#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:38:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179416 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/13/4331343.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_4331343
loop_
_publ_author_name
'Jason A. Cody'
'Kenneth B. Finch'
'Gilbert J. Reynders'
'Grant C. B. Alexander'
'Hyung G. Lim'
'Christian Näther'
'Wolfgang Bensch'
_publ_section_title
;
 Ionothermal Synthesis of Four New Nickel Thiophosphate Anions:
 [Ni(P2S8)2]2-, [Ni(P3S9)(P2S8)]3-, [Ni(P3S9)2]4-, and [(NiP3S8)4(PS4)]7-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13357
_journal_page_last               13362
_journal_paper_doi               10.1021/ic302112g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C24 H44 N8 Ni P6 S18'
_chemical_formula_weight         1266.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.397(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.0276(14)
_cell_length_b                   12.2186(7)
_cell_length_c                   22.3472(12)
_cell_measurement_temperature    173(2)
_cell_volume                     5240.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14699
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_T_max  0.8698
_exptl_absorpt_correction_T_min  0.7512
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-red and X-shape (STOE&CIE)'
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5643
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0380
_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)+(0.0596P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                4465
_reflns_number_total             5643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302112g_si_001_4.cif
_cod_data_source_block           3_Ni(P3S9)2
_cod_original_cell_volume        5240.2(5)
_cod_database_code               4331343
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.5000 1.0000 0.5000 0.01577(11) Uani 1 2 d S . .
P1 P 0.30881(3) 0.95789(5) 0.37058(3) 0.02022(15) Uani 1 1 d . . .
P2 P 0.38996(4) 0.75947(5) 0.49509(4) 0.02094(15) Uani 1 1 d . . .
P3 P 0.42758(3) 0.77888(5) 0.36304(3) 0.01839(14) Uani 1 1 d . . .
S1 S 0.38162(3) 1.06898(5) 0.42427(3) 0.02228(15) Uani 1 1 d . . .
S2 S 0.21544(4) 1.01386(6) 0.30730(4) 0.03319(19) Uani 1 1 d . . .
S3 S 0.29500(3) 0.84508(5) 0.43450(4) 0.02503(15) Uani 1 1 d . . .
S4 S 0.33185(3) 0.86286(6) 0.30478(3) 0.02424(15) Uani 1 1 d . . .
S5 S 0.36418(5) 0.64594(6) 0.54041(4) 0.03701(19) Uani 1 1 d . . .
S6 S 0.46790(4) 0.85751(5) 0.55540(3) 0.02460(15) Uani 1 1 d . . .
S7 S 0.40843(4) 0.66952(5) 0.42482(4) 0.02317(15) Uani 1 1 d . . .
S8 S 0.43433(4) 0.68536(6) 0.29567(4) 0.03049(17) Uani 1 1 d . . .
S9 S 0.50685(3) 0.88018(5) 0.41652(3) 0.01920(14) Uani 1 1 d . . .
N1 N 0.76114(15) 0.1317(2) 0.90163(14) 0.0373(6) Uani 1 1 d . . .
C1 C 0.72226(16) 0.2214(2) 0.87884(16) 0.0321(7) Uani 1 1 d . . .
H1 H 0.7243 0.2735 0.8484 0.038 Uiso 1 1 calc R . .
N2 N 0.68048(14) 0.2265(2) 0.90518(13) 0.0339(6) Uani 1 1 d . . .
C2 C 0.69228(19) 0.1361(3) 0.9463(2) 0.0524(10) Uani 1 1 d . . .
H2 H 0.6689 0.1184 0.9712 0.063 Uiso 1 1 calc R . .
C3 C 0.7432(2) 0.0775(3) 0.9445(2) 0.0516(10) Uani 1 1 d . . .
H3 H 0.7629 0.0112 0.9684 0.062 Uiso 1 1 calc R . .
C4 C 0.62857(18) 0.3128(3) 0.89089(18) 0.0432(8) Uani 1 1 d . . .
H4A H 0.6041 0.2980 0.9167 0.065 Uiso 1 1 calc R . .
H4B H 0.5950 0.3141 0.8416 0.065 Uiso 1 1 calc R . .
