#------------------------------------------------------------------------------
#$Date: 2021-12-07 03:53:47 +0100 (mar 07 de dic de 2021) $
#$Revision: 271159 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/36/7243684.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_7243684
loop_
_publ_author_name
'Yuan, Guo-Jun'
'Zhou, Hong'
'Li, Li'
'Chen, Hong'
'Ren, Xiao-Ming'
_publ_section_title
;
 Supramolecular [Na(15-crown-5)]+ cations anchored to face-sharing
 octahedral lead bromide chains featuring a rotor-like one-dimensional
 perovskite with a reversible isostructural phase transition near room
 temperature
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7787
_journal_page_last               7793
_journal_paper_doi               10.1039/D1CE01273H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         ' C10 H20 Br3 Na O5 Pb'
_chemical_formula_sum            'C10 H20 Br3 Na O5 Pb'
_chemical_formula_weight         690.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-22 deposited with the CCDC.	2021-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8558(3)
_cell_length_b                   13.8616(5)
_cell_length_c                   16.5205(7)
_cell_measurement_reflns_used    7814
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.47
_cell_volume                     1798.98(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17645
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.349
_diffrn_reflns_theta_min         2.871
_diffrn_source.source            'Ius 2.0'
_diffrn_source.type              microfocus
_exptl_absorpt_coefficient_mu    16.077
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.548
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00144(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0262
_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)+(0.0274P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1846
_reflns_number_total             2313
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01273h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7243683--7243691.cif.'
_cod_database_code               7243684
_shelx_shelxl_version_number     2018/3
_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   0.271
_shelx_estimated_absorpt_t_max   0.296
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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 0.67528(2) 0.750000 0.74963(2) 0.02015(8) Uani 1 2 d S T P . .
Br1 Br 0.43420(4) 0.60395(2) 0.81443(2) 0.02824(11) Uani 1 1 d . . . . .
Br2 Br 0.42216(6) 0.750000 0.60598(3) 0.03029(14) Uani 1 2 d S T P . .
Na1 Na 0.5585(2) 0.750000 0.44083(12) 0.0243(4) Uani 1 2 d S T P . .
O1 O 0.4717(7) 0.6286(4) 0.3459(3) 0.0289(12) Uani 0.5 1 d . . P . .
O2 O 0.3350(7) 0.8070(4) 0.3531(4) 0.0308(14) Uani 0.5 1 d . . P . .
O3 O 0.5658(6) 0.9234(3) 0.4327(3) 0.0260(12) Uani 0.5 1 d . . P . .
O4 O 0.8534(7) 0.8045(4) 0.4268(3) 0.0290(12) Uani 0.5 1 d . . P . .
O5 O 0.7425(7) 0.6181(3) 0.4472(3) 0.0310(12) Uani 0.5 1 d . . P . .
C1 C 0.2987(12) 0.6449(8) 0.3315(6) 0.033(2) Uani 0.5 1 d . . P . .
H1A H 0.269180 0.601111 0.289066 0.040 Uiso 0.5 1 d R U P . .
H1B H 0.226110 0.632382 0.376576 0.040 Uiso 0.5 1 d R U P . .
C2 C 0.2779(8) 0.750000 0.2937(4) 0.0413(15) Uani 1 2 d S T P . .
H2A H 0.341492 0.761170 0.245444 0.050 Uiso 0.5 1 d R U P . .
H2B H 0.160693 0.762560 0.282884 0.050 Uiso 0.5 1 d R U P . .
C3 C 0.3662(12) 0.9025(6) 0.3225(5) 0.0309(19) Uani 0.5 1 d . . P . .
H3A H 0.265696 0.929124 0.298954 0.037 Uiso 0.5 1 d R U P . .
H3B H 0.452193 0.899306 0.281822 0.037 Uiso 0.5 1 d R U P . .
C4 C 0.4242(12) 0.9657(9) 0.3920(7) 0.031(2) Uani 0.5 1 d . . P . .
H4A H 0.454607 1.028338 0.372243 0.037 Uiso 0.5 1 d R U P . .
H4B H 0.334397 0.973215 0.430313 0.037 Uiso 0.5 1 d R U P . .
C5 C 0.731(3) 0.959(2) 0.4096(13) 0.021(4) Uani 0.5 1 d . . P . .
H5A H 0.738274 1.026119 0.422880 0.025 Uiso 0.5 1 d R U P . .
H5B H 0.742973 0.952138 0.352430 0.025 Uiso 0.5 1 d R U P . .
C6 C 0.8596(13) 0.9023(7) 0.4526(6) 0.030(2) Uani 0.5 1 d . . P . .
