#------------------------------------------------------------------------------
#$Date: 2021-12-07 04:53:47 +0200 (Tue, 07 Dec 2021) $
#$Revision: 271159 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/36/7243683.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_7243683
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                   7.8228(3)
_cell_length_b                   13.8222(6)
_cell_length_c                   16.4334(8)
_cell_measurement_reflns_used    8688
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.48
_cell_volume                     1776.92(13)
_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      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_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       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16553
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.563
_diffrn_reflns_theta_min         2.479
_diffrn_source.source            'Ius 2.0'
_diffrn_source.type              microfocus
_exptl_absorpt_coefficient_mu    16.277
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.580
_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         2.623
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.00065(8)
_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   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2122
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0234P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1846
_reflns_number_total             2122
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01273h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7243683--7243691.cif.'
_cod_database_code               7243683
_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   0.268
_shelx_estimated_absorpt_t_max   0.293
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 0.67582(2) 0.750000 0.74938(2) 0.00985(8) Uani 1 2 d S T P . .
Br1 Br 0.43545(4) 0.60345(2) 0.81490(2) 0.01526(10) Uani 1 1 d . . . . .
Br2 Br 0.42145(5) 0.750000 0.60536(3) 0.01506(12) Uani 1 2 d S T P . .
Na1 Na 0.55824(19) 0.750000 0.43968(11) 0.0132(4) Uani 1 2 d S T P . .
O1 O 0.4704(6) 0.6289(3) 0.3451(3) 0.0170(10) Uani 0.5 1 d D . P . .
O2 O 0.3323(5) 0.8098(3) 0.3534(3) 0.0129(11) Uani 0.5 1 d D . P . .
O3 O 0.5644(5) 0.9249(3) 0.4334(3) 0.0133(10) Uani 0.5 1 d D . P . .
O4 O 0.8536(5) 0.8053(3) 0.4262(3) 0.0141(10) Uani 0.5 1 d D . P . .
O5 O 0.7427(6) 0.6182(3) 0.4469(3) 0.0145(10) Uani 0.5 1 d D . P . .
C1 C 0.2940(9) 0.6447(6) 0.3291(5) 0.0166(16) Uani 0.5 1 d D . P . .
H1A H 0.264428 0.600921 0.286693 0.020 Uiso 0.5 1 d R U P . .
H1B H 0.221358 0.632196 0.374208 0.020 Uiso 0.5 1 d R U P . .
C2 C 0.2748(6) 0.750000 0.2932(3) 0.0214(11) Uani 1 2 d DS TU P . .
H2A H 0.338396 0.766513 0.244881 0.026 Uiso 0.5 1 d R U P . .
H2B H 0.157597 0.767903 0.282321 0.026 Uiso 0.5 1 d R U P . .
C3 C 0.3672(9) 0.9040(5) 0.3217(4) 0.0136(14) Uani 0.5 1 d D . P . .
H3A H 0.266610 0.930548 0.298127 0.016 Uiso 0.5 1 d R U P . .
H3B H 0.453110 0.900730 0.280997 0.016 Uiso 0.5 1 d R U P . .
C4 C 0.4220(9) 0.9676(6) 0.3907(5) 0.0144(18) Uani 0.5 1 d D . P . .
H4A H 0.452413 1.030241 0.371037 0.017 Uiso 0.5 1 d R U P . .
H4B H 0.332203 0.975121 0.429107 0.017 Uiso 0.5 1 d R U P . .
C5 C 0.7272(15) 0.9619(14) 0.4083(13) 0.013(3) Uani 0.5 1 d D U P . .
H5A H 0.734638 1.029057 0.421588 0.016 Uiso 0.5 1 d R U P . .
H5B H 0.739338 0.955079 0.351137 0.016 Uiso 0.5 1 d R U P . .
C6 C 0.8621(9) 0.9033(5) 0.4526(4) 0.0124(15) Uani 0.5 1 d D U P . .
H6A H 0.971446 0.927196 0.437391 0.015 Uiso 0.5 1 d R U P . .
H6B H 0.849817 0.910066 0.509723 0.015 Uiso 0.5 1 d R U P . .
C7 C 0.9453(6) 0.750000 0.4790(3) 0.0247(12) Uani 1 2 d DS TU P . .
H7A H 0.908162 0.766725 0.533391 0.030 Uiso 0.5 1 d R U P . .