H4C H 0.6521 0.3839 0.9049 0.065 Uiso 1 1 calc R . .
C5 C 0.8154(2) 0.0985(3) 0.8849(2) 0.0515(10) Uani 1 1 d . . .
H5A H 0.8090 0.1399 0.8441 0.062 Uiso 1 1 calc R . .
H5B H 0.8097 0.0198 0.8730 0.062 Uiso 1 1 calc R . .
C6 C 0.88805(19) 0.1180(3) 0.9432(2) 0.0424(8) Uani 1 1 d . . .
H6A H 0.9220 0.0951 0.9294 0.064 Uiso 1 1 calc R . .
H6B H 0.8952 0.0757 0.9834 0.064 Uiso 1 1 calc R . .
H6C H 0.8942 0.1961 0.9548 0.064 Uiso 1 1 calc R . .
N11 N 0.5623(5) 0.9747(9) 0.7737(7) 0.029(2) Uani 0.50 1 d PD . 1
C11 C 0.5937(3) 0.9355(4) 0.7397(3) 0.0285(12) Uani 0.50 1 d PD . 1
H11A H 0.5822 0.9570 0.6945 0.034 Uiso 0.50 1 d PR . 1
N12 N 0.6431(3) 0.8640(4) 0.7774(3) 0.0354(12) Uani 0.50 1 d PD A 1
C12 C 0.6481(4) 0.8582(7) 0.8402(4) 0.051(2) Uani 0.50 1 d PD A 1
H12A H 0.6786 0.8125 0.8772 0.061 Uiso 0.50 1 d PR A 1
C13 C 0.6008(4) 0.9273(6) 0.8407(4) 0.0482(18) Uani 0.50 1 d PD . 1
H13A H 0.5943 0.9438 0.8787 0.058 Uiso 0.50 1 d PR . 1
C14 C 0.6868(5) 0.8028(7) 0.7566(5) 0.053(2) Uani 0.50 1 d PD A 1
H14A H 0.6736 0.8206 0.7091 0.080 Uiso 0.50 1 d PR A 1
H14B H 0.7356 0.8231 0.7869 0.080 Uiso 0.50 1 d PR A 1
H14C H 0.6810 0.7241 0.7606 0.080 Uiso 0.50 1 d PR A 1
C15 C 0.5000 1.0566(4) 0.7500 0.0537(16) Uani 1 2 d SD . 1
H15A H 0.5008 1.1084 0.7163 0.064 Uiso 1 1 d R . 1
C16 C 0.4330(8) 1.0030(11) 0.7193(11) 0.047(4) Uani 0.50 1 d PD . 1
H16A H 0.3962 1.0581 0.7057 0.071 Uiso 0.50 1 d PR . 1
H16B H 0.4258 0.9618 0.6787 0.071 Uiso 0.50 1 d PR . 1
H16C H 0.4315 0.9528 0.7527 0.071 Uiso 0.50 1 d PR . 1
N11' N 0.5698(3) 0.6553(5) 0.7603(3) 0.0302(12) Uani 0.50 1 d PD . 2
C11' C 0.6236(3) 0.7145(4) 0.8050(3) 0.0283(12) Uani 0.50 1 d PD B 2
H11B H 0.6436 0.7132 0.8536 0.034 Uiso 0.50 1 d PR B 2
N12' N 0.6453(3) 0.7754(4) 0.7698(3) 0.0315(11) Uani 0.50 1 d PD B 2
C12' C 0.6045(4) 0.7552(7) 0.7018(3) 0.0474(18) Uani 0.50 1 d PD B 2
H12B H 0.6099 0.7865 0.6658 0.057 Uiso 0.50 1 d PR B 2
C13' C 0.5563(4) 0.6808(7) 0.6946(4) 0.053(2) Uani 0.50 1 d PD . 2
H13B H 0.5196 0.6526 0.6529 0.064 Uiso 0.50 1 d PR . 2
C14' C 0.7036(3) 0.8527(5) 0.8003(4) 0.0394(16) Uani 0.50 1 d PD B 2
H14D H 0.7239 0.8526 0.8504 0.059 Uiso 0.50 1 d PR B 2