H6A H 0.968962 0.926224 0.437433 0.035 Uiso 0.5 1 d R U P . .
H6B H 0.847333 0.909094 0.509763 0.035 Uiso 0.5 1 d R U P . .
C7 C 0.9425(6) 0.750000 0.4786(4) 0.0410(15) Uani 1 2 d S T P . .
H7A H 0.905364 0.759500 0.532962 0.049 Uiso 0.5 1 d R U P . .
H7B H 1.059939 0.766940 0.474762 0.049 Uiso 0.5 1 d R U P . .
C8 C 0.9187(13) 0.6392(8) 0.4460(6) 0.037(2) Uani 0.5 1 d . . P . .
H8A H 0.974838 0.596713 0.482972 0.044 Uiso 0.5 1 d R U P . .
H8B H 0.968700 0.630454 0.393902 0.044 Uiso 0.5 1 d R U P . .
C9 C 0.692(3) 0.537(2) 0.3965(16) 0.036(6) Uani 0.5 1 d . . P . .
H9A H 0.721827 0.477880 0.423338 0.043 Uiso 0.5 1 d R U P . .
H9B H 0.754297 0.539801 0.346957 0.043 Uiso 0.5 1 d R U P . .
C10 C 0.5075(14) 0.5402(9) 0.3846(9) 0.041(3) Uani 0.5 1 d . . P . .
H10A H 0.487447 0.490694 0.345449 0.050 Uiso 0.5 1 d R U P . .
H10B H 0.439696 0.526823 0.431189 0.050 Uiso 0.5 1 d R U P . .
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
Br1 Pb1 Br1 85.881(15) 7_575 . ?
Br1 Pb1 Br1 95.598(11) 7_575 4_566 ?
Br1 Pb1 Br1 177.900(11) . 4_566 ?
Br1 Pb1 Br1 177.899(11) 7_575 6_657 ?
Br1 Pb1 Br1 95.598(12) . 6_657 ?
Br1 Pb1 Br1 82.885(14) 4_566 6_657 ?
Br1 Pb1 Br2 97.037(11) 7_575 6_657 ?
Br1 Pb1 Br2 97.038(11) . 6_657 ?
Br1 Pb1 Br2 81.314(11) 4_566 6_657 ?
Br1 Pb1 Br2 81.315(11) 6_657 6_657 ?
Br1 Pb1 Br2 82.348(11) 7_575 . ?
Br1 Pb1 Br2 82.347(11) . . ?
Br1 Pb1 Br2 99.314(11) 4_566 . ?
Br1 Pb1 Br2 99.313(11) 6_657 . ?
Br2 Pb1 Br2 179.154(15) 6_657 . ?
Pb1 Br1 Pb1 81.270(9) . 6_557 ?
Na1 Br2 Pb1 162.32(4) . 6_557 ?
Na1 Br2 Pb1 118.61(4) . . ?
Pb1 Br2 Pb1 79.072(13) 6_557 . ?
O5 Na1 O5 103.2(3) . 7_575 ?
O5 Na1 O1 69.84(18) . . ?
O5 Na1 O1 139.03(19) 7_575 . ?
O5 Na1 O1 139.03(19) . 7_575 ?
O5 Na1 O1 69.84(18) 7_575 7_575 ?
O1 Na1 O1 89.1(2) . 7_575 ?
O5 Na1 O3 140.36(19) . . ?
O5 Na1 O3 37.39(18) 7_575 . ?
O1 Na1 O3 132.11(19) . . ?
O1 Na1 O3 43.12(17) 7_575 . ?
O5 Na1 O3 37.39(18) . 7_575 ?
O5 Na1 O3 140.36(19) 7_575 7_575 ?
O1 Na1 O3 43.11(17) . 7_575 ?
O1 Na1 O3 132.11(19) 7_575 7_575 ?
O3 Na1 O3 173.0(3) . 7_575 ?
O5 Na1 O2 137.3(2) . . ?
O5 Na1 O2 102.8(2) 7_575 . ?
O1 Na1 O2 68.29(19) . . ?
O1 Na1 O2 33.90(18) 7_575 . ?
O3 Na1 O2 69.90(19) . . ?
O3 Na1 O2 108.1(2) 7_575 . ?
O5 Na1 O2 102.8(2) . 7_575 ?
O5 Na1 O2 137.3(2) 7_575 7_575 ?
O1 Na1 O2 33.90(18) . 7_575 ?
O1 Na1 O2 68.29(19) 7_575 7_575 ?
O3 Na1 O2 108.1(2) . 7_575 ?
O3 Na1 O2 69.90(19) 7_575 7_575 ?
O2 Na1 O2 38.3(3) . 7_575 ?
