#------------------------------------------------------------------------------
#$Date: 2018-09-01 18:27:48 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210310 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/03/4320377.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_4320377
loop_
_publ_author_name
'Oshio, Hiroki'
'Yamamoto, Masashi'
'Ito, Tasuku'
'Kawauchi, Hidekazu'
'Koga, Nobuaki'
'Ikoma, Tadaaki'
'Tero-Kubota, Shozo'
_publ_section_title
;
 Experimental and Theoretical Studies on Ferromagnetically Coupled Metal
 Complexes with Imino Nitroxides
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   22
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5518
_journal_page_last               5525
_journal_paper_doi               10.1021/ic0102384
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C19 H35 Cl2 N5 Ni O6'
_chemical_formula_weight         559.13
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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
_cell_angle_alpha                108.1630(10)
_cell_angle_beta                 100.6760(10)
_cell_angle_gamma                92.6140(10)
_cell_formula_units_Z            2
_cell_length_a                   6.5936(2)
_cell_length_b                   13.2244(4)
_cell_length_c                   16.2682(5)
_cell_measurement_temperature    203
_cell_volume                     1316.38(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9944
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.327
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0569P)²+1.3938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                4288
_reflns_number_total             5152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0102384_3.cif
_cod_data_source_block           '[NiCl(bisimpy)(H2O)2]Cl.2H2O'
_cod_database_code               4320377
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.56416(5) 0.11209(3) 0.76962(2) 0.01904(12) Uani 1 1 d . . .
Cl1 Cl 0.20624(10) 0.11847(6) 0.71229(5) 0.02962(18) Uani 1 1 d . . .
Cl2 Cl 0.95309(12) 0.25339(7) 0.03095(5) 0.0353(2) Uani 1 1 d . . .
O1 O 0.8291(5) 0.2452(2) 0.53151(18) 0.0526(7) Uani 1 1 d . . .
O2 O 0.5484(4) -0.30453(18) 0.63867(17) 0.0478(7) Uani 1 1 d . . .
O3 O 0.5290(3) 0.19204(17) 0.89410(13) 0.0285(5) Uani 1 1 d . . .
H3SA H 0.6436 0.2118 0.9272 0.043 Uiso 1 1 calc R . .
H3SB H 0.4414 0.2425 0.9101 0.043 Uiso 1 1 d R . .
O4 O 0.8753(3) 0.11094(17) 0.82969(14) 0.0292(5) Uani 1 1 d . . .
H4SA H 0.8991 0.1513 0.8810 0.044 Uiso 1 1 calc R . .
H4SB H 0.9518 0.1202 0.7976 0.044 Uiso 1 1 d R . .
O5S O 0.3137(4) 0.3523(2) 0.9696(2) 0.0420(6) Uani 1 1 d . . .
O6S O 0.2920(7) 0.5405(3) 0.9348(3) 0.0605(9) Uani 1 1 d . . .
N1 N 0.6402(3) 0.02429(18) 0.65435(15) 0.0203(5) Uani 1 1 d . . .
N2 N 0.6582(4) 0.23152(18) 0.71594(16) 0.0232(5) Uani 1 1 d . . .
N3 N 0.7693(4) 0.2649(2) 0.60415(18) 0.0329(6) Uani 1 1 d . . .
N4 N 0.5004(4) -0.04811(18) 0.76695(15) 0.0224(5) Uani 1 1 d . . .
N5 N 0.5059(4) -0.2218(2) 0.69514(17) 0.0306(6) Uani 1 1 d . . .
C1 C 0.7079(4) 0.0730(2) 0.60218(18) 0.0210(6) Uani 1 1 d . . .
C2 C 0.7653(4) 0.0158(2) 0.52438(19) 0.0249(6) Uani 1 1 d . . .
H2A H 0.8055 0.0501 0.4870 0.030 Uiso 1 1 calc R . .
C3 C 0.7608(4) -0.0946(2) 0.50416(19) 0.0266(6) Uani 1 1 d . . .
H3A H 0.8008 -0.1351 0.4530 0.032 Uiso 1 1 calc R . .
C4 C 0.6969(5) -0.1448(2) 0.55965(19) 0.0272(6) Uani 1 1 d . . .
H4A H 0.6968 -0.2184 0.5474 0.033 Uiso 1 1 calc R . .
C5 C 0.6333(4) -0.0819(2) 0.63408(19) 0.0227(6) Uani 1 1 d . . .
C6 C 0.7105(4) 0.1904(2) 0.64094(19) 0.0230(6) Uani 1 1 d . . .
C7 C 0.6913(6) 0.3507(3) 0.7430(2) 0.0398(8) Uani 1 1 d . . .
