#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:31:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179794 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/90/7009079.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_7009079
loop_
_publ_author_name
'Pérez-Lourido, Paulo'
'Romero, Jaime'
'García-Vázquez, José A.'
'Sousa, Antonio'
'Zheng, Yifan'
'Dilworth, Jonathan R.'
'Zubieta, Jon'
_publ_section_title
;
 Lead(II) complexes with phosphorylthiolato and thiophosphorylthiolato
 ligands
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              769
_journal_paper_doi               10.1039/a908496g
_journal_year                    2000
_chemical_formula_sum            'C38 H32 P2 Pb S4'
_chemical_formula_weight         886.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 100.455(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5560(10)
_cell_length_b                   15.6120(10)
_cell_length_c                   15.0520(10)
_cell_measurement_temperature    150(2)
_cell_volume                     3594.8(4)
_computing_cell_refinement
'DIP2000 software DENZO (Otwinowski & Minor, 1996)'
_computing_data_collection       'DIP2000 software Xpress (MAC science, 1989)'
_computing_data_reduction
'DIP2000 software DENZO (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf-nonius DIP2000 '
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6712
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    5.041
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         2.216
_refine_diff_density_min         -1.415
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.047(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         3804
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0589P)²+31.1723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                3670
_reflns_number_total             3804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908496g.txt
_cod_data_source_block           compound5
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7009079
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'
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
Pb Pb 0.78012(9) 0.14038(2) 0.26500(10) 0.03152(14) Uani 1 1 d . . .
P1 P 0.5096(3) 0.1673(4) 0.2486(3) 0.0274(10) Uani 1 1 d . . .
P2 P 1.0675(3) 0.1728(4) 0.2827(3) 0.0314(11) Uani 1 1 d . . .
S1 S 0.7231(4) 0.2508(4) 0.1437(4) 0.0480(15) Uani 1 1 d . . .
S2 S 0.8488(4) 0.2535(4) 0.3855(5) 0.0550(18) Uani 1 1 d . . .
S3 S 0.9677(6) 0.0985(6) 0.2254(6) 0.0254(19) Uani 0.50 1 d P . .
S4 S 0.6082(7) 0.0966(11) 0.3092(10) 0.048(3) Uani 0.50 1 d P . .
S3' S 0.9555(10) 0.1575(12) 0.1979(10) 0.056(4) Uani 0.50 1 d P . .
S4' S 0.6203(8) 0.1499(9) 0.3363(9) 0.039(3) Uani 0.50 1 d P . .
C11 C 0.6582(13) 0.1787(13) 0.0869(12) 0.041(5) Uani 1 1 d . . .
C12 C 0.5662(10) 0.1664(9) 0.0877(9) 0.024(3) Uani 1 1 d U . .
C13 C 0.5170(10) 0.1025(11) 0.0308(9) 0.035(5) Uani 1 1 d U . .
H13 H 0.4573 0.0982 0.0302 0.043 Uiso 1 1 calc R . .
C14 C 0.556(2) 0.046(2) -0.025(2) 0.089(9) Uani 1 1 d U . .
H14 H 0.5233 0.0029 -0.0587 0.107 Uiso 1 1 calc R . .
C15 C 0.6441(10) 0.0570(11) -0.0249(9) 0.041(4) Uani 1 1 d U . .
H15 H 0.6716 0.0209 -0.0603 0.049 Uiso 1 1 calc R . .
C16 C 0.6944(15) 0.1221(14) 0.0272(14) 0.053(6) Uani 1 1 d U . .
H16 H 0.7528 0.1284 0.0226 0.063 Uiso 1 1 calc R . .
C17 C 0.5220(12) 0.2273(9) 0.1440(10) 0.021(3) Uani 1 1 d U . .
H17A H 0.4653 0.2446 0.1108 0.025 Uiso 1 1 calc R . .
H17B H 0.5575 0.2781 0.1594 0.025 Uiso 1 1 calc R . .
C21 C 0.4097(7) 0.0926(6) 0.2154(7) 0.042(4) Uani 1 1 d G . .
C22 C 0.3284(7) 0.1272(6) 0.1744(8) 0.049(4) Uani 1 1 d G . .
H22 H 0.3219 0.1863 0.1693 0.059 Uiso 1 1 calc R . .
C23 C 0.2572(7) 0.0740(7) 0.1412(8) 0.059(4) Uani 1 1 d G . .