O5 Na1 O4 70.11(19) . . ?
O5 Na1 O4 34.51(17) 7_575 . ?
O1 Na1 O4 115.07(19) . . ?
O1 Na1 O4 89.46(18) 7_575 . ?
O3 Na1 O4 70.37(17) . . ?
O3 Na1 O4 106.29(17) 7_575 . ?
O2 Na1 O4 122.12(18) . . ?
O2 Na1 O4 137.2(2) 7_575 . ?
O5 Na1 O4 34.51(17) . 7_575 ?
O5 Na1 O4 70.11(19) 7_575 7_575 ?
O1 Na1 O4 89.46(18) . 7_575 ?
O1 Na1 O4 115.07(19) 7_575 7_575 ?
O3 Na1 O4 106.29(17) . 7_575 ?
O3 Na1 O4 70.37(17) 7_575 7_575 ?
O2 Na1 O4 137.2(2) . 7_575 ?
O2 Na1 O4 122.12(18) 7_575 7_575 ?
O4 Na1 O4 36.0(2) . 7_575 ?
O5 Na1 Br2 100.64(14) . . ?
O5 Na1 Br2 100.65(14) 7_575 . ?
O1 Na1 Br2 120.30(13) . . ?
O1 Na1 Br2 120.30(13) 7_575 . ?
O3 Na1 Br2 93.47(13) . . ?
O3 Na1 Br2 93.47(13) 7_575 . ?
O2 Na1 Br2 107.06(15) . . ?
O2 Na1 Br2 107.06(15) 7_575 . ?
O4 Na1 Br2 115.70(15) . . ?
O4 Na1 Br2 115.71(15) 7_575 . ?
O5 Na1 C10 49.7(3) . . ?
O5 Na1 C10 146.5(2) 7_575 . ?
O1 Na1 C10 26.3(3) . . ?
O1 Na1 C10 115.4(3) 7_575 . ?
O3 Na1 C10 158.3(3) . . ?
O3 Na1 C10 17.0(3) 7_575 . ?
O2 Na1 C10 91.9(3) . . ?
O2 Na1 C10 54.1(3) 7_575 . ?
O4 Na1 C10 112.7(2) . . ?
O4 Na1 C10 78.6(2) 7_575 . ?
Br2 Na1 C10 103.5(2) . . ?
C3 O1 C1 37.5(6) 7_575 . ?
C3 O1 O2 71.1(6) 7_575 7_575 ?
C1 O1 O2 33.5(4) . 7_575 ?
C3 O1 C10 88.1(8) 7_575 . ?
C1 O1 C10 114.3(7) . . ?
O2 O1 C10 131.9(7) 7_575 . ?
C3 O1 C4 68.4(7) 7_575 7_575 ?
C1 O1 C4 89.2(6) . 7_575 ?
O2 O1 C4 108.0(6) 7_575 7_575 ?
C10 O1 C4 25.5(5) . 7_575 ?
C3 O1 O3 118.6(6) 7_575 7_575 ?
C1 O1 O3 127.6(5) . 7_575 ?
O2 O1 O3 120.7(5) 7_575 7_575 ?
C10 O1 O3 36.3(6) . 7_575 ?
C4 O1 O3 50.3(5) 7_575 7_575 ?
C3 O1 Na1 141.4(7) 7_575 . ?
C1 O1 Na1 105.9(6) . . ?
O2 O1 Na1 73.5(4) 7_575 . ?
C10 O1 Na1 104.9(7) . . ?
C4 O1 Na1 109.7(6) 7_575 . ?
O3 O1 Na1 68.7(2) 7_575 . ?
C1 O2 C2 92.6(10) 7_575 . ?
C1 O2 O1 73.0(9) 7_575 7_575 ?
C2 O2 O1 124.8(6) . 7_575 ?
C1 O2 C3 31.3(8) 7_575 . ?
C2 O2 C3 110.1(6) . . ?
O1 O2 C3 41.7(4) 7_575 . ?
C1 O2 O2 145.6(9) 7_575 7_575 ?
C2 O2 O2 53.8(3) . 7_575 ?
O1 O2 O2 129.6(3) 7_575 7_575 ?
C3 O2 O2 157.0(4) . 7_575 ?
C1 O2 Na1 142.5(10) 7_575 . ?
C2 O2 Na1 119.4(4) . . ?
O1 O2 Na1 72.6(3) 7_575 . ?
C3 O2 Na1 112.9(5) . . ?
O2 O2 Na1 70.86(14) 7_575 . ?
C10 O3 C9 77.1(13) 7_575 7_575 ?
C10 O3 C4 26.2(8) 7_575 . ?
