#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/91/7019117.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_7019117
loop_
_publ_author_name
'Lin, Ya-Chi'
'Yu, Kuo-Hsuan'
'Lin, Ya-Fan'
'Lee, Gene-Hsiang'
'Wang, Yu'
'Liu, Shiuh-Tzung'
'Chen, Jwu-Ting'
_publ_section_title
;
 Synthesis, structures of (aminopyridine)nickel complexes and their use
 for catalytic ethylene polymerization.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6661
_journal_page_last               6670
_journal_paper_doi               10.1039/c2dt30151b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C18.5 H27 Br2 Cl N4 Ni'
_chemical_formula_weight         559.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.5146(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9677(2)
_cell_length_b                   16.4392(3)
_cell_length_c                   13.4252(2)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.61
_cell_volume                     2409.36(7)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39307
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.243
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.879
_refine_diff_density_min         -2.200
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0054(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0645
_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)+(0.0831P)²+9.3790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1846
_reflns_number_gt                4268
_reflns_number_total             5524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30151b.txt
_cod_data_source_block           ic8185
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C18.50 H27 Br2 Cl N4 Ni'
_cod_database_code               7019117
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.64710(8) 0.81323(6) 0.66866(7) 0.0648(3) Uani 1 1 d . . .
Br1 Br 0.75526(13) 0.71004(9) 0.77436(12) 0.0662(4) Uani 0.67 1 d P A 1
Br1' Br 0.7105(3) 0.68473(19) 0.7456(3) 0.0791(9) Uani 0.33 1 d P A 2
Br2 Br 0.67247(4) 0.98190(3) 0.37422(4) 0.0398(2) Uani 1 1 d . . .
N1 N 0.4735(6) 0.7609(3) 0.6608(4) 0.0633(16) Uani 1 1 d . A .
N2 N 0.5978(6) 0.8220(3) 0.5162(4) 0.0601(15) Uani 1 1 d . A .
N3 N 0.8102(5) 0.8778(5) 0.6636(5) 0.085(2) Uani 1 1 d . A .
N4 N 0.5919(4) 0.9273(3) 0.7109(3) 0.0439(10) Uani 1 1 d . A .
C1 C 0.4274(9) 0.7093(4) 0.7265(6) 0.077(2) Uani 1 1 d . . .
H1A H 0.4773 0.6946 0.7855 0.093 Uiso 1 1 calc R A .
C2 C 0.3131(10) 0.6780(5) 0.7113(7) 0.088(3) Uani 1 1 d . A .
H2A H 0.2829 0.6425 0.7590 0.106 Uiso 1 1 calc R . .
C3 C 0.2415(11) 0.6986(6) 0.6252(7) 0.104(4) Uani 1 1 d . . .
H3A H 0.1614 0.6765 0.6127 0.125 Uiso 1 1 calc R A .
C4 C 0.2859(9) 0.7517(6) 0.5563(6) 0.087(3) Uani 1 1 d . A .
H4A H 0.2369 0.7676 0.4973 0.105 Uiso 1 1 calc R . .
C5 C 0.4035(7) 0.7803(4) 0.5770(5) 0.0597(18) Uani 1 1 d . . .
C6 C 0.4629(7) 0.8357(3) 0.5059(5) 0.0532(15) Uani 1 1 d . A .
H6A H 0.4290 0.8245 0.4363 0.064 Uiso 1 1 calc R . .
H6B H 0.4451 0.8932 0.5214 0.064 Uiso 1 1 calc R . .
C7 C 0.6339(13) 0.7504(6) 0.4574(10) 0.115(4) Uani 1 1 d . . .
H7A H 0.6069 0.7018 0.4943 0.138 Uiso 0.67 1 calc PR A 1
H7'A H 0.6162 0.7698 0.3869 0.138 Uiso 0.33 1 d PR A 2
C8 C 0.7794(12) 0.7470(9) 0.4699(10) 0.145(6) Uani 1 1 d . A .
