#------------------------------------------------------------------------------
#$Date: 2021-12-07 06:01:44 +0200 (Tue, 07 Dec 2021) $
#$Revision: 271233 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/49/1564904.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_1564904
loop_
_publ_author_name
'Wang, Beibei'
'Liu, Heng'
'Zhang, Chunyu'
'Tang, Tao'
'Zhang, Xuequan'
_publ_section_title
;
 Propylene homopolymerization and copolymerization with ethylene by
 acenaphthene-based α-diimine nickel complexes to access EPR-like
 elastomers
;
_journal_issue                   43
_journal_name_full               'Polymer Chemistry'
_journal_page_first              6307
_journal_page_last               6318
_journal_paper_doi               10.1039/D1PY00923K
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C62 H60 Br2 N2 Ni, 2(C H2 Cl2)'
_chemical_formula_sum            'C64 H64 Br2 Cl4 N2 Ni'
_chemical_formula_weight         1221.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.0420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.961(2)
_cell_length_b                   12.0016(8)
_cell_length_c                   18.5133(13)
_cell_measurement_reflns_used    5947
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.934
_cell_measurement_theta_min      2.548
_cell_volume                     5814.1(7)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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      273.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16288
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.376
_diffrn_reflns_theta_min         1.556
_exptl_absorpt_coefficient_mu    1.933
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.806891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0547 before and 0.0216 after correction. The Ratio of minimum to maximum transmission is 0.8069. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.526
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5909
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0938P)²+13.0960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4631
_reflns_number_total             5909
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1py00923k2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 1564904--1564905.cif.'
_cod_database_code               1564904
_shelx_shelxl_version_number     2018/3
_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   0.944
_shelx_estimated_absorpt_t_min   0.910
_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. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C16(H16)
3.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_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 0.54132(2) 1.09105(4) 0.88296(3) 0.05793(18) Uani 1 1 d . . . . .
Ni01 Ni 0.500000 0.99384(5) 0.750000 0.03137(18) Uani 1 2 d S T P . .
N1 N 0.45757(10) 0.8660(2) 0.74872(17) 0.0283(6) Uani 1 1 d . . . . .
C1 C 0.47673(12) 0.7710(3) 0.7510(2) 0.0291(7) Uani 1 1 d . . . . .
C2 C 0.46427(13) 0.6540(3) 0.7546(2) 0.0328(7) Uani 1 1 d . . . . .
C3 C 0.500000 0.5902(4) 0.750000 0.0333(10) Uani 1 2 d S T P . .
C4 C 0.500000 0.4725(4) 0.750000 0.0397(11) Uani 1 2 d S T P . .
C5 C 0.46259(16) 0.4205(3) 0.7561(3) 0.0452(9) Uani 1 1 d . . . . .
H5 H 0.461218 0.343179 0.756845 0.054 Uiso 1 1 calc R . . . .
C6 C 0.42801(16) 0.4827(3) 0.7608(3) 0.0482(9) Uani 1 1 d . . . . .
H6 H 0.403714 0.445984 0.764593 0.058 Uiso 1 1 calc R . . . .
C7 C 0.42818(14) 0.6011(3) 0.7601(3) 0.0394(8) Uani 1 1 d . . . . .
H7 H 0.404480 0.641516 0.763356 0.047 Uiso 1 1 calc R . . . .
C8 C 0.41204(12) 0.8688(3) 0.7483(2) 0.0294(7) Uani 1 1 d . . . . .
C9 C 0.41793(13) 0.8635(3) 0.8294(2) 0.0330(7) Uani 1 1 d . . . . .
C10 C 0.37360(14) 0.8622(3) 0.8265(2) 0.0379(8) Uani 1 1 d . . . . .
H10 H 0.376311 0.859396 0.879248 0.045 Uiso 1 1 calc R . . . .
C11 C 0.32521(14) 0.8650(3) 0.7474(3) 0.0375(8) Uani 1 1 d . . . . .
C12 C 0.32137(13) 0.8730(3) 0.6695(2) 0.0339(7) Uani 1 1 d . . . . .
H12 H 0.289145 0.876312 0.616510 0.041 Uiso 1 1 calc R . . . .
C13 C 0.36451(12) 0.8763(3) 0.6681(2) 0.0294(7) Uani 1 1 d . . . . .
C14 C 0.47001(15) 0.8574(4) 0.9156(2) 0.0453(9) Uani 1 1 d . . . . .
H14A H 0.485557 0.787081 0.919761 0.068 Uiso 1 1 calc GR . . . .
H14B H 0.466620 0.864587 0.963675 0.068 Uiso 1 1 calc GR . . . .
H14C H 0.491023 0.916726 0.918307 0.068 Uiso 1 1 calc GR . . . .
C15 C 0.27747(16) 0.8613(4) 0.7471(3) 0.0542(10) Uani 1 1 d . . . . .
H15A H 0.247839 0.873807 0.688201 0.081 Uiso 1 1 calc GR . . . .
H15B H 0.279541 0.918172 0.785469 0.081 Uiso 1 1 calc GR . . . .
