#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:08:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179777 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/73/7007336.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_7007336
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 Na O3 P S2'
_chemical_formula_weight         370.42
_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                 102.117(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0592(11)
_cell_length_b                   8.7781(9)
_cell_length_c                   16.8189(15)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     1885.1(3)
_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 0.990
_diffrn_measured_fraction_theta_max 0.690
_diffrn_measurement_device_type  'stoe stadi 4'
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10946
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.75
_diffrn_reflns_theta_min         3.95
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.538
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4416
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0957
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2834
_refine_ls_wR_factor_ref         0.3278
_reflns_number_gt                2888
_reflns_number_total             4416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603764j.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7007336
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
Na1 Na 0.28012(14) 0.5146(2) 0.29810(11) 0.0572(6) Uani 1 1 d . . .
P1 P 0.32725(8) 0.70836(14) 0.14169(6) 0.0444(4) Uani 1 1 d . . .
S1 S 0.18682(8) 0.70632(14) 0.17111(6) 0.0474(4) Uani 1 1 d . . .
S2 S 0.42696(10) 0.55185(18) 0.19400(8) 0.0662(5) Uani 1 1 d . A .
O1 O 0.3660(2) 0.8803(4) 0.16326(17) 0.0460(7) Uani 1 1 d . . .
O2 O 0.2653(2) 0.7400(4) -0.21832(18) 0.0526(8) Uani 1 1 d . . .
C1 C 0.3081(3) 0.7021(5) 0.0327(3) 0.0396(9) Uani 1 1 d . . .
C2 C 0.3595(3) 0.6016(5) -0.0094(3) 0.0481(10) Uani 1 1 d . A .
H2A H 0.4040 0.5259 0.0198 0.058 Uiso 1 1 calc R . .
C3 C 0.3472(3) 0.6096(6) -0.0931(3) 0.0502(11) Uani 1 1 d . . .
H3A H 0.3835 0.5408 -0.1210 0.060 Uiso 1 1 calc R A .
C4 C 0.2818(3) 0.7185(5) -0.1353(2) 0.0438(10) Uani 1 1 d . A .
C5 C 0.2260(3) 0.8154(6) -0.0946(3) 0.0479(10) Uani 1 1 d . . .
H5A H 0.1780 0.8866 -0.1243 0.057 Uiso 1 1 calc R A .
C6 C 0.2402(3) 0.8084(5) -0.0119(2) 0.0423(9) Uani 1 1 d . A .
H6A H 0.2032 0.8769 0.0157 0.051 Uiso 1 1 calc R . .
C7 C 0.3159(4) 0.6384(7) -0.2643(3) 0.0606(13) Uani 1 1 d . . .
H7A H 0.2981 0.6671 -0.3218 0.091 Uiso 1 1 calc R . .
H7B H 0.2924 0.5340 -0.2579 0.091 Uiso 1 1 calc R . .
H7C H 0.3919 0.6446 -0.2446 0.091 Uiso 1 1 calc R . .
C8 C 0.4702(3) 0.9524(6) 0.1651(3) 0.0524(11) Uani 1 1 d . A .
C9 C 0.5301(3) 0.8742(7) 0.1067(3) 0.0606(13) Uani 1 1 d . . .
H9A H 0.5483 0.7700 0.1254 0.091 Uiso 1 1 calc R A .
H9B H 0.5942 0.9314 0.1057 0.091 Uiso 1 1 calc R . .
H9C H 0.4858 0.8714 0.0519 0.091 Uiso 1 1 calc R . .
C10 C 0.4426(4) 1.1145(7) 0.1358(3) 0.0640(13) Uani 1 1 d . . .
H10A H 0.4050 1.1652 0.1731 0.096 Uiso 1 1 calc R A .
H10B H 0.3980 1.1117 0.0811 0.096 Uiso 1 1 calc R . .
H10C H 0.5069 1.1709 0.1343 0.096 Uiso 1 1 calc R . .
C11 C 0.5305(4) 0.9482(10) 0.2513(3) 0.0787(19) Uani 1 1 d . . .
H11A H 0.4903 0.9999 0.2864 0.118 Uiso 1 1 calc R A .
H11B H 0.5979 0.9998 0.2551 0.118 Uiso 1 1 calc R . .
H11C H 0.5427 0.8420 0.2688 0.118 Uiso 1 1 calc R . .
