# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_s5102r_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 1995412'
loop_
_audit_author_name
_audit_author_address
'Xi Chen'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2020-04-07 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
# end Validation Reply Form
_audit_creation_date             2018-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C48 H48 N4 O20 Pb4)'
_chemical_formula_sum            'C12 H12 N O5 Pb'
_chemical_formula_weight         457.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         C24H24N2O10Pb2
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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4855(4)
_cell_length_b                   11.1137(5)
_cell_length_c                   12.4920(4)
_cell_angle_alpha                111.886(4)
_cell_angle_beta                 101.798(3)
_cell_angle_gamma                103.943(4)
_cell_volume                     1239.04(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4165
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      26.3440
_cell_measurement_theta_min      1.8610
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.632
_exptl_absorpt_correction_T_max  0.513
_exptl_absorpt_correction_T_min  0.134
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.452
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-15 3 2 0.0586
15 -3 -2 0.0586
1 5 -17 0.1157
-1 -5 17 0.1157
0 -14 0 0.0255
0 14 0 0.0255
3 -6 -12 0.0875

_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.051
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-14.9641 2.9869 2.0349 -0.9393 -0.3648 -0.1752
14.9641 -2.9869 -2.0349 0.9393 0.3648 0.1752
0.5237 4.5102 -16.9950 -0.2128 -0.1098 0.9600
-0.5237 -4.5102 16.9950 0.2128 0.1098 -0.9600
0.0091 -14.0450 0.0273 -0.4913 0.8930 0.1460
-0.0091 14.0450 -0.0273 0.4913 -0.8930 -0.1460
3.0154 -6.0182 -11.9861 -0.2794 0.5348 0.7779

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24359
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         1.859
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00 -18.00   1.00    1.00    --   -7.70  31.00  57.00   26
  2  ω    -95.00  28.00   1.00    1.00    --   -7.70 -31.00-102.00  123
  3  ω    -86.00  25.00   1.00    1.00    --   -7.70 -57.00  90.00  111
  4  ω    -94.00  16.00   1.00    1.00    --   -7.70 -57.00-180.00  110
  5  ω    -31.00  -2.00   1.00    1.00    --   -7.70 -57.00 -30.00   29
  6  ω      7.00  64.00   1.00    1.00    --   -7.70  31.00  57.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0730453000
_diffrn_orient_matrix_UB_12      0.0350721000
_diffrn_orient_matrix_UB_13      0.0240782000
_diffrn_orient_matrix_UB_21      0.0103087000
_diffrn_orient_matrix_UB_22      -0.0635949000
_diffrn_orient_matrix_UB_23      -0.0100969000
_diffrn_orient_matrix_UB_31      0.0015576000
_diffrn_orient_matrix_UB_32      -0.0105063000
_diffrn_orient_matrix_UB_33      -0.0592295000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6439
_reflns_number_total             7619
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         5.219
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.268
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7619
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0681P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0946
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H15A(0.074) H15B(0.074) H15C(0.074) H18(0.019) H16A(0.087)
 H16B(0.087) H16C(0.087) H3(0.019) H22A(0.089) H22B(0.089) H22C(0.089)
 H23A(0.095) H23B(0.095) H23C(0.095) H8(0.021) H13(0.023) H17A(0.077)
 H17B(0.077) H17C(0.077) H11(0.02) H20(0.019) H24A(0.092) H24B(0.092)
 H24C(0.092)
 Fixed X: H15A(0.784876) H15B(0.883659) H15C(0.943435) H18(0.478257)
 H16A(0.854639) H16B(0.94824) H16C(0.787842) H3(0.483186) H22A(1.171925)
 H22B(1.074419) H22C(1.198234) H23A(1.101324) H23B(1.022972) H23C(1.177189) H8(-
 0.01195) H13(0.189088) H17A(0.726324) H17B(0.69605) H17C(0.847174) H11(-
 0.202544) H20(0.52252) H24A(0.846271) H24B(0.957124) H24C(0.804816)
 Fixed Y: H15A(0.671518) H15B(0.653881) H15C(0.706183) H18(0.304261)
 H16A(0.324932) H16B(0.451729) H16C(0.389358) H3(0.517815) H22A(1.431154)
 H22B(1.289287) H22C(1.294398) H23A(1.197432) H23B(1.285172) H23C(1.356598)
 H8(0.044165) H13(-0.001096) H17A(0.514736) H17B(0.595097) H17C(0.637333) H11(-
 0.001544) H20(0.703297) H24A(1.268427) H24B(1.418335) H24C(1.391949)
 Fixed Z: H15A(-0.046279) H15B(-0.125307) H15C(0.01611) H18(0.342286) H16A(-
 0.173167) H16B(-0.182128) H16C(-0.251974) H3(0.145171) H22A(0.398348)
 H22B(0.28802) H22C(0.38634) H23A(0.52411) H23B(0.595449) H23C(0.607737) H8(-
 0.345932) H13(-0.060347) H17A(0.147072) H17B(0.070668) H17C(0.156854) H11(-
 0.106915) H20(0.496339) H24A(0.244065) H24B(0.315858) H24C(0.31992)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Pb2 Pb 0.55462(3) 0.12113(3) -0.09333(2) 0.01506(10) Uani 1 1 d . . . . .
Pb1 Pb 0.63886(3) 1.09759(3) 0.44794(2) 0.01439(10) Uani 1 1 d . . . . .
O9 O 0.7784(8) 0.3345(9) -0.0159(8) 0.052(2) Uani 1 1 d D U . . .
O3 O 0.4788(9) 0.1604(7) 0.1251(6) 0.0300(17) Uani 1 1 d . . . . .
O1 O 0.5300(7) 0.8670(6) 0.4091(6) 0.0201(14) Uani 1 1 d . . . . .
O6 O -0.3689(6) -0.0092(6) -0.2939(5) 0.0194(13) Uani 1 1 d . . . . .
O7 O -0.2324(7) 0.0866(7) -0.3809(5) 0.0241(14) Uani 1 1 d . . . . .
O2 O 0.5023(7) 0.7620(6) 0.2108(5) 0.0240(14) Uani 1 1 d . . . . .
O4 O 0.3179(7) -0.0232(7) -0.2128(5) 0.0200(14) Uani 1 1 d . . . . .
O5 O 0.2057(7) 0.0092(7) -0.3654(5) 0.0236(14) Uani 1 1 d . . . . .
O8 O 0.4625(7) 0.2798(6) 0.0188(5) 0.0264(15) Uani 1 1 d . . . . .
O10 O 0.8517(9) 1.3195(7) 0.5020(7) 0.045(2) Uani 1 1 d D U . . .
N2 N 1.0378(13) 1.3153(12) 0.4438(10) 0.069(3) Uani 1 1 d D U . . .
N1 N 0.8361(12) 0.5023(10) -0.0742(10) 0.058(3) Uani 1 1 d D U . . .
C15 C 0.8645(13) 0.6459(11) -0.0558(12) 0.049(3) Uani 1 1 d D U . . .
H15A H 0.784876 0.671518 -0.046279 0.074 Uiso 1 1 calc GR . . . .
H15B H 0.883659 0.653881 -0.125307 0.074 Uiso 1 1 calc GR . . . .
H15C H 0.943435 0.706183 0.016110 0.074 Uiso 1 1 calc GR . . . .
C18 C 0.4837(9) 0.3866(9) 0.3371(7) 0.0162(17) Uani 1 1 d . . . . .
H18 H 0.478257 0.304261 0.342286 0.019 Uiso 1 1 calc R . . . .
C16 C 0.8586(14) 0.4093(13) -0.1791(11) 0.058(4) Uani 1 1 d D U . . .
H16A H 0.854639 0.324932 -0.173167 0.087 Uiso 1 1 calc GR . . . .
H16B H 0.948240 0.451729 -0.182128 0.087 Uiso 1 1 calc GR . . . .
H16C H 0.787842 0.389358 -0.251974 0.087 Uiso 1 1 calc GR . . . .
C19 C 0.4976(9) 0.5025(9) 0.4413(7) 0.0156(17) Uani 1 1 d . . . . .
C10 C -0.2558(9) 0.0342(9) -0.3111(7) 0.0156(17) Uani 1 1 d . . . . .
C1 C 0.5107(9) 0.7619(8) 0.3102(7) 0.0151(17) Uani 1 1 d . . . . .
C5 C 0.4702(9) 0.2639(9) 0.1148(7) 0.0169(17) Uani 1 1 d . . . . .
