#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/88/7008887.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_7008887
loop_
_publ_author_name
'Pavlishchuk, Vitaly V.'
'Kolotilov, Sergey V.'
'Addison, Anthony W.'
'Butcher, Raymond J.'
'Sinn, Ekkehard'
_publ_section_title
;
 Nickel(II) complexes with dithiadiiminoamine and
 dithiabis(thiosemicarbazone) ligands †
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              335
_journal_paper_doi               10.1039/a906294g
_journal_year                    2000
_chemical_formula_sum            'C12 H27 Cl2 N4 Ni O8.5 S2'
_chemical_formula_weight         557.11
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.888(2)
_cell_length_b                   19.831(3)
_cell_length_c                   13.2864(16)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      4.96
_cell_volume                     4449.7(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_method       'ω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5007
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.41
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.4374
_exptl_absorpt_correction_T_min  0.4107
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_purple
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.74
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5007
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.301
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0474P)²+4.0131P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                2991
_reflns_number_total             5007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a906294g.txt
_cod_data_source_block           1
_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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pccn
_cod_original_formula_sum        'C12 H27 Cl2 N4 Ni O8.50 S2'
_cod_database_code               7008887
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.07264(3) 0.38334(3) 0.16815(4) 0.03310(16) Uani 1 1 d . . .
Cl1 Cl 0.19452(8) 0.59502(7) 0.08197(12) 0.0603(4) Uani 1 1 d . . .
Cl2 Cl 0.37728(7) 0.35729(6) 0.09202(10) 0.0496(3) Uani 1 1 d D . .
S1A S -0.02288(7) 0.47690(6) 0.16860(9) 0.0470(3) Uani 1 1 d . . .
S1B S -0.01114(7) 0.32634(7) 0.29028(9) 0.0487(3) Uani 1 1 d . . .
O1W O 0.2500 0.7500 0.2259(9) 0.178(4) Uani 1 2 d S . .
O11 O 0.1330(3) 0.5726(2) 0.0202(4) 0.117(2) Uani 1 1 d . . .
O12 O 0.2374(3) 0.5384(2) 0.1168(4) 0.1099(18) Uani 1 1 d . . .
O13 O 0.1583(4) 0.6316(3) 0.1611(4) 0.1218(19) Uani 1 1 d . . .
O14 O 0.2459(3) 0.6392(2) 0.0313(5) 0.130(2) Uani 1 1 d . . .
O21 O 0.4031(3) 0.3339(2) 0.1859(3) 0.1058(17) Uani 1 1 d D A .
O22 O 0.3176(6) 0.3149(5) 0.0568(6) 0.087(5) Uani 0.57(3) 1 d PD A 1
O23 O 0.4385(4) 0.3609(9) 0.0246(6) 0.128(6) Uani 0.57(3) 1 d PD A 1
O24 O 0.3468(10) 0.4220(4) 0.1032(7) 0.113(6) Uani 0.57(3) 1 d PD A 1
O22A O 0.4392(8) 0.3845(13) 0.0387(10) 0.136(10) Uani 0.43(3) 1 d PD A 2
O23A O 0.3159(12) 0.4004(14) 0.1015(13) 0.223(16) Uani 0.43(3) 1 d PD A 2
O24A O 0.350(2) 0.2984(9) 0.0377(12) 0.168(12) Uani 0.43(3) 1 d PD A 2
N1A N 0.1667(3) 0.3174(2) 0.2021(4) 0.0430(10) Uani 1 1 d . . .
H1NA H 0.146(3) 0.277(3) 0.203(4) 0.067(19) Uiso 1 1 d . . .
H2NA H 0.195(3) 0.321(3) 0.163(4) 0.048(19) Uiso 1 1 d . . .
N2A N 0.1264(2) 0.4416(2) 0.2744(3) 0.0423(9) Uani 1 1 d . . .
N1B N 0.1282(3) 0.4159(2) 0.0359(3) 0.0438(10) Uani 1 1 d . . .
H1NB H 0.105(3) 0.458(3) 0.012(4) 0.08(2) Uiso 1 1 d . . .
H2NB H 0.174(3) 0.424(3) 0.046(4) 0.059(18) Uiso 1 1 d . . .
N2B N 0.0105(2) 0.32448(17) 0.0699(3) 0.0359(8) Uani 1 1 d . . .
C1A C 0.1965(3) 0.3363(3) 0.3022(4) 0.0521(13) Uani 1 1 d . . .