C8 C 0.7372(6) 0.3741(3) 0.6602(2) 0.0387(8) Uani 1 1 d . . .
C9 C 0.8917(11) 0.3816(4) 0.8186(3) 0.102(2) Uani 1 1 d . . .
H9A H 0.9243 0.4580 0.8406 0.153 Uiso 1 1 calc R . .
H9B H 1.0055 0.3490 0.7957 0.153 Uiso 1 1 calc R . .
H9C H 0.8679 0.3567 0.8659 0.153 Uiso 1 1 calc R . .
C10 C 0.5216(11) 0.3988(4) 0.7834(5) 0.110(3) Uani 1 1 d . . .
H10A H 0.3937 0.3785 0.7400 0.165 Uiso 1 1 calc R . .
H10B H 0.5511 0.4754 0.8045 0.165 Uiso 1 1 calc R . .
H10C H 0.5092 0.3740 0.8319 0.165 Uiso 1 1 calc R . .
C11 C 0.9138(10) 0.4555(5) 0.6731(4) 0.106(2) Uani 1 1 d . . .
H11A H 1.0406 0.4328 0.6976 0.159 Uiso 1 1 calc R . .
H11B H 0.8917 0.5229 0.7129 0.159 Uiso 1 1 calc R . .
H11C H 0.9230 0.4634 0.6172 0.159 Uiso 1 1 calc R . .
C12 C 0.5363(10) 0.4010(4) 0.6078(3) 0.0852(18) Uani 1 1 d . . .
H12A H 0.5535 0.3952 0.5492 0.128 Uiso 1 1 calc R . .
H12B H 0.5106 0.4727 0.6376 0.128 Uiso 1 1 calc R . .
H12C H 0.4209 0.3516 0.6041 0.128 Uiso 1 1 calc R . .
C13 C 0.5489(4) -0.1169(2) 0.69975(19) 0.0230(6) Uani 1 1 d . . .
C14 C 0.4266(5) -0.1055(2) 0.8236(2) 0.0277(6) Uani 1 1 d . . .
C15 C 0.3731(5) -0.2244(2) 0.7602(2) 0.0356(8) Uani 1 1 d . . .
C16 C 0.6096(6) -0.0908(3) 0.9006(2) 0.0427(8) Uani 1 1 d . . .
H16A H 0.7248 -0.1227 0.8783 0.064 Uiso 1 1 calc R . .
H16B H 0.5701 -0.1247 0.9404 0.064 Uiso 1 1 calc R . .
H16C H 0.6490 -0.0158 0.9315 0.064 Uiso 1 1 calc R . .
C17 C 0.2426(5) -0.0557(3) 0.8575(2) 0.0364(8) Uani 1 1 d . . .
H17A H 0.2861 0.0167 0.8956 0.055 Uiso 1 1 calc R . .
H17B H 0.1890 -0.0963 0.8900 0.055 Uiso 1 1 calc R . .
H17C H 0.1362 -0.0559 0.8083 0.055 Uiso 1 1 calc R . .
C18 C 0.4302(8) -0.3096(3) 0.8018(3) 0.0627(13) Uani 1 1 d . . .
H18A H 0.3947 -0.3790 0.7575 0.094 Uiso 1 1 calc R . .
H18B H 0.3554 -0.3048 0.8479 0.094 Uiso 1 1 calc R . .
H18C H 0.5767 -0.2991 0.8262 0.094 Uiso 1 1 calc R . .
C19 C 0.1504(6) -0.2495(3) 0.7071(3) 0.0598(12) Uani 1 1 d . . .
H19A H 0.1152 -0.1927 0.6840 0.090 Uiso 1 1 calc R . .
H19B H 0.0582 -0.2563 0.7448 0.090 Uiso 1 1 calc R . .
H19C H 0.1376 -0.3155 0.6592 0.090 Uiso 1 1 calc R . .
H5SA H 0.285(6) 0.401(4) 0.957(3) 0.045(13) Uiso 1 1 d . . .
H5SB H 0.221(9) 0.330(5) 0.988(4) 0.09(2) Uiso 1 1 d . . .
H6SA H 0.225(7) 0.586(4) 0.936(3) 0.050(14) Uiso 1 1 d . . .
H6SB H 0.389(8) 0.567(4) 0.950(4) 0.07(2) Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 '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'
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
O3 Ni1 N1 170.95(9) . . ?
O3 Ni1 O4 85.33(8) . . ?
N1 Ni1 O4 86.14(8) . . ?
O3 Ni1 N4 99.65(9) . . ?