O3 O 0.3467(3) 0.6614(6) 0.4139(3) 0.0794(12) Uani 0.50 1 d PD A 1
C12 C 0.2991(9) 0.7350(13) 0.4735(7) 0.069(3) Uiso 0.50 1 d PD A 1
H12A H 0.2729 0.6593 0.5081 0.083 Uiso 0.50 1 calc PR A 1
H12B H 0.2405 0.8016 0.4473 0.083 Uiso 0.50 1 calc PR A 1
C13 C 0.3865(13) 0.8252(17) 0.5213(7) 0.085(4) Uiso 0.50 1 d PD A 1
H13A H 0.4206 0.7694 0.5710 0.102 Uiso 0.50 1 calc PR A 1
H13B H 0.3609 0.9244 0.5374 0.102 Uiso 0.50 1 calc PR A 1
C14 C 0.4621(9) 0.8481(14) 0.4652(9) 0.082(3) Uiso 0.50 1 d PD A 1
H14A H 0.5346 0.8616 0.4966 0.099 Uiso 0.50 1 calc PR A 1
H14B H 0.4423 0.9379 0.4297 0.099 Uiso 0.50 1 calc PR A 1
C15 C 0.4517(11) 0.702(2) 0.4156(12) 0.136(7) Uiso 0.50 1 d PD A 1
H15A H 0.4636 0.7199 0.3602 0.163 Uiso 0.50 1 calc PR A 1
H15B H 0.5008 0.6224 0.4426 0.163 Uiso 0.50 1 calc PR A 1
O3A O 0.3467(3) 0.6614(6) 0.4139(3) 0.0794(12) Uani 0.50 1 d PD A 2
C12A C 0.3163(15) 0.8068(14) 0.4332(8) 0.110(5) Uiso 0.50 1 d PD A 2
H12C H 0.2404 0.8247 0.4132 0.132 Uiso 0.50 1 calc PR A 2
H12D H 0.3569 0.8879 0.4129 0.132 Uiso 0.50 1 calc PR A 2
C14A C 0.4259(12) 0.6744(18) 0.5446(6) 0.093(4) Uiso 0.50 1 d PD A 2
H14C H 0.4018 0.5874 0.5733 0.112 Uiso 0.50 1 calc PR A 2
H14D H 0.4909 0.7159 0.5789 0.112 Uiso 0.50 1 calc PR A 2
C13A C 0.3463(18) 0.790(2) 0.5275(9) 0.118(7) Uiso 0.50 1 d PD A 2
H13C H 0.3733 0.8880 0.5529 0.141 Uiso 0.50 1 calc PR A 2
H13D H 0.2843 0.7599 0.5491 0.141 Uiso 0.50 1 calc PR A 2
C15A C 0.4459(11) 0.623(2) 0.4595(10) 0.113(5) Uiso 0.50 1 d PD A 2
H15C H 0.5027 0.6814 0.4430 0.136 Uiso 0.50 1 calc PR A 2
H15D H 0.4604 0.5121 0.4576 0.136 Uiso 0.50 1 calc PR A 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'
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'
Na Na 0.0362 0.0249 '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
O3 Na1 O1 102.59(13) . 2_545 ?
O3 Na1 S1 111.43(13) . 2_545 ?
O1 Na1 S1 65.12(9) 2_545 2_545 ?
O3 Na1 S1 109.29(14) . . ?
O1 Na1 S1 104.74(10) 2_545 . ?
S1 Na1 S1 139.26(9) 2_545 . ?
O3 Na1 S2 105.38(12) . . ?
O1 Na1 S2 151.04(12) 2_545 . ?
S1 Na1 S2 97.31(7) 2_545 . ?
S1 Na1 S2 72.85(5) . . ?
O3 Na1 C15 25.1(2) . . ?
O1 Na1 C15 125.6(3) 2_545 . ?
S1 Na1 C15 109.4(5) 2_545 . ?
S1 Na1 C15 107.9(5) . . ?
S2 Na1 C15 81.0(3) . . ?
O3 Na1 P1 107.52(12) . 2_545 ?
O1 Na1 P1 27.96(8) 2_545 2_545 ?
S1 Na1 P1 37.27(4) 2_545 2_545 ?
S1 Na1 P1 125.65(7) . 2_545 ?
S2 Na1 P1 131.52(8) . 2_545 ?
C15 Na1 P1 122.0(4) . 2_545 ?
O3 Na1 P1 106.29(13) . . ?
O1 Na1 P1 138.40(10) 2_545 . ?
