#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/22/8102232.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_8102232
loop_
_publ_author_name
'Martin Köckerling'
'Gerald Henkel'
_publ_section_title
;
 Crystal structure of bis(tetraphenylphosphonium)
 tetrakis(ethane-1,2-dithiolato)trinickelate(II) ethane-1,2-dithiole
 solvate, [(C6H5)4P]2[Ni3(SCH2CH2S)4)] · 2HSC2H4SH
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              102
_journal_volume                  223
_journal_year                    2008
_chemical_formula_structural
'[(C6H5)4P]2[Ni3(SCH2CH2S)4)] &#x00B7; 2HSC2H4SH'
_chemical_formula_sum            'C60 H68 Ni3 P2 S12'
_chemical_formula_weight         1411.99
_chemical_name_systematic
;
bis(tetraphenylphosphonium) tetrakis(ethane-1,2-dithiolato)trinickelate(II)
ethane-1,2-dithiole solvate
;
_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
_cell_angle_alpha                113.27(2)
_cell_angle_beta                 102.75(2)
_cell_angle_gamma                104.52(2)
_cell_formula_units_Z            1
_cell_length_a                   9.671(3)
_cell_length_b                   14.086(4)
_cell_length_c                   14.091(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      4.0
_cell_volume                     1592.9(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7193
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 99
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.150
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0441
_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)+(0.0931P)²+0.4901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                5868
_reflns_number_total             6779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2174.cff
_cod_data_source_block           Ni3edt4_2(H2edt)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (7
times).

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (40
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (13
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (64 times).

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        1592.9(8)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8102232
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.5000 0.01368(12) Uani 1 1 f d S . .
Ni2 Ni 0.43974(3) 0.07223(3) 0.33758(2) 0.01379(11) Uani 1 2 i d . . .
S1 S 0.37102(7) 0.10412(5) 0.48096(5) 0.01575(14) Uani 1 2 i d . . .
S2 S 0.20851(8) 0.02343(6) 0.22703(5) 0.02102(16) Uani 1 2 i d . . .
S3 S 0.65522(7) 0.09689(5) 0.44925(5) 0.01636(15) Uani 1 2 i d . . .
S4 S 0.52087(7) 0.03675(6) 0.19969(5) 0.01975(15) Uani 1 2 i d . . .
C1 C 0.1646(3) 0.0218(2) 0.4122(2) 0.0201(5) Uani 1 2 i d . . .
H1A H 0.1455 -0.0573 0.3795 0.024 Uiso 1 2 i calc R . .
H1B H 0.1135 0.0392 0.4651 0.024 Uiso 1 2 i calc R . .
C2 C 0.1061(3) 0.0516(2) 0.3232(2) 0.0222(6) Uani 1 2 i d . . .
H2A H 0.1209 0.1300 0.3570 0.027 Uiso 1 2 i calc R . .
H2B H -0.0026 0.0081 0.2833 0.027 Uiso 1 2 i calc R . .
C3 C 0.7248(3) 0.0108(3) 0.3498(2) 0.0228(6) Uani 1 2 i d . . .
H3A H 0.8297 0.0223 0.3863 0.027 Uiso 1 2 i calc R . .
H3B H 0.6619 -0.0676 0.3174 0.027 Uiso 1 2 i calc R . .
C4 C 0.7151(3) 0.0469(2) 0.2612(2) 0.0210(5) Uani 1 2 i d . . .
H4A H 0.7443 0.0000 0.2039 0.025 Uiso 1 2 i calc R . .
H4B H 0.7860 0.1233 0.2934 0.025 Uiso 1 2 i calc R . .
S5 S 0.90973(9) 0.38097(6) 0.50303(6) 0.02909(18) Uani 1 2 i d . . .
S6 S 0.43461(10) 0.35710(7) 0.36742(7) 0.0344(2) Uani 1 2 i d . . .
C29 C 0.7319(3) 0.3624(3) 0.4077(2) 0.0277(6) Uani 1 2 i d . . .