H23 H 0.2039 0.0974 0.1143 0.070 Uiso 1 1 calc R . .
C24 C 0.2672(7) -0.0138(7) 0.1491(9) 0.064(5) Uani 1 1 d G . .
H24 H 0.2206 -0.0499 0.1274 0.077 Uiso 1 1 calc R . .
C25 C 0.3485(7) -0.0483(6) 0.1901(8) 0.072(7) Uani 1 1 d G . .
H25 H 0.3550 -0.1074 0.1952 0.087 Uiso 1 1 calc R . .
C26 C 0.4197(7) 0.0049(6) 0.2232(7) 0.042(3) Uani 1 1 d G . .
H26 H 0.4730 -0.0185 0.2502 0.051 Uiso 1 1 calc R . .
C31 C 0.4436(7) 0.2552(7) 0.2922(7) 0.049(5) Uani 1 1 d G . .
C32 C 0.3867(8) 0.3070(8) 0.2337(7) 0.056(4) Uani 1 1 d G . .
H32 H 0.3803 0.2997 0.1715 0.068 Uiso 1 1 calc R . .
C33 C 0.3396(9) 0.3696(7) 0.2691(8) 0.072(6) Uani 1 1 d G . .
H33 H 0.3013 0.4046 0.2305 0.086 Uiso 1 1 calc R . .
C34 C 0.3494(10) 0.3804(8) 0.3629(8) 0.079(7) Uani 1 1 d G . .
H34 H 0.3176 0.4225 0.3861 0.095 Uiso 1 1 calc R . .
C35 C 0.4063(10) 0.3286(9) 0.4214(7) 0.086(8) Uani 1 1 d G . .
H35 H 0.4127 0.3359 0.4835 0.103 Uiso 1 1 calc R . .
C36 C 0.4534(8) 0.2660(8) 0.3860(7) 0.052(4) Uani 1 1 d G . .
H36 H 0.4916 0.2310 0.4246 0.062 Uiso 1 1 calc R . .
C41 C 0.9160(9) 0.1676(9) 0.4508(8) 0.031(4) Uani 1 1 d G . .
C42 C 1.0032(8) 0.1613(9) 0.4493(9) 0.042(5) Uani 1 1 d GU . .
C43 C 1.0525(8) 0.1024(9) 0.5009(9) 0.052(6) Uani 1 1 d GU . .
H43 H 1.1119 0.0980 0.5000 0.062 Uiso 1 1 calc R . .
C44 C 1.0145(8) 0.0498(9) 0.5540(8) 0.032(4) Uani 1 1 d GU . .
H44 H 1.0481 0.0091 0.5897 0.038 Uiso 1 1 calc R . .
C45 C 0.9273(9) 0.0561(10) 0.5554(10) 0.089(10) Uani 1 1 d GU . .
H45 H 0.9017 0.0197 0.5921 0.107 Uiso 1 1 calc R . .
C46 C 0.8780(8) 0.1150(10) 0.5039(10) 0.042(5) Uani 1 1 d GU . .
H46 H 0.8186 0.1194 0.5047 0.051 Uiso 1 1 calc R . .
C47 C 1.0478(15) 0.2122(13) 0.3856(15) 0.046(5) Uani 1 1 d . . .
H47A H 1.1040 0.2294 0.4199 0.055 Uiso 1 1 calc R . .
H47B H 1.0139 0.2642 0.3719 0.055 Uiso 1 1 calc R . .
C51 C 1.1255(8) 0.0828(6) 0.3154(8) 0.049(5) Uani 1 1 d G . .
C52 C 1.2122(9) 0.0910(8) 0.3619(9) 0.062(5) Uani 1 1 d G . .
H52 H 1.2372 0.1451 0.3712 0.075 Uiso 1 1 calc R . .
C53 C 1.2607(9) 0.0194(10) 0.3939(11) 0.101(9) Uani 1 1 d G . .
H53 H 1.3179 0.0250 0.4245 0.121 Uiso 1 1 calc R . .
C54 C 1.2226(11) -0.0604(9) 0.3794(11) 0.105(10) Uani 1 1 d G . .
H54 H 1.2543 -0.1090 0.4005 0.126 Uiso 1 1 calc R . .
C55 C 1.1359(11) -0.0686(6) 0.3330(10) 0.096(9) Uani 1 1 d G . .
