#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:08:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179777 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/73/7007374.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_7007374
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            'C18 H16 N2 Ni O8 S4'
_chemical_formula_weight         575.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 90.063(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.0075(5)
_cell_length_b                   16.375(2)
_cell_length_c                   16.191(2)
_cell_measurement_reflns_used    1607
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1885
_cell_measurement_theta_min      2.424
_cell_volume                     1062.5(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'Bruker SMART Version 5.054 (Bruker, 1998)'
_computing_data_reduction        'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS SMART 1K CCD Diffractometer'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1795
_diffrn_reflns_av_sigmaI/netI    0.1235
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5547
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.251586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         1872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0455
_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)+(0.0357P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                1642
_reflns_number_total             1872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604319d.txt
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7007374
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_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 1.0000 0.5000 -0.5000 0.0156(2) Uani 1 2 d S . .
S2 S 1.25696(19) 0.44143(4) -0.60357(5) 0.0208(2) Uani 1 1 d . . .
S1 S 0.96703(18) 0.61521(4) -0.56651(5) 0.0181(2) Uani 1 1 d . . .
O2 O 1.5079(6) 0.50940(11) -0.73647(16) 0.0243(6) Uani 1 1 d . . .
C1 C 1.1838(7) 0.60182(16) -0.6564(2) 0.0168(7) Uani 1 1 d . . .
O1 O 1.2225(5) 0.65633(11) -0.70867(15) 0.0237(5) Uani 1 1 d . . .
O3 O 1.0158(6) 0.54375(11) -1.11458(16) 0.0283(6) Uani 1 1 d . . .
C2 C 1.3386(8) 0.51748(16) -0.6733(2) 0.0173(7) Uani 1 1 d . . .
N1 N 0.5961(6) 0.66214(14) -0.84711(18) 0.0224(6) Uani 1 1 d . . .
H1A H 0.5283 0.6568 -0.7957 0.027 Uiso 1 1 calc R . .
C5 C 0.8180(7) 0.67810(16) -1.0080(2) 0.0157(7) Uani 1 1 d . . .
C9 C 1.0651(8) 0.61278(16) -1.1382(2) 0.0185(7) Uani 1 1 d . . .
C8 C 0.9389(7) 0.68896(15) -1.0958(2) 0.0181(7) Uani 1 1 d . . .
H8A H 0.7532 0.7116 -1.1291 0.022 Uiso 1 1 calc R . .
H8B H 1.1205 0.7299 -1.0957 0.022 Uiso 1 1 calc R . .
C7 C 0.5203(8) 0.60447(16) -0.9027(2) 0.0210(7) Uani 1 1 d . . .
H7A H 0.3915 0.5586 -0.8862 0.025 Uiso 1 1 calc R . .
C4 C 0.8875(8) 0.73754(17) -0.9483(2) 0.0209(7) Uani 1 1 d . . .
H4A H 1.0134 0.7845 -0.9630 0.025 Uiso 1 1 calc R . .
C6 C 0.6256(8) 0.61058(16) -0.9832(2) 0.0185(7) Uani 1 1 d . . .
H6A H 0.5687 0.5693 -1.0220 0.022 Uiso 1 1 calc R . .
C3 C 0.7769(8) 0.72895(18) -0.8693(2) 0.0235(8) Uani 1 1 d . . .
H3A H 0.8262 0.7698 -0.8295 0.028 Uiso 1 1 calc R . .
O4 O 1.2388(6) 0.63049(13) -1.20563(17) 0.0290(6) Uani 1 1 d . . .
H4C H 1.308(11) 0.586(3) -1.232(3) 0.049(12) Uiso 1 1 d . . .
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
S1 Ni1 S1 180.000(17) 3_764 . ?
S1 Ni1 S2 88.33(3) 3_764 . ?
S1 Ni1 S2 91.67(3) . . ?
S1 Ni1 S2 91.67(3) 3_764 3_764 ?
S1 Ni1 S2 88.33(3) . 3_764 ?
S2 Ni1 S2 180.0 . 3_764 ?
C2 S2 Ni1 106.05(12) . . ?
C1 S1 Ni1 106.22(10) . . ?
O1 C1 C2 118.3(3) . . ?
O1 C1 S1 123.5(2) . . ?
C2 C1 S1 118.1(2) . . ?
O2 C2 C1 117.7(3) . . ?
O2 C2 S2 125.0(2) . . ?
C1 C2 S2 117.3(3) . . ?
C7 N1 C3 120.7(3) . . ?
C4 C5 C6 117.3(3) . . ?
C4 C5 C8 120.3(3) . . ?
C6 C5 C8 122.4(3) . . ?
O3 C9 O4 123.3(3) . . ?
O3 C9 C8 125.0(3) . . ?
O4 C9 C8 111.7(2) . . ?
C9 C8 C5 115.9(2) . . ?
N1 C7 C6 121.1(3) . . ?
C3 C4 C5 120.8(3) . . ?
C7 C6 C5 119.8(3) . . ?
N1 C3 C4 120.3(3) . . ?
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 S1 2.1762(7) 3_764 ?
Ni1 S1 2.1762(7) . ?
Ni1 S2 2.1900(9) . ?
Ni1 S2 2.1900(9) 3_764 ?
S2 C2 1.712(3) . ?
S1 C1 1.710(4) . ?
O2 C2 1.235(4) . ?
C1 O1 1.240(4) . ?
C1 C2 1.538(4) . ?
O3 C9 1.209(3) . ?
N1 C7 1.339(4) . ?
N1 C3 1.361(4) . ?
C5 C4 1.400(4) . ?
C5 C6 1.407(4) . ?
C5 C8 1.513(5) . ?
C9 O4 1.328(4) . ?
C9 C8 1.511(4) . ?
C7 C6 1.375(5) . ?
C4 C3 1.361(5) . ?
