#------------------------------------------------------------------------------
#$Date: 2020-05-05 16:28:12 +0300 (Tue, 05 May 2020) $
#$Revision: 251655 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/37/7703768.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_7703768
loop_
_publ_author_name
'Wang, Chaoqun'
'Zhang, Yuxing'
'Mu, Hongliang'
'Jian, Zhongbao'
_publ_section_title
;
 Systematic studies on dibenzhydryl and pentiptycenyl substituted
 pyridine-imine nickel(ii) mediated ethylene polymerization.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4824
_journal_page_last               4833
_journal_paper_doi               10.1039/d0dt00505c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C78 H64 Br4 N4 Ni2 O2'
_chemical_formula_sum            'C78 H64 Br4 N4 Ni2 O2'
_chemical_formula_weight         1526.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2020-02-11 deposited with the CCDC.	2020-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                96.0490(10)
_cell_angle_beta                 91.8800(10)
_cell_angle_gamma                107.2170(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5838(6)
_cell_length_b                   13.0175(9)
_cell_length_c                   13.8929(9)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.479
_cell_measurement_theta_min      2.344
_cell_volume                     1642.61(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47034
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         2.344
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1408 before and 0.0830 after correction.
The Ratio of minimum to maximum transmission is 0.6699.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0046(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         7505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0284
_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/[σ²(Fo²)+(0.0319P)²+1.0684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6506
_reflns_number_total             7505
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00505c2.cif
_cod_data_source_block           Ni1
_cod_depositor_comments
'Adding full bibliography for 7703768--7703771.cif.'
_cod_database_code               7703768
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.515
_shelx_estimated_absorpt_t_min   0.461
_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:
 C00D(H00D), C00F(H00F)
2.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00E(H00E), C00G(H00G), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C012(H012), C013(H013), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C019(H019)
2.c Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.68117(2) 0.54413(2) 0.54122(2) 0.02786(7) Uani 1 1 d . . . . .
Br2 Br 0.37156(3) 0.21880(2) 0.55301(2) 0.04069(8) Uani 1 1 d . . . . .
Ni1 Ni 0.51691(3) 0.36258(2) 0.47359(2) 0.02059(7) Uani 1 1 d . . . . .
O004 O 0.09320(14) 0.28693(11) 0.04073(10) 0.0260(3) Uani 1 1 d . . . . .
N2 N 0.53167(16) 0.32845(12) 0.32809(11) 0.0168(3) Uani 1 1 d . . . . .
N1 N 0.6972(2) 0.30706(14) 0.47366(13) 0.0284(4) Uani 1 1 d . . . . .
C007 C 0.42176(18) 0.31717(14) 0.25097(13) 0.0166(3) Uani 1 1 d . . . . .
C008 C 0.42142(18) 0.40503(14) 0.20086(13) 0.0162(3) Uani 1 1 d . . . . .
C009 C 0.5012(2) 0.60653(14) 0.18521(13) 0.0187(4) Uani 1 1 d . . . . .
C00A C 0.68939(19) 0.50516(14) 0.19759(13) 0.0184(4) Uani 1 1 d . . . . .
C00B C 0.31542(19) 0.21667(14) 0.23008(13) 0.0176(3) Uani 1 1 d . . . . .
C00C C 0.6511(2) 0.30954(15) 0.30683(14) 0.0211(4) Uani 1 1 d . . . . .
H00C H 0.674802 0.301033 0.241196 0.025 Uiso 1 1 calc R . . . .
C00D C 0.32879(19) 0.12102(14) 0.28051(14) 0.0187(4) Uani 1 1 d . . . . .
H00D H 0.356510 0.149400 0.350431 0.022 Uiso 1 1 calc R . . . .
C00E C 0.2022(2) 0.20514(15) 0.16004(14) 0.0203(4) Uani 1 1 d . . . . .
H00E H 0.126754 0.138122 0.146447 0.024 Uiso 1 1 calc R . . . .
C00F C 0.54063(19) 0.51323(14) 0.22611(13) 0.0172(3) Uani 1 1 d . . . . .
H00F H 0.547872 0.529733 0.298375 0.021 Uiso 1 1 calc R . . . .
C00G C 0.31021(19) 0.38957(15) 0.12907(13) 0.0186(4) Uani 1 1 d . . . . .
H00G H 0.309497 0.446895 0.092211 0.022 Uiso 1 1 calc R . . . .
