#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:59:58 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180283 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/69/7116966.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7116966
loop_
_publ_author_name
'Wei Gao'
'Lan Xin'
'Zhiqiang Hao'
'Guodong Li'
'Ji-Hu Su'
'Lijing Zhou'
'Ying Mu'
_publ_section_title
;
 The ligand redox behavior and role in
 1,2-bis[(2,6-diisopropylphenyl)imino]-acenaphthene nickel-TMA(MAO)
 systems for ethylene polymerization
;
_journal_name_full               Chem.Commun.
_journal_page_first              7004
_journal_paper_doi               10.1039/C5cc00582E
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C38 H46 Al Br2 N2 Ni'
_chemical_formula_weight         776.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-21 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7598(11)
_cell_length_b                   18.9444(15)
_cell_length_c                   14.2281(11)
_cell_measurement_reflns_used    4531
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.32
_cell_volume                     3708.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22125
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    2.729
_exptl_absorpt_correction_T_max  0.6850
_exptl_absorpt_correction_T_min  0.5980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0503P)²+0.8671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                2837
_reflns_number_total             3661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc00582e2.cif
_cod_data_source_block           Complex_4
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7116966
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.5000 0.15060(6) 0.2500 0.0348(3) Uani 1 2 d S . .
C1 C 0.44935(17) 0.46808(13) 0.23208(16) 0.0222(5) Uani 1 1 d . . .
C2 C 0.42019(19) 0.54167(13) 0.21813(17) 0.0250(6) Uani 1 1 d . . .
C3 C 0.3395(2) 0.57561(15) 0.18307(19) 0.0321(6) Uani 1 1 d . . .
H3 H 0.2854 0.5495 0.1603 0.038 Uiso 1 1 calc R . .
C4 C 0.3390(2) 0.64988(16) 0.1818(2) 0.0401(7) Uani 1 1 d . . .
H4 H 0.2835 0.6735 0.1576 0.048 Uiso 1 1 calc R . .
C5 C 0.4157(2) 0.68960(15) 0.2144(2) 0.0389(7) Uani 1 1 d . . .
H5 H 0.4118 0.7397 0.2129 0.047 Uiso 1 1 calc R . .
C6 C 0.5000 0.65676(19) 0.2500 0.0313(9) Uani 1 2 d S . .
C7 C 0.5000 0.58287(19) 0.2500 0.0268(8) Uani 1 2 d S . .
C8 C 0.31111(18) 0.39928(13) 0.19002(18) 0.0256(6) Uani 1 1 d . . .
C9 C 0.23376(18) 0.41873(13) 0.24894(19) 0.0298(6) Uani 1 1 d . . .
C10 C 0.1400(2) 0.40735(17) 0.2143(2) 0.0409(7) Uani 1 1 d . . .
H10 H 0.0857 0.4202 0.2519 0.049 Uiso 1 1 calc R . .
C11 C 0.1244(2) 0.37804(17) 0.1271(3) 0.0476(8) Uani 1 1 d . . .
H11 H 0.0599 0.3717 0.1050 0.057 Uiso 1 1 calc R . .
C12 C 0.2015(2) 0.35780(15) 0.0718(2) 0.0401(7) Uani 1 1 d . . .
H12 H 0.1895 0.3371 0.0121 0.048 Uiso 1 1 calc R . .
C13 C 0.29691(18) 0.36721(13) 0.10188(19) 0.0289(6) Uani 1 1 d . . .
C14 C 0.2485(2) 0.44697(15) 0.3473(2) 0.0363(7) Uani 1 1 d . . .
H14 H 0.3156 0.4672 0.3507 0.044 Uiso 1 1 calc R . .
C15 C 0.2423(4) 0.3874(2) 0.4183(2) 0.0866(15) Uani 1 1 d . . .
H15A H 0.1777 0.3657 0.4150 0.130 Uiso 1 1 calc R . .
H15B H 0.2531 0.4062 0.4816 0.130 Uiso 1 1 calc R . .
H15C H 0.2919 0.3519 0.4041 0.130 Uiso 1 1 calc R . .
C16 C 0.1779(3) 0.5046(2) 0.3746(3) 0.0687(11) Uani 1 1 d . . .
H16A H 0.1931 0.5214 0.4380 0.103 Uiso 1 1 calc R . .
H16B H 0.1115 0.4859 0.3734 0.103 Uiso 1 1 calc R . .
H16C H 0.1832 0.5439 0.3300 0.103 Uiso 1 1 calc R . .
C17 C 0.3839(2) 0.34686(15) 0.04275(19) 0.0349(7) Uani 1 1 d . . .
H17 H 0.4357 0.3308 0.0871 0.042 Uiso 1 1 calc R . .
C18 C 0.4246(3) 0.41004(17) -0.0106(2) 0.0525(9) Uani 1 1 d . . .
H18A H 0.4851 0.3964 -0.0422 0.079 Uiso 1 1 calc R . .
H18B H 0.4378 0.4486 0.0336 0.079 Uiso 1 1 calc R . .
H18C H 0.3772 0.4258 -0.0575 0.079 Uiso 1 1 calc R . .
C19 C 0.3640(3) 0.2854(2) -0.0246(3) 0.0602(10) Uani 1 1 d . . .
H19A H 0.3207 0.3012 -0.0750 0.090 Uiso 1 1 calc R . .
H19B H 0.3331 0.2466 0.0100 0.090 Uiso 1 1 calc R . .