C3 C 0.4867(9) 0.5133(9) 0.2185(7) 0.0159(17) Uani 1 1 d . . . . .
H3 H 0.483186 0.517815 0.145171 0.019 Uiso 1 1 calc R . . . .
C2 C 0.5008(9) 0.6286(8) 0.3194(7) 0.0149(17) Uani 1 1 d . . . . .
C9 C -0.1283(9) 0.0243(9) -0.2359(7) 0.0164(17) Uani 1 1 d . . . . .
C22 C 1.1282(14) 1.3341(13) 0.3731(13) 0.059(4) Uani 1 1 d D U . . .
H22A H 1.171925 1.431154 0.398348 0.089 Uiso 1 1 calc GR . . . .
H22B H 1.074419 1.289287 0.288020 0.089 Uiso 1 1 calc GR . . . .
H22C H 1.198234 1.294398 0.386340 0.089 Uiso 1 1 calc GR . . . .
C6 C 0.2191(9) 0.0034(9) -0.2656(8) 0.0171(17) Uani 1 1 d . . . . .
C4 C 0.4778(9) 0.3899(9) 0.2256(7) 0.0171(18) Uani 1 1 d . . . . .
C23 C 1.0897(15) 1.2858(14) 0.5531(11) 0.063(4) Uani 1 1 d D U . . .
H23A H 1.101324 1.197432 0.524110 0.095 Uiso 1 1 calc GR . . . .
H23B H 1.022972 1.285172 0.595449 0.095 Uiso 1 1 calc GR . . . .
H23C H 1.177189 1.356598 0.607737 0.095 Uiso 1 1 calc GR . . . .
C14 C 0.7936(12) 0.4601(13) -0.0017(10) 0.053(3) Uani 1 1 d D U . . .
C8 C -0.0118(9) 0.0304(8) -0.2769(7) 0.0177(18) Uani 1 1 d . . . . .
H8 H -0.011950 0.044165 -0.345932 0.021 Uiso 1 1 calc R . . . .
C7 C 0.1025(9) 0.0155(9) -0.2121(7) 0.0174(17) Uani 1 1 d . . . . .
C13 C 0.1094(9) 0.0051(9) -0.1036(8) 0.0189(18) Uani 1 1 d . . . . .
H13 H 0.189088 -0.001096 -0.060347 0.023 Uiso 1 1 calc R . . . .
C17 C 0.7630(12) 0.5612(14) 0.1029(9) 0.051(3) Uani 1 1 d D U . . .
H17A H 0.726324 0.514736 0.147072 0.077 Uiso 1 1 calc GR . . . .
H17B H 0.696050 0.595097 0.070668 0.077 Uiso 1 1 calc GR . . . .
H17C H 0.847174 0.637333 0.156854 0.077 Uiso 1 1 calc GR . . . .
C11 C -0.1237(9) 0.0075(9) -0.1307(7) 0.0166(17) Uani 1 1 d . . . . .
H11 H -0.202544 -0.001544 -0.106915 0.020 Uiso 1 1 calc R . . . .
C12 C -0.0040(8) 0.0038(8) -0.0589(7) 0.0142(16) Uani 1 1 d . . . . .
C21 C 0.9194(14) 1.3281(14) 0.4300(11) 0.062(3) Uani 1 1 d D U . . .
C20 C 0.5089(9) 0.6229(8) 0.4282(7) 0.0159(17) Uani 1 1 d . . . . .
H20 H 0.522520 0.703297 0.496339 0.019 Uiso 1 1 calc R . . . .
C24 C 0.8780(14) 1.3542(13) 0.3167(11) 0.062(4) Uani 1 1 d D U . . .
H24A H 0.846271 1.268427 0.244065 0.092 Uiso 1 1 calc GR . . . .
H24B H 0.957124 1.418335 0.315858 0.092 Uiso 1 1 calc GR . . . .
H24C H 0.804816 1.391949 0.319920 0.092 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pb2 O9 2.597(8) . ?
Pb2 O2 2.373(6) 2_665 ?
Pb2 O4 2.397(6) . ?
Pb2 O8 2.353(6) . ?
Pb1 O1 2.354(6) . ?
Pb1 O1 2.754(6) 2_676 ?
Pb1 O7 2.346(6) 1_666 ?
Pb1 O5 2.416(6) 2_665 ?
Pb1 O10 2.648(7) . ?
O9 C14 1.305(13) . ?
O3 C5 1.225(10) . ?
O1 C1 1.281(10) . ?
O6 C10 1.260(10) . ?
O7 C10 1.248(10) . ?
O2 C1 1.228(9) . ?
O4 C6 1.269(11) . ?
O5 C6 1.253(10) . ?
O8 C5 1.265(10) . ?
O10 C21 1.271(13) . ?
N2 C22 1.451(12) . ?
N2 C23 1.544(14) . ?
N2 C21 1.268(16) . ?
N1 C15 1.469(12) . ?
N1 C16 1.440(12) . ?
N1 C14 1.273(13) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C18 H18 0.9300 . ?
C18 C19 1.399(11) . ?
C18 C4 1.396(10) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C19 C19 1.480(15) 2_666 ?
C19 C20 1.387(11) . ?
C10 C9 1.522(12) . ?
C1 C2 1.509(11) . ?
C5 C4 1.530(11) . ?
C3 H3 0.9300 . ?
C3 C2 1.371(10) . ?
C3 C4 1.389(12) . ?
C2 C20 1.370(11) . ?
C9 C8 1.415(11) . ?
C9 C11 1.387(11) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C6 C7 1.518(11) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C14 C17 1.525(14) . ?
C8 H8 0.9300 . ?
C8 C7 1.384(13) . ?
C7 C13 1.392(11) . ?
C13 H13 0.9300 . ?
C13 C12 1.413(10) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C11 H11 0.9300 . ?
C11 C12 1.405(12) . ?
C12 C12 1.491(15) 2 ?
C21 C24 1.545(15) . ?
C20 H20 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

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 Pb2 O9 75.8(2) 2_665 . ?
O2 Pb2 O4 79.4(2) 2_665 . ?
O4 Pb2 O9 155.1(2) . . ?
O8 Pb2 O9 85.6(3) . . ?
O8 Pb2 O2 74.04(19) . 2_665 ?
O8 Pb2 O4 86.0(2) . . ?
O1 Pb1 O1 79.51(19) . 2_676 ?
O1 Pb1 O5 79.0(2) . 2_665 ?
O1 Pb1 O10 155.4(3) . . ?
O7 Pb1 O1 78.8(2) 1_666 2_676 ?
O7 Pb1 O1 77.6(2) 1_666 . ?
O7 Pb1 O5 79.4(2) 1_666 2_665 ?
O7 Pb1 O10 87.0(3) 1_666 . ?
O5 Pb1 O1 152.14(19) 2_665 2_676 ?
O5 Pb1 O10 79.4(2) 2_665 . ?
O10 Pb1 O1 116.4(2) . 2_676 ?
C14 O9 Pb2 130.5(7) . . ?
Pb1 O1 Pb1 100.49(19) . 2_676 ?
C1 O1 Pb1 128.6(5) . 2_676 ?
C1 O1 Pb1 123.8(5) . . ?
C10 O7 Pb1 137.4(6) . 1_444 ?
C1 O2 Pb2 143.0(5) . 2_665 ?
C6 O4 Pb2 130.5(6) . . ?
C6 O5 Pb1 104.8(5) . 2_665 ?
C5 O8 Pb2 104.2(5) . . ?
C21 O10 Pb1 123.4(7) . . ?
C22 N2 C23 119.1(12) . . ?
C21 N2 C22 126.5(13) . . ?
C21 N2 C23 114.2(11) . . ?
C16 N1 C15 117.0(11) . . ?
C14 N1 C15 122.4(11) . . ?
C14 N1 C16 120.6(11) . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C19 C18 H18 118.8 . . ?
C4 C18 H18 118.8 . . ?
C4 C18 C19 122.4(8) . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C19 C19 122.0(9) . 2_666 ?
C20 C19 C18 115.9(7) . . ?
C20 C19 C19 122.1(9) . 2_666 ?
O6 C10 C9 116.6(7) . . ?
O7 C10 O6 129.0(8) . . ?
O7 C10 C9 114.4(7) . . ?
O1 C1 C2 116.3(7) . . ?
O2 C1 O1 125.5(8) . . ?
O2 C1 C2 118.3(7) . . ?
O3 C5 O8 125.0(7) . . ?