C00H C 0.20013(19) 0.29133(15) 0.11058(13) 0.0190(4) Uani 1 1 d . . . . .
C00I C 0.18699(19) 0.02884(15) 0.27806(14) 0.0193(4) Uani 1 1 d . . . . .
C00J C 0.7505(2) 0.30129(15) 0.38566(16) 0.0246(4) Uani 1 1 d . . . . .
C00K C 0.4538(2) 0.08104(15) 0.24316(14) 0.0207(4) Uani 1 1 d . . . . .
C00L C 0.5837(2) 0.66732(16) 0.11957(15) 0.0245(4) Uani 1 1 d . . . . .
H00L H 0.669427 0.651958 0.098343 0.029 Uiso 1 1 calc R . . . .
C00M C 0.7058(2) 0.45406(16) 0.10724(14) 0.0240(4) Uani 1 1 d . . . . .
H00M H 0.623712 0.425303 0.061707 0.029 Uiso 1 1 calc R . . . .
C00N C 0.4999(2) 0.09044(16) 0.14984(15) 0.0250(4) Uani 1 1 d . . . . .
H00N H 0.449689 0.119920 0.105241 0.030 Uiso 1 1 calc R . . . .
C00O C 0.8110(2) 0.54719(17) 0.26294(15) 0.0264(4) Uani 1 1 d . . . . .
H00O H 0.801718 0.583561 0.324252 0.032 Uiso 1 1 calc R . . . .
C00P C -0.0315(2) -0.05483(18) 0.35719(16) 0.0284(4) Uani 1 1 d . . . . .
H00P H -0.090439 -0.054558 0.410844 0.034 Uiso 1 1 calc R . . . .
C00Q C -0.0760(2) -0.13757(16) 0.28154(16) 0.0272(4) Uani 1 1 d . . . . .
H00Q H -0.165538 -0.193766 0.282564 0.033 Uiso 1 1 calc R . . . .
C00R C 0.3769(2) 0.63161(16) 0.21643(15) 0.0256(4) Uani 1 1 d . . . . .
H00R H 0.320091 0.591223 0.262290 0.031 Uiso 1 1 calc R . . . .
C00S C 0.0983(2) 0.02782(16) 0.35553(15) 0.0244(4) Uani 1 1 d . . . . .
H00S H 0.127117 0.084459 0.407908 0.029 Uiso 1 1 calc R . . . .
C00T C 0.3354(2) 0.71464(17) 0.18134(17) 0.0320(5) Uani 1 1 d . . . . .
H00T H 0.249899 0.730429 0.202553 0.038 Uiso 1 1 calc R . . . .
C00U C 0.6188(2) 0.05708(17) 0.12116(17) 0.0314(5) Uani 1 1 d . . . . .
H00U H 0.649481 0.064106 0.057220 0.038 Uiso 1 1 calc R . . . .
C00V C 0.0109(2) -0.13761(17) 0.20458(17) 0.0309(5) Uani 1 1 d . . . . .
H00V H -0.018778 -0.194156 0.152169 0.037 Uiso 1 1 calc R . . . .
C00W C 0.5421(3) 0.75065(17) 0.08445(17) 0.0328(5) Uani 1 1 d . . . . .
H00W H 0.599049 0.791484 0.038900 0.039 Uiso 1 1 calc R . . . .
C00X C 0.1422(2) -0.05526(17) 0.20310(16) 0.0282(4) Uani 1 1 d . . . . .
H00X H 0.201791 -0.056788 0.149989 0.034 Uiso 1 1 calc R . . . .
C00Y C 0.4184(3) 0.77456(17) 0.11539(17) 0.0334(5) Uani 1 1 d . . . . .
H00Y H 0.390575 0.831876 0.091467 0.040 Uiso 1 1 calc R . . . .
C00Z C 0.9458(2) 0.5364(2) 0.23928(18) 0.0361(5) Uani 1 1 d . . . . .
H00Z H 1.027932 0.564178 0.284901 0.043 Uiso 1 1 calc R . . . .
C010 C 0.5269(2) 0.03478(17) 0.30593(17) 0.0299(5) Uani 1 1 d . . . . .
H010 H 0.495261 0.025811 0.369431 0.036 Uiso 1 1 calc R . . . .
C011 C -0.0418(2) 0.20381(19) 0.04227(17) 0.0333(5) Uani 1 1 d . . . . .
