#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:14:25 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180418 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/87/7208745.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_7208745
loop_
_publ_author_name
'Park, Sunhong'
'Lee, Seul-Gi'
'Jung, Jong Hwa'
'Ikeda, Mari'
'Habata, Yoichi'
'Lee, Shim Sun'
_publ_section_title
;
 Macrocycles incorporating isomeric arms: synthesis and crystal structures
 of ligands and their mono-, di- and polynuclear supramolecular complexes
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6515
_journal_paper_doi               10.1039/c2ce25708d
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C19 H24 Cl2 N2 O9 Pb S2'
_chemical_formula_weight         766.61
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 117.185(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5333(12)
_cell_length_b                   10.1786(7)
_cell_length_c                   16.9387(12)
_cell_measurement_reflns_used    9577
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.89
_cell_measurement_theta_min      2.34
_cell_volume                     2535.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44906
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.081
_exptl_absorpt_correction_T_max  0.6760
_exptl_absorpt_correction_T_min  0.4164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.283
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0491P)²+6.4746P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                5004
_reflns_number_total             5242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25708d.txt
_cod_data_source_block           7
_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               7208745
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 -0.167801(10) -0.108842(14) -0.979365(10) 0.02265(7) Uani 1 1 d .
Cl1 Cl -0.08499(6) -0.02394(9) -1.14154(6) 0.0233(2) Uani 1 1 d .
Cl2 Cl -0.16538(11) -0.20504(13) -0.60745(11) 0.0536(4) Uani 1 1 d .
O1 O -0.1838(3) 0.0228(4) -0.8632(3) 0.0559(11) Uani 1 1 d .
O2 O -0.0278(2) 0.0771(4) -1.1472(3) 0.0424(9) Uani 1 1 d .
O3 O -0.0333(3) -0.1143(3) -1.0717(2) 0.0403(9) Uani 1 1 d .
O4 O -0.1282(3) -0.0926(3) -1.2247(2) 0.0371(8) Uani 1 1 d .
O5 O -0.1541(2) 0.0354(3) -1.1231(2) 0.0348(7) Uani 1 1 d .
O6 O -0.2272(8) -0.1482(8) -0.6858(5) 0.142(4) Uani 1 1 d .
O7 O -0.0806(6) -0.1624(8) -0.5905(11) 0.219(7) Uani 1 1 d .
O8 O -0.1647(3) -0.3460(4) -0.6137(4) 0.0682(14) Uani 1 1 d .
O9 O -0.1937(7) -0.1725(6) -0.5455(5) 0.126(3) Uani 1 1 d .
S1 S -0.07570(7) -0.28217(10) -0.81437(7) 0.0262(2) Uani 1 1 d .
S2 S -0.26819(7) -0.24918(10) -1.15389(7) 0.0257(2) Uani 1 1 d .
N1 N -0.2903(2) -0.2496(3) -0.9675(2) 0.0240(7) Uani 1 1 d .
N2 N -0.3208(2) -0.0034(3) -1.0614(2) 0.0262(7) Uani 1 1 d .
C1 C -0.0537(3) -0.4692(4) -0.9214(3) 0.0246(8) Uani 1 1 d .
C2 C -0.0745(3) -0.6021(4) -0.9227(4) 0.0332(11) Uani 1 1 d .
H2A H -0.0514 -0.6498 -0.8701 0.040 Uiso 1 1 calc R
C3 C -0.1300(3) -0.6633(4) -1.0030(4) 0.0377(11) Uani 1 1 d .
H3A H -0.1408 -0.7531 -1.0041 0.045 Uiso 1 1 calc R
C4 C -0.1689(3) -0.5930(4) -1.0802(3) 0.0309(10) Uani 1 1 d .
H4A H -0.2089 -0.6338 -1.1328 0.037 Uiso 1 1 calc R
C5 C -0.1485(3) -0.4605(4) -1.0800(3) 0.0253(8) Uani 1 1 d .
