#------------------------------------------------------------------------------
#$Date: 2020-09-11 05:13:52 +0300 (Fri, 11 Sep 2020) $
#$Revision: 256335 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/12/7241208.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_7241208
loop_
_publ_author_name
'Hammer, Arden C.'
'Jia, Xiwen'
'Zeller, Matthias'
'Coughlin, Ezra John'
'Zhang, Weiguo'
'Oertel, Catherine M.'
_publ_section_title
;
 Ligand Geometry Directs the Packing and Symmetry of One-Dimensional
 Helical Motifs in Lead Oxide Naphthoates and Biphenylcarboxylates
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01150A
_journal_year                    2020
_chemical_formula_sum            'C176 H112 O41.42 Pb16'
_chemical_formula_weight         6204.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-11-22 deposited with the CCDC.	2020-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.8392(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.3686(18)
_cell_length_b                   10.8690(5)
_cell_length_c                   27.3181(13)
_cell_measurement_reflns_used    9088
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      42.8911
_cell_measurement_theta_min      2.9178
_cell_volume                     8293.5(7)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2016/6 (Sheldrick, 2015, 2016), 
SHELXLE Rev714 (Hübschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            60989
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    16.250
_exptl_absorpt_correction_T_max  0.1081
_exptl_absorpt_correction_T_min  0.0365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.485
_exptl_crystal_description       block
_exptl_crystal_F_000             5623
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.163
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         12660
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0134P)²+64.6381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11570
_reflns_number_total             12660
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01150a2.cif
_cod_data_source_block           lead_oxide_2-naphthoate_hydrate(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7241208
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.101
_shelx_estimated_absorpt_t_max   0.246
loop_
_space_group_symop_operation_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'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.31122(2) 0.85098(2) 0.30290(2) 0.01811(3) Uani 1 1 d . . . . .
Pb2 Pb 0.24031(2) 0.61949(2) 0.17060(2) 0.01851(3) Uani 1 1 d . . . . .
Pb3 Pb 0.20510(2) 0.95280(2) 0.16349(2) 0.01831(3) Uani 1 1 d . . . . .
Pb4 Pb 0.19090(2) 0.67925(2) 0.24408(2) 0.01882(3) Uani 1 1 d . . . . .
O1 O 0.23703(9) 0.7778(2) 0.22348(12) 0.0175(5) Uani 1 1 d . . . . .
O2 O 0.26775(9) 1.0247(2) 0.26023(12) 0.0167(5) Uani 1 1 d . . . . .
O3 O 0.33195(13) 0.9313(3) 0.23418(17) 0.0361(8) Uani 1 1 d . . . . .
O4 O 0.26319(13) 0.8627(3) 0.14737(19) 0.0388(8) Uani 1 1 d . . . . .
O5 O 0.16032(11) 0.7575(3) 0.08321(15) 0.0322(7) Uani 1 1 d . . . . .
O6 O 0.15120(12) 0.6060(3) 0.12862(15) 0.0347(7) Uani 1 1 d . . . . .
O7 O 0.15410(12) 0.9292(3) 0.19749(18) 0.0364(8) Uani 1 1 d . . . . .
O8 O 0.17194(11) 1.1225(3) 0.23210(18) 0.0373(8) Uani 1 1 d . . . . .
O9 O 0.25852(13) 0.6684(3) 0.35159(14) 0.0341(8) Uani 1 1 d . . . . .
O10 O 0.28012(13) 0.8656(3) 0.36606(16) 0.0318(7) Uani 1 1 d . . . . .
O11 O 0.4323(5) 0.9209(13) 0.3470(7) 0.047(4) Uani 0.311(13) 1 d D . P . .
H11A H 0.431(7) 0.850(9) 0.357(9) 0.070 Uiso 0.311(13) 1 d D U P . .
H11B H 0.405(3) 0.942(17) 0.316(7) 0.070 Uiso 0.311(13) 1 d D U P . .
C1 C 0.30677(17) 0.8913(4) 0.1789(2) 0.0302(9) Uani 1 1 d . . . . .
C2 C 0.33049(15) 0.8747(4) 0.1486(2) 0.0258(8) Uani 1 1 d . . . . .
C3 C 0.37621(15) 0.9164(4) 0.1777(2) 0.0279(9) Uani 1 1 d . . . . .
H3 H 0.392832 0.955604 0.216938 0.033 Uiso 1 1 calc R U . . .
