#------------------------------------------------------------------------------
#$Date: 2021-12-07 06:01:44 +0200 (Tue, 07 Dec 2021) $
#$Revision: 271233 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/49/1564905.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_1564905
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_sum            'C31 H24 Br N Ni0.5'
_chemical_formula_weight         519.78
_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
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.380(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.143(4)
_cell_length_b                   12.407(2)
_cell_length_c                   17.891(3)
_cell_measurement_reflns_used    4977
_cell_measurement_temperature    207(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.00
_cell_volume                     5637.0(15)
_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-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      207(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0987
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36170
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.004
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  0.8134
_exptl_absorpt_correction_T_min  0.7039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
;
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4977
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0627
_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)+(0.0892P)²+4.3067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3185
_reflns_number_total             4977
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1py00923k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1564904--1564905.cif.'
_cod_original_cell_volume        5637.1(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C31 H24 Br N Ni0.50'
_cod_database_code               1564905
_shelx_shelxl_version_number     2017/1
_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_min   0.704
_shelx_estimated_absorpt_t_max   0.813
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
Ni1 Ni 0.000000 0.53471(7) 0.250000 0.0422(3) Uani 1 2 d S T P . .
Br1 Br 0.05046(3) 0.43953(6) 0.20407(5) 0.0801(3) Uani 1 1 d . . . . .
N1 N 0.04122(13) 0.6576(3) 0.3282(2) 0.0379(9) Uani 1 1 d . . . . .
C1 C 0.02198(16) 0.7497(4) 0.2964(3) 0.0354(11) Uani 1 1 d . . . . .
C2 C 0.03313(17) 0.8624(4) 0.3237(3) 0.0389(11) Uani 1 1 d . . . . .
C3 C 0.000000 0.9228(6) 0.250000 0.0424(17) Uani 1 2 d S T P . .
C4 C 0.000000 1.0366(6) 0.250000 0.0528(19) Uani 1 2 d S T P . .
C5 C 0.0339(2) 1.0869(5) 0.3293(4) 0.0605(15) Uani 1 1 d . . . . .
H5A H 0.035074 1.162536 0.332623 0.073 Uiso 1 1 calc R U . . .
C6 C 0.0649(2) 1.0279(5) 0.4011(4) 0.0582(15) Uani 1 1 d . . . . .
H6A H 0.086251 1.064027 0.453003 0.070 Uiso 1 1 calc R U . . .
C7 C 0.0659(2) 0.9138(5) 0.3995(3) 0.0511(13) Uani 1 1 d . . . . .
H7A H 0.088283 0.874284 0.448986 0.061 Uiso 1 1 calc R U . . .
C8 C 0.08552(17) 0.6480(4) 0.4156(3) 0.0385(11) Uani 1 1 d . . . . .
C9 C 0.13626(17) 0.6399(4) 0.4272(3) 0.0407(12) Uani 1 1 d . . . . .
C10 C 0.17657(19) 0.6253(5) 0.5110(3) 0.0545(14) Uani 1 1 d . . . . .
H10A H 0.211376 0.620044 0.521316 0.065 Uiso 1 1 calc R U . . .
C11 C 0.16744(19) 0.6182(5) 0.5798(3) 0.0528(14) Uani 1 1 d . . . . .
C12 C 0.1163(2) 0.6268(5) 0.5646(3) 0.0532(14) Uani 1 1 d . . . . .
H12A H 0.109840 0.620882 0.611045 0.064 Uiso 1 1 calc R U . . .
C13 C 0.07424(19) 0.6439(4) 0.4830(3) 0.0483(13) Uani 1 1 d . . . . .
C14 C 0.01867(19) 0.6575(5) 0.4680(3) 0.0597(15) Uani 1 1 d . . . . .
H14A H -0.005274 0.613726 0.419484 0.090 Uiso 1 1 calc R U . . .
H14B H 0.008433 0.732669 0.456053 0.090 Uiso 1 1 calc R U . . .