C9 O3 C4 101.9(12) 7_575 . ?
C10 O3 C5 91.6(12) 7_575 . ?
C9 O3 C5 14.6(18) 7_575 . ?
C4 O3 C5 115.9(11) . . ?
C10 O3 O5 134.5(8) 7_575 7_575 ?
C9 O3 O5 62.0(12) 7_575 7_575 ?
C4 O3 O5 160.2(6) . 7_575 ?
C5 O3 O5 49.4(10) . 7_575 ?
C10 O3 O1 53.0(8) 7_575 7_575 ?
C9 O3 O1 96.9(12) 7_575 7_575 ?
C4 O3 O1 57.2(5) . 7_575 ?
C5 O3 O1 107.5(10) . 7_575 ?
O5 O3 O1 110.8(4) 7_575 7_575 ?
C10 O3 Na1 120.9(8) 7_575 . ?
C9 O3 Na1 118.3(13) 7_575 . ?
C4 O3 Na1 114.7(6) . . ?
C5 O3 Na1 112.2(12) . . ?
O5 O3 Na1 68.6(3) 7_575 . ?
O1 O3 Na1 68.2(2) 7_575 . ?
C10 O3 H10B 49.5(5) 7_575 7_575 ?
C9 O3 H10B 112.3(14) 7_575 7_575 ?
C4 O3 H10B 27.8(10) . 7_575 ?
C5 O3 H10B 122.6(13) . 7_575 ?
O5 O3 H10B 165.4(8) 7_575 7_575 ?
O1 O3 H10B 82.7(7) 7_575 7_575 ?
Na1 O3 H10B 123.5(7) . 7_575 ?
C8 O4 C7 88.3(8) 7_575 . ?
C8 O4 C6 29.7(7) 7_575 . ?
C7 O4 C6 109.3(6) . . ?
C8 O4 O5 69.3(7) 7_575 7_575 ?
C7 O4 O5 126.6(5) . 7_575 ?
C6 O4 O5 39.7(4) . 7_575 ?
C8 O4 O4 142.3(7) 7_575 7_575 ?
C7 O4 O4 55.6(3) . 7_575 ?
C6 O4 O4 162.5(5) . 7_575 ?
O5 O4 O4 139.0(3) 7_575 7_575 ?
C8 O4 Na1 134.9(7) 7_575 . ?
C7 O4 Na1 105.1(4) . . ?
C6 O4 Na1 107.4(5) . . ?
O5 O4 Na1 68.3(3) 7_575 . ?
O4 O4 Na1 72.02(12) 7_575 . ?
C6 O5 C5 82.2(13) 7_575 7_575 ?
C6 O5 C8 29.6(7) 7_575 . ?
C5 O5 C8 104.1(12) 7_575 . ?
C6 O5 O4 70.1(6) 7_575 7_575 ?
C5 O5 O4 125.3(13) 7_575 7_575 ?
C8 O5 O4 40.7(4) . 7_575 ?
C6 O5 C9 94.9(12) 7_575 . ?
C5 O5 C9 13.1(19) 7_575 . ?
C8 O5 C9 114.7(12) . . ?
O4 O5 C9 127.9(12) 7_575 . ?
C6 O5 O3 140.6(8) 7_575 7_575 ?
C5 O5 O3 61.8(11) 7_575 7_575 ?
C8 O5 O3 165.6(6) . 7_575 ?
O4 O5 O3 143.8(5) 7_575 7_575 ?
C9 O5 O3 51.0(11) . 7_575 ?
C6 O5 Na1 145.4(7) 7_575 . ?
C5 O5 Na1 127.4(11) 7_575 . ?
C8 O5 Na1 116.3(5) . . ?
O4 O5 Na1 77.2(3) 7_575 . ?
C9 O5 Na1 114.4(10) . . ?
O3 O5 Na1 74.0(3) 7_575 . ?
O2 C1 C3 119.4(15) 7_575 7_575 ?
O2 C1 O1 73.5(9) 7_575 . ?
C3 C1 O1 45.9(8) 7_575 . ?
O2 C1 C2 57.0(8) 7_575 . ?
C3 C1 C2 134.2(12) 7_575 . ?
O1 C1 C2 108.3(7) . . ?
O2 C1 Na1 28.4(8) 7_575 . ?
C3 C1 Na1 93.1(10) 7_575 . ?
O1 C1 Na1 48.3(4) . . ?
C2 C1 Na1 82.3(5) . . ?
O2 C1 H1A 159.0 7_575 . ?
C3 C1 H1A 62.4 7_575 . ?
O1 C1 H1A 105.0 . . ?
C2 C1 H1A 105.6 . . ?