C4 C 0.39914(16) 0.9013(5) 0.1494(2) 0.0305(9) Uani 1 1 d . . . . .
C5 C 0.4447(2) 0.9506(7) 0.1764(3) 0.0555(18) Uani 1 1 d . . . . .
H5 H 0.460951 0.994621 0.214349 0.067 Uiso 1 1 calc R U . . .
C6 C 0.4662(2) 0.9357(8) 0.1482(3) 0.067(2) Uani 1 1 d . . . . .
H6 H 0.496977 0.969727 0.166757 0.080 Uiso 1 1 calc R U . . .
C7 C 0.39770(19) 0.8240(5) 0.0647(2) 0.0374(11) Uani 1 1 d . . . . .
H7 H 0.381903 0.780450 0.026671 0.045 Uiso 1 1 calc R U . . .
C8 C 0.37447(17) 0.8401(4) 0.0922(2) 0.0289(9) Uani 1 1 d . . . . .
C9 C 0.32727(17) 0.7989(5) 0.0630(2) 0.0340(10) Uani 1 1 d . . . . .
H9 H 0.310295 0.758343 0.024050 0.041 Uiso 1 1 calc R U . . .
C10 C 0.30570(16) 0.8171(5) 0.0904(2) 0.0328(10) Uani 1 1 d . . . . .
H10 H 0.273662 0.790423 0.069793 0.039 Uiso 1 1 calc R U . . .
C11 C 0.13421(15) 0.6949(4) 0.09019(19) 0.0278(9) Uani 1 1 d . . . . .
C12 C 0.08226(15) 0.7272(4) 0.0536(2) 0.0272(8) Uani 1 1 d . . . . .
C13 C 0.05245(17) 0.6545(4) 0.0572(2) 0.0313(9) Uani 1 1 d . . . . .
H13 H 0.064784 0.582858 0.082359 0.038 Uiso 1 1 calc R U . . .
C14 C 0.00321(17) 0.6849(5) 0.0236(2) 0.0337(10) Uani 1 1 d . . . . .
C15 C -0.0283(2) 0.6122(6) 0.0270(3) 0.0499(15) Uani 1 1 d . . . . .
H15 H -0.017050 0.539342 0.051307 0.060 Uiso 1 1 calc R U . . .
C16 C -0.0753(2) 0.6478(7) -0.0053(3) 0.0570(18) Uani 1 1 d . . . . .
H16 H -0.096450 0.597930 -0.003427 0.068 Uiso 1 1 calc R U . . .
C17 C -0.09229(19) 0.7532(8) -0.0399(3) 0.0561(18) Uani 1 1 d . . . . .
H17 H -0.124605 0.776930 -0.060154 0.067 Uiso 1 1 calc R U . . .
C18 C -0.06341(19) 0.8255(7) -0.0458(3) 0.0512(16) Uani 1 1 d . . . . .
H18 H -0.075954 0.897112 -0.071035 0.061 Uiso 1 1 calc R U . . .
C19 C -0.01431(17) 0.7921(6) -0.0137(2) 0.0386(11) Uani 1 1 d . . . . .
C20 C 0.0174(2) 0.8650(6) -0.0172(3) 0.0433(13) Uani 1 1 d . . . . .
H20 H 0.005722 0.936317 -0.042652 0.052 Uiso 1 1 calc R U . . .
C21 C 0.06448(18) 0.8329(5) 0.0159(2) 0.0358(10) Uani 1 1 d . . . . .
H21 H 0.085427 0.882455 0.013547 0.043 Uiso 1 1 calc R U . . .
C22 C 0.14394(15) 1.0299(4) 0.2099(2) 0.0265(8) Uani 1 1 d . . . . .
C23 C 0.09677(14) 1.0421(4) 0.19758(19) 0.0228(8) Uani 1 1 d . . . . .
C24 C 0.06316(15) 0.9505(4) 0.1669(2) 0.0288(9) Uani 1 1 d . . . . .
H24 H 0.070194 0.879373 0.153572 0.035 Uiso 1 1 calc R U . . .
C25 C 0.01821(17) 0.9605(5) 0.1547(2) 0.0362(11) Uani 1 1 d . . . . .
C26 C -0.0174(2) 0.8687(8) 0.1215(4) 0.073(3) Uani 1 1 d . . . . .
H26 H -0.011252 0.797357 0.107308 0.088 Uiso 1 1 calc R U . . .
