#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:12:25 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243925 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/26/7702620.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_7702620
loop_
_publ_author_name
'Yamamoto, Youhei'
'Suzuki, Takayoshi'
'Kaizaki, Sumio'
_publ_section_title
;
 Syntheses, structures, magnetic, and spectroscopic properties of
 cobalt(ii), nickel(ii) and zinc(ii) complexes containing
 2-(6-methyl)pyridyl-substituted nitronyl and imino nitroxide†
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2943
_journal_paper_doi               10.1039/b103647p
_journal_year                    2001
_chemical_formula_moiety         '(Ni Cl2 (C13 H18 N3 O))'
_chemical_formula_sum            'C13 H18 Cl2 N3 Ni O'
_chemical_formula_weight         361.91
_chemical_name_common            '[{NiCl(IMmepy)}₂(μ-Cl)₂]'
_chemical_name_systematic
;
Bis(μ-chloro)bis(chloro(2-(6'-methyl-2'-pyridyl)-4,4,5,5-
tetramethylimidazoline-1-oxy)nickel(II))
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.292(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2119(19)
_cell_length_b                   10.892(3)
_cell_length_c                   14.5148(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     1593.3(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotatiing anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0127
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4821
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0.51
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0399P)²+0.3576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                3429
_reflns_number_total             4651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            b103647p.txt
_cod_data_source_block           NiIMmepy
_cod_original_cell_volume        1593.3(5)
_cod_database_code               7702620
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ni Ni 0.60593(2) 0.11072(2) 0.458157(17) 0.02992(7) Uani 1 1 d .
Cl1 Cl 0.72063(6) 0.09427(5) 0.33619(4) 0.04597(13) Uani 1 1 d .
Cl2 Cl 0.41531(5) 0.10980(4) 0.53040(4) 0.04392(13) Uani 1 1 d .
O O 0.91694(18) 0.42756(14) 0.64487(14) 0.0605(5) Uani 1 1 d .
N1 N 0.74847(15) 0.16713(13) 0.56055(11) 0.0296(3) Uani 1 1 d .
N2 N 0.87549(17) 0.31953(15) 0.62770(13) 0.0388(4) Uani 1 1 d .
N3 N 0.59300(15) 0.30179(14) 0.43772(11) 0.0326(3) Uani 1 1 d .
C1 C 0.76823(18) 0.28448(16) 0.56222(13) 0.0317(4) Uani 1 1 d .
C2 C 0.84273(19) 0.10802(16) 0.63702(13) 0.0337(4) Uani 1 1 d .
C3 C 0.9536(2) 0.20720(18) 0.66147(16) 0.0412(4) Uani 1 1 d .
C4 C 0.8941(2) -0.01089(18) 0.60198(18) 0.0453(5) Uani 1 1 d .
H4A H 0.8258 -0.0723 0.5972 0.055 Uiso 1 1 calc R
H4B H 0.9701 -0.0381 0.6449 0.055 Uiso 1 1 calc R
H4C H 0.9188 0.0024 0.5417 0.055 Uiso 1 1 calc R
C5 C 0.7645(3) 0.0837(2) 0.71612(16) 0.0530(6) Uani 1 1 d .
H5A H 0.7385 0.1604 0.7403 0.064 Uiso 1 1 calc R
H5B H 0.8189 0.0389 0.7650 0.064 Uiso 1 1 calc R
H5C H 0.6868 0.0364 0.6929 0.064 Uiso 1 1 calc R
C6 C 1.0634(2) 0.2002(2) 0.6015(2) 0.0619(7) Uani 1 1 d .
H6A H 1.1182 0.1298 0.6195 0.075 Uiso 1 1 calc R
H6B H 1.1165 0.2733 0.6103 0.075 Uiso 1 1 calc R
H6C H 1.0244 0.1931 0.5369 0.075 Uiso 1 1 calc R
C7 C 1.0109(3) 0.2176(3) 0.76418(19) 0.0643(7) Uani 1 1 d .
H7A H 1.0503 0.1407 0.7859 0.077 Uiso 1 1 calc R
H7B H 0.9415 0.2379 0.7989 0.077 Uiso 1 1 calc R
H7C H 1.0774 0.2807 0.7727 0.077 Uiso 1 1 calc R
C8 C 0.68686(19) 0.36530(16) 0.49546(14) 0.0335(4) Uani 1 1 d .
C9 C 0.7035(2) 0.49101(17) 0.48857(17) 0.0432(5) Uani 1 1 d .