H8A H 0.8074 0.7009 0.4318 0.218 Uiso 0.67 1 calc PR B 1
H8B H 0.8082 0.7404 0.5408 0.218 Uiso 0.67 1 calc PR B 1
H8C H 0.8124 0.7976 0.4448 0.218 Uiso 0.67 1 calc PR B 1
H8'A H 0.8077 0.7009 0.4319 0.218 Uiso 0.33 1 d PR B 2
H8'B H 0.8125 0.7977 0.4451 0.218 Uiso 0.33 1 d PR B 2
H8'C H 0.8077 0.7403 0.5409 0.218 Uiso 0.33 1 d PR B 2
C9 C 0.5877(16) 0.7399(10) 0.3639(15) 0.116(6) Uani 0.67 1 d P A 1
H9A H 0.4980 0.7418 0.3604 0.175 Uiso 0.67 1 calc PR A 1
H9B H 0.6134 0.6869 0.3399 0.175 Uiso 0.67 1 calc PR A 1
H9C H 0.6172 0.7831 0.3220 0.175 Uiso 0.67 1 calc PR A 1
C9' C 0.560(4) 0.6763(10) 0.457(2) 0.122(15) Uani 0.33 1 d P A 2
H9'A H 0.4734 0.6904 0.4458 0.182 Uiso 0.33 1 calc PR A 2
H9'B H 0.5764 0.6486 0.5215 0.182 Uiso 0.33 1 calc PR A 2
H9'C H 0.5823 0.6403 0.4033 0.182 Uiso 0.33 1 calc PR A 2
C10 C 0.9252(7) 0.8503(8) 0.6628(9) 0.125(5) Uani 1 1 d . . .
H10A H 0.9409 0.7939 0.6724 0.150 Uiso 1 1 calc R A .
C11 C 1.0231(7) 0.9027(9) 0.6484(9) 0.121(5) Uani 1 1 d . A .
H11A H 1.1040 0.8818 0.6496 0.145 Uiso 1 1 calc R . .
C12 C 1.0020(7) 0.9837(8) 0.6326(7) 0.098(3) Uani 1 1 d . . .
H12A H 1.0667 1.0197 0.6204 0.117 Uiso 1 1 calc R A .
C13 C 0.8859(6) 1.0110(7) 0.6349(6) 0.077(2) Uani 1 1 d . A .
H13A H 0.8686 1.0672 0.6253 0.092 Uiso 1 1 calc R . .
C14 C 0.7914(5) 0.9573(5) 0.6513(5) 0.0610(18) Uani 1 1 d . . .
C15 C 0.6626(5) 0.9853(4) 0.6545(4) 0.0440(12) Uani 1 1 d . A .
H15A H 0.6624 1.0395 0.6867 0.053 Uiso 1 1 calc R . .
H15B H 0.6230 0.9908 0.5854 0.053 Uiso 1 1 calc R . .
C16 C 0.6072(6) 0.9435(6) 0.8212(5) 0.071(2) Uani 1 1 d . . .
H16A H 0.6953 0.9338 0.8447 0.085 Uiso 0.67 1 calc PR A 1
H16B H 0.5731 0.9986 0.8339 0.085 Uiso 0.33 1 d PR A 2
C17 C 0.5314(9) 0.8793(7) 0.8719(6) 0.090(3) Uani 1 1 d . A .
H17A H 0.5393 0.8884 0.9443 0.135 Uiso 0.67 1 calc PR C 1
H17B H 0.5617 0.8248 0.8577 0.135 Uiso 0.67 1 calc PR C 1
H17C H 0.4451 0.8838 0.8458 0.135 Uiso 0.67 1 calc PR C 1
H17D H 0.5392 0.8883 0.9444 0.135 Uiso 0.33 1 d PR C 2
H17E H 0.4451 0.8836 0.8457 0.135 Uiso 0.33 1 d PR C 2
H17F H 0.5620 0.8249 0.8576 0.135 Uiso 0.33 1 d PR C 2
C18 C 0.5757(16) 1.0278(9) 0.8542(8) 0.094(5) Uani 0.67 1 d P A 1
H18A H 0.6248 1.0677 0.8216 0.142 Uiso 0.67 1 calc PR A 1
H18B H 0.5931 1.0322 0.9270 0.142 Uiso 0.67 1 calc PR A 1
H18C H 0.4885 1.0383 0.8356 0.142 Uiso 0.67 1 calc PR A 1
C18' C 0.725(2) 0.941(3) 0.8662(17) 0.115(14) Uani 0.33 1 d P A 2
H18D H 0.7748 0.9816 0.8360 0.173 Uiso 0.33 1 calc PR A 2
H18E H 0.7593 0.8864 0.8568 0.173 Uiso 0.33 1 calc PR A 2
H18F H 0.7245 0.9517 0.9379 0.173 Uiso 0.33 1 calc PR A 2
C19 C 0.584(3) 1.5073(14) 0.401(3) 0.19(2) Uani 0.50 1 d P . .
H19A H 0.5195 1.5014 0.3474 0.230 Uiso 0.50 1 d PR . .
H19B H 0.6034 1.4536 0.4254 0.230 Uiso 0.50 1 d PR . .
