#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:08:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179777 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/73/7007370.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_7007370
loop_
_publ_author_name
'Adams, Christopher J.'
'Crawford, Paul C.'
'Guy Orpen, A.'
'Podesta, Thomas J.'
_publ_section_title
;
 Cation and anion diversity in [M(dithiooxalate)2]2- salts: structure
 robustness in crystal synthesis.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4078
_journal_page_last               4092
_journal_paper_doi               10.1039/b604319d
_journal_year                    2006
_chemical_formula_sum            'C16 H12 N2 Ni O8 S4'
_chemical_formula_weight         547.23
_chemical_name_systematic
;
?
;
_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                75.683(2)
_cell_angle_beta                 70.904(2)
_cell_angle_gamma                85.902(2)
_cell_formula_units_Z            1
_cell_length_a                   7.0457(10)
_cell_length_b                   7.5275(10)
_cell_length_c                   10.1365(14)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.461
_cell_measurement_theta_min      3.113
_cell_volume                     492.22(12)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5158
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_T_max  0.901067
_exptl_absorpt_correction_T_min  0.706660
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             278
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0410P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                1924
_reflns_number_total             2229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604319d.txt
_cod_data_source_block           3gerea
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               7007370
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 2.0000 -1.0000 0.0000 0.01713(11) Uani 1 2 d S . .
S1 S 1.94388(7) -1.17000(7) 0.21688(5) 0.02284(13) Uani 1 1 d . . .
S2 S 1.68978(7) -0.91207(7) 0.06880(5) 0.02227(13) Uani 1 1 d . . .
O3 O 1.1974(2) -0.8259(2) 0.30707(15) 0.0268(3) Uani 1 1 d . . .
O4 O 1.1466(2) -0.6478(2) 0.10785(15) 0.0248(3) Uani 1 1 d . . .
C2 C 1.8365(3) -0.7129(3) -0.2158(2) 0.0193(4) Uani 1 1 d . . .
C6 C 0.5745(3) -0.7957(3) 0.5239(2) 0.0248(4) Uani 1 1 d . . .
H6A H 0.5114 -0.8623 0.6198 0.030 Uiso 1 1 calc R . .
C3 C 1.0888(3) -0.7363(3) 0.2456(2) 0.0201(4) Uani 1 1 d . . .
O2 O 1.8122(2) -0.6008(2) -0.31840(14) 0.0261(3) Uani 1 1 d . . .
C5 C 0.7798(3) -0.8097(3) 0.4589(2) 0.0219(4) Uani 1 1 d . . .
H5A H 0.8589 -0.8841 0.5108 0.026 Uiso 1 1 calc R . .
C4 C 0.8686(3) -0.7146(3) 0.3181(2) 0.0182(4) Uani 1 1 d . . .
O1 O 1.5064(2) -0.66177(19) -0.07430(15) 0.0246(3) Uani 1 1 d . . .
C1 C 1.6608(3) -0.7514(3) -0.0745(2) 0.0188(4) Uani 1 1 d . . .
N1 N 0.5549(2) -0.5912(2) 0.31340(18) 0.0209(3) Uani 1 1 d . . .
H1A H 0.4818 -0.5188 0.2671 0.025 Uiso 1 1 calc R . .
C8 C 0.7525(3) -0.6027(3) 0.2456(2) 0.0194(4) Uani 1 1 d . . .
H8A H 0.8114 -0.5350 0.1494 0.023 Uiso 1 1 calc R . .
C7 C 0.4642(3) -0.6850(3) 0.4484(2) 0.0229(4) Uani 1 1 d . . .
H7A H 0.3235 -0.6746 0.4915 0.027 Uiso 1 1 calc R . .
