#------------------------------------------------------------------------------
#$Date: 2025-08-20 23:21:57 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301837 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/55/4315508.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_4315508
loop_
_publ_author_name
'Robert P. Davies'
'M. Giovanna Martinelli'
'Laura Patel'
'Andrew J. P. White'
_publ_section_title
;
 Facile Synthesis of Bis(dichalcogenophosphinate)s and a Remarkable
 [Li8(OH)6]2+ Polyhedron
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4626
_journal_page_last               4631
_journal_paper_doi               10.1021/ic100272y
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C30 H46 Li2 O4 P2 S4'
_chemical_formula_weight         674.73
_chemical_name_common            2
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   28.5600(7)
_cell_length_b                   28.5600(7)
_cell_length_c                   12.2070(4)
_cell_measurement_reflns_used    14865
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      2.91
_cell_volume                     8623.0(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0972
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26981
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         4.88
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3222
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3881
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0778
_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)+(0.1250P)²+35.9756P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2475
_reflns_number_gt                2397
_reflns_number_total             3880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100272y_si_001_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        8622.9(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4315508
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
C1 C 0.23409(18) 0.17563(19) 0.1659(3) 0.0433(10) Uani 1 1 d . A .
C2 C 0.2524(2) 0.2299(2) 0.1498(4) 0.0587(13) Uani 1 1 d . . .
H2 H 0.2795 0.2558 0.1967 0.070 Uiso 1 1 calc R . .
C3 C 0.2319(3) 0.2474(3) 0.0667(5) 0.0762(17) Uani 1 1 d . . .
H3 H 0.2451 0.2849 0.0564 0.091 Uiso 1 1 calc R . .
C4 C 0.1933(3) 0.2110(3) 0.0008(6) 0.087(2) Uani 1 1 d . . .
H4 H 0.1791 0.2232 -0.0559 0.104 Uiso 1 1 calc R . .
C5 C 0.1736(3) 0.1557(3) 0.0138(6) 0.089(2) Uani 1 1 d . . .
H5 H 0.1467 0.1304 -0.0343 0.107 Uiso 1 1 calc R . .
C6 C 0.1941(2) 0.1382(2) 0.0994(4) 0.0641(14) Uani 1 1 d . . .
H6 H 0.1803 0.1007 0.1111 0.077 Uiso 1 1 calc R . .
C7 C 0.1488(9) 0.0996(11) 0.588(2) 0.097(6) Uani 0.50 1 d PDU A 1
