#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:09:13 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234784 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/34/1553408.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_1553408
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_moiety         'C36 H40 Cl2 N4 Ni'
_chemical_formula_sum            'C36 H40 Cl2 N4 Ni'
_chemical_formula_weight         658.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-27 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.03(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0742(18)
_cell_length_b                   14.496(3)
_cell_length_c                   12.391(3)
_cell_measurement_reflns_used    4715
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4781
_cell_measurement_theta_min      1.4048
_cell_volume                     1613.9(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.9906
_diffrn_measured_fraction_theta_max 0.9906
_diffrn_measurement_details
;
scan:
	Number of images: 300
	           Slice: -110.0000 - 40.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.0140
	          2theta: -19.9120
scan:
	Number of images: 300
	           Slice: -110.0000 - 40.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0140
	          2theta: -19.9120
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0810
_diffrn_orient_matrix_UB_12      0.0228
_diffrn_orient_matrix_UB_13      -0.0729
_diffrn_orient_matrix_UB_21      0.0307
_diffrn_orient_matrix_UB_22      0.0403
_diffrn_orient_matrix_UB_23      0.0468
_diffrn_orient_matrix_UB_31      0.0504
_diffrn_orient_matrix_UB_32      -0.0610
_diffrn_orient_matrix_UB_33      0.0195
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10742
_diffrn_reflns_theta_full        27.4974
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8138
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             693.4891
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.4292
_refine_diff_density_min         -0.2673
_refine_diff_density_rms         0.0666
_refine_ls_d_res_high            0.7697
_refine_ls_d_res_low             6.8592
_refine_ls_goodness_of_fit_ref   1.0388
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    31
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0388
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0400P)²+0.9852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -11
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -8
_reflns_number_gt                3542
_reflns_number_total             3674
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6py02089e2.cif
_cod_data_source_block           Ni1
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1553408
_diffrn_number_total             3844
_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.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C1(H1), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C17(H17a,H17b,H17c)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.0 1.0 1.0 0.01774(9) Uani 1.000000 2 S T P
Cl1 Cl 0.08837(4) 0.86821(3) 0.91717(3) 0.02666(11) Uani 1.000000 1 . . .
N2 N 0.21708(14) 1.04544(9) 1.03768(11) 0.0199(3) Uani 1.000000 1 . . .
N1 N 0.02384(14) 1.08559(9) 0.84757(11) 0.0214(3) Uani 1.000000 1 . . .
C11 C -0.08644(19) 1.10605(13) 0.75510(14) 0.0281(4) Uani 1.000000 1 . . .
C5 C 0.25945(17) 1.09425(11) 0.95526(13) 0.0217(3) Uani 1.000000 1 . . .
C3 C 0.50740(19) 1.11702(13) 1.04236(16) 0.0302(4) Uani 1.000000 1 . . .
C7 C 0.24359(19) 1.17678(12) 0.78437(14) 0.0277(4) Uani 1.000000 1 . . .
C4 C 0.39980(18) 1.13049(12) 0.95247(15) 0.0270(4) Uani 1.000000 1 . . .
C6 C 0.15771(18) 1.11573(11) 0.85619(13) 0.0229(3) Uani 1.000000 1 . . .
C1 C 0.32111(18) 1.03288(12) 1.12373(14) 0.0247(3) Uani 1.000000 1 . . .
C16 C -0.1784(2) 1.18414(15) 0.75841(16) 0.0370(5) Uani 1.000000 1 . . .
C2 C 0.46546(19) 1.06761(12) 1.12825(15) 0.0287(4) Uani 1.000000 1 . . .
C12 C -0.1103(2) 1.04285(15) 0.66858(15) 0.0357(4) Uani 1.000000 1 . . .
C18 C -0.1624(2) 1.25240(15) 0.84994(19) 0.0447(5) Uani 1.000000 1 . . .
C9 C 0.1833(2) 1.27508(13) 0.78313(18) 0.0374(4) Uani 1.000000 1 . . .
C8 C 0.4062(2) 1.17606(15) 0.84508(17) 0.0370(4) Uani 1.000000 1 . . .
C10 C 0.2396(3) 1.14111(16) 0.66839(17) 0.0441(5) Uani 1.000000 1 . . .
C13 C -0.2289(3) 1.0595(2) 0.58571(17) 0.0542(7) Uani 1.000000 1 . . .
C15 C -0.2936(2) 1.1973(2) 0.6721(2) 0.0549(7) Uani 1.000000 1 . . .
C17 C -0.0165(3) 0.95845(16) 0.66286(17) 0.0427(5) Uani 1.000000 1 . . .
C14 C -0.3194(3) 1.1354(2) 0.5878(2) 0.0644(8) Uani 1.000000 1 . . .
H8a H 0.4710(2) 1.14193(15) 0.80347(17) 0.0444(5) Uiso 1.000000 1 R . .
H8b H 0.4438(2) 1.23853(15) 0.85561(17) 0.0444(5) Uiso 1.000000 1 R . .
H13 H -0.2469(3) 1.0182(2) 0.52793(17) 0.0650(8) Uiso 1.000000 1 R . .
H14 H -0.3979(3) 1.1448(2) 0.5321(2) 0.0772(10) Uiso 1.000000 1 R . .
H15 H -0.3539(2) 1.2491(2) 0.6719(2) 0.0658(8) Uiso 1.000000 1 R . .
H1 H 0.29660(18) 0.99973(12) 1.18297(14) 0.0296(4) Uiso 1.000000 1 R . .
H2 H 0.53427(19) 1.05728(12) 1.19003(15) 0.0345(4) Uiso 1.000000 1 R . .