C27 C -0.0610(3) 0.8825(9) 0.1098(5) 0.091(3) Uani 1 1 d . . . . .
H27 H -0.085190 0.822109 0.086211 0.110 Uiso 1 1 calc R U . . .
C28 C -0.0696(2) 0.9843(9) 0.1323(4) 0.074(2) Uani 1 1 d . . . . .
H28 H -0.099314 0.990665 0.125572 0.089 Uiso 1 1 calc R U . . .
C29 C -0.0369(2) 1.0741(7) 0.1635(3) 0.0533(16) Uani 1 1 d . . . . .
H29 H -0.044011 1.143775 0.177555 0.064 Uiso 1 1 calc R U . . .
C30 C 0.00840(16) 1.0658(5) 0.1757(2) 0.0344(10) Uani 1 1 d . . . . .
C31 C 0.0435(2) 1.1575(5) 0.2073(3) 0.0440(13) Uani 1 1 d . . . . .
H31 H 0.037326 1.228463 0.221761 0.053 Uiso 1 1 calc R U . . .
C32 C 0.08659(17) 1.1464(5) 0.2178(3) 0.0360(10) Uani 1 1 d . . . . .
H32 H 0.109735 1.210034 0.238922 0.043 Uiso 1 1 calc R U . . .
C33 C 0.27525(16) 0.7647(4) 0.38486(19) 0.0252(8) Uani 1 1 d . . . . .
C34 C 0.29171(14) 0.7559(4) 0.44996(17) 0.0194(7) Uani 1 1 d . . . . .
C35 C 0.28702(15) 0.6479(4) 0.47170(19) 0.0241(8) Uani 1 1 d . . . . .
H35 H 0.273209 0.578482 0.445026 0.029 Uiso 1 1 calc R U . . .
C36 C 0.30239(14) 0.6378(4) 0.53325(19) 0.0230(7) Uani 1 1 d . . . . .
C37 C 0.29836(17) 0.5277(5) 0.5570(2) 0.0327(10) Uani 1 1 d . . . . .
H37 H 0.284267 0.457340 0.531063 0.039 Uiso 1 1 calc R U . . .
C38 C 0.31451(18) 0.5211(5) 0.6170(2) 0.0375(11) Uani 1 1 d . . . . .
H38 H 0.312112 0.445901 0.632695 0.045 Uiso 1 1 calc R U . . .
C39 C 0.3347(2) 0.6255(5) 0.6559(2) 0.0408(12) Uani 1 1 d . . . . .
H39 H 0.345983 0.620252 0.697544 0.049 Uiso 1 1 calc R U . . .
C40 C 0.3382(2) 0.7327(5) 0.6340(2) 0.0392(11) Uani 1 1 d . . . . .
H40 H 0.351244 0.802768 0.660269 0.047 Uiso 1 1 calc R U . . .
C41 C 0.32239(15) 0.7425(4) 0.57179(19) 0.0254(8) Uani 1 1 d . . . . .
C42 C 0.32685(18) 0.8530(4) 0.5487(2) 0.0323(10) Uani 1 1 d . . . . .
H42 H 0.340529 0.923286 0.574715 0.039 Uiso 1 1 calc R U . . .
C43 C 0.31163(16) 0.8599(4) 0.4889(2) 0.0258(8) Uani 1 1 d . . . . .
H43 H 0.314529 0.935115 0.473695 0.031 Uiso 1 1 calc R U . . .
C52 C 0.4426(2) 0.8706(7) 0.0925(3) 0.0517(15) Uani 1 1 d . . . . .
H52 H 0.457795 0.858718 0.073839 0.062 Uiso 1 1 calc R U . . .
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'
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
O2 Pb1 O1 77.25(9) . . ?
O2 Pb1 O3 75.29(10) . . ?
O1 Pb1 O3 95.80(11) . . ?
O2 Pb1 O10 81.82(10) . . ?
O1 Pb1 O10 86.78(11) . . ?
O3 Pb1 O10 155.73(11) . . ?
O2 Pb1 Pb3 40.36(6) . . ?
O1 Pb1 Pb3 40.43(6) . . ?
O3 Pb1 Pb3 72.07(8) . . ?
O10 Pb1 Pb3 95.53(8) . . ?
O1 Pb2 O2 75.00(9) . 4_545 ?
O1 Pb2 O8 80.46(10) . 4_545 ?
