#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:38:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179855 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/51/7015155.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_7015155
loop_
_publ_author_name
'Lobana, Tarlok Singh'
'Kumari, Poonam'
'Sharma, Rekha'
'Castineiras, Alfonso'
'Butcher, Ray Jay'
'Akitsu, Takashiro'
'Aritake, Yoshikazu'
_publ_section_title
;
 Thiosemicarbazone derivatives of nickel and copper: the unprecedented
 coordination of furan ring in octahedral nickel(II) and of
 triphenylphosphine in three-coordinate copper(I) complexes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3219
_journal_page_last               3228
_journal_paper_doi               10.1039/c0dt01291b
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C16 H20 N6 Ni S4'
_chemical_formula_sum            'C16 H20 N6 Ni S4'
_chemical_formula_weight         483.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      41
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.768(2)
_cell_length_b                   27.394(3)
_cell_length_c                   4.8820(6)
_cell_measurement_reflns_used    1966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.163
_cell_measurement_theta_min      2.7585
_cell_volume                     1975.0(4)
_computing_cell_refinement       'APEX2 Software (Bruker, 2005)'
_computing_data_collection       'APEX2 Software (Bruker, 2005)'
_computing_data_reduction        'APEX2 Software (Bruker, 2005)'
_computing_molecular_graphics    'PLATON (Spek, 2004)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and phi 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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            11660
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_T_max  0.7741
_exptl_absorpt_correction_T_min  0.4779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1925
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0494P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                1816
_reflns_number_total             1925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01291b.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      'A e a 2'
_cod_database_code               7015155
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z+1/2'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
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 0.0000 0.0000 0.65147(14) 0.01253(15) Uani 1 2 d S . .
S1 S -0.14195(5) 0.01651(3) 0.55569(18) 0.0157(2) Uani 1 1 d . . .
S11 S 0.03104(6) 0.18306(3) 0.47992(19) 0.0174(2) Uani 1 1 d . . .
N12 N 0.01754(16) 0.06911(9) 0.6387(7) 0.0131(5) Uani 1 1 d . . .
N13 N -0.03450(19) 0.09404(9) 0.4453(6) 0.0135(5) Uani 1 1 d . . .
N14 N -0.16940(18) 0.09046(9) 0.2155(5) 0.0172(7) Uani 1 1 d . . .
H14A H -0.2214 0.0757 0.1866 0.021 Uiso 1 1 d R . .
C11 C 0.0917(2) 0.23416(11) 0.5631(7) 0.0197(7) Uani 1 1 d . . .
H11 H 0.0822 0.2652 0.4815 0.024 Uiso 1 1 d R . .
C12 C 0.1551(2) 0.22526(12) 0.7598(8) 0.0208(8) Uani 1 1 d . . .
H12 H 0.1947 0.2495 0.8311 0.025 Uiso 1 1 d R . .
C13 C 0.1554(2) 0.17635(12) 0.8449(8) 0.0187(7) Uani 1 1 d . . .
H13 H 0.1955 0.1640 0.9805 0.022 Uiso 1 1 d R . .
C14 C 0.0918(2) 0.14776(11) 0.7130(7) 0.0149(7) Uani 1 1 d . . .
C15 C 0.0781(2) 0.09596(10) 0.7660(7) 0.0136(7) Uani 1 1 d . . .
C16 C -0.1102(2) 0.07088(11) 0.3924(6) 0.0140(8) Uani 1 1 d . . .
C17 C -0.1497(2) 0.13562(11) 0.0699(8) 0.0194(7) Uani 1 1 d . . .
H17A H -0.1425 0.1623 0.2021 0.029 Uiso 1 1 d R . .
H17B H -0.1997 0.1432 -0.0549 0.029 Uiso 1 1 d R . .
H17C H -0.0937 0.1318 -0.0353 0.029 Uiso 1 1 d R . .
C18 C 0.1355(2) 0.07303(12) 0.9829(7) 0.0169(7) Uani 1 1 d . . .
H18A H 0.1313 0.0923 1.1516 0.025 Uiso 1 1 d R . .
H18B H 0.1987 0.0721 0.9212 0.025 Uiso 1 1 d R . .
