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#$Date: 2016-03-25 13:49:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179865 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/61/7016106.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_7016106
loop_
_publ_author_name
'Clark, J. M.'
'Kociok-Köhn, G'
'Harnett, N. J.'
'Hill, M. S.'
'Hill, R.'
'Molloy, K. C.'
'Saponia, H.'
'Stanton, D.'
'Sudlow, A.'
_publ_section_title
;
 Formation of PbS materials from lead xanthate precursors.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6893
_journal_page_last               6900
_journal_paper_doi               10.1039/c1dt10273g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C32 H36 N4 O4 Pb2 S8'
_chemical_formula_sum            'C32 H36 N4 O4 Pb2 S8'
_chemical_formula_weight         1211.51
_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                112.535(4)
_cell_angle_beta                 111.534(4)
_cell_angle_gamma                94.306(3)
_cell_formula_units_Z            1
_cell_length_a                   10.1779(6)
_cell_length_b                   10.5781(6)
_cell_length_c                   11.4041(8)
_cell_measurement_reflns_used    52785
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     1021.09(12)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
DENZO-SCALEPACK Z. Otwinowski and W. Minor, "
Processing of X-ray Diffraction Data Collected in Oscillation Mode ",
Methods in Enzymology, Volume 276: Macromolecular Crystallography,
part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
'WinGX publication routines, Farrugia,
L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
SHELXL97 -Program for Crystal Structure Analysis (Release 97-2).
Sheldrick, G.M., Institüt für Anorganische Chemie der Universität,
Tammanstrasse 4, D-3400 Göttingen, Germany, 1998
;
_computing_structure_solution
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '257 2.0 degree images with ω scans'
_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  0.0934
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15152
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.682
_exptl_absorpt_correction_T_max  0.4772
_exptl_absorpt_correction_T_min  0.3559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.617
_refine_diff_density_min         -3.382
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       0.0115(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0593
_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)+(0.0878P)²+6.0044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                4569
_reflns_number_total             5495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10273g.txt
_cod_data_source_block           h09kcm33
_cod_original_cell_volume        1021.09(11)
_cod_database_code               7016106
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
Pb Pb 0.11519(3) 0.13238(3) 0.18824(3) 0.03692(16) Uani 1 1 d . A .
S1 S 0.0647(3) 0.3407(3) 0.4079(3) 0.0573(7) Uani 1 1 d . . .
S2 S 0.1151(3) 0.0677(3) 0.4118(3) 0.0556(6) Uani 1 1 d . . .
S3 S -0.2220(2) 0.0362(3) 0.0583(3) 0.0420(5) Uani 1 1 d . . .
S4 S -0.0942(2) 0.1947(2) -0.0595(3) 0.0403(5) Uani 1 1 d . . .
O2 O -0.3319(7) 0.2160(8) -0.0362(8) 0.0433(14) Uani 1 1 d . . .
N1 N 0.4019(8) 0.1713(8) 0.3261(8) 0.0392(15) Uani 1 1 d . . .
N2 N 0.3017(8) 0.3677(8) 0.2423(9) 0.0441(17) Uani 1 1 d . . .
C1 C 0.0991(11) 0.2346(13) 0.4878(12) 0.057(3) Uani 1 1 d . A .
O1 O 0.1194(12) 0.2686(12) 0.6210(11) 0.048(3) Uani 0.75(3) 1 d P A 1
C2 C 0.1007(18) 0.4063(15) 0.7002(18) 0.054(4) Uani 0.75(3) 1 d P A 1
H2A H 0.1719 0.4826 0.7094 0.064 Uiso 0.75(3) 1 calc PR A 1
H2B H 0.0012 0.4140 0.6504 0.064 Uiso 0.75(3) 1 calc PR A 1
C3 C 0.124(2) 0.4203(19) 0.8389(19) 0.051(4) Uani 0.75(3) 1 d P A 1
H3A H 0.1113 0.5123 0.8934 0.077 Uiso 0.75(3) 1 calc PR A 1
H3B H 0.2225 0.4133 0.8877 0.077 Uiso 0.75(3) 1 calc PR A 1
H3C H 0.0523 0.3447 0.8289 0.077 Uiso 0.75(3) 1 calc PR A 1
O1A O 0.092(4) 0.348(4) 0.597(4) 0.064(13) Uani 0.25(3) 1 d P A 2
C2A C 0.114(8) 0.285(7) 0.689(8) 0.073(17) Uiso 0.25(3) 1 d P A 2
H2C H 0.2142 0.2721 0.7199 0.088 Uiso 0.25(3) 1 calc PR A 2
H2D H 0.0452 0.1900 0.6381 0.088 Uiso 0.25(3) 1 calc PR A 2
C3A C 0.091(9) 0.372(8) 0.820(8) 0.07(2) Uiso 0.25(3) 1 d P A 2
H3D H 0.1072 0.3236 0.8801 0.106 Uiso 0.25(3) 1 calc PR A 2
H3E H -0.0093 0.3833 0.7908 0.106 Uiso 0.25(3) 1 calc PR A 2
H3F H 0.1597 0.4656 0.8726 0.106 Uiso 0.25(3) 1 calc PR A 2
C4 C -0.2253(9) 0.1518(9) -0.0104(10) 0.0370(17) Uani 1 1 d . A .