O3 C5 C4 119.9(7) . . ?
O8 C5 C4 115.0(7) . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.2(7) . . ?
C4 C3 H3 119.9 . . ?
C3 C2 C1 119.5(7) . . ?
C20 C2 C1 120.5(7) . . ?
C20 C2 C3 120.0(8) . . ?
C8 C9 C10 118.2(7) . . ?
C11 C9 C10 122.4(7) . . ?
C11 C9 C8 119.4(8) . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O4 C6 C7 118.6(7) . . ?
O5 C6 O4 123.7(8) . . ?
O5 C6 C7 117.4(8) . . ?
C18 C4 C5 121.4(8) . . ?
C3 C4 C18 118.6(7) . . ?
C3 C4 C5 120.0(7) . . ?
N2 C23 H23A 109.5 . . ?
N2 C23 H23B 109.5 . . ?
N2 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O9 C14 C17 121.1(11) . . ?
N1 C14 O9 120.9(11) . . ?
N1 C14 C17 118.0(11) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 C9 118.6(8) . . ?
C7 C8 H8 120.7 . . ?
C8 C7 C6 118.3(7) . . ?
C8 C7 C13 121.8(7) . . ?
C13 C7 C6 119.9(8) . . ?
C7 C13 H13 119.9 . . ?
C7 C13 C12 120.3(8) . . ?
C12 C13 H13 119.9 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C9 C11 H11 118.9 . . ?
C9 C11 C12 122.3(8) . . ?
C12 C11 H11 118.9 . . ?
C13 C12 C12 120.6(9) . 2 ?
C11 C12 C13 117.3(7) . . ?
C11 C12 C12 122.1(8) . 2 ?
O10 C21 C24 128.6(13) . . ?
N2 C21 O10 122.1(13) . . ?
N2 C21 C24 109.2(11) . . ?
C19 C20 H20 118.5 . . ?
C2 C20 C19 122.9(7) . . ?
C2 C20 H20 118.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.844
_oxdiff_exptl_absorpt_empirical_full_min 0.594
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6407 8102 8137 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.3593 8120 8137 nmt -0.0008 0.9967 0.4998 1.0029 0.0016 0.5020 -0.0019
-0.0030 -1.0013

_twin_special_details            
;
Component 2 rotated by -179.9588° 
 around [0.70 0.71 -0.00] (reciprocal) or [0.67 0.66 0.33] (direct)
;
# start Validation Reply Form
_vrf_PLAT094_s5102r_twin1_hklf4  
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.57 Report
RESPONSE: There is a (relatively) large positive density close to the Pb in 
the compound. This can be attributed to the lone pair of the Pb, further 
indicated by the presence of the hemidirected coordination environments. 
This results in a large ratio between the maximum and minimum residual 
densities as it cannot easily be accounted for in the model.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rms139_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 1995413'
loop_
_audit_author_name
_audit_author_address
'Xi Chen'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2020-04-07 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_rms139_twin1_hklf4  
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.955 Why?
RESPONSE: The crystals are weakly diffracting beyond 1 \%A. The space group is P-1, so the completeness is relatively low even the resolution is 0.83 \%A, but the connectivity of the atoms in structure is clear enough.
;
_vrf_PLAT097_rms139_twin1_hklf4  
;
PROBLEM: Large Reported Max.  (Positive) Residual Density      10.43 eA-3
RESPONSE: There is a (relatively) large positive density close to the Pb in the compound. This can be attributed to the lone pair of the Pb, further indicated by the presence of the hemidirected coordination environments. This results in a large ratio between the maximum and minimum residual densities as it cannot easily be accounted for in the model.
;
_vrf_PLAT342_rms139_twin1_hklf4  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04647 Ang.
RESPONSE: Low bond precision is due to the relatively low quality of data.
;
# Added during the CSD deposition process: Tuesday 07 April 2020 04:20 PM
# end Validation Reply Form

_audit_creation_date             2020-04-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H8 O9 Pb2'
_chemical_formula_sum            'C16 H8 O9 Pb2'
_chemical_formula_weight         758.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3121(17)
_cell_length_b                   9.4816(17)
_cell_length_c                   11.803(3)
_cell_angle_alpha                81.482(17)
_cell_angle_beta                 74.95(2)
_cell_angle_gamma                73.334(18)
_cell_volume                     754.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    757
_cell_measurement_temperature    99.8(8)
_cell_measurement_theta_max      70.0930
_cell_measurement_theta_min      5.9750
_shelx_estimated_absorpt_T_max   0.346
_shelx_estimated_absorpt_T_min   0.034
_exptl_absorpt_coefficient_mu    43.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.338
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.031
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5354
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.946
_diffrn_reflns_theta_min         3.891
_diffrn_ambient_temperature      99.8(8)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  28.00   1.00    1.00    --    5.00 -66.00-103.00   55
  2  ω    -80.00   2.00   1.00    1.00    --  -44.10  66.00  31.00   82
  3  ω   -112.00 -80.00   1.00    1.00    --  -44.10 -66.00-103.00   32
  4  ω   -143.00 -77.00   1.00    1.00    -- -107.20  66.00  31.00   66
  5  ω    -76.00 -30.00   1.00    1.00    -- -107.20  66.00  31.00   46
  6  ω   -159.00 -99.00   1.00    1.00    -- -107.20 -66.00-103.00   60
  7  ω     -8.00  19.00   1.00    1.00    --    5.00  66.00  31.00   27
  8  ω    -37.00  41.00   1.00    1.00    --  -44.10  76.00-180.00   78
  9  ω    -78.00 -40.00   1.00    1.00    --  -44.10  76.00-180.00   38
 10  ω    -75.00  39.00   1.00    1.00    --  -44.10  76.00  90.00  114
 11  ω    -77.00 -15.00   1.00    1.00    --  -44.10 -66.00-103.00   62
 12  ω    -69.00 -35.00   1.00    1.00    -- -107.20  76.00-150.00   34
 13  ω   -106.00 -72.00   1.00    1.00    -- -107.20  76.00-150.00   34
 14  ω   -146.00 -98.00   1.00    1.00    -- -107.20  38.00-120.00   48
 15  ω    -47.00 -20.00   1.00    1.00    -- -107.20  76.00 -60.00   27
 16  ω   -112.00 -70.00   1.00    1.00    -- -107.20  76.00 -60.00   42
 17  ω   -195.00 -95.00   1.00    1.00    -- -107.20 -19.00  60.00  100
 18  ω    -94.00 -18.00   1.00    1.00    -- -107.20 -19.00  60.00   76
 19  ω   -147.00 -47.00   1.00    1.00    -- -107.20  76.00-180.00  100
 20  ω   -148.00-107.00   1.00    1.00    -- -107.20  76.00-150.00   41
 21  ω   -131.00 -21.00   1.00    1.00    -- -107.20  76.00  30.00  110
 22  ω    -82.00 -18.00   1.00    1.00    -- -107.20  38.00  30.00   64
 23  ω   -139.00-103.00   1.00    1.00    -- -107.20  38.00  30.00   36
 24  ω    -97.00 -18.00   1.00    1.00    -- -107.20  38.00-120.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3809
_reflns_number_total             5354
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         10.433
_refine_diff_density_min         -5.235
_refine_diff_density_rms         0.633
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     193
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1003
_refine_ls_restrained_S_all      1.182
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2797
_refine_ls_wR_factor_ref         0.3038
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.442(3)
 0.558(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Rigid body (RIGU) restrains
 C14, Pb01, O00M, C00E, C004, O006, C00D, C00O, C00V, C00F, C00Q, C005, C00R,
 C00S, O00C, O00L, C00J, C00W, Pb02, C003, C00K, C00N, O00B, O00P, O008, O009
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Rotating group:
 O4(H4A,H4B)
4.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00K(H00K), C00R(H00R), C00S(H00S), C14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Pb01 Pb 0.59710(17) 0.25606(11) 0.03299(10) 0.0396(4) Uani 1 1 d . . . . .
Pb02 Pb 0.16219(17) 1.05367(12) 0.23422(10) 0.0414(4) Uani 1 1 d . . . . .
C003 C 0.304(6) 0.066(3) 0.891(3) 0.046(7) Uani 1 1 d . . . . .
C004 C 0.549(5) 0.336(3) 0.345(3) 0.045(7) Uani 1 1 d . . . . .
C005 C 0.261(5) 0.733(3) 0.297(3) 0.037(5) Uani 1 1 d . . . . .