H01A H -0.116029 0.217180 -0.000733 0.050 Uiso 1 1 calc GR . . . .
H01B H -0.073736 0.203498 0.108564 0.050 Uiso 1 1 calc GR . . . .
H01C H -0.028709 0.133477 0.020038 0.050 Uiso 1 1 calc GR . . . .
C012 C 0.6925(2) 0.01373(18) 0.18525(19) 0.0358(5) Uani 1 1 d . . . . .
H012 H 0.775105 -0.007571 0.166112 0.043 Uiso 1 1 calc R . . . .
C013 C 0.8821(2) 0.27996(18) 0.3712(2) 0.0364(5) Uani 1 1 d . . . . .
H013 H 0.918481 0.277618 0.308444 0.044 Uiso 1 1 calc R . . . .
C014 C 0.8415(2) 0.44497(18) 0.08347(17) 0.0322(5) Uani 1 1 d . . . . .
H014 H 0.852076 0.410807 0.021438 0.039 Uiso 1 1 calc R . . . .
C015 C 0.6451(2) 0.00171(19) 0.2771(2) 0.0379(5) Uani 1 1 d . . . . .
H015 H 0.693990 -0.029540 0.320985 0.045 Uiso 1 1 calc R . . . .
C016 C 0.9612(2) 0.4853(2) 0.14951(19) 0.0375(5) Uani 1 1 d . . . . .
H016 H 1.053671 0.478091 0.133389 0.045 Uiso 1 1 calc R . . . .
C017 C 0.9593(3) 0.2621(2) 0.4506(2) 0.0474(7) Uani 1 1 d . . . . .
H017 H 1.051090 0.249213 0.443451 0.057 Uiso 1 1 calc R . . . .
C018 C 0.7705(3) 0.2867(2) 0.54878(19) 0.0455(6) Uani 1 1 d . . . . .
H018 H 0.731636 0.288209 0.610778 0.055 Uiso 1 1 calc R . . . .
C019 C 0.9017(3) 0.2634(2) 0.5392(2) 0.0535(8) Uani 1 1 d . . . . .
H019 H 0.951280 0.248330 0.593807 0.064 Uiso 1 1 calc R . . . .
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'
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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
Ni1 Br1 Ni1 94.073(11) . 2_666 ?
Br1 Ni1 Br1 85.927(11) . 2_666 ?
Br2 Ni1 Br1 130.477(13) . . ?
Br2 Ni1 Br1 95.001(13) . 2_666 ?
N2 Ni1 Br1 112.85(4) . . ?
N2 Ni1 Br1 96.26(4) . 2_666 ?
N2 Ni1 Br2 116.22(4) . . ?
N2 Ni1 N1 79.29(7) . . ?
N1 Ni1 Br1 88.22(5) . . ?
N1 Ni1 Br1 170.64(5) . 2_666 ?
N1 Ni1 Br2 94.35(5) . . ?
C00H O004 C011 116.34(15) . . ?
C007 N2 Ni1 127.75(11) . . ?
C00C N2 Ni1 113.50(13) . . ?
C00C N2 C007 118.62(16) . . ?
C00J N1 Ni1 112.51(13) . . ?
C018 N1 Ni1 128.61(18) . . ?
C018 N1 C00J 118.6(2) . . ?
C008 C007 N2 120.71(15) . . ?
C00B C007 N2 117.42(16) . . ?
C00B C007 C008 121.86(16) . . ?
C007 C008 C00F 119.87(16) . . ?
C00G C008 C007 117.83(16) . . ?
C00G C008 C00F 122.30(16) . . ?
C00L C009 C00F 122.98(17) . . ?
C00L C009 C00R 118.74(18) . . ?
C00R C009 C00F 118.27(16) . . ?
C00M C00A C00F 121.12(17) . . ?
C00O C00A C00F 119.92(17) . . ?
C00O C00A C00M 118.94(17) . . ?
C007 C00B C00D 119.61(16) . . ?
C007 C00B C00E 118.77(16) . . ?
C00E C00B C00D 121.56(16) . . ?
N2 C00C C00J 118.56(18) . . ?
C00I C00D C00B 114.34(15) . . ?
C00I C00D C00K 111.74(15) . . ?
C00K C00D C00B 111.25(15) . . ?
C00H C00E C00B 119.87(17) . . ?