C5 C -0.4545(11) 0.1827(12) -0.0070(13) 0.051(2) Uani 1 1 d . A .
H5A H -0.4202 0.2036 0.0933 0.061 Uiso 1 1 calc R . .
H5B H -0.5064 0.0815 -0.0655 0.061 Uiso 1 1 calc R . .
C6 C -0.5535(13) 0.2743(14) -0.0422(16) 0.062(3) Uani 1 1 d . . .
H6A H -0.4985 0.3737 0.0115 0.093 Uiso 1 1 calc R A .
H6B H -0.6347 0.2609 -0.0180 0.093 Uiso 1 1 calc R . .
H6C H -0.5916 0.2479 -0.1430 0.093 Uiso 1 1 calc R . .
C7 C 0.4459(11) 0.0639(10) 0.3519(11) 0.0432(19) Uani 1 1 d . A .
H7 H 0.3756 -0.0087 0.3416 0.052 Uiso 1 1 calc R . .
C8 C 0.5890(12) 0.0550(11) 0.3927(11) 0.048(2) Uani 1 1 d . . .
H8 H 0.6166 -0.0223 0.4097 0.057 Uiso 1 1 calc R A .
C9 C 0.6913(11) 0.1610(12) 0.4082(12) 0.050(2) Uani 1 1 d . A .
H9 H 0.7904 0.1570 0.4352 0.060 Uiso 1 1 calc R . .
C10 C 0.6480(10) 0.2730(11) 0.3840(12) 0.048(2) Uani 1 1 d . . .
H10 H 0.7170 0.3478 0.3958 0.058 Uiso 1 1 calc R A .
C11 C 0.5006(9) 0.2743(10) 0.3418(10) 0.0389(18) Uani 1 1 d . A .
C12 C 0.4451(9) 0.3908(9) 0.3103(10) 0.0398(18) Uani 1 1 d . A .
C13 C 0.5412(10) 0.5194(10) 0.3524(11) 0.046(2) Uani 1 1 d . . .
H13 H 0.6431 0.5369 0.4058 0.055 Uiso 1 1 calc R A .
C14 C 0.4835(13) 0.6189(11) 0.3142(12) 0.053(2) Uani 1 1 d . A .
H14 H 0.5464 0.7049 0.3385 0.064 Uiso 1 1 calc R . .
C15 C 0.3349(12) 0.5943(10) 0.2407(12) 0.049(2) Uani 1 1 d . . .
H15 H 0.2932 0.6621 0.2142 0.059 Uiso 1 1 calc R A .
C16 C 0.2490(11) 0.4662(10) 0.2070(12) 0.048(2) Uani 1 1 d . A .
H16 H 0.1464 0.4475 0.1558 0.057 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'
O O 0.0106 0.0060 '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'
N N 0.0061 0.0033 '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'
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
N1 Pb N2 60.5(2) . . ?
N1 Pb S1 99.22(18) . . ?
N2 Pb S1 80.49(19) . . ?
N1 Pb S2 81.35(18) . . ?
N2 Pb S2 121.3(2) . . ?
S1 Pb S2 62.43(9) . . ?
N1 Pb S3 166.11(18) . . ?
N2 Pb S3 132.55(18) . . ?
S1 Pb S3 80.70(7) . . ?
S2 Pb S3 86.41(7) . . ?
C1 S1 Pb 86.3(4) . . ?
O1A S1 Pb 128.4(11) . . ?
C1 S2 Pb 85.9(5) . . ?