H19C H 0.4254 0.2689 -0.0517 0.090 Uiso 1 1 calc R . .
C20 C 0.4459(2) 0.10353(17) 0.1402(2) 0.0512(8) Uani 1 1 d . . .
H20A H 0.4987 0.0843 0.1019 0.077 Uiso 1 1 calc R . .
H20B H 0.4085 0.1375 0.1030 0.077 Uiso 1 1 calc R . .
H20C H 0.4031 0.0651 0.1606 0.077 Uiso 1 1 calc R . .
Br1 Br 0.38304(2) 0.236566(16) 0.30327(2) 0.04251(12) Uani 1 1 d . . .
N1 N 0.40956(14) 0.40649(11) 0.22169(14) 0.0227(5) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.32845(2) 0.2500 0.02578(14) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C20 Al1 C20 125.5(2) . 4_655
C20 Al1 Br1 108.21(11) . 4_655
C20 Al1 Br1 107.82(10) 4_655 4_655
C20 Al1 Br1 107.82(10) . .
C20 Al1 Br1 108.21(11) 4_655 .
Br1 Al1 Br1 95.05(4) 4_655 .
N1 C1 C2 136.5(2) . .
N1 C1 C1 115.82(14) . 4_655
C2 C1 C1 107.69(14) . 4_655
C3 C2 C7 118.8(3) . .
C3 C2 C1 135.6(2) . .
C7 C2 C1 105.5(2) . .
C2 C3 C4 118.4(3) . .
C2 C3 H3 120.8 . .
C4 C3 H3 120.8 . .
C5 C4 C3 122.6(3) . .
C5 C4 H4 118.7 . .
C3 C4 H4 118.7 . .
C4 C5 C6 120.7(3) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C7 C6 C5 116.18(19) . .
C7 C6 C5 116.18(19) . 4_655
C5 C6 C5 127.6(4) . 4_655
C6 C7 C2 123.30(16) . .
C6 C7 C2 123.30(16) . 4_655
C2 C7 C2 113.4(3) . 4_655
C9 C8 C13 122.7(2) . .
C9 C8 N1 120.2(2) . .
C13 C8 N1 116.9(2) . .
C10 C9 C8 116.7(3) . .
C10 C9 C14 120.3(2) . .
C8 C9 C14 122.9(2) . .
C11 C10 C9 121.6(3) . .
C11 C10 H10 119.2 . .
C9 C10 H10 119.2 . .
C12 C11 C10 120.6(3) . .
C12 C11 H11 119.7 . .
C10 C11 H11 119.7 . .
C11 C12 C13 121.0(3) . .
C11 C12 H12 119.5 . .
C13 C12 H12 119.5 . .
C12 C13 C8 117.4(3) . .
C12 C13 C17 122.8(2) . .
C8 C13 C17 119.7(2) . .
C9 C14 C16 114.0(3) . .
C9 C14 C15 110.2(3) . .
C16 C14 C15 109.2(3) . .
C9 C14 H14 107.7 . .
C16 C14 H14 107.7 . .
C15 C14 H14 107.7 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C13 C17 C18 111.6(2) . .
C13 C17 C19 113.6(2) . .
C18 C17 C19 110.6(3) . .
C13 C17 H17 106.9 . .
C18 C17 H17 106.9 . .
C19 C17 H17 106.9 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
Al1 C20 H20A 109.5 . .
Al1 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
Al1 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
Al1 Br1 Ni1 86.85(2) . .
C1 N1 C8 121.3(2) . .
C1 N1 Ni1 112.60(16) . .
C8 N1 Ni1 126.03(16) . .
N1 Ni1 N1 83.00(12) 4_655 .
N1 Ni1 Br1 100.27(6) 4_655 4_655
N1 Ni1 Br1 150.38(6) . 4_655
N1 Ni1 Br1 150.38(6) 4_655 .
N1 Ni1 Br1 100.27(6) . .
Br1 Ni1 Br1 91.24(2) 4_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 C20 1.947(3) .
Al1 C20 1.947(3) 4_655
Al1 Br1 2.4118(8) 4_655
Al1 Br1 2.4118(8) .
C1 N1 1.297(3) .
C1 C2 1.464(3) .
C1 C1 1.484(5) 4_655
C2 C3 1.377(4) .
C2 C7 1.421(3) .
C3 C4 1.407(4) .
C3 H3 0.9500 .
C4 C5 1.377(4) .
C4 H4 0.9500 .
C5 C6 1.410(3) .
C5 H5 0.9500 .
C6 C7 1.400(5) .
C6 C5 1.410(3) 4_655
C7 C2 1.421(3) 4_655
C8 C9 1.404(3) .
C8 C13 1.407(4) .
C8 N1 1.434(3) .
C9 C10 1.397(4) .
C9 C14 1.512(4) .
C10 C11 1.376(5) .
C10 H10 0.9500 .
C11 C12 1.376(4) .
C11 H11 0.9500 .
C12 C13 1.392(4) .
C12 H12 0.9500 .
C13 C17 1.513(4) .
C14 C16 1.513(4) .
C14 C15 1.517(4) .
C14 H14 1.0000 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 C18 1.524(4) .
C17 C19 1.533(4) .
C17 H17 1.0000 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
Br1 Ni1 2.4889(4) .
N1 Ni1 1.974(2) .
Ni1 N1 1.974(2) 4_655
Ni1 Br1 2.4889(4) 4_655