H14E H 0.7390 0.8295 0.7884 0.059 Uiso 0.50 1 d PR B 2
H14F H 0.6876 0.9266 0.7827 0.059 Uiso 0.50 1 d PR B 2
C15' C 0.5287(4) 0.5771(5) 0.7776(4) 0.0386(15) Uani 0.50 1 d PD . 2
H15C H 0.5579 0.5478 0.8246 0.046 Uiso 0.50 1 d PR . 2
H15D H 0.5142 0.5151 0.7450 0.046 Uiso 0.50 1 d PR . 2
C16' C 0.4658(5) 0.6297(7) 0.7729(6) 0.057(2) Uani 0.50 1 d PD . 2
H16D H 0.4392 0.5764 0.7836 0.086 Uiso 0.50 1 d PR . 2
H16E H 0.4802 0.6904 0.8057 0.086 Uiso 0.50 1 d PR . 2
H16F H 0.4366 0.6578 0.7263 0.086 Uiso 0.50 1 d PR . 2
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'
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
S9 Ni1 S9 180.0 . 5_676
S9 Ni1 S6 84.12(2) . 5_676
S9 Ni1 S6 95.88(2) 5_676 5_676
S9 Ni1 S6 95.88(2) . .
S9 Ni1 S6 84.12(2) 5_676 .
S6 Ni1 S6 180.00(2) 5_676 .
S9 Ni1 S1 82.96(2) . 5_676
S9 Ni1 S1 97.04(2) 5_676 5_676
S6 Ni1 S1 96.93(2) 5_676 5_676
S6 Ni1 S1 83.07(2) . 5_676
S9 Ni1 S1 97.04(2) . .
S9 Ni1 S1 82.96(2) 5_676 .
S6 Ni1 S1 83.07(2) 5_676 .
S6 Ni1 S1 96.93(2) . .
S1 Ni1 S1 180.0 5_676 .
S2 P1 S1 116.51(4) . .
S2 P1 S3 105.49(4) . .
S1 P1 S3 112.22(4) . .
S2 P1 S4 102.37(4) . .
S1 P1 S4 113.25(4) . .
S3 P1 S4 105.93(4) . .
S5 P2 S6 116.79(5) . .
S5 P2 S7 103.08(4) . .
S6 P2 S7 113.65(4) . .
S5 P2 S3 103.49(5) . .
S6 P2 S3 112.87(4) . .
S7 P2 S3 105.70(4) . .
S8 P3 S9 116.77(4) . .
S8 P3 S7 104.45(4) . .
S9 P3 S7 113.57(4) . .
S8 P3 S4 103.81(4) . .
S9 P3 S4 112.49(4) . .
S7 P3 S4 104.50(4) . .
P1 S1 Ni1 116.72(3) . .
P1 S3 P2 109.18(4) . .
P3 S4 P1 110.08(4) . .
P2 S6 Ni1 117.22(4) . .
P3 S7 P2 109.30(4) . .
P3 S9 Ni1 117.91(4) . .
C1 N1 C3 108.2(3) . .
C1 N1 C5 125.5(3) . .
C3 N1 C5 126.3(3) . .
N2 C1 N1 109.2(3) . .
C1 N2 C2 108.4(3) . .
C1 N2 C4 125.3(3) . .
C2 N2 C4 126.3(3) . .
C3 C2 N2 107.1(3) . .
C2 C3 N1 107.1(3) . .
N1 C5 C6 112.7(3) . .
C16 N11 C11 117(5) 2_656 .
C16 N11 C13 92(5) 2_656 .
C11 N11 C13 104.0(7) . .
C16 N11 C15 64(4) 2_656 .
C11 N11 C15 130.2(10) . .
C13 N11 C15 125.8(9) . .
N12 C11 N11 111.3(7) . .
N12 C11 C16 113.9(9) . 2_656
C11 N12 C12 108.6(5) . .
C11 N12 C14 126.6(6) . .
C12 N12 C14 124.8(6) . .
C13 C12 N12 107.8(6) . .
C12 C13 N11 108.0(7) . .