H14C H 0.017281 0.634986 0.518729 0.090 Uiso 1 1 calc R U . . .
C15 C 0.2120(2) 0.5981(6) 0.6718(4) 0.080(2) Uani 1 1 d . . . . .
H15A H 0.201831 0.540725 0.697509 0.120 Uiso 1 1 calc R U . . .
H15B H 0.218530 0.663471 0.705315 0.120 Uiso 1 1 calc R U . . .
H15C H 0.243750 0.577561 0.670628 0.120 Uiso 1 1 calc R U . . .
C16 C 0.14635(17) 0.6514(4) 0.3518(3) 0.0434(12) Uani 1 1 d . . . . .
H16A H 0.116565 0.615480 0.302383 0.052 Uiso 1 1 calc R U . . .
C17 C 0.14425(18) 0.7685(5) 0.3275(3) 0.0509(14) Uani 1 1 d . . . . .
C18 C 0.1133(2) 0.8000(5) 0.2423(4) 0.0620(16) Uani 1 1 d . . . . .
H18A H 0.094810 0.748673 0.199116 0.074 Uiso 1 1 calc R U . . .
C19 C 0.1100(2) 0.9149(6) 0.2213(4) 0.0753(19) Uani 1 1 d . U . . .
C20 C 0.0772(3) 0.9500(7) 0.1386(5) 0.096(2) Uani 1 1 d . . . . .
H20A H 0.057509 0.900599 0.094408 0.115 Uiso 1 1 calc R U . . .
C21 C 0.0739(4) 1.0624(9) 0.1217(7) 0.116(3) Uani 1 1 d . . . . .
H21A H 0.052293 1.088792 0.065911 0.139 Uiso 1 1 calc R U . . .
C22 C 0.1029(5) 1.1325(9) 0.1887(9) 0.125(4) Uani 1 1 d . . . . .
H22A H 0.098854 1.206420 0.175512 0.151 Uiso 1 1 calc R U . . .
C23 C 0.1343(4) 1.1077(8) 0.2659(8) 0.111(3) Uani 1 1 d . . . . .
H23 H 0.153492 1.160316 0.307391 0.133 Uiso 1 1 calc R U . . .
C24 C 0.1394(3) 0.9885(6) 0.2881(6) 0.085(2) Uani 1 1 d . U . . .
C25 C 0.1707(3) 0.9537(6) 0.3704(5) 0.079(2) Uani 1 1 d . . . . .
H25A H 0.190923 1.003287 0.414067 0.095 Uiso 1 1 calc R U . . .
C26 C 0.1722(2) 0.8476(5) 0.3887(4) 0.0597(15) Uani 1 1 d . . . . .
H26A H 0.193429 0.825795 0.445935 0.072 Uiso 1 1 calc R U . . .
C27 C 0.19632(18) 0.5941(5) 0.3654(3) 0.0492(14) Uani 1 1 d . . . . .
C28 C 0.2367(2) 0.6479(5) 0.3632(4) 0.0645(16) Uani 1 1 d . . . . .
H28A H 0.234656 0.722761 0.353890 0.077 Uiso 1 1 calc R U . . .
C29 C 0.2820(2) 0.5893(6) 0.3751(4) 0.0733(19) Uani 1 1 d . . . . .
H29A H 0.309719 0.626472 0.373894 0.088 Uiso 1 1 calc R U . . .
C30 C 0.2856(2) 0.4850(7) 0.3876(4) 0.0743(19) Uani 1 1 d . . . . .
H30A H 0.315961 0.448694 0.395302 0.089 Uiso 1 1 calc R U . . .
C31 C 0.2456(3) 0.4273(6) 0.3896(5) 0.086(2) Uani 1 1 d . . . . .
H31A H 0.248137 0.352208 0.397760 0.103 Uiso 1 1 calc R U . . .
C32 C 0.2012(2) 0.4837(6) 0.3791(4) 0.0701(17) Uani 1 1 d . . . . .
