#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:52:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179159 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/20/4312086.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_4312086
loop_
_publ_author_name
'Balwant S. Chohan'
'Steven C. Shoner'
'Julie A. Kovacs'
'Michael J. Maroney'
_publ_section_title
;
 Ligand Oxidations in High-Spin Nickel Thiolate Complexes and Zinc
 Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7726
_journal_page_last               7734
_journal_paper_doi               10.1021/ic049110n
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C12 H19 N3 Ni O2 S2'
_chemical_formula_weight         360.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.81(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.626(3)
_cell_length_b                   7.605(5)
_cell_length_c                   14.902(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1505.8(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            1846
_diffrn_reflns_theta_max         22.02
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    1.569
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.772
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.501
_refine_ls_goodness_of_fit_obs   1.619
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.504
_refine_ls_restrained_S_obs      1.619
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_obs          0.0718
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1982
_refine_ls_wR_factor_obs         0.1786
_reflns_number_observed          1340
_reflns_number_total             1846
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic049110nsi20040707_015146.cif
_cod_data_source_block           bc27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4312086
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni Ni 0.78071(7) 0.00018(14) 0.10746(6) 0.0332(5) Uani 1 d . .
S1 S 0.6874(2) -0.0533(4) -0.0400(2) 0.0520(8) Uani 1 d . .
S2 S 0.9198(2) -0.1506(3) 0.1907(2) 0.0497(7) Uani 1 d . .
O1 O 0.5280(6) -0.2509(13) -0.0682(5) 0.090(3) Uani 1 d . .
O2 O 1.0982(5) -0.0884(11) 0.1626(5) 0.075(2) Uani 1 d . .
N1 N 0.6690(5) -0.1370(10) 0.1475(5) 0.044(2) Uani 1 d . .
N2 N 0.7538(7) 0.2134(11) 0.1810(6) 0.059(2) Uani 1 d . .
H2 H 0.8158(7) 0.2327(11) 0.2175(6) 0.071 Uiso 1 calc R .
N3 N 0.8857(5) 0.1531(9) 0.0679(5) 0.040(2) Uani 1 d . .
C1 C 0.5946(7) -0.1782(12) -0.0110(6) 0.048(2) Uani 1 d . .
C2 C 0.5972(6) -0.2081(11) 0.0901(7) 0.042(2) Uani 1 d . .
C3 C 0.6687(9) -0.1446(16) 0.2467(6) 0.075(4) Uani 1 d . .
H3A H 0.7087(9) -0.2441(16) 0.2744(6) 0.090 Uiso 1 calc R .
H3B H 0.6003(9) -0.1624(16) 0.2538(6) 0.090 Uiso 1 calc R .
C4 C 0.7099(11) 0.0197(15) 0.2956(7) 0.074(4) Uani 1 d . .
H4A H 0.6816(11) 0.0303(15) 0.3496(7) 0.089 Uiso 1 calc R .
H4B H 0.7819(11) 0.0034(15) 0.3173(7) 0.089 Uiso 1 calc R .
C5 C 0.6951(8) 0.1828(15) 0.2484(7) 0.061(3) Uani 1 d . .
H5A H 0.7094(8) 0.2763(15) 0.2937(7) 0.073 Uiso 1 calc R .
H5B H 0.6245(8) 0.1920(15) 0.2181(7) 0.073 Uiso 1 calc R .
C6 C 0.7357(8) 0.3770(12) 0.1324(8) 0.060(3) Uani 1 d . .
H6A H 0.7324(8) 0.4688(12) 0.1769(8) 0.071 Uiso 1 calc R .
H6B H 0.6700(8) 0.3705(12) 0.0909(8) 0.071 Uiso 1 calc R .
C7 C 0.8103(12) 0.4326(15) 0.0776(9) 0.089(4) Uani 1 d . .
H7A H 0.7803(12) 0.5306(15) 0.0396(9) 0.106 Uiso 1 calc R .
H7B H 0.8681(12) 0.4791(15) 0.1212(9) 0.106 Uiso 1 calc R .
C8 C 0.8491(7) 0.3135(12) 0.0180(7) 0.054(3) Uani 1 d . .
H8A H 0.9036(7) 0.3698(12) -0.0034(7) 0.064 Uiso 1 calc R .