H55 H 1.1110 -0.1227 0.3236 0.115 Uiso 1 1 calc R . .
C56 C 1.0874(10) 0.0030(6) 0.3010(7) 0.052(4) Uani 1 1 d G . .
H56 H 1.0301 -0.0026 0.2703 0.062 Uiso 1 1 calc R . .
C61 C 1.1028(8) 0.2417(6) 0.2031(7) 0.056(5) Uani 1 1 d G . .
C62 C 1.1350(8) 0.2100(7) 0.1299(7) 0.052(4) Uani 1 1 d G . .
H62 H 1.1442 0.1514 0.1256 0.063 Uiso 1 1 calc R . .
C63 C 1.1536(8) 0.2633(7) 0.0633(7) 0.061(4) Uani 1 1 d G . .
H63 H 1.1752 0.2412 0.0144 0.073 Uiso 1 1 calc R . .
C64 C 1.1400(9) 0.3484(7) 0.0700(8) 0.054(4) Uani 1 1 d G . .
H64 H 1.1522 0.3854 0.0255 0.065 Uiso 1 1 calc R . .
C65 C 1.1079(10) 0.3801(6) 0.1432(8) 0.078(6) Uani 1 1 d G . .
H65 H 1.0987 0.4387 0.1475 0.093 Uiso 1 1 calc R . .
C66 C 1.0893(9) 0.3268(6) 0.2098(8) 0.059(5) Uani 1 1 d G . .
H66 H 1.0677 0.3488 0.2587 0.071 Uiso 1 1 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'
Pb Pb -3.3944 10.1111 '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'
P P 0.1023 0.0942 '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
S1 Pb S2 94.90(9) . . ?
S1 Pb S4' 91.2(3) . . ?
S2 Pb S4' 88.8(4) . . ?
S1 Pb S4 96.1(3) . . ?
S2 Pb S4 105.8(4) . . ?
S4' Pb S4 18.3(4) . . ?
S1 Pb S3' 85.5(4) . . ?
S2 Pb S3' 84.0(3) . . ?
S4' Pb S3' 171.7(3) . . ?
S4 Pb S3' 169.9(5) . . ?
C17 P1 C31 94.2(6) . . ?
C17 P1 C21 106.6(7) . . ?
C31 P1 C21 93.7(5) . . ?
C17 P1 S4 118.6(7) . . ?
C31 P1 S4 131.9(7) . . ?
C21 P1 S4 107.7(6) . . ?
C17 P1 S4' 114.7(7) . . ?
C31 P1 S4' 109.1(6) . . ?
C21 P1 S4' 130.3(6) . . ?
S4 P1 S4' 27.2(5) . . ?
C51 P2 C47 101.8(9) . . ?
C51 P2 C61 119.1(6) . . ?
C47 P2 C61 120.9(8) . . ?
C51 P2 S3' 116.6(7) . . ?
C47 P2 S3' 109.8(9) . . ?
C61 P2 S3' 89.0(7) . . ?
C51 P2 S3 88.6(6) . . ?
C47 P2 S3 109.8(8) . . ?
C61 P2 S3 111.8(6) . . ?
S3' P2 S3 29.5(6) . . ?
C11 S1 Pb 90.6(7) . . ?
C41 S2 Pb 90.0(5) . . ?
S3' S3 P2 73.9(10) . . ?
S4' S4 P1 77.4(12) . . ?
S4' S4 Pb 76.9(10) . . ?
P1 S4 Pb 115.3(6) . . ?
S3 S3' P2 76.6(11) . . ?
S3 S3' Pb 84.2(9) . . ?
P2 S3' Pb 121.7(6) . . ?
S4 S4' P1 75.5(11) . . ?
S4 S4' Pb 84.8(11) . . ?
P1 S4' Pb 117.4(5) . . ?
C16 C11 C12 115.0(15) . . ?
C16 C11 S1 118.0(15) . . ?
C12 C11 S1 127.0(15) . . ?
C13 C12 C11 120.4(13) . . ?
C13 C12 C17 121.3(13) . . ?
C11 C12 C17 118.1(14) . . ?
C14 C13 C12 123.1(16) . . ?
C15 C14 C13 116(2) . . ?
C14 C15 C16 122.3(18) . . ?
C15 C16 C11 122.7(17) . . ?
C12 C17 P1 106.4(10) . . ?
