#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:56:25 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239910 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/05/4350511.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_4350511
loop_
_publ_author_name
'Senda, Shunsuke'
'Ohki, Yasuhiro'
'Hirayama, Tomoko'
'Toda, Daisuke'
'Chen, Jing-Lin'
'Matsumoto, Tsuyoshi'
'Kawaguchi, Hiroyuki'
'Tatsumi, Kazuyuki'
_publ_section_title
;
 Mono{hydrotris(mercaptoimidazolyl)borato} complexes of manganese(II),
 iron(II), cobalt(II), and nickel(II) halides.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9914
_journal_page_last               9925
_journal_paper_doi               10.1021/ic0610132
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C14 H24 Cl2 N4 Ni S2 '
_chemical_formula_sum            'C14 H24 Cl2 N4 Ni S2'
_chemical_formula_weight         442.10
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 125.169(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7566(111)
_cell_length_b                   8.5754(52)
_cell_length_c                   16.6980(113)
_cell_measurement_reflns_used    2730
_cell_measurement_temperature    173.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     1961(2)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9902
_diffrn_measured_fraction_theta_max 0.9902
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7734
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2198
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00063|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                1763
_reflns_number_total             2223
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic0610132si20060906_094900.cif
_cod_data_source_block           Ni(imi(tBu))2Cl2
_cod_original_cell_volume        1961.4(22)
_cod_original_formula_sum        'C14 H24 Cl2 N4 Ni S2 '
_cod_database_code               4350511
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+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_calc_flag
_atom_site_refinement_flags
Ni(1) Ni 1.0000 0.77899(5) 0.7500 0.0234(1) Uani 1.00 d S
Cl(1) Cl 1.13106(4) 0.87682(7) 0.88904(4) 0.0317(2) Uani 1.00 d .
S(1) S 0.94814(5) 0.62463(7) 0.82258(4) 0.0300(2) Uani 1.00 d .
N(1) N 0.8190(1) 0.5175(2) 0.6371(1) 0.0243(5) Uani 1.00 d .
N(2) N 0.8575(1) 0.3404(2) 0.7460(1) 0.0210(5) Uani 1.00 d .
C(1) C 0.8741(2) 0.4900(3) 0.7341(2) 0.0220(5) Uani 1.00 d .
C(2) C 0.7664(2) 0.3874(3) 0.5868(2) 0.0278(6) Uani 1.00 d .
C(3) C 0.7897(2) 0.2775(3) 0.6539(2) 0.0261(6) Uani 1.00 d .
C(4) C 0.9001(2) 0.2570(3) 0.8422(2) 0.0249(6) Uani 1.00 d .
C(5) C 0.8646(2) 0.3377(3) 0.8970(2) 0.0345(7) Uani 1.00 d .
C(6) C 1.0113(2) 0.2556(3) 0.9000(2) 0.0381(7) Uani 1.00 d .
C(7) C 0.8634(2) 0.0895(3) 0.8203(2) 0.0372(7) Uani 1.00 d .
H(1) H 0.8117 0.6080 0.6155 0.0912 Uiso 1.00 calc .
H(2) H 0.7207 0.3773 0.5162 0.0326 Uiso 1.00 calc .
H(3) H 0.7639 0.1724 0.6410 0.0301 Uiso 1.00 calc .
H(4) H 0.8919 0.2858 0.9592 0.0408 Uiso 1.00 calc .
H(5) H 0.8855 0.4459 0.9086 0.0408 Uiso 1.00 calc .
H(6) H 0.7940 0.3332 0.8584 0.0408 Uiso 1.00 calc .
H(7) H 1.0387 0.2021 0.9614 0.0470 Uiso 1.00 calc .
H(8) H 1.0303 0.2022 0.8619 0.0470 Uiso 1.00 calc .
H(9) H 1.0355 0.3621 0.9123 0.0470 Uiso 1.00 calc .
H(10) H 0.7927 0.0887 0.7824 0.0443 Uiso 1.00 calc .
H(11) H 0.8844 0.0383 0.7838 0.0443 Uiso 1.00 calc .