C12 C13 C16 115.4(10) . 2_656
C16 C15 C16 126.1(12) . 2_656
C16 C15 N11 113.1(5) 2_656 2_656
C16 C15 N11 113.1(5) . .
N11 C15 N11 100.6(9) 2_656 .
N11 C16 C15 102(4) 2_656 .
N11 C16 C13 74(5) 2_656 2_656
C15 C16 C13 130.6(16) . 2_656
N11 C16 C11 51(5) 2_656 2_656
C15 C16 C11 123.8(14) . 2_656
C13 C16 C11 92.0(9) 2_656 2_656
C16' N11' C11' 167.9(10) 2_656 .
C16' N11' C13' 61.3(8) 2_656 .
C11' N11' C13' 108.9(6) . .
C16' N11' C15' 64.2(9) 2_656 .
C11' N11' C15' 125.8(5) . .
C13' N11' C15' 125.3(6) . .
N11' C11' N12' 107.8(5) . .
C11' N12' C12' 109.1(5) . .
C11' N12' C14' 124.8(6) . .
C12' N12' C14' 126.0(6) . .
C13' C12' N12' 107.9(6) . .
C16' C13' C12' 142.5(9) 2_656 .
C12' C13' N11' 106.2(6) . .
C15' C15' C16' 68.9(7) 2_656 2_656
C15' C15' C16' 58.5(7) 2_656 .
C16' C15' C16' 101.4(7) 2_656 .
C15' C15' N11' 101.0(7) 2_656 .
C16' C15' N11' 111.7(5) . .
N11' C16' C13' 82.1(9) 2_656 2_656
N11' C16' C15' 82.2(11) 2_656 2_656
C13' C16' C15' 163.5(11) 2_656 2_656
N11' C16' C15' 131.6(13) 2_656 .
C13' C16' C15' 143.9(11) 2_656 .
C15' C16' C15' 52.6(6) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S9 2.4337(6) .
Ni1 S9 2.4337(6) 5_676
Ni1 S6 2.4338(7) 5_676
Ni1 S6 2.4338(7) .
Ni1 S1 2.4579(7) 5_676
Ni1 S1 2.4579(7) .
P1 S2 1.9603(9) .
P1 S1 1.9914(9) .
P1 S3 2.1118(10) .
P1 S4 2.1214(10) .
P2 S5 1.9587(10) .
P2 S6 1.9818(9) .
P2 S7 2.1134(10) .
P2 S3 2.1266(10) .
P3 S8 1.9531(9) .
P3 S9 1.9901(9) .
P3 S7 2.1074(10) .
P3 S4 2.1212(9) .
N1 C1 1.328(4) .
N1 C3 1.374(5) .
N1 C5 1.473(5) .
C1 N2 1.315(4) .
N2 C2 1.378(4) .
N2 C4 1.471(4) .
C2 C3 1.347(6) .
C5 C6 1.507(5) .
N11 C16 0.37(2) 2_656
N11 C11 1.344(13) .
N11 C13 1.432(13) .
N11 C15 1.565(10) .
C11 N12 1.325(7) .
C11 C16 1.55(2) 2_656
N12 C12 1.354(8) .
N12 C14 1.464(8) .
C12 C13 1.345(10) .
C13 C16 1.49(2) 2_656
C15 C16 1.444(15) .
C15 C16 1.444(15) 2_656
C15 N11 1.565(10) 2_656
C16 N11 0.37(2) 2_656
C16 C13 1.49(2) 2_656
C16 C11 1.55(2) 2_656
N11' C16' 0.833(10) 2_656
N11' C11' 1.328(8) .
N11' C13' 1.383(9) .
N11' C15' 1.491(9) .
C11' N12' 1.332(7) .
N12' C12' 1.355(8) .
N12' C14' 1.465(8) .
C12' C13' 1.346(10) .
C13' C16' 1.225(12) 2_656
C15' C15' 1.262(14) 2_656
C15' C16' 1.356(12) 2_656
C15' C16' 1.484(10) .
C16' N11' 0.833(10) 2_656
C16' C13' 1.225(12) 2_656
C16' C15' 1.356(12) 2_656