O006 O 0.825(4) 0.133(3) 0.358(2) 0.051(5) Uani 1 1 d . . . . .
O008 O -0.297(3) 0.508(2) 0.991(2) 0.044(5) Uani 1 1 d . . . . .
O009 O -0.255(3) 0.680(2) 0.846(2) 0.045(5) Uani 1 1 d . . . . .
O00B O 0.449(4) -0.025(2) 0.831(2) 0.046(5) Uani 1 1 d . . . . .
O00C O 0.130(3) 0.827(2) 0.3611(18) 0.042(5) Uani 1 1 d . . . . .
C00D C 0.455(5) 0.303(3) 0.461(3) 0.040(6) Uani 1 1 d . . . . .
H00D H 0.498639 0.207376 0.498232 0.048 Uiso 1 1 calc R U . . .
C00E C 0.737(5) 0.228(3) 0.288(3) 0.040(5) Uani 1 1 d . . . . .
C00F C 0.241(5) 0.543(3) 0.463(3) 0.044(6) Uani 1 1 d . . . . .
H00F H 0.137363 0.617966 0.503069 0.053 Uiso 1 1 calc R U . . .
C00J C 0.216(5) 0.203(3) 0.829(3) 0.043(6) Uani 1 1 d . . . . .
C00K C 0.064(4) 0.305(3) 0.892(3) 0.039(5) Uani 1 1 d . . . . .
H00K H 0.012484 0.282494 0.973622 0.046 Uiso 1 1 calc R U . . .
O00L O 0.340(3) 0.764(2) 0.1909(18) 0.041(5) Uani 1 1 d . . . . .
O00M O 0.801(4) 0.240(3) 0.181(2) 0.048(5) Uani 1 1 d . . . . .
C00N C -0.200(5) 0.551(4) 0.896(3) 0.048(7) Uani 1 1 d . . . . .
C00O C 0.296(5) 0.407(3) 0.526(3) 0.039(5) Uani 1 1 d . . . . .
O00P O 0.230(4) 0.033(3) 0.998(2) 0.065(8) Uani 1 1 d . . . . .
C00Q C 0.213(5) 0.369(3) 0.651(3) 0.041(6) Uani 1 1 d . . . . .
C00R C 0.287(5) 0.235(3) 0.710(3) 0.044(7) Uani 1 1 d . . . . .
H00R H 0.390120 0.161925 0.667359 0.053 Uiso 1 1 calc R U . . .
C00S C 0.065(5) 0.469(3) 0.709(3) 0.041(6) Uani 1 1 d . . . . .
H00S H 0.010303 0.559956 0.668962 0.050 Uiso 1 1 calc R U . . .
C00V C 0.330(4) 0.579(3) 0.341(3) 0.033(5) Uani 1 1 d . . . . .
C00W C -0.015(5) 0.440(3) 0.838(3) 0.040(6) Uani 1 1 d . . . . .
C14 C 0.482(5) 0.478(4) 0.289(3) 0.051(8) Uani 1 1 d . . . . .
H14 H 0.548097 0.500743 0.210622 0.061 Uiso 1 1 calc R U . . .
O4 O 0.199(4) 1.078(3) 0.445(2) 0.054(6) Uani 1 1 d . . . . .
H4A H 0.141311 1.019699 0.497580 0.080 Uiso 1 1 d R U . . .
H4B H 0.135615 1.166172 0.467917 0.080 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pb01 O008 2.66(2) 1_654 ?
Pb01 O008 2.68(2) 2_566 ?
Pb01 O009 2.49(2) 2_566 ?
Pb01 O00B 2.57(2) 2_656 ?
Pb01 O00L 2.59(2) 2_665 ?
Pb01 O00M 2.54(2) . ?
Pb01 O00P 2.70(3) 2_656 ?
Pb02 O006 2.48(2) 1_465 ?
Pb02 O00B 2.69(3) 2_666 ?
Pb02 O00C 2.468(19) . ?
Pb02 O00L 2.74(2) . ?
Pb02 O00P 2.73(3) 1_564 ?
Pb02 O4 2.63(3) . ?
C003 O00B 1.28(4) . ?
C003 C00J 1.46(4) . ?
C003 O00P 1.26(4) . ?
C004 C00D 1.40(4) . ?
C004 C00E 1.52(4) . ?
C004 C14 1.42(4) . ?
C005 O00C 1.26(4) . ?
C005 O00L 1.27(4) . ?
C005 C00V 1.46(4) . ?
O006 C00E 1.27(4) . ?
O008 C00N 1.24(4) . ?
O009 C00N 1.28(4) . ?
C00D H00D 0.9500 . ?
C00D C00O 1.42(4) . ?
C00E O00M 1.22(4) . ?
C00F H00F 0.9500 . ?
C00F C00O 1.40(4) . ?
C00F C00V 1.45(4) . ?
C00J C00K 1.37(5) . ?
C00J C00R 1.39(5) . ?
C00K H00K 0.9500 . ?
C00K C00W 1.38(4) . ?
C00N C00W 1.53(5) . ?
C00O C00Q 1.47(4) . ?
C00Q C00R 1.39(4) . ?
C00Q C00S 1.33(4) . ?
C00R H00R 0.9500 . ?
C00S H00S 0.9500 . ?
C00S C00W 1.50(4) . ?
C00V C14 1.32(5) . ?
C14 H14 0.9500 . ?
O4 H4A 0.8741 . ?
O4 H4B 0.8735 . ?

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
O008 Pb01 O008 67.4(8) 1_654 2_566 ?
O008 Pb01 O00P 137.4(8) 1_654 2_656 ?
O008 Pb01 O00P 148.0(9) 2_566 2_656 ?
O009 Pb01 O008 105.0(7) 2_566 1_654 ?
O009 Pb01 O008 50.3(7) 2_566 2_566 ?
O009 Pb01 O00B 73.3(7) 2_566 2_656 ?
O009 Pb01 O00L 119.8(7) 2_566 2_665 ?
O009 Pb01 O00M 103.0(8) 2_566 . ?
O009 Pb01 O00P 117.1(8) 2_566 2_656 ?
O00B Pb01 O008 150.1(8) 2_656 1_654 ?
O00B Pb01 O008 122.6(7) 2_656 2_566 ?
O00B Pb01 O00L 117.1(7) 2_656 2_665 ?
O00B Pb01 O00P 49.8(8) 2_656 2_656 ?
O00L Pb01 O008 90.1(7) 2_665 1_654 ?
O00L Pb01 O008 87.3(7) 2_665 2_566 ?
O00L Pb01 O00P 75.1(7) 2_665 2_656 ?
O00M Pb01 O008 75.5(7) . 1_654 ?
O00M Pb01 O008 121.5(8) . 2_566 ?
O00M Pb01 O00B 75.9(8) . 2_656 ?
O00M Pb01 O00L 137.1(7) . 2_665 ?
O00M Pb01 O00P 88.6(8) . 2_656 ?
O006 Pb02 O00B 156.1(8) 1_465 2_666 ?
O006 Pb02 O00L 122.2(7) 1_465 . ?
O006 Pb02 O00P 121.7(9) 1_465 1_564 ?
O006 Pb02 O4 73.4(8) 1_465 . ?
O00B Pb02 O00L 72.7(7) 2_666 . ?
O00B Pb02 O00P 79.2(8) 2_666 1_564 ?
O00C Pb02 O006 78.1(7) . 1_465 ?
O00C Pb02 O00B 104.3(7) . 2_666 ?
O00C Pb02 O00L 50.3(6) . . ?
O00C Pb02 O00P 116.0(7) . 1_564 ?
O00C Pb02 O4 70.2(7) . . ?
O00P Pb02 O00L 72.2(7) 1_564 . ?
O4 Pb02 O00B 84.9(8) . 2_666 ?
O4 Pb02 O00L 105.4(7) . . ?
O4 Pb02 O00P 164.0(9) . 1_564 ?
O00B C003 C00J 117(3) . . ?
O00P C003 O00B 122(3) . . ?
O00P C003 C00J 121(3) . . ?
C00D C004 C00E 119(3) . . ?
C00D C004 C14 119(3) . . ?
C14 C004 C00E 121(3) . . ?
O00C C005 O00L 123(3) . . ?
O00C C005 C00V 122(3) . . ?
O00L C005 C00V 115(3) . . ?
C00E O006 Pb02 102(2) . 1_645 ?
Pb01 O008 Pb01 112.6(8) 1_456 2_566 ?
C00N O008 Pb01 89.0(19) . 2_566 ?
