#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:08:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179777 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/73/7007338.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_7007338
loop_
_publ_author_name
'Shi, Weifeng'
'Shafaei-Fallah, Maryam'
'Anson, Christopher E.'
'Rothenberger, Alexander'
_publ_section_title
;
 Metal thiophosphonates and related compounds: an emerging area of
 supramolecular coordination chemistry.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3257
_journal_page_last               3262
_journal_paper_doi               10.1039/b603764j
_journal_year                    2006
_chemical_formula_sum            'C15 H24 K O3 P S2'
_chemical_formula_weight         386.53
_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                96.849(6)
_cell_angle_beta                 102.612(6)
_cell_angle_gamma                111.286(7)
_cell_formula_units_Z            2
_cell_length_a                   8.264(6)
_cell_length_b                   11.2990(9)
_cell_length_c                   11.3100(8)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     937.1(7)
_computing_cell_refinement       'kuma ccd'
_computing_data_collection       'kuma ccd'
_computing_data_reduction        'kuma ccd'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.638
_diffrn_measurement_device_type  'stoe stadi IV'
_diffrn_measurement_method       rotation
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7578
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.83
_diffrn_reflns_theta_min         3.86
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0327
_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)+(0.1100P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                3473
_reflns_number_total             4099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603764j.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7007338
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
P1 P 0.42961(7) 0.31269(5) 0.26777(5) 0.01669(16) Uani 1 1 d . . .
K1 K 0.55732(6) 0.36255(5) 0.60413(4) 0.02319(16) Uani 1 1 d . . .
S1 S 0.34180(8) 0.15995(5) 0.34146(5) 0.02442(17) Uani 1 1 d . . .
S2 S 0.65845(7) 0.46024(5) 0.36516(5) 0.02139(16) Uani 1 1 d . . .
C1 C 0.4519(3) 0.2640(2) 0.11531(18) 0.0170(4) Uani 1 1 d . . .
C2 C 0.5254(3) 0.3614(2) 0.0526(2) 0.0211(4) Uani 1 1 d . . .
H2A H 0.5741 0.4503 0.0941 0.025 Uiso 1 1 calc R . .
C3 C 0.5277(3) 0.3298(2) -0.06776(19) 0.0215(4) Uani 1 1 d . . .
H3A H 0.5773 0.3967 -0.1092 0.026 Uiso 1 1 calc R . .
C4 C 0.4574(3) 0.1999(2) -0.12924(19) 0.0186(4) Uani 1 1 d . . .
C5 C 0.3922(3) 0.1020(2) -0.0671(2) 0.0232(5) Uani 1 1 d . . .
H5A H 0.3501 0.0132 -0.1073 0.028 Uiso 1 1 calc R . .
C6 C 0.3892(3) 0.1353(2) 0.0548(2) 0.0229(4) Uani 1 1 d . . .
H6A H 0.3432 0.0683 0.0971 0.027 Uiso 1 1 calc R . .
C7 C 0.3790(4) 0.0478(2) -0.3202(2) 0.0299(5) Uani 1 1 d . . .
H7A H 0.3830 0.0468 -0.4062 0.045 Uiso 1 1 calc R . .
H7B H 0.2529 0.0059 -0.3188 0.045 Uiso 1 1 calc R . .
H7C H 0.4480 0.0004 -0.2829 0.045 Uiso 1 1 calc R . .
C8 C 0.0875(3) 0.3194(2) 0.1873(2) 0.0221(4) Uani 1 1 d . . .
C9 C 0.0443(3) 0.4239(3) 0.1326(3) 0.0347(6) Uani 1 1 d . . .
H9A H 0.0805 0.5006 0.1988 0.052 Uiso 1 1 calc R . .
H9B H -0.0861 0.3909 0.0924 0.052 Uiso 1 1 calc R . .
H9C H 0.1105 0.4479 0.0711 0.052 Uiso 1 1 calc R . .
C10 C 0.0029(3) 0.2903(3) 0.2926(2) 0.0343(6) Uani 1 1 d . . .
H10A H 0.0498 0.3697 0.3575 0.051 Uiso 1 1 calc R . .
H10B H 0.0332 0.2230 0.3272 0.051 Uiso 1 1 calc R . .
H10C H -0.1289 0.2595 0.2609 0.051 Uiso 1 1 calc R . .
C11 C 0.0252(3) 0.1973(2) 0.0869(2) 0.0294(5) Uani 1 1 d . . .