H29A H 0.7527 0.4169 0.3818 0.033 Uiso 1 2 i calc R . .
H29B H 0.6913 0.2888 0.3440 0.033 Uiso 1 2 i calc R . .
C30 C 0.6132(4) 0.3752(3) 0.4610(2) 0.0289(6) Uani 1 2 i d . . .
H30A H 0.6542 0.4489 0.5248 0.035 Uiso 1 2 i calc R . .
H30B H 0.5928 0.3208 0.4870 0.035 Uiso 1 2 i calc R . .
HS5 H 0.868(5) 0.298(3) 0.509(3) 0.050(12) Uiso 1 2 i d . . .
HS6 H 0.400(6) 0.261(4) 0.326(4) 0.071(15) Uiso 1 2 i d . . .
P P 0.31440(7) 0.63806(5) 0.94011(5) 0.01590(15) Uani 1 2 i d . . .
C5 C 0.1930(3) 0.6970(2) 0.8875(2) 0.0179(5) Uani 1 2 i d . . .
C6 C 0.0686(3) 0.6300(2) 0.7869(2) 0.0211(5) Uani 1 2 i d . . .
H6A H 0.0513 0.5552 0.7449 0.025 Uiso 1 2 i calc R . .
C7 C -0.0282(3) 0.6762(3) 0.7505(2) 0.0262(6) Uani 1 2 i d . . .
H7A H -0.1103 0.6322 0.6835 0.031 Uiso 1 2 i calc R . .
C8 C -0.0035(4) 0.7871(3) 0.8131(3) 0.0263(6) Uani 1 2 i d . . .
H8A H -0.0713 0.8168 0.7897 0.032 Uiso 1 2 i calc R . .
C9 C 0.1218(4) 0.8541(3) 0.9103(3) 0.0300(7) Uani 1 2 i d . . .
H9A H 0.1397 0.9294 0.9506 0.036 Uiso 1 2 i calc R . .
C10 C 0.2214(4) 0.8102(2) 0.9484(2) 0.0276(6) Uani 1 2 i d . . .
H10A H 0.3059 0.8557 1.0137 0.033 Uiso 1 2 i calc R . .
C11 C 0.2733(3) 0.5015(2) 0.8313(2) 0.0194(5) Uani 1 2 i d . . .
C12 C 0.1341(3) 0.4143(2) 0.7973(2) 0.0236(6) Uani 1 2 i d . . .
H12A H 0.0679 0.4250 0.8358 0.028 Uiso 1 2 i calc R . .
C13 C 0.0957(4) 0.3120(3) 0.7059(3) 0.0349(7) Uani 1 2 i d . . .
H13A H 0.0024 0.2546 0.6817 0.042 Uiso 1 2 i calc R . .
C14 C 0.1964(4) 0.2957(3) 0.6508(3) 0.0406(8) Uani 1 2 i d . . .
H14A H 0.1717 0.2263 0.5912 0.049 Uiso 1 2 i calc R . .
C15 C 0.3330(4) 0.3808(3) 0.6831(3) 0.0421(9) Uani 1 2 i d . . .
H15A H 0.3987 0.3692 0.6443 0.050 Uiso 1 2 i calc R . .
C16 C 0.3726(4) 0.4850(2) 0.7747(2) 0.0281(6) Uani 1 2 i d . . .
H16A H 0.4650 0.5426 0.7973 0.034 Uiso 1 2 i calc R . .
C17 C 0.5111(3) 0.7222(2) 0.9815(2) 0.0173(5) Uani 1 2 i d . . .
C18 C 0.6226(3) 0.7214(2) 1.0637(2) 0.0236(6) Uani 1 2 i d . . .
H18A H 0.5940 0.6839 1.1020 0.028 Uiso 1 2 i calc R . .
C19 C 0.7762(3) 0.7774(2) 1.0870(3) 0.0277(6) Uani 1 2 i d . . .