H7A H 0.1316 0.0910 0.5147 0.117 Uiso 0.50 1 calc PR A 1
H7B H 0.1656 0.1391 0.5991 0.117 Uiso 0.50 1 calc PR A 1
C7A C 0.1511(9) 0.1004(13) 0.556(2) 0.106(8) Uani 0.50 1 d PDU A 2
H7C H 0.1415 0.0926 0.4777 0.128 Uiso 0.50 1 calc PR A 2
H7D H 0.1634 0.1389 0.5716 0.128 Uiso 0.50 1 calc PR A 2
C8 C 0.1066(11) 0.0711(10) 0.673(2) 0.105(6) Uani 0.50 1 d PDU A 1
H8A H 0.0697 0.0542 0.6413 0.126 Uiso 0.50 1 calc PR A 1
H8B H 0.1097 0.0955 0.7333 0.126 Uiso 0.50 1 calc PR A 1
C8A C 0.1062(11) 0.0630(12) 0.6299(16) 0.105(7) Uani 0.50 1 d PDU A 2
H8C H 0.0844 0.0275 0.5938 0.126 Uiso 0.50 1 calc PR A 2
H8D H 0.0823 0.0780 0.6457 0.126 Uiso 0.50 1 calc PR A 2
C9 C 0.1209(8) 0.0298(7) 0.7086(18) 0.098(5) Uani 0.50 1 d PDU A 1
H9A H 0.0990 -0.0045 0.6682 0.118 Uiso 0.50 1 calc PR A 1
H9B H 0.1138 0.0225 0.7880 0.118 Uiso 0.50 1 calc PR A 1
C9A C 0.1296(10) 0.0563(11) 0.7343(17) 0.126(7) Uani 0.50 1 d PDU A 2
H9C H 0.1439 0.0886 0.7819 0.151 Uiso 0.50 1 calc PR A 2
H9D H 0.1036 0.0237 0.7757 0.151 Uiso 0.50 1 calc PR A 2
C10 C 0.1798(10) 0.0522(12) 0.6849(17) 0.074(6) Uani 0.50 1 d PDU A 1
H10B H 0.2021 0.0740 0.7475 0.088 Uiso 0.50 1 calc PR A 1
H10A H 0.1876 0.0227 0.6704 0.088 Uiso 0.50 1 calc PR A 1
C10A C 0.1732(14) 0.0499(16) 0.682(3) 0.116(10) Uani 0.50 1 d PDU A 2
H10D H 0.2035 0.0603 0.7340 0.139 Uiso 0.50 1 calc PR A 2
H10C H 0.1593 0.0121 0.6589 0.139 Uiso 0.50 1 calc PR A 2
C11 C 0.3482(11) 0.0981(15) 0.4774(19) 0.098(6) Uani 0.34 1 d PDU A 1
H11B H 0.3824 0.1332 0.4759 0.118 Uiso 0.34 1 calc PR A 1
H11A H 0.3353 0.0869 0.4014 0.118 Uiso 0.34 1 calc PR A 1
C14B C 0.3149(10) 0.0579(9) 0.495(2) 0.092(6) Uani 0.33 1 d PDU A 4
H14E H 0.3217 0.0634 0.4155 0.110 Uiso 0.33 1 calc PR A 4
H14F H 0.2835 0.0215 0.5087 0.110 Uiso 0.33 1 calc PR A 4
C11B C 0.3608(8) 0.1466(10) 0.565(3) 0.116(8) Uani 0.33 1 d PDU A 4
H11F H 0.3598 0.1690 0.6254 0.139 Uiso 0.33 1 calc PR A 4
H11E H 0.3745 0.1693 0.4982 0.139 Uiso 0.33 1 calc PR A 4
C12 C 0.3554(16) 0.0556(13) 0.536(2) 0.094(8) Uani 0.34 1 d PDU A 1
H12B H 0.3224 0.0195 0.5333 0.113 Uiso 0.34 1 calc PR A 1
H12A H 0.3867 0.0532 0.5081 0.113 Uiso 0.34 1 calc PR A 1
C13B C 0.3643(15) 0.0663(16) 0.556(4) 0.097(8) Uani 0.33 1 d PDU A 4
H13E H 0.3532 0.0418 0.6205 0.116 Uiso 0.33 1 calc PR A 4
H13F H 0.3867 0.0576 0.5080 0.116 Uiso 0.33 1 calc PR A 4
C12B C 0.3965(18) 0.1239(15) 0.594(5) 0.106(9) Uani 0.33 1 d PDU A 4
H12E H 0.4032 0.1260 0.6739 0.127 Uiso 0.33 1 calc PR A 4
H12F H 0.4316 0.1433 0.5552 0.127 Uiso 0.33 1 calc PR A 4
C13 C 0.3654(14) 0.0800(16) 0.649(3) 0.100(8) Uani 0.34 1 d PDU A 1
H13A H 0.3606 0.0534 0.7058 0.120 Uiso 0.34 1 calc PR A 1