H11A H 0.0525 0.1301 0.1239 0.044 Uiso 1 1 calc R . .
H11B H 0.0885 0.2176 0.0233 0.044 Uiso 1 1 calc R . .
H11C H -0.1056 0.1655 0.0489 0.044 Uiso 1 1 calc R . .
C12 C 0.8890(3) 0.2528(3) 0.5628(2) 0.0309(5) Uani 1 1 d . . .
H12A H 0.9688 0.3415 0.5595 0.037 Uiso 1 1 calc R . .
H12B H 0.8016 0.2093 0.4798 0.037 Uiso 1 1 calc R . .
C13 C 0.9996(4) 0.1755(3) 0.6017(3) 0.0376(6) Uani 1 1 d . . .
H13A H 0.9286 0.0810 0.5682 0.045 Uiso 1 1 calc R . .
H13B H 1.1112 0.2033 0.5745 0.045 Uiso 1 1 calc R . .
C14 C 1.0426(3) 0.2094(3) 0.7415(3) 0.0385(6) Uani 1 1 d . . .
H14A H 1.1474 0.2939 0.7774 0.046 Uiso 1 1 calc R . .
H14B H 1.0682 0.1410 0.7791 0.046 Uiso 1 1 calc R . .
C15 C 0.8702(3) 0.2168(3) 0.7602(2) 0.0296(5) Uani 1 1 d . . .
H15A H 0.7846 0.1305 0.7647 0.036 Uiso 1 1 calc R . .
H15B H 0.8971 0.2798 0.8379 0.036 Uiso 1 1 calc R . .
O1 O 0.28732(18) 0.38101(13) 0.23995(13) 0.0181(3) Uani 1 1 d . . .
O2 O 0.4566(2) 0.17980(15) -0.25084(14) 0.0242(4) Uani 1 1 d . . .
O3 O 0.7955(2) 0.25837(19) 0.65533(15) 0.0323(4) Uani 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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
O1 P1 C1 103.30(8) . . ?
O1 P1 S1 113.00(7) . . ?
C1 P1 S1 110.55(7) . . ?
O1 P1 S2 103.07(7) . . ?
C1 P1 S2 108.10(7) . . ?
S1 P1 S2 117.64(3) . . ?
O1 P1 K1 103.11(6) . . ?
C1 P1 K1 153.25(7) . . ?
S1 P1 K1 61.90(2) . . ?
S2 P1 K1 61.44(2) . . ?
O1 P1 K1 46.53(5) . 2_666 ?
C1 P1 K1 125.00(7) . 2_666 ?
S1 P1 K1 123.09(3) . 2_666 ?
S2 P1 K1 57.87(4) . 2_666 ?
K1 P1 K1 72.510(17) . 2_666 ?
O3 K1 O2 69.03(6) . 1_556 ?
O3 K1 O1 107.36(6) . 2_666 ?
O2 K1 O1 108.86(4) 1_556 2_666 ?
O3 K1 S2 160.81(5) . 2_666 ?
O2 K1 S2 105.87(4) 1_556 2_666 ?
O1 K1 S2 55.72(4) 2_666 2_666 ?
O3 K1 S2 97.16(5) . . ?
O2 K1 S2 155.23(4) 1_556 . ?
O1 K1 S2 94.68(3) 2_666 . ?
S2 K1 S2 93.56(2) 2_666 . ?
O3 K1 S1 92.80(5) . . ?
O2 K1 S1 95.60(4) 1_556 . ?
O1 K1 S1 152.49(3) 2_666 . ?
S2 K1 S1 106.24(3) 2_666 . ?
S2 K1 S1 63.67(2) . . ?
O3 K1 C12 22.05(5) . . ?
O2 K1 C12 88.52(6) 1_556 . ?
O1 K1 C12 111.72(6) 2_666 . ?
S2 K1 C12 163.12(5) 2_666 . ?
S2 K1 C12 75.32(5) . . ?
S1 K1 C12 80.50(5) . . ?
O3 K1 P1 104.47(4) . . ?
O2 K1 P1 128.35(4) 1_556 . ?
O1 K1 P1 121.27(3) 2_666 . ?
S2 K1 P1 93.17(2) 2_666 . ?
S2 K1 P1 32.959(18) . . ?
S1 K1 P1 32.781(14) . . ?
C12 K1 P1 84.36(5) . . ?
O3 K1 P1 131.57(5) . 2_666 ?