Na1 C1 H1A 152.7 . . ?
O2 C1 H1B 90.9 7_575 . ?
C3 C1 H1B 111.4 7_575 . ?
O1 C1 H1B 114.8 . . ?
C2 C1 H1B 114.2 . . ?
Na1 C1 H1B 91.4 . . ?
H1A C1 H1B 108.2 . . ?
O2 C2 O2 72.5(7) 7_575 . ?
O2 C2 C1 102.6(7) 7_575 7_575 ?
O2 C2 C1 30.4(4) . 7_575 ?
O2 C2 C1 30.4(4) 7_575 . ?
O2 C2 C1 102.6(7) . . ?
C1 C2 C1 132.2(10) 7_575 . ?
O2 C2 H2A 122.3 7_575 . ?
O2 C2 H2A 110.0 . . ?
C1 C2 H2A 97.2 7_575 . ?
C1 C2 H2A 115.0 . . ?
O2 C2 H2B 124.7 7_575 . ?
O2 C2 H2B 110.7 . . ?
C1 C2 H2B 90.3 7_575 . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.6 . . ?
O2 C2 H2A 110.0(4) 7_575 7_575 ?
O2 C2 H2A 122.3(4) . 7_575 ?
C1 C2 H2A 115.0(5) 7_575 7_575 ?
C1 C2 H2A 97.2(5) . 7_575 ?
H2A C2 H2A 18.7 . 7_575 ?
H2B C2 H2A 112.2 . 7_575 ?
O2 C2 H2B 110.7(3) 7_575 7_575 ?
O2 C2 H2B 124.7(4) . 7_575 ?
C1 C2 H2B 109.8(4) 7_575 7_575 ?
C1 C2 H2B 90.3(4) . 7_575 ?
H2A C2 H2B 112.2 . 7_575 ?
H2B C2 H2B 21.0 . 7_575 ?
H2A C2 H2B 108.6 7_575 7_575 ?
C1 C3 O1 96.5(11) 7_575 7_575 ?
C1 C3 O2 29.3(8) 7_575 . ?
O1 C3 O2 67.2(6) 7_575 . ?
C1 C3 C4 119.9(12) 7_575 . ?
O1 C3 C4 73.2(7) 7_575 . ?
O2 C3 C4 108.5(8) . . ?
C1 C3 C10 130.9(12) 7_575 7_575 ?
O1 C3 C10 55.7(6) 7_575 7_575 ?
O2 C3 C10 109.2(7) . 7_575 ?
C4 C3 C10 23.0(4) . 7_575 ?
C1 C3 H3A 81.7 7_575 . ?
O1 C3 H3A 177.2 7_575 . ?
O2 C3 H3A 110.9 . . ?
C4 C3 H3A 109.6 . . ?
C10 C3 H3A 127.1 7_575 . ?
C1 C3 H3B 121.6 7_575 . ?
O1 C3 H3B 70.7 7_575 . ?
O2 C3 H3B 109.0 . . ?
C4 C3 H3B 110.4 . . ?
C10 C3 H3B 89.2 7_575 . ?
H3A C3 H3B 108.4 . . ?
C1 C3 H1A 63.9(8) 7_575 7_575 ?
O1 C3 H1A 149.7(11) 7_575 7_575 ?
O2 C3 H1A 91.1(7) . 7_575 ?
C4 C3 H1A 135.9(11) . 7_575 ?
C10 C3 H1A 154.5(10) 7_575 7_575 ?
H3A C3 H1A 27.5 . 7_575 ?
H3B C3 H1A 99.0 . 7_575 ?
C10 C4 O3 43.5(19) 7_575 . ?
C10 C4 C3 95(2) 7_575 . ?
O3 C4 C3 110.8(8) . . ?
C10 C4 O1 64.9(18) 7_575 7_575 ?
O3 C4 O1 72.5(6) . 7_575 ?
C3 C4 O1 38.4(4) . 7_575 ?
C10 C4 H4A 78.8 7_575 . ?
O3 C4 H4A 109.8 . . ?
C3 C4 H4A 110.0 . . ?
O1 C4 H4A 122.3 7_575 . ?
C10 C4 H4B 148.8 7_575 . ?
O3 C4 H4B 107.9 . . ?
C3 C4 H4B 110.1 . . ?
O1 C4 H4B 126.4 7_575 . ?
H4A C4 H4B 108.1 . . ?
C10 C4 H10B 91(3) 7_575 7_575 ?
O3 C4 H10B 57.5(12) . 7_575 ?
C3 C4 H10B 152(3) . 7_575 ?
O1 C4 H10B 124(2) 7_575 7_575 ?