H13B H 0.4021 0.1120 0.6548 0.120 Uiso 0.34 1 calc PR A 1
C12A C 0.3893(16) 0.1195(13) 0.591(4) 0.103(9) Uani 0.33 1 d PDU A 3
H12C H 0.3986 0.1446 0.6533 0.124 Uiso 0.33 1 calc PR A 3
H12D H 0.4234 0.1236 0.5609 0.124 Uiso 0.33 1 calc PR A 3
C13A C 0.3543(11) 0.0626(12) 0.630(3) 0.086(6) Uani 0.33 1 d PDU A 3
H13C H 0.3518 0.0353 0.5769 0.103 Uiso 0.33 1 calc PR A 3
H13D H 0.3655 0.0561 0.7028 0.103 Uiso 0.33 1 calc PR A 3
C14 C 0.3224(12) 0.0952(13) 0.6548(13) 0.096(7) Uani 0.34 1 d PDU A 1
H14A H 0.2905 0.0670 0.6945 0.115 Uiso 0.34 1 calc PR A 1
H14B H 0.3361 0.1298 0.6949 0.115 Uiso 0.34 1 calc PR A 1
C11A C 0.3623(7) 0.1348(14) 0.504(2) 0.092(7) Uani 0.33 1 d PDU A 3
H11C H 0.3739 0.1738 0.5050 0.111 Uiso 0.33 1 calc PR A 3
H11D H 0.3673 0.1241 0.4293 0.111 Uiso 0.33 1 calc PR A 3
C14A C 0.3043(9) 0.0665(9) 0.6349(19) 0.082(6) Uani 0.33 1 d PDU A 3
H14C H 0.2718 0.0302 0.6276 0.098 Uiso 0.33 1 calc PR A 3
H14D H 0.3022 0.0824 0.7055 0.098 Uiso 0.33 1 calc PR A 3
C15 C 0.33331(19) 0.1806(2) 0.2191(4) 0.0507(11) Uani 1 1 d . . .
H15A H 0.3504 0.2200 0.2054 0.061 Uiso 1 1 calc R . .
H15B H 0.3554 0.1751 0.2746 0.061 Uiso 1 1 calc R . .
Li1 Li 0.2483(4) 0.1078(4) 0.4885(7) 0.059(2) Uani 1 1 d . A .
O1 O 0.19025(18) 0.08513(18) 0.5904(3) 0.0748(12) Uani 1 1 d D . .
O2 O 0.30711(17) 0.10086(19) 0.5448(3) 0.0781(12) Uani 1 1 d D . .
P1 P 0.26479(5) 0.15561(5) 0.27404(9) 0.0422(3) Uani 1 1 d . . .
S1 S 0.22535(6) 0.07645(5) 0.29516(10) 0.0619(4) Uani 1 1 d . A .
S2 S 0.27381(6) 0.19812(5) 0.41071(10) 0.0589(4) Uani 1 1 d . A .
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'
S S 0.1246 0.1234 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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
C6 C1 C2 119.4(4) . . ?
C6 C1 P1 121.7(4) . . ?
C2 C1 P1 118.9(4) . . ?
C1 C2 C3 121.3(6) . . ?
C4 C3 C2 119.6(6) . . ?
C3 C4 C5 121.2(6) . . ?
C4 C5 C6 118.9(6) . . ?
C1 C6 C5 119.6(6) . . ?
O1 C7 C8 112.8(13) . . ?
O1 C7A C8A 97.3(16) . . ?
C7 C8 C9 99.7(15) . . ?
C7A C8A C9A 109(2) . . ?
C8 C9 C10 107.3(17) . . ?
C10A C9A C8A 96(2) . . ?
O1 C10 C9 105.0(14) . . ?
O1 C10A C9A 105.2(16) . . ?
O2 C11 C12 102(2) . . ?
O2 C14B C13B 101(2) . . ?
O2 C11B C12B 107(2) . . ?
C13 C12 C11 98(3) . . ?
C12B C13B C14B 110(3) . . ?
C11B C12B C13B 103(3) . . ?
C14 C13 C12 101(2) . . ?
C11A C12A C13A 112(3) . . ?
C14A C13A C12A 94(3) . . ?
O2 C14 C13 108.8(19) . . ?
O2 C11A C12A 96(2) . . ?
O2 C14A C13A 106.9(18) . . ?
C15 C15 P1 112.7(4) 13 . ?
O1 Li1 O2 112.9(4) . . ?
O1 Li1 S2 110.8(4) . . ?
O2 Li1 S2 115.2(4) . . ?
O1 Li1 S1 117.9(5) . . ?
O2 Li1 S1 112.9(4) . . ?
S2 Li1 S1 84.2(3) . . ?
O1 Li1 P1 131.4(4) . . ?