H3 H 0.60331(19) 1.14024(13) 1.04456(16) 0.0362(4) Uiso 1.000000 1 R . .
H18a H -0.2470(10) 1.2481(8) 0.8884(9) 0.0671(8) Uiso 1.000000 1 GR . .
H18b H -0.0733(10) 1.2394(7) 0.8990(8) 0.0671(8) Uiso 1.000000 1 GR . .
H18c H -0.157(2) 1.31358(18) 0.8211(2) 0.0671(8) Uiso 1.000000 1 GR . .
H9a H 0.0821(6) 1.2758(2) 0.7479(12) 0.0561(7) Uiso 1.000000 1 GR . .
H9b H 0.1872(17) 1.2970(4) 0.85660(19) 0.0561(7) Uiso 1.000000 1 GR . .
H9c H 0.2427(11) 1.3144(3) 0.7441(11) 0.0561(7) Uiso 1.000000 1 GR . .
H10a H 0.2784(18) 1.0794(5) 0.67025(17) 0.0661(8) Uiso 1.000000 1 GR . .
H10b H 0.1388(4) 1.1411(11) 0.6324(5) 0.0661(8) Uiso 1.000000 1 GR . .
H10c H 0.2992(16) 1.1803(7) 0.6294(4) 0.0661(8) Uiso 1.000000 1 GR . .
H17a H 0.0858(4) 0.9733(3) 0.6873(13) 0.0641(7) Uiso 1.000000 1 GR . .
H17b H -0.0486(13) 0.9112(4) 0.7086(11) 0.0641(7) Uiso 1.000000 1 GR . .
H17c H -0.0266(15) 0.9368(7) 0.5890(3) 0.0641(7) Uiso 1.000000 1 GR . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Ni 0.35663 1.12491 12.83760 7.29200 4.44380 2.38000 3.87850 0.25650 12.17630
66.34210 1.03410005569
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
Cl1 Ni1 Cl1 180.0 3_577 .
N2 Ni1 Cl1 90.85(4) 3_577 .
N2 Ni1 Cl1 89.15(4) . .
N2 Ni1 Cl1 90.85(4) . 3_577
N2 Ni1 Cl1 89.15(4) 3_577 3_577
N2 Ni1 N2 180.0 3_577 .
N1 Ni1 Cl1 89.84(3) . 3_577
N1 Ni1 Cl1 90.16(3) . .
N1 Ni1 Cl1 90.16(3) 3_577 3_577
N1 Ni1 Cl1 89.84(3) 3_577 .
N1 Ni1 N2 79.47(5) 3_577 3_577
N1 Ni1 N2 100.53(5) 3_577 .
N1 Ni1 N2 100.53(5) . 3_577
N1 Ni1 N2 79.47(5) . .
N1 Ni1 N1 180.0 3_577 .
C5 N2 Ni1 111.18(10) . .
C1 N2 Ni1 133.03(11) . .
C1 N2 C5 115.73(13) . .
C11 N1 Ni1 129.05(10) . .
C6 N1 Ni1 108.24(11) . .
C6 N1 C11 122.72(14) . .
C16 C11 N1 119.31(17) . .
C12 C11 N1 119.23(16) . .
C12 C11 C16 121.14(17) . .
C4 C5 N2 125.60(16) . .
C6 C5 N2 122.45(14) . .
C6 C5 C4 111.95(15) . .
C2 C3 C4 116.93(16) . .
C9 C7 C6 109.43(14) . .
C8 C7 C6 103.78(14) . .
C8 C7 C9 108.95(16) . .
C10 C7 C6 113.75(15) . .
C10 C7 C9 110.27(17) . .
C10 C7 C8 110.41(16) . .
C3 C4 C5 118.26(16) . .
C8 C4 C5 109.92(16) . .
C8 C4 C3 131.78(16) . .
C5 C6 N1 118.51(14) . .
C7 C6 N1 134.22(15) . .
C7 C6 C5 107.22(13) . .
C2 C1 N2 122.52(16) . .
C18 C16 C11 123.89(18) . .
C15 C16 C11 117.9(2) . .
C15 C16 C18 118.2(2) . .
C1 C2 C3 120.94(16) . .
C13 C12 C11 117.9(2) . .
C17 C12 C11 122.76(17) . .
C17 C12 C13 119.3(2) . .
C4 C8 C7 106.31(14) . .
C14 C13 C12 121.6(2) . .
C14 C15 C16 121.5(2) . .
C15 C14 C13 119.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 Cl1 2.3613(5) 3_577
Ni1 Cl1 2.3613(5) .
Ni1 N2 2.0676(13) 3_577
Ni1 N2 2.0676(13) .
Ni1 N1 2.2952(14) .
Ni1 N1 2.2952(14) 3_577
N2 C5 1.342(2) .
N2 C1 1.334(2) .
N1 C11 1.443(2) .
N1 C6 1.281(2) .
C11 C16 1.410(3) .
C11 C12 1.404(3) .
C5 C4 1.383(2) .
C5 C6 1.463(2) .
C3 C4 1.388(3) .
C3 C2 1.380(3) .
C7 C6 1.541(2) .
C7 C9 1.526(3) .
C7 C8 1.560(3) .
C7 C10 1.523(3) .
C4 C8 1.494(3) .
C1 C2 1.397(2) .
C16 C18 1.497(3) .
C16 C15 1.400(3) .
C12 C13 1.401(3) .
C12 C17 1.498(3) .
C13 C14 1.376(4) .
C15 C14 1.372(4) .