H1AA H 0.2486 0.3168 0.3124 0.056(14) Uiso 1 1 calc R . .
H1AB H 0.1614 0.3187 0.3537 0.037(12) Uiso 1 1 calc R . .
C2A C 0.2014(3) 0.4123(3) 0.3107(4) 0.0544(14) Uani 1 1 d . . .
H2AA H 0.2102 0.4252 0.3802 0.050(14) Uiso 1 1 calc R . .
H2AB H 0.2452 0.4291 0.2706 0.057(15) Uiso 1 1 calc R . .
C3A C 0.1012(3) 0.4976(2) 0.3081(4) 0.0490(12) Uani 1 1 d . . .
C31A C 0.1409(5) 0.5405(3) 0.3866(5) 0.0800(19) Uani 1 1 d . . .
H31D H 0.1880 0.5184 0.4098 0.20(5) Uiso 1 1 calc R . .
H31E H 0.1054 0.5472 0.4421 0.16(4) Uiso 1 1 calc R . .
H31F H 0.1545 0.5834 0.3578 0.21(5) Uiso 1 1 calc R . .
C4A C 0.0256(3) 0.5260(3) 0.2650(4) 0.0583(14) Uani 1 1 d . . .
H4AA H 0.0372 0.5702 0.2374 0.077(18) Uiso 1 1 calc R . .
H4AB H -0.0116 0.5324 0.3199 0.062(16) Uiso 1 1 calc R . .
C5A C -0.1038(3) 0.4388(3) 0.2374(4) 0.0604(15) Uani 1 1 d . . .
H5AA H -0.1370 0.4745 0.2643 0.064(16) Uiso 1 1 calc R . .
H5AB H -0.1358 0.4129 0.1907 0.043(13) Uiso 1 1 calc R . .
C1B C 0.1178(3) 0.3620(2) -0.0383(3) 0.0469(12) Uani 1 1 d . . .
H1BA H 0.1542 0.3254 -0.0237 0.028(11) Uiso 1 1 calc R . .
H1BB H 0.1298 0.3790 -0.1050 0.042(12) Uiso 1 1 calc R . .
C2B C 0.0336(3) 0.3361(3) -0.0355(3) 0.0453(12) Uani 1 1 d . . .
H2BA H -0.0016 0.3688 -0.0661 0.054(14) Uiso 1 1 calc R . .
H2BB H 0.0298 0.2943 -0.0732 0.09(2) Uiso 1 1 calc R . .
C3B C -0.0467(3) 0.2860(2) 0.0926(4) 0.0417(11) Uani 1 1 d . . .
C31B C -0.0964(3) 0.2455(3) 0.0215(5) 0.0621(15) Uani 1 1 d . . .
H31A H -0.0802 0.2545 -0.0464 0.17(4) Uiso 1 1 calc R . .
H31B H -0.1511 0.2576 0.0296 0.14(3) Uiso 1 1 calc R . .
H31C H -0.0898 0.1984 0.0358 0.13(3) Uiso 1 1 calc R . .
C4B C -0.0671(3) 0.2760(3) 0.2020(4) 0.0576(14) Uani 1 1 d . . .
H4BA H -0.0592 0.2288 0.2186 0.11(2) Uiso 1 1 calc R . .
H4BB H -0.1229 0.2858 0.2112 0.073(17) Uiso 1 1 calc R . .
C5B C -0.0791(3) 0.3928(3) 0.3236(4) 0.0625(15) Uani 1 1 d . . .
H5BA H -0.1263 0.3726 0.3522 0.064(17) Uiso 1 1 calc R . .
H5BB H -0.0548 0.4203 0.3756 0.08(2) 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
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'
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
N2A Ni N2B 175.03(15) . . ?
N2A Ni N1B 101.94(16) . . ?
N2B Ni N1B 82.52(16) . . ?
N2A Ni N1A 82.37(16) . . ?
N2B Ni N1A 99.78(16) . . ?
N1B Ni N1A 91.9(2) . . ?
N2A Ni S1B 93.49(11) . . ?
N2B Ni S1B 82.05(11) . . ?
N1B Ni S1B 164.57(13) . . ?
N1A Ni S1B 90.42(16) . . ?
N2A Ni S1A 82.13(11) . . ?
N2B Ni S1A 95.49(10) . . ?
N1B Ni S1A 93.65(14) . . ?
N1A Ni S1A 164.31(13) . . ?
S1B Ni S1A 88.13(5) . . ?