C4 S3 Pb 87.0(3) . . ?
C4 O2 C5 118.6(7) . . ?
C11 N1 C7 118.9(8) . . ?
C11 N1 Pb 122.9(6) . . ?
C7 N1 Pb 116.5(6) . . ?
C12 N2 C16 118.6(8) . . ?
C12 N2 Pb 121.3(6) . . ?
C16 N2 Pb 120.0(6) . . ?
O1 C1 S1 125.8(9) . . ?
O1A C1 S1 83(2) . . ?
O1 C1 S2 109.8(10) . . ?
O1A C1 S2 153(2) . . ?
S1 C1 S2 124.4(7) . . ?
C1 O1 C2 117.3(11) . . ?
C3 C2 O1 108.5(12) . . ?
C3 C2 H2A 110.0 . . ?
O1 C2 H2A 110.0 . . ?
C3 C2 H2B 110.0 . . ?
O1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 O1A C2A 97(4) . . ?
C1 O1A S1 54.8(15) . . ?
C2A O1A S1 151(4) . . ?
O1A C2A C3A 113(5) . . ?
O1A C2A H2C 109.0 . . ?
C3A C2A H2C 109.0 . . ?
O1A C2A H2D 109.0 . . ?
C3A C2A H2D 109.0 . . ?
H2C C2A H2D 107.8 . . ?
C2A C3A H3D 109.5 . . ?
C2A C3A H3E 109.5 . . ?
H3D C3A H3E 109.5 . . ?
C2A C3A H3F 109.5 . . ?
H3D C3A H3F 109.5 . . ?
H3E C3A H3F 109.5 . . ?
O2 C4 S3 123.3(6) . . ?
O2 C4 S4 113.0(7) . . ?
S3 C4 S4 123.6(5) . . ?
O2 C5 C6 106.1(9) . . ?
O2 C5 H5A 110.5 . . ?
C6 C5 H5A 110.5 . . ?
O2 C5 H5B 110.5 . . ?
C6 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 C8 122.7(9) . . ?
N1 C7 H7 118.7 . . ?
C8 C7 H7 118.7 . . ?
C7 C8 C9 118.6(9) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
C8 C9 C10 119.4(9) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C11 118.8(9) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N1 C11 C10 121.6(9) . . ?
N1 C11 C12 116.6(8) . . ?
C10 C11 C12 121.8(8) . . ?
N2 C12 C13 121.5(9) . . ?
N2 C12 C11 117.0(8) . . ?
C13 C12 C11 121.4(8) . . ?
C14 C13 C12 118.4(9) . . ?
C14 C13 H13 120.8 . . ?
C12 C13 H13 120.8 . . ?
C15 C14 C13 120.3(9) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 117.1(9) . . ?
C14 C15 H15 121.5 . . ?
C16 C15 H15 121.5 . . ?
N2 C16 C15 124.0(9) . . ?
N2 C16 H16 118.0 . . ?
C15 C16 H16 118.0 . . ?
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 N1 2.667(7) . ?
Pb N2 2.727(8) . ?
Pb S1 2.877(3) . ?
Pb S2 2.882(3) . ?
Pb S3 3.098(2) . ?
S1 C1 1.680(15) . ?
S1 O1A 2.04(4) . ?
S2 C1 1.693(12) . ?
S3 C4 1.683(9) . ?
S4 C4 1.718(8) . ?
O2 C4 1.324(11) . ?
O2 C5 1.456(12) . ?
N1 C11 1.335(11) . ?
N1 C7 1.346(12) . ?
N2 C12 1.327(12) . ?
N2 C16 1.335(13) . ?
C1 O1 1.349(16) . ?
C1 O1A 1.39(3) . ?
O1 C2 1.461(18) . ?
C2 C3 1.46(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
O1A C2A 1.41(9) . ?
C2A C3A 1.54(11) . ?
C2A H2C 0.9900 . ?
C2A H2D 0.9900 . ?
C3A H3D 0.9800 . ?
C3A H3E 0.9800 . ?
C3A H3F 0.9800 . ?
C5 C6 1.504(14) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.379(14) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(15) . ?
C8 H8 0.9500 . ?
C9 C10 1.383(15) . ?
C9 H9 0.9500 . ?
C10 C11 1.400(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.504(13) . ?
C12 C13 1.412(12) . ?
C13 C14 1.379(15) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(16) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(14) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