H7B H 1.062733 0.774165 0.475190 0.030 Uiso 0.5 1 d R U P . .
C8 C 0.9211(8) 0.6406(6) 0.4457(5) 0.0177(17) Uani 0.5 1 d D . P . .
H8A H 0.977266 0.598151 0.482625 0.021 Uiso 0.5 1 d R U P . .
H8B H 0.971125 0.631891 0.393554 0.021 Uiso 0.5 1 d R U P . .
C9 C 0.6947(17) 0.5368(14) 0.3983(14) 0.021(4) Uani 0.5 1 d D U P . .
H9A H 0.724355 0.477964 0.425180 0.025 Uiso 0.5 1 d R U P . .
H9B H 0.756828 0.539886 0.348799 0.025 Uiso 0.5 1 d R U P . .
C10 C 0.5042(10) 0.5408(6) 0.3861(6) 0.0186(19) Uani 0.5 1 d D . P . .
H10A H 0.484144 0.491264 0.346910 0.022 Uiso 0.5 1 d R U P . .
H10B H 0.436392 0.527394 0.432644 0.022 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 86.141(13) 7_575 . ?
Br1 Pb1 Br1 95.402(11) 7_575 4_566 ?
Br1 Pb1 Br1 177.679(9) . 4_566 ?
Br1 Pb1 Br1 177.678(10) 7_575 6_657 ?
Br1 Pb1 Br1 95.402(10) . 6_657 ?
Br1 Pb1 Br1 83.004(13) 4_566 6_657 ?
Br1 Pb1 Br2 96.589(10) 7_575 6_657 ?
Br1 Pb1 Br2 96.590(10) . 6_657 ?
Br1 Pb1 Br2 81.523(9) 4_566 6_657 ?
Br1 Pb1 Br2 81.523(9) 6_657 6_657 ?
Br1 Pb1 Br2 82.524(9) 7_575 . ?
Br1 Pb1 Br2 82.523(9) . . ?
Br1 Pb1 Br2 99.384(10) 4_566 . ?
Br1 Pb1 Br2 99.383(10) 6_657 . ?
Br2 Pb1 Br2 178.778(13) 6_657 . ?
Pb1 Br1 Pb1 80.981(8) . 6_557 ?
Na1 Br2 Pb1 162.63(3) . 6_557 ?
Na1 Br2 Pb1 118.49(3) . . ?
Pb1 Br2 Pb1 78.888(12) 6_557 . ?
O5 Na1 O5 103.0(2) 7_575 . ?
O5 Na1 O1 70.28(15) 7_575 7_575 ?
O5 Na1 O1 139.54(17) . 7_575 ?
O5 Na1 O1 139.54(17) 7_575 . ?
O5 Na1 O1 70.28(15) . . ?
O1 Na1 O1 89.1(2) 7_575 . ?
O5 Na1 O2 138.82(17) 7_575 7_575 ?
O5 Na1 O2 102.46(15) . 7_575 ?
O1 Na1 O2 69.29(16) 7_575 7_575 ?
O1 Na1 O2 33.40(15) . 7_575 ?
O5 Na1 O2 102.46(15) 7_575 . ?
O5 Na1 O2 138.82(17) . . ?
O1 Na1 O2 33.40(15) 7_575 . ?
O1 Na1 O2 69.28(16) . . ?
O2 Na1 O2 40.1(2) 7_575 . ?
O5 Na1 O3 37.61(14) 7_575 . ?
O5 Na1 O3 140.51(16) . . ?
O1 Na1 O3 43.73(15) 7_575 . ?
O1 Na1 O3 132.74(17) . . ?
O2 Na1 O3 109.40(16) 7_575 . ?
O2 Na1 O3 69.34(15) . . ?
O5 Na1 O3 140.51(16) 7_575 7_575 ?
O5 Na1 O3 37.61(14) . 7_575 ?
O1 Na1 O3 132.74(17) 7_575 7_575 ?
O1 Na1 O3 43.73(15) . 7_575 ?
O2 Na1 O3 69.33(15) 7_575 7_575 ?
O2 Na1 O3 109.40(16) . 7_575 ?
O3 Na1 O3 174.6(2) . 7_575 ?
O5 Na1 O4 70.32(15) 7_575 7_575 ?
O5 Na1 O4 34.24(14) . 7_575 ?
O1 Na1 O4 115.63(17) 7_575 7_575 ?
O1 Na1 O4 89.63(15) . 7_575 ?