O2 Li1 P1 115.5(4) . . ?
S2 Li1 P1 43.02(14) . . ?
S1 Li1 P1 42.36(14) . . ?
C10A O1 C10 7(2) . . ?
C10A O1 C7 100.4(14) . . ?
C10 O1 C7 106.0(11) . . ?
C10A O1 C7A 113.4(15) . . ?
C10 O1 C7A 119.6(13) . . ?
C7 O1 C7A 15.6(18) . . ?
C10A O1 Li1 133.5(12) . . ?
C10 O1 Li1 127.8(8) . . ?
C7 O1 Li1 126.1(9) . . ?
C7A O1 Li1 112.3(10) . . ?
C14 O2 C14A 30.4(12) . . ?
C14 O2 C11B 72.8(18) . . ?
C14A O2 C11B 99.1(17) . . ?
C14 O2 C11A 96.2(16) . . ?
C14A O2 C11A 112.7(15) . . ?
C11B O2 C11A 32.9(14) . . ?
C14 O2 C11 102.7(15) . . ?
C14A O2 C11 99.4(15) . . ?
C11B O2 C11 68.2(17) . . ?
C11A O2 C11 38.7(14) . . ?
C14 O2 C14B 96.3(15) . . ?
C14A O2 C14B 74.4(15) . . ?
C11B O2 C14B 106.5(16) . . ?
C11A O2 C14B 81.4(17) . . ?
C11 O2 C14B 43.1(14) . . ?
C14 O2 Li1 132.4(11) . . ?
C14A O2 Li1 126.0(10) . . ?
C11B O2 Li1 123.6(13) . . ?
C11A O2 Li1 121.1(11) . . ?
C11 O2 Li1 124.9(10) . . ?
C14B O2 Li1 116.2(9) . . ?
C1 P1 C15 101.5(2) . . ?
C1 P1 S1 111.37(16) . . ?
C15 P1 S1 112.27(17) . . ?
C1 P1 S2 110.39(15) . . ?
C15 P1 S2 106.15(16) . . ?
S1 P1 S2 114.34(7) . . ?
C1 P1 Li1 144.5(2) . . ?
C15 P1 Li1 113.9(2) . . ?
S1 P1 Li1 58.29(19) . . ?
S2 P1 Li1 58.06(19) . . ?
P1 S1 Li1 79.3(2) . . ?
P1 S2 Li1 78.9(2) . . ?
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
C1 C6 1.374(7) . ?
C1 C2 1.381(7) . ?
C1 P1 1.827(4) . ?
C2 C3 1.382(8) . ?
C3 C4 1.340(10) . ?
C4 C5 1.395(10) . ?
C5 C6 1.407(8) . ?
C7 O1 1.436(11) . ?
C7 C8 1.486(14) . ?
C7A O1 1.450(13) . ?
C7A C8A 1.493(15) . ?
C8 C9 1.495(15) . ?
C8A C9A 1.495(15) . ?
C9 C10 1.498(15) . ?
C9A C10A 1.487(16) . ?
C10 O1 1.423(11) . ?
C10A O1 1.421(13) . ?
C11 O2 1.469(14) . ?
C11 C12 1.509(16) . ?
C14B O2 1.481(13) . ?
C14B C13B 1.506(16) . ?
C11B O2 1.453(15) . ?
C11B C12B 1.500(16) . ?
C12 C13 1.499(16) . ?
C13B C12B 1.502(16) . ?
C13 C14 1.499(15) . ?
C12A C11A 1.500(15) . ?
C12A C13A 1.500(16) . ?
C13A C14A 1.491(15) . ?
C14 O2 1.445(14) . ?
C11A O2 1.465(14) . ?
C14A O2 1.448(13) . ?
C15 C15 1.510(9) 13 ?
C15 P1 1.842(5) . ?
Li1 O1 1.908(9) . ?
Li1 O2 1.915(10) . ?
Li1 S2 2.491(9) . ?
Li1 S1 2.494(9) . ?
Li1 P1 2.881(8) . ?
P1 S1 1.9749(17) . ?
P1 S2 2.0028(16) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139132002
