#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:09:13 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234784 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/34/1553407.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_1553407
loop_
_publ_author_name
'Zhang, Youfu'
'Huang, Chuanbing'
'Wang, Xinxin'
'Mahmood, Qaiser'
'Hao, Xiang'
'Hu, Xinquan'
'Guo, Cun-Yue'
'Solan, Gregory A.'
'Sun, Wen-Hua'
_publ_section_title
;
 Highly branched unsaturated polyethylenes achievable using strained
 imino-cyclopenta[b]pyridyl-nickel precatalysts
;
_journal_issue                   6
_journal_name_full               'Polymer Chemistry'
_journal_page_first              995
_journal_paper_doi               10.1039/C6PY02089E
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C42 H54 Cl4 N4 Ni2 O2'
_chemical_formula_weight         906.07
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-11-27 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                91.22(3)
_cell_angle_beta                 109.68(3)
_cell_angle_gamma                108.69(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7278(19)
_cell_length_b                   10.550(2)
_cell_length_c                   11.522(2)
_cell_measurement_reflns_used    3235
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4791
_cell_measurement_theta_min      2.4414
_cell_volume                     1043.6(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13422
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7440
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0661P)²+0.4788P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                4621
_reflns_number_total             4730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6py02089e2.cif
_cod_data_source_block           Ni2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1043.6(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1553407
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.05169(3) 0.46863(3) 0.88123(2) 0.01626(11) Uani 1 1 d .
Cl1 Cl -0.09305(6) 0.32786(5) 0.98807(5) 0.01931(14) Uani 1 1 d .
Cl2 Cl -0.16817(7) 0.50118(6) 0.73103(5) 0.02389(14) Uani 1 1 d .
O1 O 0.25007(19) 0.45712(17) 1.03256(15) 0.0249(4) Uani 1 1 d .
N2 N 0.1935(2) 0.57161(19) 0.78969(17) 0.0188(4) Uani 1 1 d .
N1 N 0.0482(2) 0.29612(18) 0.76928(16) 0.0151(3) Uani 1 1 d .
C7 C 0.1514(2) 0.2734(2) 0.59103(19) 0.0179(4) Uani 1 1 d .
C12 C -0.1823(3) 0.0883(2) 0.6909(2) 0.0194(4) Uani 1 1 d .
C16 C 0.0602(3) 0.0833(2) 0.8458(2) 0.0210(4) Uani 1 1 d .
C6 C 0.1249(2) 0.3385(2) 0.69804(19) 0.0160(4) Uani 1 1 d .
C5 C 0.2061(2) 0.4844(2) 0.7117(2) 0.0175(4) Uani 1 1 d .
C14 C -0.1652(3) -0.1220(2) 0.7641(3) 0.0291(5) Uani 1 1 d .
H14 H -0.2119 -0.2166 0.7615 0.035 Uiso 1 1 calc R
C13 C -0.2489(3) -0.0506(2) 0.6899(2) 0.0243(5) Uani 1 1 d .
H13 H -0.3539 -0.0971 0.6370 0.029 Uiso 1 1 calc R
C17 C -0.2825(3) 0.1610(2) 0.6124(2) 0.0231(5) Uani 1 1 d .
H17A H -0.3289 0.1163 0.5248 0.028 Uiso 1 1 calc R
H17B H -0.2168 0.2554 0.6147 0.028 Uiso 1 1 calc R
C11 C -0.0264(2) 0.1534(2) 0.7675(2) 0.0172(4) Uani 1 1 d .
C4 C 0.2968(2) 0.5156(2) 0.6397(2) 0.0197(4) Uani 1 1 d .
C10 C 0.1900(3) 0.1445(2) 0.6123(2) 0.0262(5) Uani 1 1 d .
H10C H 0.2808 0.1621 0.6892 0.039 Uiso 1 1 calc R
H10A H 0.2133 0.1156 0.5419 0.039 Uiso 1 1 calc R
H10B H 0.1007 0.0731 0.6195 0.039 Uiso 1 1 calc R
C19 C 0.2276(3) 0.1545(2) 0.9305(2) 0.0265(5) Uani 1 1 d .
H19B H 0.2287 0.1970 1.0084 0.032 Uiso 1 1 calc R
H19A H 0.2768 0.2279 0.8896 0.032 Uiso 1 1 calc R
C3 C 0.3817(3) 0.6517(2) 0.6462(2) 0.0269(5) Uani 1 1 d .
H3 H 0.4465 0.6797 0.5987 0.032 Uiso 1 1 calc R
C1 C 0.2737(3) 0.7016(2) 0.7947(2) 0.0249(5) Uani 1 1 d .