O2 Na1 O4 122.14(15) 7_575 7_575 ?
O2 Na1 O4 138.30(17) . 7_575 ?
O3 Na1 O4 106.85(15) . 7_575 ?
O3 Na1 O4 70.41(14) 7_575 7_575 ?
O5 Na1 O4 34.24(14) 7_575 . ?
O5 Na1 O4 70.32(15) . . ?
O1 Na1 O4 89.63(15) 7_575 . ?
O1 Na1 O4 115.63(17) . . ?
O2 Na1 O4 138.30(17) 7_575 . ?
O2 Na1 O4 122.14(15) . . ?
O3 Na1 O4 70.41(14) . . ?
O3 Na1 O4 106.85(14) 7_575 . ?
O4 Na1 O4 36.5(2) 7_575 . ?
O5 Na1 Br2 100.35(12) 7_575 . ?
O5 Na1 Br2 100.35(12) . . ?
O1 Na1 Br2 120.09(11) 7_575 . ?
O1 Na1 Br2 120.09(11) . . ?
O2 Na1 Br2 106.20(13) 7_575 . ?
O2 Na1 Br2 106.20(13) . . ?
O3 Na1 Br2 92.69(12) . . ?
O3 Na1 Br2 92.69(12) 7_575 . ?
O4 Na1 Br2 115.50(13) 7_575 . ?
O4 Na1 Br2 115.50(13) . . ?
O5 Na1 C10 147.4(2) 7_575 . ?
O5 Na1 C10 50.12(17) . . ?
O1 Na1 C10 115.9(2) 7_575 . ?
O1 Na1 C10 26.80(19) . . ?
O2 Na1 C10 53.42(19) 7_575 . ?
O2 Na1 C10 93.1(2) . . ?
O3 Na1 C10 159.5(2) . . ?
O3 Na1 C10 17.09(19) 7_575 . ?
O4 Na1 C10 78.94(17) 7_575 . ?
O4 Na1 C10 113.65(19) . . ?
Br2 Na1 C10 102.59(18) . . ?
C3 O1 O2 71.7(5) 7_575 7_575 ?
C3 O1 C10 86.7(6) 7_575 . ?
O2 O1 C10 128.8(5) 7_575 . ?
C3 O1 C1 38.5(5) 7_575 . ?
O2 O1 C1 33.2(3) 7_575 . ?
C10 O1 C1 113.6(5) . . ?
C3 O1 C4 66.7(5) 7_575 7_575 ?
O2 O1 C4 106.5(5) 7_575 7_575 ?
C10 O1 C4 24.7(3) . 7_575 ?
C1 O1 C4 89.1(5) . 7_575 ?
C3 O1 O3 116.9(5) 7_575 7_575 ?
O2 O1 O3 119.8(4) 7_575 7_575 ?
C10 O1 O3 34.9(4) . 7_575 ?
C1 O1 O3 127.7(4) . 7_575 ?
C4 O1 O3 50.2(3) 7_575 7_575 ?
C3 O1 Na1 143.1(5) 7_575 . ?
O2 O1 Na1 74.4(3) 7_575 . ?
C10 O1 Na1 103.8(5) . . ?
C1 O1 Na1 107.0(4) . . ?
C4 O1 Na1 110.6(4) 7_575 . ?
O3 O1 Na1 69.2(2) 7_575 . ?
C1 O2 C2 89.5(7) 7_575 . ?
C1 O2 O1 76.3(7) 7_575 7_575 ?
C2 O2 O1 123.9(5) . 7_575 ?
C1 O2 C3 34.6(6) 7_575 . ?
C2 O2 C3 110.5(5) . . ?
O1 O2 C3 41.8(3) 7_575 . ?
C1 O2 O2 141.5(7) 7_575 7_575 ?
C2 O2 O2 52.7(3) . 7_575 ?
O1 O2 O2 127.8(3) 7_575 7_575 ?
C3 O2 O2 155.7(3) . 7_575 ?
C1 O2 Na1 146.6(7) 7_575 . ?
C2 O2 Na1 117.4(3) . . ?
O1 O2 Na1 72.2(3) 7_575 . ?
C3 O2 Na1 112.8(4) . . ?
O2 O2 Na1 69.94(11) 7_575 . ?
C10 O3 C9 80.4(8) 7_575 7_575 ?
C10 O3 C5 91.4(8) 7_575 . ?