C00N O008 Pb01 125(2) . 1_456 ?
C00N O009 Pb01 97(2) . 2_566 ?
Pb01 O00B Pb02 106.1(8) 2_656 2_666 ?
C003 O00B Pb01 95.6(19) . 2_656 ?
C003 O00B Pb02 134(2) . 2_666 ?
C005 O00C Pb02 98.9(17) . . ?
C004 C00D H00D 118.8 . . ?
C004 C00D C00O 122(3) . . ?
C00O C00D H00D 118.8 . . ?
O006 C00E C004 116(3) . . ?
O00M C00E C004 120(3) . . ?
O00M C00E O006 124(3) . . ?
C00O C00F H00F 117.5 . . ?
C00O C00F C00V 125(3) . . ?
C00V C00F H00F 117.5 . . ?
C00K C00J C003 118(3) . . ?
C00K C00J C00R 120(3) . . ?
C00R C00J C003 121(3) . . ?
C00J C00K H00K 120.0 . . ?
C00J C00K C00W 120(3) . . ?
C00W C00K H00K 120.0 . . ?
Pb01 O00L Pb02 107.8(7) 2_665 . ?
C005 O00L Pb01 153(2) . 2_665 ?
C005 O00L Pb02 86.0(17) . . ?
C00E O00M Pb01 124(2) . . ?
O008 C00N O009 122(3) . . ?
O008 C00N C00W 117(3) . . ?
O009 C00N C00W 121(3) . . ?
C00D C00O C00Q 119(3) . . ?
C00F C00O C00D 114(3) . . ?
C00F C00O C00Q 126(3) . . ?
Pb01 O00P Pb02 105.0(7) 2_656 1_546 ?
C003 O00P Pb01 89.8(19) . 2_656 ?
C003 O00P Pb02 153(3) . 1_546 ?
C00R C00Q C00O 123(3) . . ?
C00S C00Q C00O 118(3) . . ?
C00S C00Q C00R 119(3) . . ?
C00J C00R C00Q 122(3) . . ?
C00J C00R H00R 119.0 . . ?
C00Q C00R H00R 119.0 . . ?
C00Q C00S H00S 120.2 . . ?
C00Q C00S C00W 120(3) . . ?
C00W C00S H00S 120.2 . . ?
C00F C00V C005 115(3) . . ?
C14 C00V C005 127(3) . . ?
C14 C00V C00F 117(3) . . ?
C00K C00W C00N 124(3) . . ?
C00K C00W C00S 119(3) . . ?
C00S C00W C00N 117(3) . . ?
C004 C14 H14 118.8 . . ?
C00V C14 C004 122(3) . . ?
C00V C14 H14 118.8 . . ?
Pb02 O4 H4A 110.5 . . ?
Pb02 O4 H4B 110.3 . . ?
H4A O4 H4B 103.5 . . ?

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
Pb01 O008 C00N O009 130(3) 1_456 . . . ?
Pb01 O008 C00N O009 13(4) 2_566 . . . ?
Pb01 O008 C00N C00W -48(4) 1_456 . . . ?
Pb01 O008 C00N C00W -165(3) 2_566 . . . ?
Pb01 O009 C00N O008 -14(4) 2_566 . . . ?
Pb01 O009 C00N C00W 164(3) 2_566 . . . ?
Pb02 O006 C00E C004 -161(2) 1_645 . . . ?
Pb02 O006 C00E O00M 17(4) 1_645 . . . ?
C003 C00J C00K C00W 176(3) . . . . ?
C003 C00J C00R C00Q -176(3) . . . . ?
C004 C00D C00O C00F 1(5) . . . . ?
C004 C00D C00O C00Q -176(3) . . . . ?
C004 C00E O00M Pb01 -52(4) . . . . ?
C005 C00V C14 C004 173(3) . . . . ?
O006 C00E O00M Pb01 131(3) . . . . ?
O008 C00N C00W C00K -9(5) . . . . ?
O008 C00N C00W C00S 160(3) . . . . ?
O009 C00N C00W C00K 172(3) . . . . ?
O009 C00N C00W C00S -18(5) . . . . ?
O00B C003 C00J C00K -178(3) . . . . ?
O00B C003 C00J C00R 0(5) . . . . ?
O00B C003 O00P Pb01 -18(4) . . . 2_656 ?
O00B C003 O00P Pb02 107(5) . . . 1_546 ?
O00C C005 O00L Pb01 -111(4) . . . 2_665 ?
O00C C005 O00L Pb02 11(3) . . . . ?
O00C C005 C00V C00F -2(4) . . . . ?
O00C C005 C00V C14 -171(3) . . . . ?
C00D C004 C00E O006 -17(5) . . . . ?
C00D C004 C00E O00M 166(3) . . . . ?
C00D C004 C14 C00V -2(6) . . . . ?
C00D C00O C00Q C00R 2(5) . . . . ?
C00D C00O C00Q C00S 180(3) . . . . ?
C00E C004 C00D C00O 170(3) . . . . ?
C00E C004 C14 C00V -173(3) . . . . ?
C00F C00O C00Q C00R -175(3) . . . . ?
C00F C00O C00Q C00S 3(5) . . . . ?
C00F C00V C14 C004 4(5) . . . . ?
C00J C003 O00B Pb01 -156(3) . . . 2_656 ?
C00J C003 O00B Pb02 85(4) . . . 2_666 ?
C00J C003 O00P Pb01 157(3) . . . 2_656 ?
C00J C003 O00P Pb02 -79(6) . . . 1_546 ?
C00J C00K C00W C00N 171(3) . . . . ?
C00J C00K C00W C00S 2(5) . . . . ?
C00K C00J C00R C00Q 2(5) . . . . ?
O00L C005 O00C Pb02 -13(3) . . . . ?
O00L C005 C00V C00F 180(3) . . . . ?
O00L C005 C00V C14 11(5) . . . . ?
C00O C00F C00V C005 -174(3) . . . . ?
C00O C00F C00V C14 -4(5) . . . . ?
C00O C00Q C00R C00J 176(3) . . . . ?
C00O C00Q C00S C00W -176(3) . . . . ?
O00P C003 O00B Pb01 19(4) . . . 2_656 ?
O00P C003 O00B Pb02 -100(4) . . . 2_666 ?
O00P C003 C00J C00K 7(5) . . . . ?
O00P C003 C00J C00R -175(4) . . . . ?
C00Q C00S C00W C00K -2(5) . . . . ?
C00Q C00S C00W C00N -173(3) . . . . ?
C00R C00J C00K C00W -2(5) . . . . ?
C00R C00Q C00S C00W 2(5) . . . . ?
C00S C00Q C00R C00J -2(5) . . . . ?
C00V C005 O00C Pb02 169(2) . . . . ?
C00V C005 O00L Pb01 68(5) . . . 2_665 ?
C00V C005 O00L Pb02 -170(2) . . . . ?
C00V C00F C00O C00D 1(5) . . . . ?
C00V C00F C00O C00Q 178(3) . . . . ?
C14 C004 C00D C00O -1(5) . . . . ?
C14 C004 C00E O006 154(4) . . . . ?
C14 C004 C00E O00M -23(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.442(3)
2 0.558(3)

_twin_special_details            
;
Component 2 rotated by -179.9275° 
 around [0.33 0.88 0.33] (reciprocal) or [0.26 0.96 0.09] (direct)
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pb_based_MOF
_database_code_depnum_ccdc_archive 'CCDC 2018703'
loop_
_audit_author_name
_audit_author_address
'xi chen'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2020-07-23 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT699_Pb_based_MOF        
;
PROBLEM: Missing _exptl_crystal_description Value .......     Please Do !
RESPONSE: powder
;
# Added during the CSD deposition process: Thursday 23 July 2020 11:46 PM
# end Validation Reply Form

_chemical_name_mineral           Pb_based_MOF
_chemical_formula_moiety         'C8 H3 O4 Pb'
_chemical_formula_sum            'C8 H3 O4 Pb'
_chemical_formula_weight         370.30
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,z

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/m
_symmetry_space_group_name_Hall  '-C 2y'
_cell_length_a                   9.3908(7)
_cell_length_b                   18.8473(8)
_cell_length_c                   4.6739(3)
_cell_angle_alpha                90
_cell_angle_beta                 118.995(5)
_cell_angle_gamma                90
_cell_volume                     723.55(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_exptl_crystal_density_diffrn    3.39939
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Diamond I11 Powder Diffractometer'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.824869
_diffrn_source                   Synchrotron
_refine_ls_goodness_of_fit_all   1.55728682
_refine_ls_R_factor_all          0.775186427
_refine_ls_shift/su_max          0.001
_pd_char_colour                  ?