C6 C -0.0877(3) -0.4023(4) -1.0013(3) 0.0243(9) Uani 1 1 d .
H6A H -0.0693 -0.3161 -1.0020 0.029 Uiso 1 1 calc R
C7 C -0.1956(3) -0.3769(4) -1.1642(3) 0.0284(9) Uani 1 1 d .
H7A H -0.2323 -0.4335 -1.2139 0.034 Uiso 1 1 calc R
H7B H -0.1498 -0.3359 -1.1768 0.034 Uiso 1 1 calc R
C8 C -0.3461(3) -0.3372(5) -1.1244(3) 0.0299(9) Uani 1 1 d .
H8A H -0.4034 -0.3632 -1.1673 0.036 Uiso 1 1 calc R
C9 C -0.3140(3) -0.3661(4) -1.0277(3) 0.0284(9) Uani 1 1 d .
H9A H -0.3611 -0.4155 -1.0218 0.034 Uiso 1 1 calc R
H9B H -0.2609 -0.4223 -1.0074 0.034 Uiso 1 1 calc R
C10 C -0.3724(3) -0.1678(5) -0.9888(3) 0.0317(10) Uani 1 1 d .
H10A H -0.3664 -0.1293 -0.9341 0.038 Uiso 1 1 calc R
H10B H -0.4249 -0.2254 -1.0111 0.038 Uiso 1 1 calc R
C11 C -0.3914(3) -0.0585(4) -1.0554(3) 0.0245(8) Uani 1 1 d .
C12 C -0.4789(3) -0.0095(4) -1.1018(3) 0.0319(10) Uani 1 1 d .
H12A H -0.5274 -0.0517 -1.0989 0.038 Uiso 1 1 calc R
C13 C -0.4933(3) 0.1023(4) -1.1523(4) 0.0356(11) Uani 1 1 d .
H13A H -0.5512 0.1383 -1.1822 0.043 Uiso 1 1 calc R
C14 C -0.4196(3) 0.1610(4) -1.1577(3) 0.0332(10) Uani 1 1 d .
H14A H -0.4273 0.2369 -1.1910 0.040 Uiso 1 1 calc R
C15 C -0.3356(3) 0.1037(4) -1.1129(3) 0.0301(10) Uani 1 1 d .
H15A H -0.2868 0.1404 -1.1182 0.036 Uiso 1 1 calc R
C16 C -0.2599(3) -0.2975(5) -0.8737(3) 0.0297(9) Uani 1 1 d .
H16A H -0.3091 -0.3485 -0.8728 0.036 Uiso 1 1 calc R
H16B H -0.2508 -0.2214 -0.8360 0.036 Uiso 1 1 calc R
C17 C -0.1744(3) -0.3800(4) -0.8330(3) 0.0293(10) Uani 1 1 d .
H17A H -0.1800 -0.4526 -0.8723 0.035 Uiso 1 1 calc R
H17B H -0.1667 -0.4162 -0.7770 0.035 Uiso 1 1 calc R
C18 C -0.0027(3) -0.3957(4) -0.8370(3) 0.0280(10) Uani 1 1 d .
H18A H 0.0460 -0.3465 -0.8402 0.034 Uiso 1 1 calc R
H18B H 0.0246 -0.4578 -0.7884 0.034 Uiso 1 1 calc R
C19 C -0.1122(6) 0.0645(8) -0.7803(5) 0.072(2) Uani 1 1 d .