H9 H 0.7694 0.5322 0.5286 0.052 Uiso 1 1 calc R
C10 C 0.6189(3) 0.55320(19) 0.42003(18) 0.0502(6) Uani 1 1 d .
H10 H 0.6266 0.6377 0.4137 0.060 Uiso 1 1 calc R
C11 C 0.5238(2) 0.48981(19) 0.36169(17) 0.0461(5) Uani 1 1 d .
H11 H 0.4664 0.5315 0.3159 0.055 Uiso 1 1 calc R
C12 C 0.5125(2) 0.36226(19) 0.37074(15) 0.0394(4) Uani 1 1 d .
C13 C 0.4116(3) 0.2901(2) 0.30743(19) 0.0602(7) Uani 1 1 d .
H13A H 0.3552 0.2476 0.3437 0.073 Uiso 1 1 calc R
H13B H 0.4555 0.2317 0.2734 0.073 Uiso 1 1 calc R
H13C H 0.3591 0.3446 0.2644 0.073 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
Ni Ni 0.3393 1.1124 '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'
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'
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_3
N1 Ni N3 79.78(6) .
N1 Ni Cl1 101.38(5) .
N3 Ni Cl1 89.81(5) .
N1 Ni Cl2 103.00(5) .
N3 Ni Cl2 91.69(4) .
Cl1 Ni Cl2 155.45(3) .
N1 Ni Cl2 108.44(4) 3_656
N3 Ni Cl2 170.94(5) 3_656
Cl1 Ni Cl2 92.19(2) 3_656
Cl2 Ni Cl2 82.849(18) 3_656
Ni Cl2 Ni 97.150(18) 3_656
C1 N1 C2 109.41(15) .
C1 N1 Ni 114.19(13) .
C2 N1 Ni 136.39(11) .
O N2 C1 126.62(18) .
O N2 C3 123.56(17) .
C1 N2 C3 108.66(15) .
C12 N3 C8 119.14(17) .
C12 N3 Ni 127.27(14) .
C8 N3 Ni 113.29(12) .
N1 C1 N2 112.93(17) .
N1 C1 C8 120.76(17) .
N2 C1 C8 126.20(16) .
N1 C2 C4 109.60(16) .
N1 C2 C5 106.35(17) .
C4 C2 C5 110.84(18) .
N1 C2 C3 103.13(15) .
C4 C2 C3 112.93(17) .
C5 C2 C3 113.44(17) .
N2 C3 C7 111.19(18) .
N2 C3 C6 104.78(19) .
C7 C3 C6 111.2(2) .
N2 C3 C2 99.33(15) .
C7 C3 C2 115.2(2) .
C6 C3 C2 114.02(17) .
C2 C4 H4A 109.5 .
C2 C4 H4B 109.5 .
H4A C4 H4B 109.5 .
C2 C4 H4C 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
C2 C5 H5A 109.5 .
C2 C5 H5B 109.5 .
H5A C5 H5B 109.5 .
C2 C5 H5C 109.5 .
H5A C5 H5C 109.5 .
H5B C5 H5C 109.5 .
C3 C6 H6A 109.5 .
C3 C6 H6B 109.5 .
H6A C6 H6B 109.5 .
C3 C6 H6C 109.5 .
H6A C6 H6C 109.5 .
H6B C6 H6C 109.5 .
C3 C7 H7A 109.5 .
C3 C7 H7B 109.5 .
H7A C7 H7B 109.5 .
C3 C7 H7C 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
N3 C8 C9 122.84(19) .
N3 C8 C1 111.78(15) .
C9 C8 C1 125.35(19) .
C10 C9 C8 117.7(2) .
C10 C9 H9 121.1 .
C8 C9 H9 121.1 .
C11 C10 C9 119.76(19) .
C11 C10 H10 120.1 .
C9 C10 H10 120.1 .
C10 C11 C12 120.2(2) .
C10 C11 H11 119.9 .
C12 C11 H11 119.9 .
N3 C12 C11 120.3(2) .
N3 C12 C13 118.07(19) .
C11 C12 C13 121.6(2) .
C12 C13 H13A 109.5 .
C12 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
C12 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni N1 2.0016(15) .
Ni N3 2.1033(16) .
Ni Cl1 2.2820(6) .
Ni Cl2 2.3554(7) .
Ni Cl2 2.4197(8) 3_656
Cl2 Ni 2.4197(8) 3_656
O N2 1.262(2) .