_pd_meas_scan_method             continuous
_pd_proc_ls_prof_R_factor        1.33439581
_pd_proc_ls_prof_wR_expected     1.14771012
_pd_proc_ls_prof_wR_factor       1.78731384
_pd_spec_mount_mode              transmission
_pd_spec_mounting                'borosilicate capillary'
_pd_spec_shape                   cylinder

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Pb1 Pb 4 0.5 0.72324(6) 1 1 0.81(4)
C1 C 4 0.2982(7) 0.5 1.3349(14) 1 0.5(2)
C2 C 8 0.2390(5) 0.5645(3) 1.1690(7) 1 0.5(2)
C3 C 8 0.1205(3) 0.5645(3) 0.8372(7) 1 0.5(2)
C4 C 4 0.0612(5) 0.5 0.6714(14) 1 0.5(2)
C7 C 8 0.3044(7) 0.6357(5) 1.3522(13) 1 0.5(2)
O1 O 8 0.3777(15) 0.6337(5) 1.670(2) 1 0.5(2)
O2 O 8 0.2809(13) 0.6920(5) 1.1739(15) 1 0.5(2)
H1 H 4 0.3911(8) 0.5 1.5949(14) 1 0.6(2)
H3 H 8 0.0740(3) 0.6150(3) 0.7072(7) 1 0.6(2)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O2 2.620(12) . . no
Pb1 O1 2.197(9) . 1_554 no
Pb1 O2 2.620(12) . 2_657 no
Pb1 O1 2.197(9) . 2_658 no
Pb1 O2 2.845(11) . 7_567 no
Pb1 O2 2.845(11) . 8_565 no
O1 C7 1.300(10) . . no
O2 C7 1.300(12) . . no
C1 C2 1.404(6) . . no
C1 C2 1.404(6) . 4_565 no
C2 C3 1.404(4) . . no
C2 C7 1.550(10) . . no
C3 C4 1.404(6) . . no
C4 C4 1.450(8) . 2_556 no
C1 H1 1.100(8) . . no
C3 H3 1.099(7) . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O2 79.8(4) 1_554 . . no
O2 Pb1 O2 154.0(3) . . 2_657 no
O1 Pb1 O2 80.3(4) 2_658 . . no
O2 Pb1 O2 57.0(3) . . 7_567 no
O2 Pb1 O2 142.8(2) . . 8_565 no
O1 Pb1 O2 80.3(4) 1_554 . 2_657 no
O1 Pb1 O1 79.7(3) 1_554 . 2_658 no
O1 Pb1 O2 97.7(4) 1_554 . 7_567 no
O1 Pb1 O2 136.8(4) 1_554 . 8_565 no
O1 Pb1 O2 79.8(4) 2_658 . 2_657 no
O2 Pb1 O2 142.8(2) 2_657 . 7_567 no
O2 Pb1 O2 57.0(3) 2_657 . 8_565 no
O1 Pb1 O2 136.8(4) 2_658 . 7_567 no
O1 Pb1 O2 97.7(4) 2_658 . 8_565 no
O2 Pb1 O2 111.7(3) 7_567 . 8_565 no
Pb1 O1 C7 125.9(7) 1_556 . . no
Pb1 O2 C7 117.9(8) . . . no
Pb1 O2 Pb1 123.0(3) . . 7_567 no
Pb1 O2 C7 119.2(8) 7_567 . . no
C2 C1 C2 120.0(5) . . 4_565 no
C1 C2 C3 120.0(5) . . . no
C1 C2 C7 120.0(4) . . . no
C3 C2 C7 120.0(5) . . . no
C2 C3 C4 120.0(5) . . . no
C3 C4 C4 120.0(3) . . 2_556 no
C3 C4 C3 120.0(5) . . 4_565 no
C3 C4 C4 120.0(3) 4_565 . 2_556 no
O1 C7 O2 126.0(9) . . . no
O1 C7 C2 117.1(7) . . . no
O2 C7 C2 117.0(5) . . . no
C2 C1 H1 120.0(3) . . . no
C2 C1 H1 120.0(3) 4_565 . . no
C2 C3 H3 120.0(5) . . . no
C4 C3 H3 120.0(4) . . . no

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
O1 Pb1 O2 C7 75.0(6) 1_554 . . . no
O2 Pb1 O2 C7 34.4(9) 2_657 . . . no
O1 Pb1 O2 C7 -6.2(6) 2_658 . . . no
O2 Pb1 O2 C7 -178.9(7) 7_567 . . . no
O2 Pb1 O2 C7 -96.1(7) 8_565 . . . no
Pb1 O1 C7 O2 -5.1(18) 1_556 . . . no
Pb1 O1 C7 C2 175.0(7) 1_556 . . . no
Pb1 O2 C7 O1 92.1(11) . . . . no
Pb1 O2 C7 C2 93.2(7) 7_567 . . . no
Pb1 O2 C7 C2 -87.9(7) . . . . no
Pb1 O2 C7 O1 -86.8(12) 7_567 . . . no
C2 C1 C2 C3 0.0(9) 4_565 . . . no
C2 C1 C2 C7 -180.0(6) 4_565 . . . no
C1 C2 C3 C4 0.0(7) . . . . no
C1 C2 C7 O2 161.7(8) . . . . no
C7 C2 C3 C4 -180.0(5) . . . . no
C1 C2 C7 O1 -18.3(11) . . . . no
C3 C2 C7 O1 161.6(9) . . . . no
C3 C2 C7 O2 -18.4(10) . . . . no
C2 C3 C4 C3 -0.1(7) . . . 4_565 no
C2 C3 C4 C4 -180.0(5) . . . 2_556 no

loop_
_pd_meas_2theta_scan
_pd_proc_intensity_total
_pd_calc_intensity_total
_pd_proc_ls_weight
2.50000 8928.39961 8904.69250 0.00011
2.50400 8840.02033 8903.72578 0.00011
2.50800 9004.86507 8902.76317 0.00011
2.51200 9045.79411 8901.80462 0.00011
2.51600 9002.03253 8900.85011 0.00011
2.52000 8987.97421 8899.89963 0.00011
2.52400 8874.34351 8898.95315 0.00011
2.52800 8933.13833 8898.01064 0.00011
2.53200 9030.95937 8897.07208 0.00011
2.53600 8971.78093 8896.13745 0.00011
2.54000 8929.44829 8895.20672 0.00011
2.54400 8801.92540 8894.27986 0.00011
2.54800 9017.70196 8893.35687 0.00011
2.55200 8913.48034 8892.43771 0.00011
2.55600 9000.14122 8891.52235 0.00011
2.56000 8977.82684 8890.61079 0.00011
2.56400 8799.42338 8889.70298 0.00011
2.56800 8866.58877 8888.79892 0.00011
2.57200 8991.22649 8887.89857 0.00011
2.57600 8893.42730 8887.00192 0.00011
2.58000 8945.53346 8886.10894 0.00011
2.58400 8910.69167 8885.21961 0.00011
2.58800 8861.78560 8884.33390 0.00011
2.59200 8891.94136 8883.45179 0.00011
2.59600 8997.10599 8882.57327 0.00011
2.60000 8985.09515 8881.69831 0.00011
2.60400 8931.02399 8880.82688 0.00011
2.60800 9019.17860 8879.95896 0.00011
2.61200 9044.41594 8879.09454 0.00011
2.61600 8977.58828 8878.23358 0.00011
2.62000 8942.90740 8877.37608 0.00011
2.62400 9010.17461 8876.52199 0.00011
2.62800 9006.36137 8875.67131 0.00011
2.63200 8945.74387 8874.82401 0.00011
2.63600 8841.57095 8873.98007 0.00011
2.64000 8842.01865 8873.41965 0.00011
2.64400 8826.23869 8872.58313 0.00011
2.64800 8989.86597 8871.74991 0.00011
2.65200 8800.46412 8870.91997 0.00011
2.65600 9031.84382 8870.09328 0.00011
2.66000 8924.86038 8869.26983 0.00011
2.66400 8853.75493 8868.44958 0.00011
2.66800 8993.01973 8867.63253 0.00011
2.67200 8851.99149 8866.81865 0.00011
2.67600 8855.53625 8866.00793 0.00011
2.68000 8867.36952 8865.20036 0.00011
2.68400 9221.82718 8864.39594 0.00011
2.68800 8943.61056 8863.59465 0.00011
2.69200 8913.95629 8862.79650 0.00011
2.69600 8887.35391 8862.00158 0.00011
2.70000 8871.42013 8861.20998 0.00011
2.70400 8925.52701 8860.42127 0.00011
2.70800 8942.54845 8859.63498 0.00011
2.71200 8938.69375 8858.85165 0.00011
2.71600 8754.46516 8858.07126 0.00011
2.72000 8735.46695 8857.29379 0.00011
2.72400 8932.77212 8856.51922 0.00011
2.72800 8850.87377 8855.74754 0.00011
2.73200 8860.28030 8854.97871 0.00011
2.73600 8815.53648 8854.21273 0.00011
2.74000 8897.42018 8853.44957 0.00011
2.74400 8810.07675 8852.68920 0.00011