H19A H -0.1372 0.1141 -0.7484 0.108 Uiso 1 1 calc R
H19B H -0.0703 0.1184 -0.7906 0.108 Uiso 1 1 calc R
H19C H -0.0808 -0.0110 -0.7460 0.108 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'
N N 0.0061 0.0033 '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
O1 Pb1 N2 76.30(14)
O1 Pb1 N1 82.32(13)
N2 Pb1 N1 69.43(11)
O1 Pb1 S2 145.20(11)
N2 Pb1 S2 72.19(9)
N1 Pb1 S2 73.17(8)
O1 Pb1 S1 77.11(11)
N2 Pb1 S1 135.18(9)
N1 Pb1 S1 71.78(8)
S2 Pb1 S1 116.41(3)
O2 Cl1 O3 110.7(2)
O2 Cl1 O4 109.4(2)
O3 Cl1 O4 109.8(2)
O2 Cl1 O5 109.0(2)
O3 Cl1 O5 108.8(2)
O4 Cl1 O5 109.1(2)
O7 Cl2 O9 116.0(8)
O7 Cl2 O6 107.9(8)
O9 Cl2 O6 105.8(5)
O7 Cl2 O8 106.9(4)
O9 Cl2 O8 108.3(4)
O6 Cl2 O8 112.0(5)
C19 O1 Pb1 126.7(4)
C17 S1 C18 104.1(2)
C17 S1 Pb1 97.21(15)
C18 S1 Pb1 105.83(16)
C8 S2 C7 104.7(2)
C8 S2 Pb1 96.10(15)
C7 S2 Pb1 109.85(15)
C10 N1 C9 110.6(3)
C10 N1 C16 105.3(3)
C9 N1 C16 108.6(3)
C10 N1 Pb1 109.5(2)
C9 N1 Pb1 111.1(2)
C16 N1 Pb1 111.6(2)
C11 N2 C15 118.8(4)
C11 N2 Pb1 118.2(3)
C15 N2 Pb1 123.0(3)
C6 C1 C2 118.4(4)
C6 C1 C18 119.4(4)
C2 C1 C18 122.1(4)
C3 C2 C1 119.9(4)
C4 C3 C2 120.8(4)
C3 C4 C5 119.9(4)
C6 C5 C4 119.1(4)
C6 C5 C7 119.7(4)
C4 C5 C7 121.1(4)
C1 C6 C5 121.5(4)
C5 C7 S2 112.4(3)
C9 C8 S2 117.0(3)
N1 C9 C8 116.1(4)
N1 C10 C11 116.7(3)
N2 C11 C12 121.7(4)
N2 C11 C10 118.2(4)
C12 C11 C10 119.7(4)
C13 C12 C11 119.3(4)
C12 C13 C14 119.0(4)
C15 C14 C13 118.3(4)
N2 C15 C14 122.7(4)
N1 C16 C17 116.8(4)
C16 C17 S1 110.7(3)
C1 C18 S1 112.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pb1 O1 2.492(4)
Pb1 N2 2.504(3)
Pb1 N1 2.563(3)
Pb1 S2 3.0085(11)
Pb1 S1 3.0583(11)
Cl1 O2 1.430(3)
Cl1 O3 1.432(3)
Cl1 O4 1.437(4)
Cl1 O5 1.446(3)
Cl2 O7 1.366(8)
Cl2 O9 1.372(6)
Cl2 O6 1.379(7)
Cl2 O8 1.439(4)
O1 C19 1.427(9)
S1 C17 1.812(5)
S1 C18 1.835(5)
S2 C8 1.817(5)
S2 C7 1.831(5)
N1 C10 1.488(5)
N1 C9 1.495(6)
N1 C16 1.512(5)
N2 C11 1.339(5)
N2 C15 1.347(6)
C1 C6 1.384(6)
C1 C2 1.393(6)
C1 C18 1.487(6)
C2 C3 1.393(7)
C3 C4 1.366(7)
C4 C5 1.390(6)
C5 C6 1.384(6)
C5 C7 1.533(6)
C8 C9 1.502(7)
C10 C11 1.511(6)
C11 C12 1.386(6)
C12 C13 1.377(7)
C13 C14 1.399(7)
C14 C15 1.371(7)
C16 C17 1.514(6)