C9 O3 C5 11.2(13) 7_575 . ?
C10 O3 C4 24.2(6) 7_575 . ?
C9 O3 C4 103.1(7) 7_575 . ?
C5 O3 C4 113.6(7) . . ?
C10 O3 O5 135.0(6) 7_575 7_575 ?
C9 O3 O5 60.2(6) 7_575 7_575 ?
C5 O3 O5 51.1(6) . 7_575 ?
C4 O3 O5 158.7(5) . 7_575 ?
C10 O3 O1 52.3(5) 7_575 7_575 ?
C9 O3 O1 97.7(11) 7_575 7_575 ?
C5 O3 O1 106.3(10) . 7_575 ?
C4 O3 O1 57.2(4) . 7_575 ?
O5 O3 O1 109.2(3) 7_575 7_575 ?
C10 O3 Na1 119.0(6) 7_575 . ?
C9 O3 Na1 116.5(9) 7_575 . ?
C5 O3 Na1 112.7(8) . . ?
C4 O3 Na1 114.4(4) . . ?
O5 O3 Na1 67.9(2) 7_575 . ?
O1 O3 Na1 67.1(2) 7_575 . ?
C10 O3 H10B 49.8(4) 7_575 7_575 ?
C9 O3 H10B 115.6(9) 7_575 7_575 ?
C5 O3 H10B 122.9(8) . 7_575 ?
C4 O3 H10B 29.0(7) . 7_575 ?
O5 O3 H10B 167.3(6) 7_575 7_575 ?
O1 O3 H10B 82.9(5) 7_575 7_575 ?
Na1 O3 H10B 122.2(5) . 7_575 ?
C8 O4 C7 86.3(6) 7_575 . ?
C8 O4 O5 71.2(5) 7_575 7_575 ?
C7 O4 O5 126.3(4) . 7_575 ?
C8 O4 C6 30.8(5) 7_575 . ?
C7 O4 C6 108.4(5) . . ?
O5 O4 C6 40.7(3) 7_575 . ?
C8 O4 O4 140.4(5) 7_575 7_575 ?
C7 O4 O4 55.8(2) . 7_575 ?
O5 O4 O4 138.6(3) 7_575 7_575 ?
C6 O4 O4 162.0(3) . 7_575 ?
C8 O4 Na1 136.6(6) 7_575 . ?
C7 O4 Na1 105.3(3) . . ?
O5 O4 Na1 68.3(3) 7_575 . ?
C6 O4 Na1 108.3(4) . . ?
O4 O4 Na1 71.76(10) 7_575 . ?
C6 O5 C5 82.9(7) 7_575 7_575 ?
C6 O5 O4 70.4(5) 7_575 7_575 ?
C5 O5 O4 125.9(10) 7_575 7_575 ?
C6 O5 C9 93.7(8) 7_575 . ?
C5 O5 C9 11.2(13) 7_575 . ?
O4 O5 C9 128.1(10) 7_575 . ?
C6 O5 C8 30.7(4) 7_575 . ?
C5 O5 C8 105.8(7) 7_575 . ?
O4 O5 C8 39.9(3) 7_575 . ?
C9 O5 C8 114.8(7) . . ?
C6 O5 O3 139.4(6) 7_575 7_575 ?
C5 O5 O3 60.4(6) 7_575 7_575 ?
O4 O5 O3 144.8(4) 7_575 7_575 ?
C9 O5 O3 51.3(7) . 7_575 ?
C8 O5 O3 166.1(5) . 7_575 ?
C6 O5 Na1 146.0(5) 7_575 . ?
C5 O5 Na1 126.3(8) 7_575 . ?
O4 O5 Na1 77.4(3) 7_575 . ?
C9 O5 Na1 115.2(7) . . ?
C8 O5 Na1 115.8(4) . . ?
O3 O5 Na1 74.5(2) 7_575 . ?
O2 C1 C3 114.8(10) 7_575 7_575 ?
O2 C1 O1 70.5(6) 7_575 . ?
C3 C1 O1 44.5(6) 7_575 . ?
O2 C1 C2 60.0(7) 7_575 . ?
C3 C1 C2 134.9(9) 7_575 . ?
O1 C1 C2 107.6(5) . . ?
O2 C1 Na1 25.3(6) 7_575 . ?
C3 C1 Na1 90.4(7) 7_575 . ?
O1 C1 Na1 47.1(3) . . ?