2.74800 8792.10895 8851.93162 0.00011
2.75200 8860.07540 8851.17681 0.00011
2.75600 8873.69818 8850.42473 0.00011
2.76000 8791.66829 8849.67538 0.00011
2.76400 8789.03084 8848.92873 0.00011
2.76800 8867.59758 8848.18476 0.00011
2.77200 8871.56626 8847.44345 0.00011
2.77600 8789.10926 8846.70479 0.00011
2.78000 8784.67669 8845.96876 0.00011
2.78400 9003.46171 8845.23533 0.00011
2.78800 9007.69607 8844.50449 0.00011
2.79200 9053.51371 8843.77622 0.00011
2.79600 8813.74728 8843.05050 0.00011
2.80000 8753.28699 8842.32730 0.00011
2.80400 8880.07338 8841.60662 0.00011
2.80800 8911.12586 8840.88843 0.00011
2.81200 8893.06428 8840.17272 0.00011
2.81600 8735.23516 8839.45945 0.00011
2.82000 8771.24656 8838.74863 0.00011
2.82400 8859.14682 8838.04022 0.00011
2.82800 8891.28346 8837.33422 0.00011
2.83200 8987.42140 8836.63059 0.00011
2.83600 8761.00097 8835.92933 0.00011
2.84000 8775.11551 8835.23041 0.00011
2.84400 8641.88929 8834.53381 0.00012
2.84800 8689.48841 8833.83953 0.00012
2.85200 8848.96425 8833.14753 0.00011
2.85600 8845.00404 8832.45781 0.00011
2.86000 9065.01226 8831.77034 0.00011
2.86400 8782.73599 8831.08511 0.00011
2.86800 8757.01235 8830.40209 0.00011
2.87200 8839.96087 8829.72128 0.00011
2.87600 8869.16438 8829.04265 0.00011
2.88000 8815.05546 8828.36618 0.00011
2.88400 8696.51671 8827.69187 0.00011
2.88800 8805.39083 8827.01968 0.00011
2.89200 8903.67946 8826.34961 0.00011
2.89600 8893.85111 8825.68163 0.00011
2.90000 8825.12680 8825.01573 0.00011
2.90400 8764.14388 8824.35189 0.00011
2.90800 8932.15801 8823.69009 0.00011
2.91200 8814.15747 8823.03032 0.00011
2.91600 8743.97717 8822.37257 0.00011
2.92000 8842.65673 8821.71680 0.00011
2.92400 8762.99654 8821.06301 0.00011
2.92800 8745.62145 8820.41118 0.00011
2.93200 8717.20782 8819.76129 0.00011
2.93600 8803.74154 8819.11333 0.00011
2.94000 8668.13838 8818.46727 0.00012
2.94400 8920.19339 8817.82311 0.00011
2.94800 8775.48974 8817.18082 0.00011
2.95200 8782.55200 8816.54239 0.00011
2.95600 8866.56363 8815.91458 0.00011
2.96000 8774.67892 8815.30132 0.00011
2.96400 8777.64855 8814.70386 0.00011
2.96800 8649.38825 8814.12404 0.00012
2.97200 8906.69248 8813.56414 0.00011
2.97600 8733.16680 8813.02703 0.00011
2.98000 8682.06557 8812.51642 0.00012
2.98400 8725.57913 8812.03726 0.00011
2.98800 8807.60635 8811.59644 0.00011
2.99200 8997.19078 8811.20400 0.00011
2.99600 8840.67375 8810.87580 0.00011
3.00000 8817.94695 8810.63998 0.00011
3.00400 8931.95911 8810.55961 0.00011
3.00800 8871.24356 8810.84006 0.00011
3.01200 8850.57995 8811.58996 0.00011
3.01600 8828.76605 8811.69176 0.00011
3.02000 8938.45700 8811.10114 0.00011
3.02400 8924.70026 8810.51222 0.00011
3.02800 8993.47974 8809.92498 0.00011
3.03200 8759.21292 8809.33942 0.00011
3.03600 8840.04809 8808.75550 0.00011
3.04000 8801.29842 8808.17323 0.00011
3.04400 8689.31404 8807.59259 0.00012
3.04800 8724.33040 8807.01356 0.00011
3.05200 8796.78417 8806.43612 0.00011
3.05600 8809.30048 8805.86028 0.00011
3.06000 8736.63654 8805.28600 0.00011
3.06400 8837.23148 8804.71328 0.00011
3.06800 8754.91151 8804.14211 0.00011
3.07200 8739.63506 8803.57247 0.00011
3.07600 8740.05039 8803.00434 0.00011
3.08000 8746.08705 8802.43772 0.00011
3.08400 8959.24427 8801.87259 0.00011
3.08800 8776.62748 8801.30894 0.00011
3.09200 8844.82738 8800.74675 0.00011
3.09600 8752.84433 8800.18601 0.00011
3.10000 8695.10551 8799.62671 0.00012
3.10400 8621.70165 8799.06884 0.00012
3.10800 8849.38150 8798.51238 0.00011
3.11200 8857.27567 8797.95759 0.00011
3.11600 8863.18593 8797.40568 0.00011
3.12000 8743.14133 8796.85834 0.00011
3.12400 8857.37281 8796.31998 0.00011
3.12800 8846.86894 8795.79731 0.00011
3.13200 8757.95039 8795.27488 0.00011
3.13600 8627.04102 8794.74730 0.00012
3.14000 8698.35925 8794.23325 0.00011
3.14400 8710.10496 8793.73782 0.00011
3.14800 8789.39957 8793.27170 0.00011
3.15200 8715.61383 8792.86673 0.00011
3.15600 8633.53889 8792.56988 0.00012
3.16000 8842.20275 8792.25912 0.00011
3.16400 8832.57425 8791.72216 0.00011
3.16800 8743.49965 8791.18643 0.00011
3.17200 8677.92714 8790.65192 0.00012
3.17600 8646.05637 8790.11861 0.00012
3.18000 8723.73701 8789.58650 0.00011
3.18400 8654.77465 8789.05745 0.00012
3.18800 8726.89137 8788.52771 0.00011
3.19200 8811.23362 8787.99913 0.00011
3.19600 8765.96645 8787.47169 0.00011
3.20000 8649.46232 8786.94540 0.00012
3.20400 8603.10895 8786.42023 0.00012
3.20800 8774.60390 8785.89618 0.00011
3.21200 8674.04289 8785.37323 0.00012
3.21600 8608.73983 8784.85137 0.00012
3.22000 8604.06819 8784.33060 0.00012
3.22400 8768.30916 8783.81090 0.00011
3.22800 8778.24151 8783.29226 0.00011
3.23200 8900.59331 8782.77467 0.00011
3.23600 8797.50594 8782.25811 0.00011
3.24000 8797.36745 8781.74259 0.00011
3.24400 8643.21311 8781.22809 0.00012
3.24800 8628.23437 8780.71460 0.00012
3.25200 8875.96011 8780.20211 0.00011
3.25600 8689.36224 8779.69060 0.00012
3.26000 8609.20564 8779.18007 0.00012
3.26400 8667.89720 8778.67051 0.00012
3.26800 8764.18087 8778.16191 0.00011
3.27200 8774.33865 8777.65426 0.00011
3.27600 8758.81408 8777.14754 0.00011
3.28000 8734.85669 8776.64175 0.00011
3.28400 8727.41467 8776.13688 0.00011
3.28800 8638.31569 8775.63292 0.00012
3.29200 8666.74774 8775.12986 0.00012
3.29600 8643.46572 8774.62769 0.00012
3.30000 8687.45320 8774.12641 0.00012
3.30400 8659.01865 8773.62599 0.00012
3.30800 8736.87664 8773.12644 0.00011
3.31200 8656.62394 8772.62773 0.00012
3.31600 8681.22023 8772.12988 0.00012
3.32000 8691.07944 8771.63286 0.00012
3.32400 8799.54555 8771.13666 0.00011
3.32800 8765.91788 8770.64128 0.00011
3.33200 8714.19393 8770.14672 0.00011
3.33600 8726.98692 8769.65293 0.00011