O2 Pb2 O8 80.59(11) 4_545 4_545 ?
O1 Pb2 O6 78.78(10) . . ?
O2 Pb2 O6 67.33(10) 4_545 . ?
O8 Pb2 O6 145.29(12) 4_545 . ?
O1 Pb2 Pb4 41.45(7) . . ?
O2 Pb2 Pb4 41.14(6) 4_545 . ?
O8 Pb2 Pb4 96.77(8) 4_545 . ?
O6 Pb2 Pb4 50.11(8) . . ?
O1 Pb3 O2 75.97(9) . . ?
O1 Pb3 O7 78.54(10) . . ?
O2 Pb3 O7 90.81(11) . . ?
O1 Pb3 O4 73.15(11) . . ?
O2 Pb3 O4 91.06(11) . . ?
O7 Pb3 O4 150.25(11) . . ?
O1 Pb3 O5 73.82(10) . . ?
O2 Pb3 O5 148.63(10) . . ?
O7 Pb3 O5 91.33(11) . . ?
O4 Pb3 O5 72.32(11) . . ?
O1 Pb3 Pb1 40.12(6) . . ?
O2 Pb3 Pb1 39.30(6) . . ?
O7 Pb3 Pb1 95.73(8) . . ?
O4 Pb3 Pb1 68.07(9) . . ?
O5 Pb3 Pb1 109.39(7) . . ?
O2 Pb4 O1 75.86(9) 4_545 . ?
O2 Pb4 O9 80.64(10) 4_545 . ?
O1 Pb4 O9 89.90(11) . . ?
O2 Pb4 O6 66.90(10) 4_545 . ?
O1 Pb4 O6 77.70(10) . . ?
O9 Pb4 O6 147.13(11) . . ?
O2 Pb4 Pb2 42.05(6) 4_545 . ?
O1 Pb4 Pb2 41.52(6) . . ?
O9 Pb4 Pb2 102.93(9) . . ?
O6 Pb4 Pb2 48.74(7) . . ?
Pb1 O1 Pb4 120.29(11) . . ?
Pb1 O1 Pb2 112.69(11) . . ?
Pb4 O1 Pb2 97.03(10) . . ?
Pb1 O1 Pb3 99.45(10) . . ?
Pb4 O1 Pb3 116.64(11) . . ?
Pb2 O1 Pb3 111.30(11) . . ?
Pb1 O2 Pb4 112.85(11) . 4 ?
Pb1 O2 Pb3 100.34(10) . . ?
Pb4 O2 Pb3 112.76(11) 4 . ?
Pb1 O2 Pb2 109.66(10) . 4 ?
Pb4 O2 Pb2 96.80(9) 4 4 ?
Pb3 O2 Pb2 124.92(11) . 4 ?
C1 O3 Pb1 116.7(3) . . ?
C1 O4 Pb3 124.4(3) . . ?
C11 O5 Pb3 114.6(3) . . ?
C11 O6 Pb2 98.7(3) . . ?
C11 O6 Pb4 112.8(3) . . ?
Pb2 O6 Pb4 81.15(9) . . ?
C22 O7 Pb3 113.6(3) . . ?
C22 O8 Pb2 125.2(3) . 4 ?
C33 O9 Pb4 120.9(3) . . ?
C33 O10 Pb1 116.2(3) . . ?
H11A O11 H11B 108(4) . . ?
O4 C1 O3 124.8(4) . . ?
O4 C1 C2 117.0(4) . . ?
O3 C1 C2 118.2(4) . . ?
C3 C2 C10 119.9(4) . . ?
C3 C2 C1 119.9(4) . . ?
C10 C2 C1 120.2(4) . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C8 119.6(4) . . ?
C5 C4 C3 121.4(4) . . ?
C8 C4 C3 119.0(4) . . ?
C6 C5 C4 120.6(5) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C52 120.0(5) . . ?
C5 C6 H6 120.0 . . ?
C52 C6 H6 120.0 . . ?
C52 C7 C8 120.6(5) . . ?
C52 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C4 C8 C9 119.4(4) . . ?
C4 C8 C7 118.7(4) . . ?
C9 C8 C7 121.9(4) . . ?
C10 C9 C8 120.5(4) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C2 120.8(4) . . ?
C9 C10 H10 119.6 . . ?
C2 C10 H10 119.6 . . ?
O5 C11 O6 121.2(4) . . ?
O5 C11 C12 119.2(4) . . ?