H18C H 0.1143 0.0397 1.0180 0.025 Uiso 1 1 d 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'
S S 0.1246 0.1234 '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'
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'
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
N12 Ni1 N12 176.3(2) 2 . y
N12 Ni1 S1 93.88(7) 2 . y
N12 Ni1 S1 85.32(8) . . y
N12 Ni1 S1 85.32(8) 2 2 y
N12 Ni1 S1 93.88(7) . 2 y
S1 Ni1 S1 155.40(6) . 2 y
C16 S1 Ni1 90.92(11) . . ?
C11 S11 C14 91.69(16) . . ?
C15 N12 N13 114.9(2) . . ?
C15 N12 Ni1 129.1(2) . . ?
N13 N12 Ni1 115.6(2) . . ?
C16 N13 N12 111.5(2) . . ?
C16 N14 C17 121.6(3) . . ?
C16 N14 H14A 119.2 . . ?
C17 N14 H14A 119.2 . . ?
C12 C11 S11 112.4(2) . . ?
C12 C11 H11 123.8 . . ?
S11 C11 H11 123.8 . . ?
C11 C12 C13 112.4(3) . . ?
C11 C12 H12 123.8 . . ?
C13 C12 H12 123.8 . . ?
C14 C13 C12 113.7(3) . . ?
C14 C13 H13 123.2 . . ?
C12 C13 H13 123.2 . . ?
C13 C14 C15 124.3(3) . . ?
C13 C14 S11 109.9(2) . . ?
C15 C14 S11 125.8(2) . . ?
N12 C15 C14 123.8(3) . . ?
N12 C15 C18 119.1(3) . . ?
C14 C15 C18 117.1(3) . . ?
N13 C16 N14 119.3(3) . . ?
N13 C16 S1 123.4(2) . . ?
N14 C16 S1 117.2(2) . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
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 N12 1.912(2) 2 y
Ni1 N12 1.912(2) . y
Ni1 S1 2.1950(8) . y
Ni1 S1 2.1950(8) 2 y
S1 C16 1.753(3) . ?
S11 C11 1.711(3) . ?
S11 C14 1.742(3) . ?
N12 C15 1.314(4) . ?
N12 N13 1.396(4) . ?
N13 C16 1.311(4) . ?
N14 C16 1.341(4) . ?
N14 C17 1.456(4) . ?
N14 H14A 0.8800 . ?
C11 C12 1.363(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.403(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.457(4) . ?
C15 C18 1.495(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N14 H14A S1 0.88 2.67 3.532(3) 168.3 3_454
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N12 Ni1 S1 C16 -149.72(14) 2 . . . ?
N12 Ni1 S1 C16 26.61(15) . . . . ?
S1 Ni1 S1 C16 -62.49(10) 2 . . . ?
N12 Ni1 N12 C15 -129.5(3) 2 . . . ?
S1 Ni1 N12 C15 152.7(3) . . . . ?
S1 Ni1 N12 C15 -52.0(3) 2 . . . ?
N12 Ni1 N12 N13 42.7(2) 2 . . . ?
S1 Ni1 N12 N13 -35.1(2) . . . . ?
S1 Ni1 N12 N13 120.3(2) 2 . . . ?
C15 N12 N13 C16 -159.4(3) . . . . ?
Ni1 N12 N13 C16 27.2(3) . . . . ?
C14 S11 C11 C12 -0.3(3) . . . . ?
S11 C11 C12 C13 0.2(4) . . . . ?
C11 C12 C13 C14 -0.1(4) . . . . ?
C12 C13 C14 C15 -179.5(3) . . . . ?
C12 C13 C14 S11 -0.1(4) . . . . ?
C11 S11 C14 C13 0.2(3) . . . . ?
C11 S11 C14 C15 179.6(3) . . . . ?
N13 N12 C15 C14 -0.3(4) . . . . ?
Ni1 N12 C15 C14 172.0(2) . . . . ?
N13 N12 C15 C18 178.3(3) . . . . ?
Ni1 N12 C15 C18 -9.4(5) . . . . ?
C13 C14 C15 N12 -179.8(3) . . . . ?
S11 C14 C15 N12 0.9(5) . . . . ?
C13 C14 C15 C18 1.6(5) . . . . ?
S11 C14 C15 C18 -177.7(2) . . . . ?
N12 N13 C16 N14 178.4(3) . . . . ?
N12 N13 C16 S1 2.0(4) . . . . ?
C17 N14 C16 N13 3.2(5) . . . . ?
C17 N14 C16 S1 179.8(2) . . . . ?
Ni1 S1 C16 N13 -23.6(3) . . . . ?
Ni1 S1 C16 N14 160.0(2) . . . . ?