C008 C00F C009 112.43(15) . . ?
C00A C00F C008 111.31(14) . . ?
C00A C00F C009 112.70(14) . . ?
C00H C00G C008 120.80(17) . . ?
O004 C00H C00E 123.64(17) . . ?
O004 C00H C00G 115.60(16) . . ?
C00E C00H C00G 120.76(17) . . ?
C00S C00I C00D 118.52(17) . . ?
C00X C00I C00D 123.33(17) . . ?
C00X C00I C00S 118.14(17) . . ?
N1 C00J C00C 113.77(17) . . ?
N1 C00J C013 122.4(2) . . ?
C013 C00J C00C 123.6(2) . . ?
C00N C00K C00D 123.08(17) . . ?
C00N C00K C010 118.35(18) . . ?
C010 C00K C00D 118.56(18) . . ?
C009 C00L C00W 120.46(19) . . ?
C014 C00M C00A 120.32(19) . . ?
C00K C00N C00U 120.6(2) . . ?
C00Z C00O C00A 120.4(2) . . ?
C00Q C00P C00S 120.58(19) . . ?
C00V C00Q C00P 119.17(18) . . ?
C00T C00R C009 120.79(19) . . ?
C00P C00S C00I 120.80(19) . . ?
C00Y C00T C00R 119.9(2) . . ?
C012 C00U C00N 120.3(2) . . ?
C00Q C00V C00X 120.4(2) . . ?
C00Y C00W C00L 120.4(2) . . ?
C00I C00X C00V 120.88(19) . . ?
C00W C00Y C00T 119.7(2) . . ?
C016 C00Z C00O 120.3(2) . . ?
C015 C010 C00K 120.9(2) . . ?
C015 C012 C00U 119.4(2) . . ?
C017 C013 C00J 118.3(3) . . ?
C016 C014 C00M 120.3(2) . . ?
C012 C015 C010 120.5(2) . . ?
C014 C016 C00Z 119.66(19) . . ?
C019 C017 C013 119.2(2) . . ?
N1 C018 C019 121.9(3) . . ?
C017 C019 C018 119.5(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Ni1 2.4858(3) . ?
Br1 Ni1 2.5519(3) 2_666 ?
Br2 Ni1 2.3777(3) . ?
Ni1 N2 2.0422(15) . ?
Ni1 N1 2.0606(18) . ?
O004 C00H 1.372(2) . ?
O004 C011 1.423(2) . ?
N2 C007 1.442(2) . ?
N2 C00C 1.277(2) . ?
N1 C00J 1.344(3) . ?
N1 C018 1.332(3) . ?
C007 C008 1.401(2) . ?
C007 C00B 1.395(2) . ?
C008 C00F 1.526(2) . ?
C008 C00G 1.390(3) . ?
C009 C00F 1.531(2) . ?
C009 C00L 1.383(3) . ?
C009 C00R 1.396(3) . ?
C00A C00F 1.522(2) . ?
C00A C00M 1.393(3) . ?
C00A C00O 1.389(3) . ?
C00B C00D 1.526(2) . ?
C00B C00E 1.397(3) . ?
C00C C00J 1.461(3) . ?
C00D C00I 1.520(2) . ?
C00D C00K 1.526(3) . ?
C00E C00H 1.381(3) . ?
C00G C00H 1.389(3) . ?
C00I C00S 1.392(3) . ?
C00I C00X 1.385(3) . ?
C00J C013 1.386(3) . ?
C00K C00N 1.389(3) . ?
C00K C010 1.391(3) . ?
C00L C00W 1.389(3) . ?
C00M C014 1.387(3) . ?
C00N C00U 1.390(3) . ?
C00O C00Z 1.386(3) . ?
C00P C00Q 1.381(3) . ?
C00P C00S 1.386(3) . ?
C00Q C00V 1.377(3) . ?
C00R C00T 1.385(3) . ?
C00T C00Y 1.383(3) . ?
C00U C012 1.383(3) . ?
C00V C00X 1.393(3) . ?
C00W C00Y 1.383(3) . ?
C00Z C016 1.384(3) . ?
C010 C015 1.382(3) . ?
C012 C015 1.378(4) . ?
C013 C017 1.385(4) . ?
C014 C016 1.381(3) . ?
C017 C019 1.366(4) . ?
C018 C019 1.386(4) . ?
