#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:08:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179777 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/73/7007368.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_7007368
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 H24 N2 Ni O8 S4'
_chemical_formula_weight         559.32
_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                92.959(2)
_cell_angle_beta                 104.109(2)
_cell_angle_gamma                103.856(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5505(10)
_cell_length_b                   7.9751(10)
_cell_length_c                   9.9141(13)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.099
_cell_volume                     558.28(13)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5846
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.825075
_exptl_absorpt_correction_T_min  0.650585
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             290
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.254
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0263
_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)+(0.0461P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                2319
_reflns_number_total             2533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604319d.txt
_cod_data_source_block           4kellya
_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               7007368
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 0.5000 0.0000 0.0000 0.01782(10) Uani 1 2 d S . .
S2 S 0.26645(5) 0.07370(5) 0.05660(4) 0.02309(11) Uani 1 1 d . . .
S1 S 0.48332(6) -0.18899(5) 0.15010(5) 0.02834(12) Uani 1 1 d . . .
O2 O 0.3140(2) 0.41093(18) -0.21292(15) 0.0423(3) Uani 1 1 d . . .
O1 O 0.11473(16) 0.32651(15) -0.02441(12) 0.0271(3) Uani 1 1 d . . .
C1 C 0.3470(2) 0.2965(2) -0.14070(17) 0.0251(3) Uani 1 1 d . . .
C2 C 0.2289(2) 0.24436(19) -0.03551(16) 0.0207(3) Uani 1 1 d . . .
O3 O -0.50428(16) 0.79075(16) -0.46376(14) 0.0306(3) Uani 1 1 d . . .
O4 O -0.26181(17) 1.01934(15) -0.45276(14) 0.0324(3) Uani 1 1 d . . .
N1 N 0.05126(18) 0.60096(17) -0.20019(14) 0.0219(3) Uani 1 1 d . . .
C8 C -0.3292(2) 0.8601(2) -0.44248(16) 0.0229(3) Uani 1 1 d . . .
C4 C 0.0015(2) 0.85512(19) -0.32007(17) 0.0229(3) Uani 1 1 d . . .
H4A H 0.0555 0.9443 -0.3752 0.027 Uiso 1 1 calc R . .
H4B H -0.0123 0.9158 -0.2351 0.027 Uiso 1 1 calc R . .
C3 C 0.1352(2) 0.7406(2) -0.27760(17) 0.0235(3) Uani 1 1 d . . .
H3A H 0.1585 0.6878 -0.3621 0.028 Uiso 1 1 calc R . .
H3B H 0.2579 0.8117 -0.2174 0.028 Uiso 1 1 calc R . .
C5 C -0.1936(2) 0.74723(19) -0.40771(15) 0.0214(3) Uani 1 1 d . . .
H5A H -0.1776 0.6995 -0.4979 0.026 Uiso 1 1 calc R . .
C7 C -0.1308(2) 0.48699(19) -0.28991(18) 0.0261(3) Uani 1 1 d . . .
H7A H -0.1822 0.3937 -0.2370 0.031 Uiso 1 1 calc R . .
H7B H -0.1082 0.4318 -0.3737 0.031 Uiso 1 1 calc R . .
C6 C -0.2726(2) 0.59295(19) -0.33482(17) 0.0242(3) Uani 1 1 d . . .
H6A H -0.3061 0.6363 -0.2515 0.029 Uiso 1 1 calc R . .
H6B H -0.3893 0.5175 -0.3994 0.029 Uiso 1 1 calc R . .
H1A H 0.029(3) 0.649(2) -0.122(2) 0.032(5) Uiso 1 1 d . . .
H1B H 0.132(3) 0.523(3) -0.182(3) 0.065(8) Uiso 1 1 d . . .
H4C H -0.346(5) 1.082(5) -0.477(4) 0.024(9) Uiso 0.50 1 d P . .
H3C H -0.558(5) 0.852(4) -0.491(4) 0.010(8) Uiso 0.50 1 d P . .
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_655 . ?
S2 Ni1 S1 92.522(15) 2_655 . ?
S2 Ni1 S1 87.479(15) . . ?
S2 Ni1 S1 87.478(15) 2_655 2_655 ?
S2 Ni1 S1 92.521(15) . 2_655 ?
S1 Ni1 S1 180.0 . 2_655 ?
C2 S2 Ni1 106.13(5) . . ?
C1 S1 Ni1 105.81(6) 2_655 . ?
O2 C1 C2 118.16(14) . . ?
O2 C1 S1 123.95(13) . 2_655 ?
C2 C1 S1 117.89(11) . 2_655 ?
O1 C2 C1 117.69(13) . . ?
O1 C2 S2 124.84(12) . . ?
C1 C2 S2 117.47(11) . . ?
C3 N1 C7 111.11(12) . . ?
O3 C8 O4 123.22(14) . . ?
O3 C8 C5 118.58(14) . . ?
O4 C8 C5 118.17(14) . . ?
C3 C4 C5 111.08(12) . . ?
N1 C3 C4 109.85(12) . . ?
C8 C5 C6 111.47(13) . . ?
C8 C5 C4 110.83(12) . . ?
C6 C5 C4 111.53(12) . . ?
N1 C7 C6 110.19(12) . . ?
C7 C6 C5 111.60(13) . . ?
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 2.1714(4) 2_655 ?
Ni1 S2 2.1714(4) . ?
Ni1 S1 2.1758(4) . ?
Ni1 S1 2.1758(4) 2_655 ?
S2 C2 1.7186(15) . ?
S1 C1 1.7205(16) 2_655 ?
O2 C1 1.224(2) . ?
O1 C2 1.2222(18) . ?
C1 C2 1.542(2) . ?
C1 S1 1.7205(16) 2_655 ?
O3 C8 1.2651(19) . ?
O4 C8 1.2691(19) . ?
N1 C3 1.4891(19) . ?
N1 C7 1.4930(19) . ?
C8 C5 1.509(2) . ?
C4 C3 1.518(2) . ?
C4 C5 1.536(2) . ?
C5 C6 1.530(2) . ?
C7 C6 1.516(2) . ?