O6 C11 C12 119.5(4) . . ?
C13 C12 C21 120.3(4) . . ?
C13 C12 C11 120.0(4) . . ?
C21 C12 C11 119.6(4) . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C19 119.5(5) . . ?
C15 C14 C13 122.0(5) . . ?
C19 C14 C13 118.5(4) . . ?
C16 C15 C14 119.5(7) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C17 C16 C15 121.6(6) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 121.1(5) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 119.6(6) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C14 C19 C20 119.5(4) . . ?
C14 C19 C18 118.7(5) . . ?
C20 C19 C18 121.8(6) . . ?
C21 C20 C19 120.3(5) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C12 120.6(5) . . ?
C20 C21 H21 119.7 . . ?
C12 C21 H21 119.7 . . ?
O7 C22 O8 123.1(4) . . ?
O7 C22 C23 118.7(4) . . ?
O8 C22 C23 118.2(4) . . ?
C24 C23 C32 119.5(4) . . ?
C24 C23 C22 120.2(4) . . ?
C32 C23 C22 120.3(4) . . ?
C23 C24 C25 121.0(4) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C26 121.9(5) . . ?
C24 C25 C30 119.1(4) . . ?
C26 C25 C30 119.1(5) . . ?
C27 C26 C25 120.1(6) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 120.3(6) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C29 C28 C27 121.3(6) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 120.7(6) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C31 C30 C25 118.7(4) . . ?
C31 C30 C29 122.8(5) . . ?
C25 C30 C29 118.4(5) . . ?
C32 C31 C30 121.0(5) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C31 C32 C23 120.7(5) . . ?
C31 C32 H32 119.7 . . ?
C23 C32 H32 119.7 . . ?
O10 C33 O9 122.9(4) . . ?
O10 C33 C34 119.1(4) . . ?
O9 C33 C34 117.9(4) . . ?
C35 C34 C43 119.8(4) . . ?
C35 C34 C33 120.5(4) . . ?
C43 C34 C33 119.7(4) . . ?
C34 C35 C36 121.3(4) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C37 C36 C41 119.1(4) . . ?
C37 C36 C35 122.6(4) . . ?
C41 C36 C35 118.3(4) . . ?
C38 C37 C36 120.7(5) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C37 C38 C39 120.3(5) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C40 C39 C38 120.2(4) . . ?
C40 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C39 C40 C41 121.0(5) . . ?
C39 C40 H40 119.5 . . ?
C41 C40 H40 119.5 . . ?
C42 C41 C36 119.7(4) . . ?
C42 C41 C40 121.8(4) . . ?
C36 C41 C40 118.6(4) . . ?
C43 C42 C41 120.7(4) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C42 C43 C34 120.2(4) . . ?
C42 C43 H43 119.9 . . ?
C34 C43 H43 119.9 . . ?
C7 C52 C6 120.4(5) . . ?
C7 C52 H52 119.8 . . ?
C6 C52 H52 119.8 . . ?
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
Pb1 O2 2.256(3) . ?
Pb1 O1 2.289(3) . ?
Pb1 O3 2.552(3) . ?
Pb1 O10 2.557(3) . ?
Pb1 Pb3 3.5041(2) . ?
Pb2 O1 2.295(3) . ?
Pb2 O2 2.318(3) 4_545 ?
Pb2 O8 2.565(3) 4_545 ?
Pb2 O6 2.615(3) . ?
Pb2 Pb4 3.4364(2) . ?
Pb3 O1 2.304(3) . ?
Pb3 O2 2.307(3) . ?
Pb3 O7 2.497(3) . ?
Pb3 O4 2.547(3) . ?
Pb3 O5 2.750(3) . ?
Pb4 O2 2.277(3) 4_545 ?
Pb4 O1 2.292(3) . ?
Pb4 O9 2.396(3) . ?
Pb4 O6 2.668(3) . ?
O3 C1 1.269(6) . ?
O4 C1 1.259(6) . ?
O5 C11 1.252(6) . ?
O6 C11 1.274(6) . ?
O7 C22 1.262(6) . ?
O8 C22 1.275(5) . ?
O9 C33 1.270(5) . ?
O10 C33 1.267(5) . ?
O11 H11A 0.84(2) . ?
O11 H11B 0.84(2) . ?
C1 C2 1.508(6) . ?
C2 C3 1.369(6) . ?
C2 C10 1.407(6) . ?