3.34000 8851.14045 8769.16100 0.00011
3.34400 8787.84501 8768.67465 0.00011
3.34800 8714.11695 8768.20188 0.00011
3.35200 8685.70112 8767.75165 0.00012
3.35600 8682.54278 8767.29376 0.00012
3.36000 8710.25218 8766.80466 0.00011
3.36400 8707.66871 8766.31631 0.00011
3.36800 8808.76596 8765.82868 0.00011
3.37200 8788.65948 8765.34178 0.00011
3.37600 8706.53604 8764.85560 0.00011
3.38000 8635.84122 8764.37013 0.00012
3.38400 8592.45939 8763.88537 0.00012
3.38800 8688.13339 8763.40129 0.00012
3.39200 8786.21571 8762.91791 0.00011
3.39600 8756.94056 8762.43521 0.00011
3.40000 8795.85769 8761.95317 0.00011
3.40400 8829.33768 8761.47181 0.00011
3.40800 8872.73950 8760.99110 0.00011
3.41200 8795.23779 8760.51104 0.00011
3.41600 8811.72357 8760.03163 0.00011
3.42000 8759.78637 8759.55285 0.00011
3.42400 8664.07641 8759.07471 0.00012
3.42800 8714.71691 8758.59719 0.00011
3.43200 8874.71973 8758.12028 0.00011
3.43600 8588.79973 8757.64399 0.00012
3.44000 8659.20911 8757.16830 0.00012
3.44400 8533.38615 8756.69321 0.00012
3.44800 8654.25715 8756.21871 0.00012
3.45200 8761.94035 8755.74479 0.00011
3.45600 8752.05344 8755.27146 0.00011
3.46000 8662.65380 8754.79870 0.00012
3.46400 8622.01530 8754.32650 0.00012
3.46800 8656.51220 8753.85486 0.00012
3.47200 8744.99281 8753.38379 0.00011
3.47600 8730.56097 8752.91326 0.00011
3.48000 8718.58535 8752.44327 0.00011
3.48400 8699.13573 8751.97383 0.00011
3.48800 8695.89694 8751.50492 0.00011
3.49200 8695.26036 8751.03653 0.00012
3.49600 8671.03169 8750.56867 0.00012
3.50000 8633.02716 8750.10133 0.00012
3.50400 8590.49972 8749.63450 0.00012
3.50800 8688.98375 8749.16818 0.00012
3.51200 8637.01471 8748.70236 0.00012
3.51600 8607.50292 8748.23705 0.00012
3.52000 8530.33617 8747.77222 0.00012
3.52400 8608.68522 8747.30789 0.00012
3.52800 8724.96858 8746.84404 0.00011
3.53200 8718.89140 8746.38068 0.00011
3.53600 8709.22908 8745.91779 0.00011
3.54000 8661.71585 8745.45537 0.00012
3.54400 8602.54487 8744.99342 0.00012
3.54800 8571.76071 8744.53195 0.00012
3.55200 8591.35872 8744.07093 0.00012
3.55600 8598.24661 8743.61038 0.00012
3.56000 8723.17496 8743.15029 0.00011
3.56400 8664.27696 8742.69067 0.00012
3.56800 8613.26843 8742.23155 0.00012
3.57200 8634.53184 8741.77295 0.00012
3.57600 8584.79601 8741.31498 0.00012
3.58000 8788.03879 8740.85779 0.00011
3.58400 8708.10694 8740.40169 0.00011
3.58800 8651.26659 8739.94727 0.00012
3.59200 8703.63382 8739.49554 0.00011
3.59600 8688.34115 8739.04831 0.00012
3.60000 8585.29880 8738.60866 0.00012
3.60400 8578.55875 8738.18174 0.00012
3.60800 8683.56991 8737.77595 0.00012
3.61200 8647.45316 8737.40468 0.00012
3.61600 8697.98988 8737.08873 0.00011
3.62000 8714.54332 8736.85958 0.00011
3.62400 8611.11479 8736.76378 0.00012
3.62800 8794.96809 8736.86819 0.00011
3.63200 8684.62583 8737.26639 0.00012
3.63600 8692.06867 8738.08551 0.00012
3.64000 8703.57896 8739.49317 0.00011
3.64400 8705.65863 8741.70334 0.00011
3.64800 8648.61739 8744.97976 0.00012
3.65200 8759.09321 8749.63527 0.00011
3.65600 8742.42038 8756.02495 0.00011
3.66000 8764.73102 8764.53157 0.00011
3.66400 8741.21539 8775.54168 0.00011
3.66800 8721.16356 8789.41211 0.00011
3.67200 8747.10367 8806.42778 0.00011
3.67600 8905.59361 8826.75334 0.00011
3.68000 8929.47901 8850.38310 0.00011
3.68400 8875.64353 8877.09530 0.00011
3.68800 8986.85752 8906.41783 0.00011
3.69200 8836.94227 8937.61239 0.00011
3.69600 8834.82876 8969.68359 0.00011
3.70000 9157.69453 9001.41639 0.00011
3.70400 9140.61342 9031.44252 0.00011
3.70800 8991.32011 9058.33203 0.00011
3.71200 9022.43017 9080.70219 0.00011
3.71600 8994.24570 9097.33242 0.00011
3.72000 9139.53262 9107.27227 0.00011
3.72400 9354.06957 9109.92896 0.00011
3.72800 9130.38019 9105.12341 0.00011
3.73200 9035.09960 9093.10740 0.00011
3.73600 9018.43992 9074.53953 0.00011
3.74000 8916.69816 9050.42308 0.00011
3.74400 8957.26516 9022.01421 0.00011
3.74800 8963.76942 8990.71182 0.00011
3.75200 9046.65380 8957.94267 0.00011
3.75600 8970.65128 8925.05484 0.00011
3.76000 8984.57124 8893.22991 0.00011
3.76400 8811.48002 8863.42141 0.00011
3.76800 8834.68245 8836.32221 0.00011
3.77200 8866.69702 8812.36017 0.00011
3.77600 8753.61796 8791.71744 0.00011
3.78000 8878.23302 8774.36733 0.00011
3.78400 8742.30831 8760.12117 0.00011
3.78800 8684.33554 8748.67853 0.00012
3.79200 8800.03374 8739.67477 0.00011
3.79600 8806.82629 8732.72188 0.00011
3.80000 8653.80855 8727.44039 0.00012
3.80400 8734.16570 8723.48160 0.00011
3.80800 8699.82694 8720.54077 0.00011
3.81200 8566.70960 8718.36270 0.00012
3.81600 8603.72391 8716.74165 0.00012
3.82000 8517.15100 8715.51734 0.00012
3.82400 8528.12141 8714.56886 0.00012
3.82800 8639.45891 8713.80766 0.00012
3.83200 8719.05831 8713.17076 0.00011
3.83600 8521.41378 8712.61453 0.00012
3.84000 8745.26837 8712.10958 0.00011
3.84400 8796.39630 8711.63660 0.00011
3.84800 8744.03649 8711.18319 0.00011
3.85200 8614.75905 8710.74164 0.00012
3.85600 8664.02509 8710.30721 0.00012
3.86000 8722.40016 8709.87709 0.00011
3.86400 8747.27713 8709.44966 0.00011
3.86800 8681.69249 8709.02398 0.00012
3.87200 8642.38497 8708.59956 0.00012
3.87600 8726.57615 8708.17612 0.00011
3.88000 8740.87364 8707.75351 0.00011
3.88400 8788.92582 8707.33168 0.00011
3.88800 8571.91613 8706.91059 0.00012
3.89200 8570.23163 8706.49024 0.00012
3.89600 8488.66562 8706.07063 0.00012
3.90000 8532.47897 8705.65177 0.00012
3.90400 8802.68237 8705.23368 0.00011
3.90800 8688.69888 8704.81636 0.00012
3.91200 8619.48002 8704.39982 0.00012
3.91600 8698.43717 8703.98410 0.00011
3.92000 8660.89191 8703.56920 0.00012
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