S1 Na1 P1 127.22(7) 2_545 . ?
S1 Na1 P1 37.14(3) . . ?
S2 Na1 P1 36.40(4) . . ?
C15 Na1 P1 90.2(4) . . ?
P1 Na1 P1 146.15(8) 2_545 . ?
O1 P1 C1 103.21(17) . . ?
O1 P1 S2 113.98(13) . . ?
C1 P1 S2 111.81(14) . . ?
O1 P1 S1 102.39(11) . . ?
C1 P1 S1 108.30(14) . . ?
S2 P1 S1 116.01(7) . . ?
O1 P1 Na1 45.43(10) . 2 ?
C1 P1 Na1 111.23(13) . 2 ?
S2 P1 Na1 135.85(8) . 2 ?
S1 P1 Na1 57.18(5) . 2 ?
O1 P1 Na1 114.00(11) . . ?
C1 P1 Na1 142.02(15) . . ?
S2 P1 Na1 60.01(5) . . ?
S1 P1 Na1 57.51(5) . . ?
Na1 P1 Na1 90.74(3) 2 . ?
P1 S1 Na1 85.55(6) . 2 ?
P1 S1 Na1 85.35(6) . . ?
Na1 S1 Na1 114.83(5) 2 . ?
P1 S2 Na1 83.59(6) . . ?
C8 O1 P1 130.1(3) . . ?
C8 O1 Na1 123.3(3) . 2 ?
P1 O1 Na1 106.61(13) . 2 ?
C4 O2 C7 118.1(4) . . ?
C2 C1 C6 118.2(4) . . ?
C2 C1 P1 124.1(3) . . ?
C6 C1 P1 117.6(3) . . ?
C3 C2 C1 121.4(4) . . ?
C4 C3 C2 119.1(4) . . ?
C3 C4 O2 124.4(4) . . ?
C3 C4 C5 120.3(4) . . ?
O2 C4 C5 115.3(4) . . ?
C6 C5 C4 120.0(4) . . ?
C5 C6 C1 120.9(4) . . ?
O1 C8 C11 107.5(4) . . ?
O1 C8 C10 103.6(3) . . ?
C11 C8 C10 112.1(5) . . ?
O1 C8 C9 112.3(4) . . ?
C11 C8 C9 111.9(4) . . ?
C10 C8 C9 109.1(4) . . ?
C15 O3 C12 115.7(9) . . ?
C15 O3 Na1 110.1(7) . . ?
C12 O3 Na1 133.4(5) . . ?
O3 C12 C13 102.9(8) . . ?
C12 C13 C14 105.1(7) . . ?
C13 C14 C15 103.6(8) . . ?
O3 C15 C14 101.4(9) . . ?
O3 C15 Na1 44.8(5) . . ?
C14 C15 Na1 139.5(10) . . ?
C13A C14A C15A 105.9(8) . . ?
C14A C13A C12A 106.6(8) . . ?
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
Na1 O3 2.345(5) . ?
Na1 O1 2.445(3) 2_545 ?
Na1 S1 2.772(2) 2_545 ?
Na1 S1 2.790(2) . ?
Na1 S2 2.874(2) . ?
Na1 C15 3.124(14) . ?
Na1 P1 3.288(2) 2_545 ?
Na1 P1 3.297(2) . ?
P1 O1 1.609(3) . ?
P1 C1 1.799(4) . ?
P1 S2 1.9688(16) . ?
P1 S1 1.9973(14) . ?
P1 Na1 3.288(2) 2 ?
S1 Na1 2.772(2) 2 ?
O1 C8 1.495(5) . ?
O1 Na1 2.445(3) 2 ?
O2 C4 1.380(5) . ?
O2 C7 1.429(6) . ?
C1 C2 1.388(6) . ?
C1 C6 1.393(6) . ?
C2 C3 1.385(6) . ?
C3 C4 1.375(6) . ?
C4 C5 1.390(6) . ?
C5 C6 1.366(6) . ?
C8 C11 1.497(7) . ?
C8 C10 1.525(8) . ?
C8 C9 1.539(6) . ?
O3 C15 1.411(11) . ?
O3 C12 1.438(9) . ?
C12 C13 1.480(16) . ?
C13 C14 1.516(19) . ?
C14 C15 1.523(19) . ?
C12A C13A 1.560(19) . ?
C14A C13A 1.44(2) . ?
C14A C15A 1.57(2) . ?