H15C H 0.274936 0.789644 0.767278 0.081 Uiso 1 1 calc GR . . . .
C16 C 0.36089(13) 0.8822(3) 0.5820(2) 0.0311(7) Uani 1 1 d . . . . .
H16 H 0.390098 0.926588 0.594455 0.037 Uiso 1 1 calc R . . . .
C17 C 0.31296(13) 0.9431(3) 0.5094(2) 0.0347(7) Uani 1 1 d . . . . .
C18 C 0.30946(16) 1.0568(3) 0.5186(3) 0.0490(9) Uani 1 1 d . . . . .
H18 H 0.336068 1.093816 0.568114 0.059 Uiso 1 1 calc R . . . .
C19 C 0.26629(19) 1.1156(4) 0.4542(3) 0.0591(11) Uani 1 1 d . . . . .
H19 H 0.264042 1.191670 0.461076 0.071 Uiso 1 1 calc R . . . .
C20 C 0.22651(16) 1.0615(4) 0.3796(3) 0.0575(12) Uani 1 1 d . . . . .
H20 H 0.197728 1.100943 0.336473 0.069 Uiso 1 1 calc R . . . .
C21 C 0.23001(16) 0.9512(4) 0.3702(3) 0.0548(11) Uani 1 1 d . . . . .
H21 H 0.203351 0.914876 0.320374 0.066 Uiso 1 1 calc R . . . .
C22 C 0.27272(15) 0.8908(3) 0.4338(3) 0.0450(9) Uani 1 1 d . . . . .
H22 H 0.274475 0.814892 0.425805 0.054 Uiso 1 1 calc R . . . .
C23 C 0.36703(12) 0.7663(3) 0.5549(2) 0.0327(7) Uani 1 1 d . . . . .
C24 C 0.33903(14) 0.6760(3) 0.5507(2) 0.0404(8) Uani 1 1 d . . . . .
H24 H 0.316309 0.684864 0.566351 0.048 Uiso 1 1 calc R . . . .
C25 C 0.34420(16) 0.5713(3) 0.5233(3) 0.0454(9) Uani 1 1 d . . . . .
H25 H 0.324180 0.512323 0.519530 0.055 Uiso 1 1 calc R . . . .
C26 C 0.37878(15) 0.5541(3) 0.5015(2) 0.0432(9) Uani 1 1 d . . . . .
C27 C 0.40683(16) 0.6454(3) 0.5066(3) 0.0466(9) Uani 1 1 d . . . . .
H27 H 0.430345 0.636603 0.492720 0.056 Uiso 1 1 calc R . . . .
C28 C 0.40084(14) 0.7503(3) 0.5321(2) 0.0398(8) Uani 1 1 d . . . . .
H28 H 0.419865 0.810086 0.533717 0.048 Uiso 1 1 calc R . . . .
C29 C 0.38288(17) 0.4404(4) 0.4680(3) 0.0526(10) Uani 1 1 d . . . . .
C30 C 0.4377(2) 0.4177(5) 0.4979(5) 0.100(2) Uani 1 1 d . U . . .
H30A H 0.447752 0.472650 0.472887 0.150 Uiso 1 1 calc GR . . . .
H30B H 0.439678 0.344920 0.478439 0.150 Uiso 1 1 calc GR . . . .
H30C H 0.460224 0.421262 0.561077 0.150 Uiso 1 1 calc GR . . . .
C31 C 0.3644(3) 0.3448(4) 0.4983(4) 0.096(2) Uani 1 1 d . . . . .
H31A H 0.382398 0.347247 0.561259 0.144 Uiso 1 1 calc GR . . . .
H31B H 0.370830 0.274867 0.481226 0.144 Uiso 1 1 calc GR . . . .
H31C H 0.328404 0.352718 0.471222 0.144 Uiso 1 1 calc GR . . . .
C32 C 0.3493(2) 0.4431(4) 0.3677(3) 0.0678(14) Uani 1 1 d . . . . .
H32A H 0.314251 0.452760 0.347115 0.102 Uiso 1 1 calc GR . . . .
H32B H 0.352867 0.374352 0.345298 0.102 Uiso 1 1 calc GR . . . .
H32C H 0.359488 0.503998 0.347472 0.102 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.40937(10) 0.8178(2) 0.3333(2) 0.1408(9) Uani 1 1 d . . . . .
Cl2 Cl 0.29885(8) 0.84487(15) 0.20692(13) 0.1122(6) Uani 1 1 d . . . . .
C33 C 0.3463(3) 0.8355(6) 0.3130(5) 0.108(2) Uani 1 1 d . . . . .
H33A H 0.339854 0.772770 0.338419 0.129 Uiso 1 1 calc R . . . .
H33B H 0.346720 0.902391 0.342856 0.129 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
Br1 Ni01 Br1 119.92(4) 2_656 . ?
N1 Ni01 Br1 111.02(7) 2_656 2_656 ?
N1 Ni01 Br1 113.25(7) 2_656 . ?
N1 Ni01 Br1 111.02(7) . . ?
