#------------------------------------------------------------------------------
#$Date: 2021-02-05 00:27:37 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261525 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/75/7127527.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_7127527
loop_
_publ_author_name
'Chen, Xi'
'Zhang, Zhongyue'
'Chen, Jin'
'Sapchenko, Sergei'
'Han, Xue'
'da-Silva, Ivan'
'Li, Ming'
'Vitorica-Yrezabal, Inigo J'
'Whitehead, George'
'Tang, Chiu C.'
'Awaga, Kunio'
'Yang, Sihai'
'Schröder, Martin'
_publ_section_title
;
 Enhanced proton conductivity in a flexible metal-organic framework
 promoted by single-crystal-to-single-crystal transformation.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              65
_journal_page_last               68
_journal_paper_doi               10.1039/d0cc05270a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '0.25(C48 H48 N4 O20 Pb4)'
_chemical_formula_sum            'C12 H12 N O5 Pb'
_chemical_formula_weight         457.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-04-07 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                111.886(4)
_cell_angle_beta                 101.798(3)
_cell_angle_gamma                103.943(4)
_cell_formula_units_Z            4
_cell_length_a                   10.4855(4)
_cell_length_b                   11.1137(5)
_cell_length_c                   12.4920(4)
_cell_measurement_reflns_used    4165
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      26.3440
_cell_measurement_theta_min      1.8610
_cell_volume                     1239.04(11)
_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)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_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_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_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_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.051
_refine_diff_density_max         5.219
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.268
_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_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0358
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6439
_reflns_number_total             7619
_reflns_threshold_expression     'I > 2σ(I)'
_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)
;
_cod_data_source_file            d0cc05270a2.cif
_cod_data_source_block           s5102r_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7127527--7127529.cif.'
_cod_original_cell_volume        1239.04(9)
_cod_database_code               7127527
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C24H24N2O10Pb2
_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.
;
_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)
;
_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_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 . . . .
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'
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
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 . . ?
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_
_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
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