H1 H 0.2666 0.7673 0.8479 0.030 Uiso 1 1 calc R
C15 C -0.0129(3) -0.0543(2) 0.8421(2) 0.0258(5) Uani 1 1 d .
H15 H 0.0433 -0.1032 0.8946 0.031 Uiso 1 1 calc R
C9 C 0.0029(3) 0.2464(3) 0.4745(2) 0.0270(5) Uani 1 1 d .
H9C H -0.0203 0.3301 0.4624 0.040 Uiso 1 1 calc R
H9B H -0.0847 0.1769 0.4859 0.040 Uiso 1 1 calc R
H9A H 0.0194 0.2153 0.4012 0.040 Uiso 1 1 calc R
C18 C -0.4124(3) 0.1616(3) 0.6583(3) 0.0316(6) Uani 1 1 d .
H18C H -0.3670 0.2020 0.7461 0.047 Uiso 1 1 calc R
H18B H -0.4828 0.0686 0.6495 0.047 Uiso 1 1 calc R
H18A H -0.4708 0.2147 0.6087 0.047 Uiso 1 1 calc R
C8 C 0.2880(3) 0.3885(2) 0.5723(2) 0.0223(4) Uani 1 1 d .
H8B H 0.3871 0.3712 0.6079 0.027 Uiso 1 1 calc R
H8A H 0.2659 0.3950 0.4827 0.027 Uiso 1 1 calc R
C2 C 0.3679(3) 0.7445(2) 0.7247(2) 0.0289(5) Uani 1 1 d .
H2 H 0.4232 0.8382 0.7308 0.035 Uiso 1 1 calc R
C20 C 0.3262(4) 0.0649(3) 0.9644(4) 0.0501(9) Uani 1 1 d .
H20B H 0.4346 0.1208 1.0125 0.075 Uiso 1 1 calc R
H20A H 0.3209 0.0174 0.8881 0.075 Uiso 1 1 calc R
H20C H 0.2868 -0.0013 1.0144 0.075 Uiso 1 1 calc R
C21 C 0.3988(3) 0.5657(3) 1.0766(3) 0.0365(6) Uani 1 1 d .
H21B H 0.4747 0.5380 1.1409 0.055 Uiso 1 1 calc R
H21C H 0.3881 0.6459 1.1117 0.055 Uiso 1 1 calc R
H21A H 0.4346 0.5871 1.0070 0.055 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'
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'
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
N2 Ni1 O1 91.22(7) . .
N2 Ni1 N1 80.75(7) . .
O1 Ni1 N1 90.58(7) . .
N2 Ni1 Cl1 171.89(6) . .
O1 Ni1 Cl1 83.74(6) . .
N1 Ni1 Cl1 92.92(5) . .
N2 Ni1 Cl2 90.77(6) . .
O1 Ni1 Cl2 173.11(5) . .
N1 Ni1 Cl2 96.25(6) . .
Cl1 Ni1 Cl2 94.97(3) . .
N2 Ni1 Cl1 93.79(6) . 2_567
O1 Ni1 Cl1 84.13(6) . 2_567
N1 Ni1 Cl1 172.34(5) . 2_567
Cl1 Ni1 Cl1 92.01(3) . 2_567
Cl2 Ni1 Cl1 89.16(4) . 2_567
N2 Ni1 Ni1 138.65(6) . 2_567
O1 Ni1 Ni1 81.26(5) . 2_567
N1 Ni1 Ni1 139.44(5) . 2_567
Cl1 Ni1 Ni1 46.86(2) . 2_567
Cl2 Ni1 Ni1 92.91(3) . 2_567
Cl1 Ni1 Ni1 45.15(2) 2_567 2_567
Ni1 Cl1 Ni1 87.99(3) . 2_567
C21 O1 Ni1 122.25(16) . .
C1 N2 C5 116.06(19) . .
C1 N2 Ni1 133.92(16) . .
C5 N2 Ni1 110.00(14) . .
C6 N1 C11 121.08(18) . .
C6 N1 Ni1 109.84(14) . .
C11 N1 Ni1 129.08(13) . .
C10 C7 C6 116.02(18) . .
C10 C7 C9 110.59(19) . .
C6 C7 C9 106.52(17) . .
C10 C7 C8 111.27(18) . .
C6 C7 C8 103.61(17) . .
C9 C7 C8 108.35(19) . .
C13 C12 C11 118.0(2) . .
C13 C12 C17 118.6(2) . .
C11 C12 C17 123.3(2) . .
C15 C16 C11 117.9(2) . .
C15 C16 C19 120.7(2) . .
C11 C16 C19 121.4(2) . .
N1 C6 C5 117.64(18) . .
N1 C6 C7 135.6(2) . .
C5 C6 C7 106.68(18) . .
N2 C5 C4 126.4(2) . .
N2 C5 C6 121.58(19) . .
