#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/67/7026779.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_7026779
loop_
_publ_author_name
'Park, In-Hyeok'
'Park, Ki-Min'
'Lee, Shim Sung'
_publ_section_title
;
 Preparation and characterisation of divalent hard and soft metal (M = Ca,
 Co, Cu, Zn, Cd, Hg and Pb) complexes of 1,10-dithia-18-crown-6:
 structural versatility.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9696
_journal_page_last               9704
_journal_paper_doi               10.1039/c0dt00696c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C12 H24 Cl2 O12 Pb S2'
_chemical_formula_sum            'C12 H24 Cl2 O12 Pb S2'
_chemical_formula_weight         702.52
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.4210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4360(3)
_cell_length_b                   10.3907(3)
_cell_length_c                   12.0754(4)
_cell_measurement_reflns_used    5953
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.62
_cell_volume                     1029.57(6)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9350
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    8.715
_exptl_absorpt_correction_T_max  0.4211
_exptl_absorpt_correction_T_min  0.2103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0098(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2383
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0209
_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)+(0.0311P)²+0.3870P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0551
_reflns_number_gt                2147
_reflns_number_total             2383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00696c.txt
_cod_data_source_block           compound9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7026779
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
Pb1 Pb 0.5000 0.0000 0.0000 0.01434(9) Uani 1 2 d S
S1 S 0.44904(9) 0.28820(8) 0.04471(7) 0.01919(18) Uani 1 1 d .
O1 O 0.7513(2) 0.16026(19) 0.06122(19) 0.0210(5) Uani 1 1 d .
O2 O 0.8012(2) -0.10084(19) 0.09575(17) 0.0178(4) Uani 1 1 d .
C1 C 0.5861(4) 0.3227(3) -0.0478(3) 0.0199(7) Uani 1 1 d .
H1A H 0.5529 0.2732 -0.1194 0.024 Uiso 1 1 calc R
H1B H 0.5821 0.4155 -0.0668 0.024 Uiso 1 1 calc R
C2 C 0.7566(4) 0.2853(3) 0.0143(3) 0.0243(7) Uani 1 1 d .
H2A H 0.8297 0.2853 -0.0391 0.029 Uiso 1 1 calc R
H2B H 0.7994 0.3479 0.0758 0.029 Uiso 1 1 calc R
C3 C 0.9116(3) 0.1098(3) 0.1090(3) 0.0213(6) Uani 1 1 d .
H3A H 0.9772 0.1739 0.1607 0.026 Uiso 1 1 calc R
H3B H 0.9678 0.0901 0.0476 0.026 Uiso 1 1 calc R
C4 C 0.8933(5) -0.0104(2) 0.1736(4) 0.0198(8) Uani 1 1 d .
H4A H 1.0019 -0.0465 0.2090 0.024 Uiso 1 1 calc R
H4B H 0.8365 0.0091 0.2348 0.024 Uiso 1 1 calc R
C5 C 0.8059(3) -0.2284(3) 0.1424(2) 0.0199(6) Uani 1 1 d .
H5A H 0.7349 -0.2331 0.1970 0.024 Uiso 1 1 calc R
H5B H 0.9186 -0.2499 0.1834 0.024 Uiso 1 1 calc R
C6 C 0.7480(4) -0.3225(3) 0.0467(3) 0.0223(7) Uani 1 1 d .
H6A H 0.7443 -0.4092 0.0799 0.027 Uiso 1 1 calc R
H6B H 0.8294 -0.3251 -0.0006 0.027 Uiso 1 1 calc R
Cl1 Cl 0.37703(9) -0.03220(8) 0.25093(7) 0.01743(16) Uani 1 1 d .
O3 O 0.5333(3) -0.0529(3) 0.2214(2) 0.0359(6) Uani 1 1 d .
O4 O 0.3027(3) -0.1536(2) 0.2617(2) 0.0440(7) Uani 1 1 d .
O5 O 0.2811(4) 0.0366(4) 0.1622(3) 0.0600(9) Uani 1 1 d U
O6 O 0.4029(6) 0.0339(4) 0.3537(4) 0.0761(14) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O1 Pb1 O1 180.0 3_655 .
O1 Pb1 O3 92.35(7) 3_655 .
O1 Pb1 O3 87.65(7) . .
O1 Pb1 O3 87.65(7) 3_655 3_655
O1 Pb1 O3 92.35(7) . 3_655
O3 Pb1 O3 180.0 . 3_655
O1 Pb1 O2 118.56(5) 3_655 .
O1 Pb1 O2 61.44(5) . .
O3 Pb1 O2 68.21(6) . .
O3 Pb1 O2 111.79(6) 3_655 .
O1 Pb1 O2 61.44(5) 3_655 3_655
O1 Pb1 O2 118.56(5) . 3_655
O3 Pb1 O2 111.79(6) . 3_655
O3 Pb1 O2 68.21(6) 3_655 3_655
O2 Pb1 O2 180.0 . 3_655
O1 Pb1 S1 121.37(5) 3_655 .
O1 Pb1 S1 58.63(5) . .
O3 Pb1 S1 90.64(7) . .
O3 Pb1 S1 89.36(7) 3_655 .
O2 Pb1 S1 116.69(4) . .
O2 Pb1 S1 63.31(4) 3_655 .
O1 Pb1 S1 58.63(5) 3_655 3_655
O1 Pb1 S1 121.37(5) . 3_655
O3 Pb1 S1 89.36(7) . 3_655
O3 Pb1 S1 90.64(7) 3_655 3_655
O2 Pb1 S1 63.31(4) . 3_655
O2 Pb1 S1 116.69(4) 3_655 3_655
S1 Pb1 S1 180.0 . 3_655
C6 S1 C1 102.22(16) 3_655 .
C6 S1 Pb1 103.29(11) 3_655 .
C1 S1 Pb1 87.14(10) . .
C2 O1 C3 112.3(2) . .
C2 O1 Pb1 123.89(18) . .
C3 O1 Pb1 119.76(16) . .
C4 O2 C5 112.8(2) . .
C4 O2 Pb1 109.64(17) . .
C5 O2 Pb1 117.14(16) . .
C2 C1 S1 108.2(2) . .
O1 C2 C1 108.6(2) . .
O1 C3 C4 108.2(2) . .
O2 C4 C3 108.2(3) . .
O2 C5 C6 108.9(2) . .
C5 C6 S1 115.5(2) . 3_655
O5 Cl1 O6 112.3(3) . .
O5 Cl1 O4 109.7(2) . .
O6 Cl1 O4 109.6(2) . .
O5 Cl1 O3 106.65(18) . .
O6 Cl1 O3 109.1(2) . .
O4 Cl1 O3 109.42(16) . .
Cl1 O3 Pb1 108.78(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.6621(19) 3_655
Pb1 O1 2.6622(19) .
Pb1 O3 2.680(2) .
Pb1 O3 2.680(2) 3_655
Pb1 O2 2.744(2) .
Pb1 O2 2.744(2) 3_655
Pb1 S1 3.0906(8) .
Pb1 S1 3.0906(8) 3_655
S1 C6 1.805(3) 3_655
S1 C1 1.820(3) .
O1 C2 1.422(4) .
O1 C3 1.440(3) .
O2 C4 1.425(4) .
O2 C5 1.437(3) .
C1 C2 1.511(4) .
C3 C4 1.499(4) .
C5 C6 1.505(4) .
C6 S1 1.805(3) 3_655
Cl1 O5 1.382(3) .
Cl1 O6 1.391(4) .
Cl1 O4 1.428(2) .
Cl1 O3 1.459(2) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139162344