H32A H 0.174046 0.445749 0.381376 0.084 Uiso 1 1 calc R U . . .
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'
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'
Br Br -0.2901 2.4595 '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
N1 Ni1 N1 82.0(2) . 2 ?
N1 Ni1 Br1 111.33(10) . . ?
N1 Ni1 Br1 113.72(11) 2 . ?
N1 Ni1 Br1 113.72(11) . 2 ?
N1 Ni1 Br1 111.33(10) 2 2 ?
Br1 Ni1 Br1 119.03(6) . 2 ?
C1 N1 C8 120.9(4) . . ?
C1 N1 Ni1 112.6(3) . . ?
C8 N1 Ni1 126.3(3) . . ?
N1 C1 C2 136.8(4) . . ?
N1 C1 C1 115.9(3) . 2 ?
C2 C1 C1 107.2(2) . 2 ?
C7 C2 C3 120.1(5) . . ?
C7 C2 C1 134.9(5) . . ?
C3 C2 C1 104.9(4) . . ?
C2 C3 C2 115.7(6) 2 . ?
C2 C3 C4 122.2(3) 2 . ?
C2 C3 C4 122.2(3) . . ?
C3 C4 C5 116.1(4) . 2 ?
C3 C4 C5 116.1(4) . . ?
C5 C4 C5 127.7(8) 2 . ?
C6 C5 C4 121.4(6) . . ?
C6 C5 H5A 119.3 . . ?
C4 C5 H5A 119.3 . . ?
C5 C6 C7 121.8(5) . . ?
C5 C6 H6A 119.1 . . ?
C7 C6 H6A 119.1 . . ?
C2 C7 C6 118.2(5) . . ?
C2 C7 H7A 120.9 . . ?
C6 C7 H7A 120.9 . . ?
C9 C8 C13 123.4(4) . . ?
C9 C8 N1 118.8(4) . . ?
C13 C8 N1 117.8(4) . . ?
C10 C9 C8 116.4(4) . . ?
C10 C9 C16 122.7(4) . . ?
C8 C9 C16 120.9(4) . . ?
C11 C10 C9 122.6(5) . . ?
C11 C10 H10A 118.7 . . ?
C9 C10 H10A 118.7 . . ?
C12 C11 C10 118.7(5) . . ?
C12 C11 C15 119.0(5) . . ?
C10 C11 C15 122.2(5) . . ?
C11 C12 C13 121.9(5) . . ?
C11 C12 H12A 119.0 . . ?
C13 C12 H12A 119.0 . . ?
C12 C13 C8 117.0(4) . . ?
C12 C13 C14 121.3(5) . . ?
C8 C13 C14 121.7(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C9 110.3(4) . . ?
C17 C16 C27 113.2(4) . . ?
C9 C16 C27 113.4(4) . . ?
C17 C16 H16A 106.4 . . ?
C9 C16 H16A 106.4 . . ?
C27 C16 H16A 106.4 . . ?
C18 C17 C26 118.4(6) . . ?
C18 C17 C16 119.9(5) . . ?
C26 C17 C16 121.7(5) . . ?
C17 C18 C19 118.6(6) . . ?
C17 C18 H18A 120.7 . . ?
C19 C18 H18A 120.7 . . ?
C20 C19 C24 121.2(8) . . ?
C20 C19 C18 120.3(8) . . ?
C24 C19 C18 118.5(6) . . ?
C19 C20 C21 118.4(9) . . ?
C19 C20 H20A 120.8 . . ?
C21 C20 H20A 120.8 . . ?
C22 C21 C20 119.0(9) . . ?
C22 C21 H21A 120.5 . . ?
C20 C21 H21A 120.5 . . ?
C23 C22 C21 126.9(12) . . ?
C23 C22 H22A 116.6 . . ?
C21 C22 H22A 116.6 . . ?
C22 C23 C24 116.7(11) . . ?
C22 C23 H23 121.7 . . ?
C24 C23 H23 121.7 . . ?
C25 C24 C19 121.0(7) . . ?