H4A C4 H10B 98.2 . 7_575 ?
H4B C4 H10B 58.2 . 7_575 ?
C9 C5 O5 119(9) 7_575 7_575 ?
C9 C5 O3 59(7) 7_575 . ?
O5 C5 O3 68.8(12) 7_575 . ?
C9 C5 C6 157(10) 7_575 . ?
O5 C5 C6 40.8(9) 7_575 . ?
O3 C5 C6 108.1(16) . . ?
C9 C5 C10 24(7) 7_575 7_575 ?
O5 C5 C10 101.1(15) 7_575 7_575 ?
O3 C5 C10 35.5(7) . 7_575 ?
C6 C5 C10 141.9(18) . 7_575 ?
C9 C5 H5A 91.5 7_575 . ?
O5 C5 H5A 135.9 7_575 . ?
O3 C5 H5A 109.1 . . ?
C6 C5 H5A 111.6 . . ?
C10 C5 H5A 96.0 7_575 . ?
C9 C5 H5B 61.9 7_575 . ?
O5 C5 H5B 113.8 7_575 . ?
O3 C5 H5B 108.6 . . ?
C6 C5 H5B 111.0 . . ?
C10 C5 H5B 82.6 7_575 . ?
H5A C5 H5B 108.5 . . ?
C9 C5 H9A 86(9) 7_575 7_575 ?
O5 C5 H9A 135(4) 7_575 7_575 ?
O3 C5 H9A 101(3) . 7_575 ?
C6 C5 H9A 117(3) . 7_575 ?
C10 C5 H9A 89(3) 7_575 7_575 ?
H5A C5 H9A 8.1 . 7_575 ?
H5B C5 H9A 110.5 . 7_575 ?
C8 C6 O5 110.7(17) 7_575 7_575 ?
C8 C6 O4 40.9(12) 7_575 . ?
O5 C6 O4 70.2(7) 7_575 . ?
C8 C6 C5 140.5(19) 7_575 . ?
O5 C6 C5 56.9(11) 7_575 . ?
O4 C6 C5 110.1(13) . . ?
C8 C6 C9 137.2(18) 7_575 7_575 ?
O5 C6 C9 53.1(10) 7_575 7_575 ?
O4 C6 C9 105.5(11) . 7_575 ?
C5 C6 C9 5(2) . 7_575 ?
C8 C6 H6A 70.7 7_575 . ?
O5 C6 H6A 159.1 7_575 . ?
O4 C6 H6A 106.5 . . ?
C5 C6 H6A 107.9 . . ?
C9 C6 H6A 110.8 7_575 . ?
C8 C6 H6B 106.4 7_575 . ?
O5 C6 H6B 91.4 7_575 . ?
O4 C6 H6B 112.8 . . ?
C5 C6 H6B 111.0 . . ?
C9 C6 H6B 112.7 7_575 . ?
H6A C6 H6B 108.4 . . ?
O4 C7 O4 68.8(6) . 7_575 ?
O4 C7 C8 105.1(6) . . ?
O4 C7 C8 37.0(4) 7_575 . ?
O4 C7 C8 37.0(4) . 7_575 ?
O4 C7 C8 105.1(6) 7_575 7_575 ?
C8 C7 C8 139.4(9) . 7_575 ?
O4 C7 Na1 50.1(3) . . ?
O4 C7 Na1 50.1(3) 7_575 . ?
C8 C7 Na1 79.8(4) . . ?
C8 C7 Na1 79.8(4) 7_575 . ?
O4 C7 H7A 111.3 . . ?
O4 C7 H7A 121.3 7_575 . ?
C8 C7 H7A 113.8 . . ?
C8 C7 H7A 98.3 7_575 . ?
Na1 C7 H7A 83.8 . . ?
O4 C7 H7B 108.9 . . ?
O4 C7 H7B 127.1 7_575 . ?
C8 C7 H7B 108.6 . . ?
C8 C7 H7B 81.8 7_575 . ?
Na1 C7 H7B 159.0 . . ?
H7A C7 H7B 108.9 . . ?
O4 C7 H7A 121.3(4) . 7_575 ?
O4 C7 H7A 111.3(4) 7_575 7_575 ?
C8 C7 H7A 98.3(4) . 7_575 ?
C8 C7 H7A 113.8(4) 7_575 7_575 ?
Na1 C7 H7A 83.77(13) . 7_575 ?
H7A C7 H7A 15.9 . 7_575 ?
H7B C7 H7A 113.0 . 7_575 ?
O4 C7 H7B 127.1(3) . 7_575 ?
O4 C7 H7B 108.9(3) 7_575 7_575 ?
C8 C7 H7B 81.8(4) . 7_575 ?