H19A H 0.8512 0.7784 1.1420 0.033 Uiso 1 2 i calc R . .
C20 C 0.8178(3) 0.8319(2) 1.0281(3) 0.0279(6) Uani 1 2 i d . . .
H20A H 0.9208 0.8681 1.0432 0.034 Uiso 1 2 i calc R . .
C21 C 0.7078(4) 0.8328(3) 0.9476(2) 0.0286(6) Uani 1 2 i d . . .
H21A H 0.7367 0.8698 0.9089 0.034 Uiso 1 2 i calc R . .
C22 C 0.5537(3) 0.7783(2) 0.9245(2) 0.0240(6) Uani 1 2 i d . . .
H22A H 0.4793 0.7794 0.8709 0.029 Uiso 1 2 i calc R . .
C23 C 0.2845(3) 0.6295(2) 1.0588(2) 0.0209(5) Uani 1 2 i d . . .
C24 C 0.2909(4) 0.7257(3) 1.1456(2) 0.0309(7) Uani 1 2 i d . . .
H24A H 0.3040 0.7906 1.1397 0.037 Uiso 1 2 i calc R . .
C25 C 0.2775(4) 0.7234(3) 1.2413(3) 0.0392(8) Uani 1 2 i d . . .
H25A H 0.2825 0.7872 1.2998 0.047 Uiso 1 2 i calc R . .
C26 C 0.2569(4) 0.6262(4) 1.2494(3) 0.0410(9) Uani 1 2 i d . . .
H26A H 0.2468 0.6249 1.3130 0.049 Uiso 1 2 i calc R . .
C27 C 0.2511(4) 0.5319(3) 1.1642(3) 0.0393(8) Uani 1 2 i d . . .
H27A H 0.2373 0.4672 1.1705 0.047 Uiso 1 2 i calc R . .
C28 C 0.2657(4) 0.5324(3) 1.0680(3) 0.0288(6) Uani 1 2 i d . . .
H28A H 0.2629 0.4687 1.0107 0.035 Uiso 1 2 i 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'
P P 0.1023 0.0942 '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
S3 Ni1 S3 180.00 . 2_656 y
S3 Ni1 S1 82.34(3) . . y
S3 Ni1 S1 97.66(3) 2_656 . y
S3 Ni1 S1 97.66(3) . 2_656 y
S3 Ni1 S1 82.34(3) 2_656 2_656 y
S1 Ni1 S1 180.00 . 2_656 y
S3 Ni1 Ni2 131.35(3) . 2_656 n
S3 Ni1 Ni2 48.65(3) 2_656 2_656 n
S1 Ni1 Ni2 131.04(2) . 2_656 n
S1 Ni1 Ni2 48.96(2) 2_656 2_656 n
S3 Ni1 Ni2 48.65(3) . . n
S3 Ni1 Ni2 131.35(3) 2_656 . n
S1 Ni1 Ni2 48.96(2) . . n
S1 Ni1 Ni2 131.04(2) 2_656 . n
Ni2 Ni1 Ni2 180.0 2_656 . y
S3 Ni2 S4 92.49(4) . . y
S3 Ni2 S2 170.93(3) . . y
S4 Ni2 S2 90.65(4) . . y
S3 Ni2 S1 83.70(4) . . y
S4 Ni2 S1 175.84(3) . . y
S2 Ni2 S1 92.89(4) . . y
S3 Ni2 Ni1 49.68(2) . . n
S4 Ni2 Ni1 126.30(3) . . n
S2 Ni2 Ni1 122.18(3) . . n
S1 Ni2 Ni1 49.71(2) . . n
C1 S1 Ni2 100.43(10) . . n
C1 S1 Ni1 111.36(9) . . n
Ni2 S1 Ni1 81.33(3) . . n
C2 S2 Ni2 101.93(9) . . n
C3 S3 Ni2 100.25(10) . . n
C3 S3 Ni1 112.82(10) . . n
Ni2 S3 Ni1 81.68(3) . . n
C4 S4 Ni2 102.50(9) . . n
C2 C1 S1 107.09(19) . . n