C3 C4 1.432(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.404(7) . ?
C4 C8 1.405(6) . ?
C5 C6 1.382(7) . ?
C5 H5 0.9500 . ?
C6 C52 1.399(9) . ?
C6 H6 0.9500 . ?
C7 C52 1.369(8) . ?
C7 C8 1.424(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.411(6) . ?
C9 C10 1.371(6) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.498(6) . ?
C12 C13 1.368(6) . ?
C12 C21 1.407(7) . ?
C13 C14 1.423(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.413(7) . ?
C14 C19 1.416(8) . ?
C15 C16 1.376(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.368(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.375(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.431(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.422(8) . ?
C20 C21 1.366(7) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.492(5) . ?
C23 C24 1.373(6) . ?
C23 C32 1.401(6) . ?
C24 C25 1.414(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.416(7) . ?
C25 C30 1.417(7) . ?
C26 C27 1.375(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(11) . ?
C27 H27 0.9500 . ?
C28 C29 1.346(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.424(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.401(7) . ?
C31 C32 1.374(7) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.497(5) . ?
C34 C35 1.371(5) . ?
C34 C43 1.409(6) . ?
C35 C36 1.419(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.410(6) . ?
C36 C41 1.411(6) . ?
C37 C38 1.368(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.412(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.348(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.431(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.410(6) . ?
C42 C43 1.372(6) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C52 H52 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb3 O4 C1 O3 26.3(7) . . . . ?
Pb3 O4 C1 C2 -154.6(3) . . . . ?
Pb1 O3 C1 O4 32.4(6) . . . . ?
Pb1 O3 C1 C2 -146.8(3) . . . . ?
O4 C1 C2 C3 172.9(4) . . . . ?
O3 C1 C2 C3 -7.9(6) . . . . ?
O4 C1 C2 C10 -6.8(6) . . . . ?
O3 C1 C2 C10 172.4(4) . . . . ?
C10 C2 C3 C4 -0.3(7) . . . . ?
C1 C2 C3 C4 -180.0(4) . . . . ?
C2 C3 C4 C5 175.7(5) . . . . ?
C2 C3 C4 C8 -1.7(7) . . . . ?
C8 C4 C5 C6 -2.3(10) . . . . ?
C3 C4 C5 C6 -179.6(7) . . . . ?
C4 C5 C6 C52 -0.3(13) . . . . ?
C5 C4 C8 C9 -175.2(6) . . . . ?
C3 C4 C8 C9 2.2(7) . . . . ?
C5 C4 C8 C7 3.4(8) . . . . ?
C3 C4 C8 C7 -179.2(5) . . . . ?
C52 C7 C8 C4 -2.0(8) . . . . ?
C52 C7 C8 C9 176.5(6) . . . . ?
C4 C8 C9 C10 -0.7(8) . . . . ?
C7 C8 C9 C10 -179.3(5) . . . . ?
C8 C9 C10 C2 -1.3(8) . . . . ?
C3 C2 C10 C9 1.8(7) . . . . ?
C1 C2 C10 C9 -178.5(5) . . . . ?
Pb3 O5 C11 O6 -87.3(5) . . . . ?
Pb3 O5 C11 C12 91.4(4) . . . . ?
Pb2 O6 C11 O5 -0.3(5) . . . . ?
Pb4 O6 C11 O5 83.7(5) . . . . ?
Pb2 O6 C11 C12 -178.9(3) . . . . ?
Pb4 O6 C11 C12 -94.9(4) . . . . ?
O5 C11 C12 C13 175.2(4) . . . . ?
O6 C11 C12 C13 -6.1(6) . . . . ?
O5 C11 C12 C21 -5.2(6) . . . . ?
O6 C11 C12 C21 173.4(4) . . . . ?
C21 C12 C13 C14 -0.7(7) . . . . ?
C11 C12 C13 C14 178.9(4) . . . . ?
C12 C13 C14 C15 -179.3(5) . . . . ?
C12 C13 C14 C19 0.1(7) . . . . ?
C19 C14 C15 C16 -1.1(8) . . . . ?
C13 C14 C15 C16 178.3(5) . . . . ?
C14 C15 C16 C17 -1.1(10) . . . . ?
C15 C16 C17 C18 2.6(10) . . . . ?
C16 C17 C18 C19 -2.0(9) . . . . ?
C15 C14 C19 C20 -179.9(5) . . . . ?
