matrix_UB_23      0.0207
_diffrn_orient_matrix_UB_31      -0.0393
_diffrn_orient_matrix_UB_32      0.0298
_diffrn_orient_matrix_UB_33      0.0289
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42112
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.164
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.753
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5675
_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    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         13572
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+14.4722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11196
_reflns_number_total             13572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj02464e1.cif
_cod_data_source_block           Ni1
_cod_depositor_comments
'Adding full bibliography for 7055772--7055773.cif.'
_cod_database_code               7055772
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.570
_diffrn_number_total             17034
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8585(9) 0.1415(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 C27-C24
 1.54 with sigma of 0.01
 C25A-C24
 1.51 with sigma of 0.01
 C23-C25A
 2.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C58 \\sim C11B \\sim C10B \\sim C6A \\sim C11A \\sim C10A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C27 \\sim C27A \\sim C25 \\sim C25A \\sim C24 \\sim C28A \\sim C28: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C11A) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C10B)
\\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11B) \\sim Ueq, Uanis(C28A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C27A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H59C)=Sof(H59D)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C10B)=Sof(H10G)=
 Sof(H10H)=Sof(H10I)=Sof(C11B)=Sof(H11G)=Sof(H11H)=Sof(H11I)=1-FVAR(1)
 Sof(H59A)=Sof(H59B)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C10A)=Sof(H10D)=
 Sof(H10E)=Sof(H10F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=FVAR(1)
 Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(C28A)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(H25E)=1-FVAR(2)
 Sof(H26A)=Sof(H26B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C26(H26C,H26D), C25(H25A,H25B), C9(H9A,H9B), C8(H8A,H8B),
 C59(H59A,H59B), C59(H59C,H59D), C6A(H6AA,H6AB), C43(H43A,H43B), C42(H42A,H42B),
  C58(H58A,H58B), C27A(H27D,H27E)
6.b Me refined with riding coordinates:
 C25A(H25C,H25D,H25E)
6.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C33(H33), C32(H32), C31(H31), C1(H1), C2(H2),
 C3(H3), C14(H14), C15(H15), C16(H16), C51(H51), C52(H52), C53(H53), C62(H62),
 C63(H63), C64(H64), C35(H35), C36(H36), C37(H37), C48(H48), C49(H49),
 C35A(H35A)
6.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C34A(H34A,H34B,H34C), C30A(H30A,
 H30B,H30C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C17A(H17A,H17B,H17C),
 C13A(H13A,H13B,H13C), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C66(H66A,
 H66B,H66C), C65(H65A,H65B,H65C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C4AA(H4AA,H4AB,H4AC), C1AA(H1AA,H1AB,
 H1AC), C10B(H10G,H10H,H10I), C11B(H11G,H11H,H11I), C28A(H28D,H28E,H28F)
6.e Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O1(H1A)
;
_shelx_res_checksum              88826
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'