H8B H 0.7963(7) 0.2849(12) -0.0352(7) 0.064 Uiso 1 calc R .
C9 C 0.9801(6) 0.1217(11) 0.0929(6) 0.038(2) Uani 1 d . .
C10 C 1.0105(7) -0.0402(12) 0.1490(6) 0.046(2) Uani 1 d . .
C11 C 0.5108(8) -0.3076(15) 0.1115(8) 0.067(3) Uani 1 d . .
H11A H 0.5199(8) -0.3190(15) 0.1770(8) 0.101 Uiso 1 calc R .
H11B H 0.5076(8) -0.4223(15) 0.0842(8) 0.101 Uiso 1 calc R .
H11C H 0.4493(8) -0.2454(15) 0.0872(8) 0.101 Uiso 1 calc R .
C12 C 1.0607(7) 0.2355(15) 0.0706(7) 0.059(3) Uani 1 d . .
H12A H 1.0306(7) 0.3340(15) 0.0345(7) 0.088 Uiso 1 calc R .
H12B H 1.0998(7) 0.1687(15) 0.0364(7) 0.088 Uiso 1 calc R .
H12C H 1.1036(7) 0.2770(15) 0.1266(7) 0.088 Uiso 1 calc R .
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'
S S 0.1246 0.1234 '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
N3 Ni N2 85.6(3) . . ?
N3 Ni N1 175.7(3) . . ?
N2 Ni N1 90.8(3) . . ?
N3 Ni S1 95.7(2) . . ?
N2 Ni S1 121.6(3) . . ?
N1 Ni S1 84.2(2) . . ?
N3 Ni S2 83.9(2) . . ?
N2 Ni S2 109.2(3) . . ?
N1 Ni S2 99.5(2) . . ?
S1 Ni S2 129.10(11) . . ?
C1 S1 Ni 98.0(3) . . ?
C10 S2 Ni 97.6(3) . . ?
C2 N1 C3 118.9(8) . . ?
C2 N1 Ni 122.3(6) . . ?
C3 N1 Ni 118.7(6) . . ?
C6 N2 C5 115.8(8) . . ?
C6 N2 Ni 116.8(6) . . ?
C5 N2 Ni 116.3(6) . . ?
C9 N3 C8 120.9(7) . . ?
C9 N3 Ni 122.4(6) . . ?
C8 N3 Ni 116.4(5) . . ?
O1 C1 C2 118.2(9) . . ?
O1 C1 S1 123.2(8) . . ?
C2 C1 S1 118.6(6) . . ?
N1 C2 C11 126.8(9) . . ?
N1 C2 C1 116.8(7) . . ?
C11 C2 C1 116.3(8) . . ?
N1 C3 C4 111.7(8) . . ?
C5 C4 C3 119.6(10) . . ?
C4 C5 N2 116.7(9) . . ?
N2 C6 C7 117.3(9) . . ?
C8 C7 C6 122.8(10) . . ?
C7 C8 N3 109.9(8) . . ?
N3 C9 C12 124.6(8) . . ?
N3 C9 C10 117.0(8) . . ?
C12 C9 C10 118.4(8) . . ?
O2 C10 C9 118.6(9) . . ?
O2 C10 S2 123.2(8) . . ?
C9 C10 S2 118.2(7) . . ?
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 N3 2.031(7) . ?
Ni N2 2.036(8) . ?
Ni N1 2.040(7) . ?
Ni S1 2.317(2) . ?
Ni S2 2.324(3) . ?
S1 C1 1.711(9) . ?
S2 C10 1.720(10) . ?
O1 C1 1.230(11) . ?
O2 C10 1.223(11) . ?
N1 C2 1.270(11) . ?
N1 C3 1.480(11) . ?
N2 C6 1.433(12) . ?
N2 C5 1.435(11) . ?
N3 C9 1.279(11) . ?
N3 C8 1.457(11) . ?
C1 C2 1.516(13) . ?
C2 C11 1.492(12) . ?
C3 C4 1.492(15) . ?
C4 C5 1.418(14) . ?
C6 C7 1.50(2) . ?
C7 C8 1.448(15) . ?
C9 C12 1.493(12) . ?
C9 C10 1.495(12) . ?