C1 C2 S2 109.96(19) . . n
C4 C3 S3 106.63(19) . . n
C3 C4 S4 110.88(19) . . n
C30 C29 S5 112.2(2) . . n
C29 C30 S6 113.0(2) . . n
C17 P C5 110.27(13) . . n
C17 P C11 108.89(13) . . n
C5 P C11 108.10(13) . . n
C17 P C23 108.00(13) . . n
C5 P C23 111.31(13) . . n
C11 P C23 110.25(13) . . n
C10 C5 C6 119.9(3) . . n
C10 C5 P 119.5(2) . . n
C6 C5 P 120.6(2) . . n
C7 C6 C5 119.6(3) . . n
C8 C7 C6 120.4(3) . . n
C9 C8 C7 120.2(3) . . n
C8 C9 C10 120.7(3) . . n
C9 C10 C5 119.2(3) . . n
C16 C11 C12 120.1(3) . . n
C16 C11 P 119.8(2) . . n
C12 C11 P 119.9(2) . . n
C13 C12 C11 119.7(3) . . n
C14 C13 C12 119.8(3) . . n
C15 C14 C13 121.0(3) . . n
C14 C15 C16 119.8(3) . . n
C11 C16 C15 119.5(3) . . n
C22 C17 C18 120.5(3) . . n
C22 C17 P 119.8(2) . . n
C18 C17 P 119.4(2) . . n
C19 C18 C17 119.0(3) . . n
C18 C19 C20 120.0(3) . . n
C21 C20 C19 120.7(3) . . n
C20 C21 C22 119.8(3) . . n
C17 C22 C21 120.0(3) . . n
C28 C23 C24 120.3(3) . . n
C28 C23 P 121.5(2) . . n
C24 C23 P 118.0(2) . . n
C25 C24 C23 119.2(3) . . n
C26 C25 C24 120.2(3) . . n
C27 C26 C25 120.5(3) . . n
C26 C27 C28 120.4(3) . . n
C23 C28 C27 119.3(3) . . n
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 2.2044(8) . y
Ni1 S3 2.2012(8) . y
Ni2 S1 2.1795(9) . y
Ni2 S2 2.1784(11) . y
Ni2 S3 2.1673(10) . y
Ni2 S4 2.1779(9) . y
Ni1 Ni2 2.8567(8) . y
Ni1 S1 2.2044(8) 2_656 n
Ni1 S3 2.2012(8) 2_656 n
Ni1 Ni2 2.8567(8) 2_656 n
S1 C1 1.834(3) . n
S2 C2 1.827(3) . n
S3 C3 1.835(3) . n
S4 C4 1.830(3) . n
C1 C2 1.514(4) . n
C3 C4 1.517(4) . n
S5 C29 1.819(3) . n
S6 C30 1.815(3) . n
C29 C30 1.513(4) . n
P C17 1.788(3) . n
P C5 1.791(3) . n
P C11 1.796(3) . n
P C23 1.803(3) . n
C5 C10 1.397(4) . n
C5 C6 1.403(4) . n
C6 C7 1.386(4) . n
C7 C8 1.381(4) . n
C8 C9 1.381(5) . n
C9 C10 1.389(4) . n
C11 C16 1.385(4) . n
C11 C12 1.404(4) . n
C12 C13 1.388(4) . n
C13 C14 1.381(5) . n
C14 C15 1.378(5) . n
C15 C16 1.404(4) . n
C17 C22 1.386(4) . n
C17 C18 1.404(4) . n
C18 C19 1.389(4) . n
C19 C20 1.392(4) . n
C20 C21 1.379(4) . n
C21 C22 1.389(4) . n
C23 C28 1.394(4) . n
C23 C24 1.397(4) . n
C24 C25 1.394(5) . n
C25 C26 1.387(6) . n
C26 C27 1.371(6) . n
C27 C28 1.395(5) . n