N1 Ni1 N4 77.20(9) . . ?
O4 Ni1 N4 89.19(9) . . ?
O3 Ni1 N2 106.43(9) . . ?
N1 Ni1 N2 76.60(9) . . ?
O4 Ni1 N2 90.23(9) . . ?
N4 Ni1 N2 153.78(9) . . ?
O3 Ni1 Cl1 90.46(6) . . ?
N1 Ni1 Cl1 98.03(7) . . ?
O4 Ni1 Cl1 175.74(6) . . ?
N4 Ni1 Cl1 90.89(7) . . ?
N2 Ni1 Cl1 91.57(6) . . ?
C5 N1 C1 120.3(2) . . ?
C5 N1 Ni1 119.23(19) . . ?
C1 N1 Ni1 120.37(19) . . ?
C6 N2 C7 109.6(2) . . ?
C6 N2 Ni1 112.48(19) . . ?
C7 N2 Ni1 137.9(2) . . ?
O1 N3 C6 126.2(3) . . ?
O1 N3 C8 124.4(3) . . ?
C6 N3 C8 109.2(2) . . ?
C13 N4 C14 109.2(2) . . ?
C13 N4 Ni1 112.24(18) . . ?
C14 N4 Ni1 138.44(18) . . ?
O2 N5 C13 126.6(3) . . ?
O2 N5 C15 124.3(3) . . ?
C13 N5 C15 108.6(2) . . ?
N1 C1 C2 121.8(3) . . ?
N1 C1 C6 109.9(2) . . ?
C2 C1 C6 128.3(3) . . ?
C1 C2 C3 117.7(3) . . ?
C4 C3 C2 120.5(3) . . ?
C3 C4 C5 118.0(3) . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C13 110.3(2) . . ?
C4 C5 C13 128.1(3) . . ?
N2 C6 N3 113.9(3) . . ?
N2 C6 C1 120.6(3) . . ?
N3 C6 C1 125.5(3) . . ?
C10 C7 N2 110.7(3) . . ?
C10 C7 C8 119.7(4) . . ?
N2 C7 C8 104.6(3) . . ?
C10 C7 C9 106.7(5) . . ?
N2 C7 C9 103.8(3) . . ?
C8 C7 C9 110.2(3) . . ?
C11 C8 N3 112.3(4) . . ?
C11 C8 C7 118.0(4) . . ?
N3 C8 C7 101.2(2) . . ?
C11 C8 C12 110.0(4) . . ?
N3 C8 C12 104.4(3) . . ?
C7 C8 C12 109.9(4) . . ?
N4 C13 N5 113.7(3) . . ?
N4 C13 C5 120.8(2) . . ?
N5 C13 C5 125.4(3) . . ?
N4 C14 C17 109.8(2) . . ?
N4 C14 C16 105.6(3) . . ?
C17 C14 C16 110.3(3) . . ?
N4 C14 C15 103.4(2) . . ?
C17 C14 C15 113.9(3) . . ?
C16 C14 C15 113.2(3) . . ?
N5 C15 C18 110.5(3) . . ?
N5 C15 C19 105.6(3) . . ?
C18 C15 C19 110.9(3) . . ?
N5 C15 C14 99.3(2) . . ?
C18 C15 C14 115.9(3) . . ?
C19 C15 C14 113.5(3) . . ?
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 O3 2.033(2) . ?
Ni1 N1 2.040(2) . ?
Ni1 O4 2.106(2) . ?
Ni1 N4 2.126(2) . ?
Ni1 N2 2.148(2) . ?
Ni1 Cl1 2.3870(8) . ?
O1 N3 1.269(4) . ?
O2 N5 1.271(3) . ?
N1 C5 1.336(4) . ?
N1 C1 1.338(4) . ?
N2 C6 1.290(4) . ?
N2 C7 1.492(4) . ?
N3 C6 1.379(4) . ?
N3 C8 1.496(4) . ?
N4 C13 1.289(4) . ?
N4 C14 1.493(4) . ?
N5 C13 1.378(4) . ?
N5 C15 1.501(4) . ?
C1 C2 1.387(4) . ?
C1 C6 1.480(4) . ?
C2 C3 1.390(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.388(4) . ?
C5 C13 1.473(4) . ?
C7 C10 1.471(6) . ?
C7 C8 1.550(5) . ?
C7 C9 1.569(7) . ?
C8 C11 1.488(6) . ?
C8 C12 1.556(6) . ?
C14 C17 1.518(4) . ?
C14 C16 1.526(5) . ?
C14 C15 1.570(4) . ?
C15 C18 1.512(5) . ?
C15 C19 1.523(6) . ?