C4 C5 C6 111.97(19) . .
C15 C14 C13 119.4(2) . .
C15 C14 H14 120.3 . .
C13 C14 H14 120.3 . .
C14 C13 C12 121.4(2) . .
C14 C13 H13 119.3 . .
C12 C13 H13 119.3 . .
C12 C17 C18 111.7(2) . .
C12 C17 H17A 109.3 . .
C18 C17 H17A 109.3 . .
C12 C17 H17B 109.3 . .
C18 C17 H17B 109.3 . .
H17A C17 H17B 107.9 . .
C12 C11 C16 121.5(2) . .
C12 C11 N1 119.92(19) . .
C16 C11 N1 118.59(19) . .
C5 C4 C3 117.3(2) . .
C5 C4 C8 109.97(19) . .
C3 C4 C8 132.7(2) . .
C7 C10 H10C 109.5 . .
C7 C10 H10A 109.5 . .
H10C C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10C C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C16 C19 C20 115.2(2) . .
C16 C19 H19B 108.5 . .
C20 C19 H19B 108.5 . .
C16 C19 H19A 108.5 . .
C20 C19 H19A 108.5 . .
H19B C19 H19A 107.5 . .
C2 C3 C4 117.3(2) . .
C2 C3 H3 121.3 . .
C4 C3 H3 121.3 . .
N2 C1 C2 122.3(2) . .
N2 C1 H1 118.9 . .
C2 C1 H1 118.9 . .
C14 C15 C16 121.8(2) . .
C14 C15 H15 119.1 . .
C16 C15 H15 119.1 . .
C7 C9 H9C 109.5 . .
C7 C9 H9B 109.5 . .
H9C C9 H9B 109.5 . .
C7 C9 H9A 109.5 . .
H9C C9 H9A 109.5 . .
H9B C9 H9A 109.5 . .
C17 C18 H18C 109.5 . .
C17 C18 H18B 109.5 . .
H18C C18 H18B 109.5 . .
C17 C18 H18A 109.5 . .
H18C C18 H18A 109.5 . .
H18B C18 H18A 109.5 . .
C4 C8 C7 105.21(17) . .
C4 C8 H8B 110.7 . .
C7 C8 H8B 110.7 . .
C4 C8 H8A 110.7 . .
C7 C8 H8A 110.7 . .
H8B C8 H8A 108.8 . .
C3 C2 C1 120.6(2) . .
C3 C2 H2 119.7 . .
C1 C2 H2 119.7 . .
C19 C20 H20B 109.5 . .
C19 C20 H20A 109.5 . .
H20B C20 H20A 109.5 . .
C19 C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
O1 C21 H21B 109.5 . .
O1 C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
O1 C21 H21A 109.5 . .
H21B C21 H21A 109.5 . .
H21C C21 H21A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 2.065(2) .
Ni1 O1 2.1614(18) .
Ni1 N1 2.1925(19) .
Ni1 Cl1 2.3682(9) .
Ni1 Cl2 2.3855(10) .
Ni1 Cl1 2.4372(10) 2_567
Ni1 Ni1 3.3383(8) 2_567
Cl1 Ni1 2.4372(10) 2_567
O1 C21 1.443(3) .
N2 C1 1.331(3) .
N2 C5 1.334(3) .
N1 C6 1.283(3) .
N1 C11 1.443(3) .
C7 C10 1.526(3) .
C7 C6 1.533(3) .
C7 C9 1.544(3) .
C7 C8 1.567(3) .
C12 C13 1.397(3) .
C12 C11 1.398(3) .
C12 C17 1.508(3) .
C16 C15 1.389(3) .
C16 C11 1.409(3) .
C16 C19 1.512(3) .
C6 C5 1.464(3) .
C5 C4 1.377(3) .
C14 C15 1.382(4) .
C14 C13 1.383(4) .
C14 H14 0.9500 .
C13 H13 0.9500 .
C17 C18 1.527(3) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C4 C3 1.394(3) .
C4 C8 1.498(3) .
C10 H10C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C19 C20 1.520(4) .
C19 H19B 0.9900 .
C19 H19A 0.9900 .
C3 C2 1.387(4) .
C3 H3 0.9500 .
C1 C2 1.395(3) .
C1 H1 0.9500 .
C15 H15 0.9500 .
C9 H9C 0.9800 .
C9 H9B 0.9800 .
C9 H9A 0.9800 .
C18 H18C 0.9800 .
C18 H18B 0.9800 .
C18 H18A 0.9800 .
C8 H8B 0.9900 .
C8 H8A 0.9900 .
C2 H2 0.9500 .
C20 H20B 0.9800 .
C20 H20A 0.9800 .
C20 H20C 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C21 H21A 0.9800 .