N1 C1 1.294(2) .
N1 C2 1.493(2) .
N2 C1 1.383(2) .
N2 C3 1.499(3) .
N3 C12 1.341(3) .
N3 C8 1.356(2) .
C1 C8 1.464(3) .
C2 C4 1.516(3) .
C2 C5 1.524(3) .
C2 C3 1.564(3) .
C3 C7 1.515(3) .
C3 C6 1.528(3) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.385(2) .
C9 C10 1.385(3) .
C9 H9 0.9300 .
C10 C11 1.368(4) .
C10 H10 0.9300 .
C11 C12 1.402(3) .
C11 H11 0.9300 .
C12 C13 1.489(3) .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Ni Cl2 Ni -107.35(5) . 3_656
N3 Ni Cl2 Ni 172.75(5) . 3_656
Cl1 Ni Cl2 Ni 79.52(5) . 3_656
Cl2 Ni Cl2 Ni 0.0 3_656 3_656
N3 Ni N1 C1 -3.29(13) . .
Cl1 Ni N1 C1 84.43(13) . .
Cl2 Ni N1 C1 -92.66(13) . .
Cl2 Ni N1 C1 -179.35(12) 3_656 .
N3 Ni N1 C2 178.04(18) . .
Cl1 Ni N1 C2 -94.24(17) . .
Cl2 Ni N1 C2 88.66(17) . .
Cl2 Ni N1 C2 1.97(18) 3_656 .
N1 Ni N3 C12 177.77(17) . .
Cl1 Ni N3 C12 76.16(16) . .
Cl2 Ni N3 C12 -79.33(16) . .
Cl2 Ni N3 C12 -26.7(4) 3_656 .
N1 Ni N3 C8 4.05(13) . .
Cl1 Ni N3 C8 -97.55(13) . .
Cl2 Ni N3 C8 106.96(13) . .
Cl2 Ni N3 C8 159.6(2) 3_656 .
C2 N1 C1 N2 4.9(2) . .
Ni N1 C1 N2 -174.11(12) . .
C2 N1 C1 C8 -178.76(16) . .
Ni N1 C1 C8 2.2(2) . .
O N2 C1 N1 -179.5(2) . .
C3 N2 C1 N1 12.6(2) . .
O N2 C1 C8 4.4(3) . .
C3 N2 C1 C8 -163.53(18) . .
C1 N1 C2 C4 -139.72(17) . .
Ni N1 C2 C4 39.0(2) . .
C1 N1 C2 C5 100.40(19) . .
Ni N1 C2 C5 -80.9(2) . .
C1 N1 C2 C3 -19.2(2) . .
Ni N1 C2 C3 159.50(14) . .
O N2 C3 C7 47.2(3) . .
C1 N2 C3 C7 -144.4(2) . .
O N2 C3 C6 -73.0(3) . .
C1 N2 C3 C6 95.36(19) . .
O N2 C3 C2 168.95(19) . .
C1 N2 C3 C2 -22.7(2) . .
N1 C2 C3 N2 24.11(19) . .
C4 C2 C3 N2 142.31(18) . .
C5 C2 C3 N2 -90.5(2) . .
N1 C2 C3 C7 142.92(18) . .
C4 C2 C3 C7 -98.9(2) . .
C5 C2 C3 C7 28.3(3) . .
N1 C2 C3 C6 -86.8(2) . .
C4 C2 C3 C6 31.4(3) . .
C5 C2 C3 C6 158.6(2) . .
C12 N3 C8 C9 0.1(3) . .
Ni N3 C8 C9 174.38(16) . .
C12 N3 C8 C1 -178.23(17) . .
Ni N3 C8 C1 -3.95(19) . .
N1 C1 C8 N3 1.3(3) . .
N2 C1 C8 N3 177.10(18) . .
N1 C1 C8 C9 -177.0(2) . .
N2 C1 C8 C9 -1.2(3) . .
N3 C8 C9 C10 0.7(3) . .
C1 C8 C9 C10 178.8(2) . .
C8 C9 C10 C11 -0.6(3) . .
C9 C10 C11 C12 -0.4(4) . .
C8 N3 C12 C11 -1.1(3) . .
Ni N3 C12 C11 -174.50(15) . .
C8 N3 C12 C13 179.1(2) . .
Ni N3 C12 C13 5.7(3) . .
C10 C11 C12 N3 1.3(3) . .
C10 C11 C12 C13 -179.0(2) . .