C2 C1 Na1 81.4(4) . . ?
O2 C1 H1A 162.3 7_575 . ?
C3 C1 H1A 64.9 7_575 . ?
O1 C1 H1A 105.8 . . ?
C2 C1 H1A 106.8 . . ?
Na1 C1 H1A 152.4 . . ?
O2 C1 H1B 88.8 7_575 . ?
C3 C1 H1B 110.7 7_575 . ?
O1 C1 H1B 114.2 . . ?
C2 C1 H1B 113.8 . . ?
Na1 C1 H1B 91.6 . . ?
H1A C1 H1B 108.1 . . ?
O2 C2 O2 74.5(5) . 7_575 ?
O2 C2 C1 30.6(3) . 7_575 ?
O2 C2 C1 104.8(6) 7_575 7_575 ?
O2 C2 C1 104.8(6) . . ?
O2 C2 C1 30.6(3) 7_575 . ?
C1 C2 C1 134.5(7) 7_575 . ?
O2 C2 H2A 106.5 . . ?
O2 C2 H2A 124.8 7_575 . ?
C1 C2 H2A 92.4 7_575 . ?
C1 C2 H2A 118.5 . . ?
O2 C2 H2B 106.9 . . ?
O2 C2 H2B 127.0 7_575 . ?
C1 C2 H2B 85.6 7_575 . ?
C1 C2 H2B 113.3 . . ?
H2A C2 H2B 106.1 . . ?
O2 C2 H2A 124.8(3) . 7_575 ?
O2 C2 H2A 106.5(3) 7_575 7_575 ?
C1 C2 H2A 118.5(4) 7_575 7_575 ?
C1 C2 H2A 92.4(4) . 7_575 ?
H2A C2 H2A 27.4 . 7_575 ?
H2B C2 H2A 113.5 . 7_575 ?
O2 C2 H2B 127.0(3) . 7_575 ?
O2 C2 H2B 106.9(3) 7_575 7_575 ?
C1 C2 H2B 113.3(3) 7_575 7_575 ?
C1 C2 H2B 85.6(3) . 7_575 ?
H2A C2 H2B 113.5 . 7_575 ?
H2B C2 H2B 29.7 . 7_575 ?
H2A C2 H2B 106.1 7_575 7_575 ?
C1 C3 O1 97.0(8) 7_575 7_575 ?
C1 C3 O2 30.7(6) 7_575 . ?
O1 C3 O2 66.5(5) 7_575 . ?
C1 C3 C4 121.5(9) 7_575 . ?
O1 C3 C4 75.3(6) 7_575 . ?
O2 C3 C4 108.3(6) . . ?
C1 C3 C10 131.5(9) 7_575 7_575 ?
O1 C3 C10 56.9(5) 7_575 7_575 ?
O2 C3 C10 107.8(5) . 7_575 ?
C4 C3 C10 22.8(3) . 7_575 ?
C1 C3 H3A 79.4 7_575 . ?
O1 C3 H3A 175.7 7_575 . ?
O2 C3 H3A 110.1 . . ?
C4 C3 H3A 108.6 . . ?
C10 C3 H3A 127.3 7_575 . ?
C1 C3 H3B 121.0 7_575 . ?
O1 C3 H3B 71.2 7_575 . ?
O2 C3 H3B 110.4 . . ?
C4 C3 H3B 111.0 . . ?
C10 C3 H3B 90.7 7_575 . ?
H3A C3 H3B 108.5 . . ?
C1 C3 H1A 60.5(6) 7_575 7_575 ?
O1 C3 H1A 147.6(8) 7_575 7_575 ?
O2 C3 H1A 89.7(5) . 7_575 ?
C4 C3 H1A 135.4(8) . 7_575 ?
C10 C3 H1A 155.5(8) 7_575 7_575 ?
H3A C3 H1A 28.2 . 7_575 ?
H3B C3 H1A 99.3 . 7_575 ?
C10 C4 O3 39.7(12) 7_575 . ?
C10 C4 C3 95.1(13) 7_575 . ?
O3 C4 C3 110.5(6) . . ?
C10 C4 O1 64.0(11) 7_575 7_575 ?
O3 C4 O1 72.6(4) . 7_575 ?
C3 C4 O1 38.0(3) . 7_575 ?
C10 C4 H4A 82.9 7_575 . ?
O3 C4 H4A 110.1 . . ?