Cl1 Cl 0.5135(19) 1.5335(6) 0.5468(11) 0.299(11) Uani 0.50 1 d P . .
Cl2 Cl 0.6991(9) 1.5116(5) 0.4144(9) 0.168(4) Uani 0.50 1 d P . .
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'
Cl Cl 0.1484 0.1585 '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
N4 Ni N2 98.75(18) . .
N4 Ni N1 95.62(19) . .
N2 Ni N1 80.1(2) . .
N4 Ni N3 79.7(2) . .
N2 Ni N3 94.3(3) . .
N1 Ni N3 172.2(2) . .
N4 Ni Br1' 138.90(16) . .
N2 Ni Br1' 121.26(17) . .
N1 Ni Br1' 83.40(18) . .
N3 Ni Br1' 104.23(18) . .
N4 Ni Br1 127.53(14) . .
N2 Ni Br1 133.49(14) . .
N1 Ni Br1 97.65(16) . .
N3 Ni Br1 90.13(16) . .
Br1' Ni Br1 17.14(7) . .
C5 N1 C1 118.4(7) . .
C5 N1 Ni 113.1(4) . .
C1 N1 Ni 128.4(6) . .
C6 N2 C7 112.5(8) . .
C6 N2 Ni 105.4(3) . .
C7 N2 Ni 114.3(6) . .
C14 N3 C10 117.7(8) . .
C14 N3 Ni 112.4(4) . .
C10 N3 Ni 129.7(8) . .
C15 N4 C16 112.1(5) . .
C15 N4 Ni 105.2(3) . .
C16 N4 Ni 115.1(5) . .
C2 C1 N1 122.5(9) . .
C1 C2 C3 118.7(7) . .
C2 C3 C4 120.2(9) . .
C5 C4 C3 117.5(9) . .
N1 C5 C4 122.6(6) . .
N1 C5 C6 115.3(6) . .
C4 C5 C6 122.1(7) . .
N2 C6 C5 109.5(6) . .
C9 C7 C9' 74.0(16) . .
C9 C7 N2 120.7(12) . .
C9' C7 N2 119.0(11) . .
C9 C7 C8 112.7(10) . .
C9' C7 C8 121.3(17) . .
N2 C7 C8 106.7(10) . .
N3 C10 C11 121.8(10) . .
C12 C11 C10 120.0(8) . .
C13 C12 C11 117.8(9) . .
C12 C13 C14 120.6(10) . .
N3 C14 C13 122.1(7) . .
N3 C14 C15 115.8(6) . .
C13 C14 C15 122.0(7) . .
N4 C15 C14 111.1(5) . .
C18' C16 N4 116.1(13) . .
C18' C16 C18 98(2) . .
N4 C16 C18 116.6(7) . .
C18' C16 C17 107.8(15) . .
N4 C16 C17 107.4(7) . .
C18 C16 C17 110.6(8) . .
Cl2 C19 Cl1 135(3) . 3_686
Cl2 C19 Cl1 107(2) . .
Cl1 C19 Cl1 49.1(17) 3_686 .
C19 Cl1 Cl1 88.6(18) 3_686 3_686
C19 Cl1 C19 130.9(17) 3_686 .
Cl1 Cl1 C19 42.3(8) 3_686 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni N4 2.067(5) .
Ni N2 2.071(6) .
Ni N1 2.082(7) .
Ni N3 2.087(7) .
Ni Br1' 2.424(3) .
Ni Br1 2.4444(14) .
N1 C5 1.339(10) .
N1 C1 1.356(8) .
N2 C6 1.490(9) .
N2 C7 1.492(9) .
N3 C14 1.331(11) .
N3 C10 1.341(9) .
N4 C15 1.483(7) .
N4 C16 1.499(8) .
C1 C2 1.352(13) .
C2 C3 1.376(15) .
C3 C4 1.393(11) .
C4 C5 1.375(11) .
C5 C6 1.511(8) .
C7 C9 1.32(2) .
C7 C9' 1.46(3) .
C7 C8 1.590(18) .
C10 C11 1.404(15) .
C11 C12 1.364(16) .
C12 C13 1.354(12) .
C13 C14 1.395(11) .
C14 C15 1.490(8) .
C16 C18' 1.37(2) .
C16 C18 1.504(17) .
C16 C17 1.542(11) .
C19 Cl2 1.26(3) .
C19 Cl1 1.49(4) 3_686
C19 Cl1 2.22(5) .
Cl1 C19 1.49(4) 3_686
Cl1 Cl1 1.68(3) 3_686