O2 K1 P1 113.96(4) 1_556 2_666 ?
O1 K1 P1 24.21(3) 2_666 2_666 ?
S2 K1 P1 32.066(19) 2_666 2_666 ?
S2 K1 P1 90.673(18) . 2_666 ?
S1 K1 P1 132.43(2) . 2_666 ?
C12 K1 P1 133.53(5) . 2_666 ?
P1 K1 P1 107.490(17) . 2_666 ?
O3 K1 K1 140.98(4) . 2_666 ?
O2 K1 K1 149.92(4) 1_556 2_666 ?
O1 K1 K1 69.59(3) 2_666 2_666 ?
S2 K1 K1 47.145(14) 2_666 2_666 ?
S2 K1 K1 46.41(2) . 2_666 ?
S1 K1 K1 82.945(19) . 2_666 ?
C12 K1 K1 120.55(5) . 2_666 ?
P1 K1 K1 54.816(14) . 2_666 ?
P1 K1 K1 52.674(14) 2_666 2_666 ?
P1 S1 K1 85.32(3) . . ?
P1 S2 K1 90.06(5) . 2_666 ?
P1 S2 K1 85.60(3) . . ?
K1 S2 K1 86.44(2) 2_666 . ?
C6 C1 C2 118.46(19) . . ?
C6 C1 P1 122.98(16) . . ?
C2 C1 P1 118.42(16) . . ?
C3 C2 C1 120.82(19) . . ?
C2 C3 C4 120.07(19) . . ?
O2 C4 C5 124.80(19) . . ?
O2 C4 C3 115.15(18) . . ?
C5 C4 C3 120.05(19) . . ?
C4 C5 C6 119.3(2) . . ?
C1 C6 C5 121.2(2) . . ?
O1 C8 C9 103.29(17) . . ?
O1 C8 C10 108.50(18) . . ?
C9 C8 C10 110.7(2) . . ?
O1 C8 C11 112.43(18) . . ?
C9 C8 C11 110.3(2) . . ?
C10 C8 C11 111.3(2) . . ?
O3 C12 C13 105.9(2) . . ?
O3 C12 K1 43.42(10) . . ?
C13 C12 K1 148.75(17) . . ?
C14 C13 C12 101.8(2) . . ?
C13 C14 C15 102.55(19) . . ?
O3 C15 C14 105.8(2) . . ?
C8 O1 P1 129.11(13) . . ?
C8 O1 K1 117.55(12) . 2_666 ?
P1 O1 K1 109.25(7) . 2_666 ?
C4 O2 C7 117.55(17) . . ?
C4 O2 K1 128.94(12) . 1_554 ?
C7 O2 K1 113.25(12) . 1_554 ?
C15 O3 C12 109.86(18) . . ?
C15 O3 K1 135.23(14) . . ?
C12 O3 K1 114.54(14) . . ?
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
P1 O1 1.6226(17) . ?
P1 C1 1.816(2) . ?
P1 S1 1.9742(8) . ?
P1 S2 1.9830(10) . ?
P1 K1 3.6342(7) . ?
P1 K1 3.7352(8) 2_666 ?
K1 O3 2.635(2) . ?
K1 O2 2.7935(16) 1_556 ?
K1 O1 2.8715(15) 2_666 ?
K1 S2 3.1632(13) 2_666 ?
K1 S2 3.2015(8) . ?
K1 S1 3.2164(8) . ?
K1 C12 3.487(3) . ?
K1 P1 3.7352(8) 2_666 ?
K1 K1 4.3588(10) 2_666 ?
S2 K1 3.1632(13) 2_666 ?
C1 C6 1.383(3) . ?
C1 C2 1.404(3) . ?
C2 C3 1.372(3) . ?
C3 C4 1.392(3) . ?
C4 O2 1.365(2) . ?
C4 C5 1.388(3) . ?
C5 C6 1.393(3) . ?
C7 O2 1.435(3) . ?
C8 O1 1.484(3) . ?
C8 C9 1.513(3) . ?
C8 C10 1.517(3) . ?
C8 C11 1.521(3) . ?
C12 O3 1.439(3) . ?
C12 C13 1.512(4) . ?
C13 C14 1.512(4) . ?
C14 C15 1.514(4) . ?
C15 O3 1.426(3) . ?
O1 K1 2.8715(15) 2_666 ?
O2 K1 2.7934(16) 1_554 ?