H4B H 1.256(4) -0.668(4) 0.074(3) 0.039(8) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01341(18) 0.01847(19) 0.01705(18) -0.00119(13) -0.00443(13) 0.00295(13)
S1 0.0159(2) 0.0269(3) 0.0191(2) 0.00048(19) -0.00232(19) 0.00598(19)
S2 0.0156(2) 0.0262(3) 0.0193(2) 0.00093(19) -0.00361(19) 0.00459(19)
O3 0.0190(7) 0.0303(8) 0.0276(8) 0.0012(6) -0.0096(6) 0.0051(6)
O4 0.0162(7) 0.0331(9) 0.0189(7) -0.0002(6) -0.0026(6) 0.0050(6)
C2 0.0177(9) 0.0193(10) 0.0217(10) -0.0052(8) -0.0078(8) 0.0029(7)
C6 0.0224(10) 0.0276(11) 0.0189(10) -0.0004(8) -0.0029(8) 0.0003(8)
C3 0.0185(9) 0.0200(10) 0.0216(10) -0.0040(8) -0.0071(8) 0.0011(7)
O2 0.0236(7) 0.0296(8) 0.0209(7) 0.0004(6) -0.0073(6) 0.0057(6)
C5 0.0222(10) 0.0216(10) 0.0226(10) -0.0025(8) -0.0109(8) 0.0041(8)
C4 0.0174(9) 0.0166(9) 0.0201(9) -0.0034(7) -0.0062(8) 0.0013(7)
O1 0.0156(7) 0.0278(8) 0.0246(7) 0.0003(6) -0.0047(6) 0.0061(6)
C1 0.0162(9) 0.0185(9) 0.0213(10) -0.0033(7) -0.0066(8) 0.0008(7)
N1 0.0178(8) 0.0220(9) 0.0240(8) -0.0029(7) -0.0111(7) 0.0052(6)
C8 0.0195(9) 0.0193(9) 0.0190(9) -0.0030(7) -0.0070(8) 0.0007(7)
C7 0.0178(9) 0.0273(11) 0.0217(10) -0.0061(8) -0.0035(8) -0.0004(8)
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
S2 Ni1 S2 180.0 2_935 . ?
S2 Ni1 S1 92.526(18) 2_935 . ?
S2 Ni1 S1 87.475(18) . . ?
S2 Ni1 S1 87.474(18) 2_935 2_935 ?
S2 Ni1 S1 92.526(18) . 2_935 ?
S1 Ni1 S1 180.0 . 2_935 ?
C2 S1 Ni1 105.68(7) 2_935 . ?
C1 S2 Ni1 105.63(7) . . ?
O2 C2 C1 118.05(16) . . ?
O2 C2 S1 124.67(15) . 2_935 ?
C1 C2 S1 117.28(14) . 2_935 ?
C7 C6 C5 119.25(18) . . ?
O3 C3 O4 125.04(18) . . ?
O3 C3 C4 122.97(17) . . ?
O4 C3 C4 111.99(16) . . ?
C4 C5 C6 119.63(18) . . ?
C8 C4 C5 119.44(17) . . ?
C8 C4 C3 120.90(17) . . ?
C5 C4 C3 119.65(17) . . ?
O1 C1 C2 116.40(17) . . ?
O1 C1 S2 124.88(15) . . ?
C2 C1 S2 118.71(14) . . ?
C7 N1 C8 122.90(18) . . ?
N1 C8 C4 118.89(18) . . ?
N1 C7 C6 119.86(18) . . ?
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 S2 2.1739(5) 2_935 ?
Ni1 S2 2.1739(5) . ?
Ni1 S1 2.1769(5) . ?
Ni1 S1 2.1769(5) 2_935 ?
S1 C2 1.723(2) 2_935 ?
S2 C1 1.704(2) . ?
O3 C3 1.208(2) . ?
O4 C3 1.329(2) . ?
C2 O2 1.219(2) . ?
C2 C1 1.534(3) . ?
C2 S1 1.723(2) 2_935 ?
C6 C7 1.365(3) . ?
C6 C5 1.388(3) . ?
C3 C4 1.500(3) . ?
C5 C4 1.384(3) . ?
C4 C8 1.381(3) . ?
O1 C1 1.238(2) . ?
N1 C7 1.340(3) . ?
N1 C8 1.343(2) . ?