C13 C14 C19 C20 0.7(7) . . . . ?
C15 C14 C19 C18 1.6(7) . . . . ?
C13 C14 C19 C18 -177.8(5) . . . . ?
C17 C18 C19 C14 -0.2(8) . . . . ?
C17 C18 C19 C20 -178.6(6) . . . . ?
C14 C19 C20 C21 -1.0(8) . . . . ?
C18 C19 C20 C21 177.5(5) . . . . ?
C19 C20 C21 C12 0.4(9) . . . . ?
C13 C12 C21 C20 0.4(8) . . . . ?
C11 C12 C21 C20 -179.1(5) . . . . ?
Pb3 O7 C22 O8 -32.0(6) . . . . ?
Pb3 O7 C22 C23 147.4(3) . . . . ?
Pb2 O8 C22 O7 -53.2(6) 4 . . . ?
Pb2 O8 C22 C23 127.4(3) 4 . . . ?
O7 C22 C23 C24 -7.4(6) . . . . ?
O8 C22 C23 C24 172.1(4) . . . . ?
O7 C22 C23 C32 172.0(4) . . . . ?
O8 C22 C23 C32 -8.6(6) . . . . ?
C32 C23 C24 C25 0.7(7) . . . . ?
C22 C23 C24 C25 -179.9(4) . . . . ?
C23 C24 C25 C26 178.2(6) . . . . ?
C23 C24 C25 C30 -1.2(8) . . . . ?
C24 C25 C26 C27 -179.1(8) . . . . ?
C30 C25 C26 C27 0.3(12) . . . . ?
C25 C26 C27 C28 -2.3(16) . . . . ?
C26 C27 C28 C29 3.0(16) . . . . ?
C27 C28 C29 C30 -1.5(13) . . . . ?
C24 C25 C30 C31 0.8(8) . . . . ?
C26 C25 C30 C31 -178.6(6) . . . . ?
C24 C25 C30 C29 -179.5(5) . . . . ?
C26 C25 C30 C29 1.1(9) . . . . ?
C28 C29 C30 C31 179.2(7) . . . . ?
C28 C29 C30 C25 -0.5(10) . . . . ?
C25 C30 C31 C32 0.2(9) . . . . ?
C29 C30 C31 C32 -179.5(6) . . . . ?
C30 C31 C32 C23 -0.7(9) . . . . ?
C24 C23 C32 C31 0.2(8) . . . . ?
C22 C23 C32 C31 -179.1(5) . . . . ?
Pb1 O10 C33 O9 -40.9(6) . . . . ?
Pb1 O10 C33 C34 136.4(3) . . . . ?
Pb4 O9 C33 O10 -41.9(6) . . . . ?
Pb4 O9 C33 C34 140.8(3) . . . . ?
O10 C33 C34 C35 -179.8(4) . . . . ?
O9 C33 C34 C35 -2.4(6) . . . . ?
O10 C33 C34 C43 0.9(6) . . . . ?
O9 C33 C34 C43 178.4(4) . . . . ?
C43 C34 C35 C36 -0.7(6) . . . . ?
C33 C34 C35 C36 -180.0(4) . . . . ?
C34 C35 C36 C37 -179.5(4) . . . . ?
C34 C35 C36 C41 0.6(6) . . . . ?
C41 C36 C37 C38 -1.4(7) . . . . ?
C35 C36 C37 C38 178.7(4) . . . . ?
C36 C37 C38 C39 1.2(7) . . . . ?
C37 C38 C39 C40 0.2(8) . . . . ?
C38 C39 C40 C41 -1.3(8) . . . . ?
C37 C36 C41 C42 179.7(4) . . . . ?
C35 C36 C41 C42 -0.4(6) . . . . ?
C37 C36 C41 C40 0.4(6) . . . . ?
C35 C36 C41 C40 -179.7(4) . . . . ?
C39 C40 C41 C42 -178.3(5) . . . . ?
C39 C40 C41 C36 1.0(7) . . . . ?
C36 C41 C42 C43 0.5(7) . . . . ?
C40 C41 C42 C43 179.7(5) . . . . ?
C41 C42 C43 C34 -0.6(7) . . . . ?
C35 C34 C43 C42 0.8(6) . . . . ?
C33 C34 C43 C42 180.0(4) . . . . ?
C8 C7 C52 C6 -0.5(10) . . . . ?
C5 C6 C52 C7 1.6(12) . . . . ?