C8 C7 H7B 108.6(4) 7_575 7_575 ?
Na1 C7 H7B 159.03(9) . 7_575 ?
H7A C7 H7B 113.0 . 7_575 ?
H7B C7 H7B 28.5 . 7_575 ?
H7A C7 H7B 108.9 7_575 7_575 ?
C6 C8 O4 109.4(17) 7_575 7_575 ?
C6 C8 O5 39.7(11) 7_575 . ?
O4 C8 O5 70.1(7) 7_575 . ?
C6 C8 C7 138.1(16) 7_575 . ?
O4 C8 C7 54.7(7) 7_575 . ?
O5 C8 C7 107.5(7) . . ?
C6 C8 H8A 73.8 7_575 . ?
O4 C8 H8A 158.8 7_575 . ?
O5 C8 H8A 108.4 . . ?
C7 C8 H8A 108.4 . . ?
C6 C8 H8B 106.8 7_575 . ?
O4 C8 H8B 91.4 7_575 . ?
O5 C8 H8B 112.9 . . ?
C7 C8 H8B 111.6 . . ?
H8A C8 H8B 108.0 . . ?
C6 C8 H6A 64.4(11) 7_575 7_575 ?
O4 C8 H6A 151.4(16) 7_575 7_575 ?
O5 C8 H6A 101.6(8) . 7_575 ?
C7 C8 H6A 148.5(11) . 7_575 ?
H8A C8 H6A 49.4 . 7_575 ?
H8B C8 H6A 66.0 . 7_575 ?
C5 C9 O3 107(8) 7_575 7_575 ?
C5 C9 O5 48(8) 7_575 . ?
O3 C9 O5 67.0(14) 7_575 . ?
C5 C9 C10 150(9) 7_575 . ?
O3 C9 C10 44.1(10) 7_575 . ?
O5 C9 C10 109(2) . . ?
C5 C9 C6 19(8) 7_575 7_575 ?
O3 C9 C6 97.0(17) 7_575 7_575 ?
O5 C9 C6 32.0(6) . 7_575 ?
C10 C9 C6 140(2) . 7_575 ?
C5 C9 H9A 71.0 7_575 . ?
O3 C9 H9A 109.8 7_575 . ?
O5 C9 H9A 109.1 . . ?
C10 C9 H9A 109.3 . . ?
C6 C9 H9A 89.1 7_575 . ?
C5 C9 H9B 94.2 7_575 . ?
O3 C9 H9B 140.9 7_575 . ?
O5 C9 H9B 108.6 . . ?
C10 C9 H9B 113.0 . . ?
C6 C9 H9B 92.7 7_575 . ?
H9A C9 H9B 108.1 . . ?
C5 C9 H5B 95(9) 7_575 7_575 ?
O3 C9 H5B 133(4) 7_575 7_575 ?
O5 C9 H5B 103(4) . 7_575 ?
C10 C9 H5B 110(3) . 7_575 ?
C6 C9 H5B 91(3) 7_575 7_575 ?
H9A C9 H5B 116.1 . 7_575 ?
H9B C9 H5B 8.2 . 7_575 ?
C4 C10 O3 110(3) 7_575 7_575 ?
C4 C10 O1 90(2) 7_575 . ?
O3 C10 O1 90.7(9) 7_575 . ?
C4 C10 C9 160(3) 7_575 . ?
O3 C10 C9 58.7(12) 7_575 . ?
O1 C10 C9 106.7(14) . . ?
C4 C10 C3 62.0(19) 7_575 7_575 ?
O3 C10 C3 121.1(11) 7_575 7_575 ?
O1 C10 C3 36.3(5) . 7_575 ?
C9 C10 C3 137.7(14) . 7_575 ?
C4 C10 C5 155(3) 7_575 7_575 ?
O3 C10 C5 52.9(9) 7_575 7_575 ?
O1 C10 C5 107.0(11) . 7_575 ?
C9 C10 C5 6.0(18) . 7_575 ?
C3 C10 C5 140.1(12) 7_575 7_575 ?
C4 C10 Na1 101(2) 7_575 . ?
O3 C10 Na1 42.2(6) 7_575 . ?
O1 C10 Na1 48.9(5) . . ?
C9 C10 Na1 82.1(13) . . ?
C3 C10 Na1 80.0(5) 7_575 . ?
C5 C10 Na1 78.3(10) 7_575 . ?
C4 C10 H10A 82.8 7_575 . ?
O3 C10 H10A 158.7 7_575 . ?
O1 C10 H10A 106.5 . . ?
C9 C10 H10A 103.3 . . ?
C3 C10 H10A 79.6 7_575 . ?