N1 Ni01 Br1 113.25(7) . 2_656 ?
N1 Ni01 N1 82.38(15) 2_656 . ?
C1 N1 Ni01 111.5(2) . . ?
C1 N1 C8 118.6(3) . . ?
C8 N1 Ni01 129.9(2) . . ?
N1 C1 C1 117.21(17) . 2_656 ?
N1 C1 C2 135.5(3) . . ?
C2 C1 C1 107.28(18) . 2_656 ?
C3 C2 C1 105.4(3) . . ?
C7 C2 C1 134.9(3) . . ?
C7 C2 C3 119.7(3) . . ?
C2 C3 C2 114.6(4) 2_656 . ?
C4 C3 C2 122.7(2) . 2_656 ?
C4 C3 C2 122.7(2) . . ?
C5 C4 C3 116.3(2) . . ?
C5 C4 C3 116.3(2) 2_656 . ?
C5 C4 C5 127.4(5) 2_656 . ?
C6 C5 C4 120.9(4) . . ?
C5 C6 C7 122.3(4) . . ?
C2 C7 C6 118.1(3) . . ?
C9 C8 N1 118.4(3) . . ?
C13 C8 N1 119.0(3) . . ?
C13 C8 C9 122.6(3) . . ?
C8 C9 C14 121.5(3) . . ?
C10 C9 C8 116.9(3) . . ?
C10 C9 C14 121.5(3) . . ?
C9 C10 C11 122.3(3) . . ?
C10 C11 C15 120.6(3) . . ?
C12 C11 C10 118.7(3) . . ?
C12 C11 C15 120.7(4) . . ?
C11 C12 C13 121.8(3) . . ?
C8 C13 C12 117.6(3) . . ?
C8 C13 C16 119.9(3) . . ?
C12 C13 C16 122.4(3) . . ?
C17 C16 C13 112.1(3) . . ?
C17 C16 C23 113.6(3) . . ?
C23 C16 C13 110.6(3) . . ?
C18 C17 C16 118.3(3) . . ?
C18 C17 C22 118.3(3) . . ?
C22 C17 C16 123.4(3) . . ?
C17 C18 C19 120.2(4) . . ?
C20 C19 C18 120.4(4) . . ?
C21 C20 C19 119.4(4) . . ?
C20 C21 C22 121.1(4) . . ?
C21 C22 C17 120.5(4) . . ?
C24 C23 C16 122.1(3) . . ?
C24 C23 C28 118.0(3) . . ?
C28 C23 C16 119.9(3) . . ?
C23 C24 C25 121.2(3) . . ?
C26 C25 C24 121.1(4) . . ?
C25 C26 C29 121.0(4) . . ?
C27 C26 C25 116.9(3) . . ?
C27 C26 C29 121.9(4) . . ?
C26 C27 C28 121.9(3) . . ?
C23 C28 C27 120.8(3) . . ?
C30 C29 C26 111.0(4) . . ?
C30 C29 C31 109.7(5) . . ?
C31 C29 C26 112.1(4) . . ?
C32 C29 C26 108.0(3) . . ?
C32 C29 C30 107.8(4) . . ?
C32 C29 C31 108.2(5) . . ?
Cl2 C33 Cl1 113.5(4) . . ?
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 Ni01 2.3305(5) . ?
Ni01 N1 2.039(3) 2_656 ?
Ni01 N1 2.039(3) . ?
N1 C1 1.283(4) . ?
N1 C8 1.451(4) . ?
C1 C1 1.510(6) 2_656 ?
C1 C2 1.472(4) . ?
C2 C3 1.418(4) . ?
C2 C7 1.371(5) . ?
C3 C4 1.412(7) . ?
C4 C5 1.409(5) 2_656 ?
C4 C5 1.409(5) . ?
C5 C6 1.378(6) . ?
C6 C7 1.420(5) . ?
C8 C9 1.403(4) . ?
C8 C13 1.390(5) . ?
C9 C10 1.387(5) . ?
C9 C14 1.508(5) . ?
C10 C11 1.392(5) . ?
C11 C12 1.378(5) . ?
C11 C15 1.523(5) . ?
C12 C13 1.395(5) . ?
C13 C16 1.532(4) . ?
C16 C17 1.523(5) . ?
C16 C23 1.529(5) . ?
C17 C18 1.388(6) . ?
C17 C22 1.393(5) . ?
C18 C19 1.391(6) . ?
C19 C20 1.389(7) . ?
C20 C21 1.348(7) . ?
C21 C22 1.389(6) . ?
C23 C24 1.379(5) . ?
C23 C28 1.381(5) . ?
C24 C25 1.400(5) . ?
C25 C26 1.392(6) . ?
C26 C27 1.384(6) . ?
C26 C29 1.536(5) . ?
C27 C28 1.395(5) . ?
C29 C30 1.530(7) . ?
C29 C31 1.535(8) . ?
C29 C32 1.520(6) . ?
Cl1 C33 1.840(9) . ?
Cl2 C33 1.658(8) . ?