H(12) H 0.8900 0.0344 0.8817 0.0443 Uiso 1.00 calc .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Ni Ni 0.339 1.112
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
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
_geom_angle_publ_flag
Cl(1) Ni(1) Cl(1) 136.13(4) . 2_756 yes
Cl(1) Ni(1) S(1) 96.47(4) . . yes
Cl(1) Ni(1) S(1) 108.76(5) . 2_756 yes
Cl(1) Ni(1) S(1) 108.76(5) 2_756 . yes
Cl(1) Ni(1) S(1) 96.47(4) 2_756 2_756 yes
S(1) Ni(1) S(1) 108.94(4) . 2_756 yes
Ni(1) S(1) C(1) 103.96(8) . . yes
C(1) N(1) C(2) 110.4(2) . . yes
C(1) N(2) C(3) 108.2(2) . . yes
C(1) N(2) C(4) 126.5(2) . . yes
C(3) N(2) C(4) 125.2(2) . . yes
S(1) C(1) N(1) 125.0(2) . . yes
S(1) C(1) N(2) 128.4(2) . . yes
N(1) C(1) N(2) 106.6(2) . . yes
N(1) C(2) C(3) 106.6(2) . . yes
N(2) C(3) C(2) 108.1(2) . . yes
N(2) C(4) C(5) 108.4(2) . . yes
N(2) C(4) C(6) 109.5(2) . . yes
N(2) C(4) C(7) 108.3(2) . . yes
C(5) C(4) C(6) 112.5(2) . . yes
C(5) C(4) C(7) 109.3(2) . . yes
C(6) C(4) C(7) 108.8(2) . . yes
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
Ni(1) Cl(1) 2.2457(8) . yes
Ni(1) Cl(1) 2.2457(8) 2_756 yes
Ni(1) S(1) 2.2780(8) . yes
Ni(1) S(1) 2.2780(8) 2_756 yes
S(1) C(1) 1.715(2) . yes
N(1) C(1) 1.345(3) . yes
N(1) C(2) 1.369(3) . yes
N(2) C(1) 1.351(3) . yes
N(2) C(3) 1.390(3) . yes
N(2) C(4) 1.510(3) . yes
C(2) C(3) 1.339(3) . yes
C(4) C(5) 1.517(3) . yes
C(4) C(6) 1.527(4) . yes
C(4) C(7) 1.522(3) . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Cl(1) C(2) 3.392(2) 8_565
Cl(1) N(1) 3.588(2) 8_565
N(1) C(7) 3.568(4) 6_656
C(2) C(2) 3.524(5) 7_656
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni(1) S(1) C(1) N(1) -32.1(2) . . . yes
Ni(1) S(1) C(1) N(2) 149.2(2) . . . yes
Ni(1) S(1) C(1) N(1) -32.1(2) 2_756 2_756 2_756 yes
Ni(1) S(1) C(1) N(2) 149.2(2) 2_756 2_756 2_756 yes
Cl(1) Ni(1) S(1) C(1) -159.98(8) . . . yes
Cl(1) Ni(1) S(1) C(1) 56.44(8) . 2_756 2_756 yes
S(1) Ni(1) S(1) C(1) -47.58(8) . 2_756 2_756 yes
S(1) C(1) N(1) C(2) -178.2(2) . . . yes
S(1) C(1) N(2) C(3) 178.0(2) . . . yes
S(1) C(1) N(2) C(4) 1.2(3) . . . yes
N(1) C(1) N(2) C(3) -0.9(2) . . . yes
N(1) C(1) N(2) C(4) -177.7(2) . . . yes
N(1) C(2) C(3) N(2) -0.4(3) . . . yes
N(2) C(1) N(1) C(2) 0.7(3) . . . yes
C(1) N(1) C(2) C(3) -0.2(3) . . . yes
C(1) N(2) C(3) C(2) 0.8(3) . . . yes
C(1) N(2) C(4) C(5) 62.9(3) . . . yes
C(1) N(2) C(4) C(6) -60.2(3) . . . yes
C(1) N(2) C(4) C(7) -178.6(2) . . . yes
C(2) C(3) N(2) C(4) 177.6(2) . . . yes
C(3) N(2) C(4) C(5) -113.3(2) . . . yes
C(3) N(2) C(4) C(6) 123.6(2) . . . yes
C(3) N(2) C(4) C(7) 5.1(3) . . . yes
C(3) N(2) C(4) C(7) 5.1(3) . . . yes