C26 C21 C22 119.7 . . ?
C26 C21 P1 120.2(6) . . ?
C22 C21 P1 119.8(6) . . ?
C23 C22 C21 121.2 . . ?
C24 C23 C22 119.2 . . ?
C23 C24 C25 119.7 . . ?
C26 C25 C24 121.2 . . ?
C21 C26 C25 119.2 . . ?
C32 C31 C36 120.6 . . ?
C32 C31 P1 121.6(6) . . ?
C36 C31 P1 117.9(6) . . ?
C33 C32 C31 119.2 . . ?
C32 C33 C34 120.2 . . ?
C35 C34 C33 120.6 . . ?
C36 C35 C34 119.2 . . ?
C35 C36 C31 120.2 . . ?
C46 C41 C42 120.5 . . ?
C46 C41 S2 118.9(8) . . ?
C42 C41 S2 120.4(8) . . ?
C43 C42 C41 120.1 . . ?
C43 C42 C47 116.5(12) . . ?
C41 C42 C47 123.1(12) . . ?
C42 C43 C44 119.3 . . ?
C43 C44 C45 120.5 . . ?
C46 C45 C44 120.1 . . ?
C45 C46 C41 119.4 . . ?
C42 C47 P2 123.7(14) . . ?
C56 C51 C52 120.4 . . ?
C56 C51 P2 120.8(7) . . ?
C52 C51 P2 118.8(7) . . ?
C53 C52 C51 120.8 . . ?
C54 C53 C52 118.8 . . ?
C53 C54 C55 120.4 . . ?
C56 C55 C54 120.8 . . ?
C51 C56 C55 118.8 . . ?
C66 C61 C62 119.7 . . ?
C66 C61 P2 118.3(6) . . ?
C62 C61 P2 121.6(6) . . ?
C63 C62 C61 121.3 . . ?
C64 C63 C62 119.0 . . ?
C63 C64 C65 119.7 . . ?
C66 C65 C64 121.3 . . ?
C61 C66 C65 119.0 . . ?
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
Pb S1 2.550(5) . ?
Pb S2 2.617(6) . ?
Pb S4' 2.885(12) . ?
Pb S4 2.950(12) . ?
Pb S3' 3.088(14) . ?
P1 C17 1.872(15) . ?
P1 C31 1.901(11) . ?
P1 C21 1.935(12) . ?
P1 S4 1.973(13) . ?
P1 S4' 1.989(14) . ?
P2 C51 1.694(12) . ?
P2 C47 1.74(2) . ?
P2 C61 1.771(12) . ?
P2 S3' 1.978(17) . ?
P2 S3 2.003(10) . ?
S1 C11 1.64(2) . ?
S2 C41 1.866(14) . ?
S3 S3' 1.01(2) . ?
S4 S4' 0.930(19) . ?
C11 C16 1.44(3) . ?
C11 C12 1.44(2) . ?
C12 C13 1.442(17) . ?
C12 C17 1.52(2) . ?
C13 C14 1.42(3) . ?
C14 C15 1.39(3) . ?
C15 C16 1.43(2) . ?
C21 C26 1.380(7) . ?
C21 C22 1.409(7) . ?
C22 C23 1.402(7) . ?
C23 C24 1.381(7) . ?
C24 C25 1.409(7) . ?
C25 C26 1.402(7) . ?
C31 C32 1.389(7) . ?
C31 C36 1.403(7) . ?
C32 C33 1.384(7) . ?
C33 C34 1.403(7) . ?
C34 C35 1.389(7) . ?
C35 C36 1.384(7) . ?
C41 C46 1.354(8) . ?
C41 C42 1.365(8) . ?
C42 C43 1.349(8) . ?
C42 C47 1.51(3) . ?
C43 C44 1.354(8) . ?
C44 C45 1.364(8) . ?
C45 C46 1.349(8) . ?
C51 C56 1.380(8) . ?
C51 C52 1.407(8) . ?
C52 C53 1.385(8) . ?
C53 C54 1.380(8) . ?
C54 C55 1.407(8) . ?
C55 C56 1.385(8) . ?
C61 C66 1.351(7) . ?
C61 C62 1.382(7) . ?
C62 C63 1.373(7) . ?
C63 C64 1.351(7) . ?
C64 C65 1.382(7) . ?
C65 C66 1.373(7) . ?