C5 C10 H10A 108.7 7_575 . ?
Na1 C10 H10A 154.6 . . ?
C4 C10 H10B 44.4 7_575 . ?
O3 C10 H10B 74.1 7_575 . ?
O1 C10 H10B 115.0 . . ?
C9 C10 H10B 116.0 . . ?
C3 C10 H10B 102.2 7_575 . ?
C5 C10 H10B 111.1 7_575 . ?
Na1 C10 H10B 90.7 . . ?
H10A C10 H10B 108.3 . . ?
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 Br1 2.9718(4) 7_575 ?
Pb1 Br1 2.9718(4) . ?
Pb1 Br1 3.0588(4) 4_566 ?
Pb1 Br1 3.0588(4) 6_657 ?
Pb1 Br2 3.0743(5) 6_657 ?
Pb1 Br2 3.0962(5) . ?
Br2 Na1 2.931(2) . ?
Na1 O5 2.333(5) . ?
Na1 O5 2.333(6) 7_575 ?
Na1 O1 2.399(6) . ?
Na1 O1 2.399(6) 7_575 ?
Na1 O3 2.408(5) . ?
Na1 O3 2.408(5) 7_575 ?
Na1 O2 2.410(6) . ?
Na1 O2 2.410(6) 7_575 ?
Na1 O4 2.448(6) . ?
Na1 O4 2.448(6) 7_575 ?
Na1 C10 3.079(13) . ?
O1 C3 1.011(9) 7_575 ?
O1 C1 1.398(10) . ?
O1 O2 1.402(7) 7_575 ?
O1 C10 1.410(14) . ?
O1 C4 1.557(12) 7_575 ?
O1 O3 1.766(7) 7_575 ?
O2 C1 0.808(9) 7_575 ?
O2 C2 1.337(7) . ?
O2 C3 1.438(9) . ?
O2 O2 1.581(12) 7_575 ?
O3 C10 1.046(14) 7_575 ?
O3 C9 1.28(3) 7_575 ?
O3 C4 1.426(12) . ?
O3 C5 1.44(2) . ?
O3 O5 1.522(7) 7_575 ?
O3 H10B 1.207(10) 7_575 ?
O4 C8 0.986(10) 7_575 ?
O4 C7 1.338(7) . ?
O4 C6 1.421(10) . ?
O4 O5 1.422(7) 7_575 ?
O4 O4 1.511(10) 7_575 ?
O5 C6 0.966(10) 7_575 ?
O5 C5 1.24(3) 7_575 ?
O5 C8 1.415(11) . ?
O5 C9 1.46(3) . ?
C1 C3 0.858(10) 7_575 ?
C1 C2 1.593(10) . ?
C1 H1A 0.9560 . ?
C1 H1B 0.9539 . ?
C2 H2A 0.9540 . ?
C2 H2B 0.9543 . ?
C2 H2A 0.9540 7_575 ?
C2 H2B 0.9543 7_575 ?
C3 C4 1.513(15) . ?
C3 C10 1.707(17) 7_575 ?
C3 H3A 0.9548 . ?
C3 H3B 0.9542 . ?
C4 C10 0.671(11) 7_575 ?
C4 H4A 0.9579 . ?
C4 H4B 0.9540 . ?
C4 H10B 0.67(2) 7_575 ?
C5 C9 0.38(4) 7_575 ?
C5 C6 1.46(2) . ?
C5 C10 1.80(3) 7_575 ?
C5 H5A 0.9584 . ?
C5 H5B 0.9539 . ?
C5 H9A 0.91(6) 7_575 ?
C6 C8 0.747(9) 7_575 ?
C6 C9 1.82(3) 7_575 ?
C6 H6A 0.9546 . ?
C6 H6B 0.9540 . ?
C7 C8 1.638(11) . ?
C7 C8 1.638(11) 7_575 ?
C7 H7A 0.9541 . ?
C7 H7B 0.9544 . ?
C7 H7A 0.9540 7_575 ?
C7 H7B 0.9544 7_575 ?
C8 H8A 0.9558 . ?
C8 H8B 0.9541 . ?
C9 C10 1.46(3) . ?
C9 H9A 0.9571 . ?
C9 H9B 0.9540 . ?
C10 H10A 0.9561 . ?
C10 H10B 0.9542 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C10 H10B O3 0.95 2.67 3.473(14) 142.5 3_646 yes
C10 H10A Br1 0.96 3.01 3.875(15) 150.7 5_666 yes
C6 H6B Br1 0.95 2.99 3.894(10) 158.9 4_566 yes
C3 H3A Br1 0.95 2.90 3.658(8) 137.3 8_665 yes