C25 C24 C23 121.1(9) . . ?
C19 C24 C23 117.8(8) . . ?
C26 C25 C24 119.5(7) . . ?
C26 C25 H25A 120.2 . . ?
C24 C25 H25A 120.2 . . ?
C25 C26 C17 123.9(6) . . ?
C25 C26 H26A 118.1 . . ?
C17 C26 H26A 118.1 . . ?
C28 C27 C32 118.0(5) . . ?
C28 C27 C16 122.2(5) . . ?
C32 C27 C16 119.7(5) . . ?
C27 C28 C29 119.4(6) . . ?
C27 C28 H28A 120.3 . . ?
C29 C28 H28A 120.3 . . ?
C30 C29 C28 121.4(6) . . ?
C30 C29 H29A 119.3 . . ?
C28 C29 H29A 119.3 . . ?
C29 C30 C31 121.1(6) . . ?
C29 C30 H30A 119.4 . . ?
C31 C30 H30A 119.4 . . ?
C30 C31 C32 118.2(7) . . ?
C30 C31 H31A 120.9 . . ?
C32 C31 H31A 120.9 . . ?
C27 C32 C31 121.8(6) . . ?
C27 C32 H32A 119.1 . . ?
C31 C32 H32A 119.1 . . ?
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
Ni1 N1 2.019(4) . ?
Ni1 N1 2.019(4) 2 ?
Ni1 Br1 2.3277(8) . ?
Ni1 Br1 2.3277(8) 2 ?
N1 C1 1.278(6) . ?
N1 C8 1.464(6) . ?
C1 C2 1.463(7) . ?
C1 C1 1.520(8) 2 ?
C2 C7 1.373(7) . ?
C2 C3 1.409(6) . ?
C3 C4 1.412(10) . ?
C4 C5 1.415(7) 2 ?
C4 C5 1.415(7) . ?
C5 C6 1.365(8) . ?
C5 H5A 0.9400 . ?
C6 C7 1.417(7) . ?
C6 H6A 0.9400 . ?
C7 H7A 0.9400 . ?
C8 C9 1.392(6) . ?
C8 C13 1.398(7) . ?
C9 C10 1.390(7) . ?
C9 C16 1.522(7) . ?
C10 C11 1.383(7) . ?
C10 H10A 0.9400 . ?
C11 C12 1.382(7) . ?
C11 C15 1.537(7) . ?
C12 C13 1.387(7) . ?
C12 H12A 0.9400 . ?
C13 C14 1.515(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.509(8) . ?
C16 C27 1.529(6) . ?
C16 H16A 0.9900 . ?
C17 C18 1.393(7) . ?
C17 C26 1.397(8) . ?
C18 C19 1.465(9) . ?
C18 H18A 0.9400 . ?
C19 C20 1.381(10) . ?
C19 C24 1.410(10) . ?
C20 C21 1.420(11) . ?
C20 H20A 0.9400 . ?
C21 C22 1.384(13) . ?
C21 H21A 0.9400 . ?
C22 C23 1.264(13) . ?
C22 H22A 0.9400 . ?
C23 C24 1.520(12) . ?
C23 H23 0.9400 . ?
C24 C25 1.367(10) . ?
C25 C26 1.351(9) . ?
C25 H25A 0.9400 . ?
C26 H26A 0.9400 . ?
C27 C28 1.371(7) . ?
C27 C32 1.386(8) . ?
C28 C29 1.427(8) . ?
C28 H28A 0.9400 . ?
C29 C30 1.309(9) . ?
C29 H29A 0.9400 . ?
C30 C31 1.385(10) . ?
C30 H30A 0.9400 . ?
C31 C32 1.399(9) . ?
C31 H31A 0.9400 . ?
C32 H32A 0.9400 . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.250 0.250 0.500 332.0 66.0
2 0.750 0.250 0.000 332.1 66.3
3 0.250 0.750 0.000 332.1 66.3
4 0.750 0.750 0.500 332.0 66.0