O11 Cl1 O14 112.2(4) . . ?
O11 Cl1 O12 108.7(3) . . ?
O14 Cl1 O12 109.6(3) . . ?
O11 Cl1 O13 106.2(4) . . ?
O14 Cl1 O13 107.6(3) . . ?
O12 Cl1 O13 112.6(4) . . ?
O23A Cl2 O23 127.4(9) . . ?
O23A Cl2 O22A 112.6(6) . . ?
O23 Cl2 O22A 21.2(13) . . ?
O23A Cl2 O24 28.5(11) . . ?
O23 Cl2 O24 107.5(8) . . ?
O22A Cl2 O24 88.6(10) . . ?
O23A Cl2 O22 81.8(13) . . ?
O23 Cl2 O22 111.0(4) . . ?
O22A Cl2 O22 127.9(10) . . ?
O24 Cl2 O22 109.0(4) . . ?
O23A Cl2 O21 111.4(7) . . ?
O23 Cl2 O21 111.4(4) . . ?
O22A Cl2 O21 110.6(6) . . ?
O24 Cl2 O21 109.0(3) . . ?
O22 Cl2 O21 108.9(3) . . ?
O23A Cl2 O24A 108.5(6) . . ?
O23 Cl2 O24A 87.2(15) . . ?
O22A Cl2 O24A 107.3(7) . . ?
O24 Cl2 O24A 133.1(11) . . ?
O22 Cl2 O24A 28.2(14) . . ?
O21 Cl2 O24A 105.9(5) . . ?
C4A S1A C5A 102.1(3) . . ?
C4A S1A Ni 96.42(17) . . ?
C5A S1A Ni 100.48(18) . . ?
C5B S1B C4B 103.4(3) . . ?
C5B S1B Ni 101.19(18) . . ?
C4B S1B Ni 97.37(16) . . ?
C1A N1A Ni 107.1(3) . . ?
C3A N2A C2A 121.1(4) . . ?
C3A N2A Ni 126.2(3) . . ?
C2A N2A Ni 112.7(3) . . ?
C1B N1B Ni 106.6(3) . . ?
C3B N2B C2B 121.5(4) . . ?
C3B N2B Ni 125.7(3) . . ?
C2B N2B Ni 112.5(3) . . ?
N1A C1A C2A 109.8(4) . . ?
N2A C2A C1A 108.7(4) . . ?
N2A C3A C31A 126.2(5) . . ?
N2A C3A C4A 118.5(4) . . ?
C31A C3A C4A 115.3(5) . . ?
C3A C4A S1A 116.8(3) . . ?
C5B C5A S1A 115.0(4) . . ?
N1B C1B C2B 110.1(4) . . ?
N2B C2B C1B 109.0(4) . . ?
N2B C3B C31B 126.9(5) . . ?
N2B C3B C4B 118.9(4) . . ?
C31B C3B C4B 114.2(4) . . ?
C3B C4B S1B 115.7(3) . . ?
C5A C5B S1B 115.3(4) . . ?
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 N2A 2.037(4) . ?
Ni N2B 2.042(3) . ?
Ni N1B 2.094(4) . ?
Ni N1A 2.106(4) . ?
Ni S1B 2.4317(13) . ?
Ni S1A 2.4586(13) . ?
Cl1 O11 1.397(4) . ?
Cl1 O14 1.405(5) . ?
Cl1 O12 1.414(4) . ?
Cl1 O13 1.416(5) . ?
Cl2 O23A 1.350(11) . ?
Cl2 O23 1.370(5) . ?
Cl2 O22A 1.374(10) . ?
Cl2 O24 1.391(5) . ?
Cl2 O22 1.393(5) . ?
Cl2 O21 1.400(4) . ?
Cl2 O24A 1.446(10) . ?
S1A C4A 1.806(5) . ?
S1A C5A 1.810(5) . ?
S1B C5B 1.803(5) . ?
S1B C4B 1.807(5) . ?
N1A C1A 1.470(6) . ?
N2A C3A 1.270(6) . ?
N2A C2A 1.473(6) . ?
N1B C1B 1.464(6) . ?
N2B C3B 1.267(5) . ?
N2B C2B 1.472(5) . ?
C1A C2A 1.515(7) . ?
C3A C31A 1.504(7) . ?
C3A C4A 1.510(7) . ?
C5A C5B 1.522(7) . ?
C1B C2B 1.513(6) . ?
C3B C31B 1.498(6) . ?
C3B C4B 1.507(7) . ?