C3 C4 H4A 110.3 . . ?
O1 C4 H4A 123.1 7_575 . ?
C10 C4 H4B 145.1 7_575 . ?
O3 C4 H4B 107.1 . . ?
C3 C4 H4B 110.8 . . ?
O1 C4 H4B 125.9 7_575 . ?
H4A C4 H4B 108.1 . . ?
C10 C4 H10B 88.6(14) 7_575 7_575 ?
O3 C4 H10B 55.9(7) . 7_575 ?
C3 C4 H10B 148.0(16) . 7_575 ?
O1 C4 H10B 120.8(13) 7_575 7_575 ?
H4A C4 H10B 101.7 . 7_575 ?
H4B C4 H10B 57.0 . 7_575 ?
C9 C5 O5 113(6) 7_575 7_575 ?
C9 C5 O3 55(6) 7_575 . ?
O5 C5 O3 68.5(7) 7_575 . ?
C9 C5 C6 151(8) 7_575 . ?
O5 C5 C6 40.1(5) 7_575 . ?
O3 C5 C6 106.8(9) . . ?
C9 C5 C10 21(7) 7_575 7_575 ?
O5 C5 C10 100.1(9) 7_575 7_575 ?
O3 C5 C10 35.1(5) . 7_575 ?
C6 C5 C10 140.2(10) . 7_575 ?
C9 C5 H5A 96.7 7_575 . ?
O5 C5 H5A 136.1 7_575 . ?
O3 C5 H5A 109.5 . . ?
C6 C5 H5A 111.6 . . ?
C10 C5 H5A 97.2 7_575 . ?
C9 C5 H5B 63.6 7_575 . ?
O5 C5 H5B 113.2 7_575 . ?
O3 C5 H5B 109.8 . . ?
C6 C5 H5B 110.6 . . ?
C10 C5 H5B 83.8 7_575 . ?
H5A C5 H5B 108.5 . . ?
C9 C5 H9A 95(8) 7_575 7_575 ?
O5 C5 H9A 132(3) 7_575 7_575 ?
O3 C5 H9A 103(2) . 7_575 ?
C6 C5 H9A 112(2) . 7_575 ?
C10 C5 H9A 93.4(16) 7_575 7_575 ?
H5A C5 H9A 7.2 . 7_575 ?
H5B C5 H9A 114.2 . 7_575 ?
C9 C5 H9B 71(8) 7_575 7_575 ?
O5 C5 H9B 116(3) 7_575 7_575 ?
O3 C5 H9B 118(2) . 7_575 ?
C6 C5 H9B 107(2) . 7_575 ?
C10 C5 H9B 91.5(16) 7_575 7_575 ?
H5A C5 H9B 103.4 . 7_575 ?
H5B C5 H9B 8.7 . 7_575 ?
H9A C5 H9B 109.7 7_575 7_575 ?
C8 C6 O5 108.5(10) 7_575 7_575 ?
C8 C6 O4 40.1(7) 7_575 . ?
O5 C6 O4 68.9(5) 7_575 . ?
C8 C6 C5 140.1(14) 7_575 . ?
O5 C6 C5 57.0(7) 7_575 . ?
O4 C6 C5 109.3(10) . . ?
C8 C6 C9 137.0(13) 7_575 7_575 ?
O5 C6 C9 52.9(6) 7_575 7_575 ?
O4 C6 C9 104.8(9) . 7_575 ?
C5 C6 C9 4.7(14) . 7_575 ?
C8 C6 H6A 72.3 7_575 . ?
O5 C6 H6A 159.1 7_575 . ?
O4 C6 H6A 107.0 . . ?
C5 C6 H6A 108.3 . . ?
C9 C6 H6A 111.6 7_575 . ?
C8 C6 H6B 106.5 7_575 . ?
O5 C6 H6B 91.6 7_575 . ?
O4 C6 H6B 113.0 . . ?
C5 C6 H6B 110.6 . . ?
C9 C6 H6B 111.9 7_575 . ?
H6A C6 H6B 108.4 . . ?
O4 C7 O4 68.4(5) 7_575 . ?
O4 C7 C8 104.3(5) 7_575 7_575 ?
O4 C7 C8 36.7(3) . 7_575 ?
O4 C7 C8 36.7(3) 7_575 . ?
O4 C7 C8 104.3(5) . . ?
C8 C7 C8 138.1(7) 7_575 . ?
O4 C7 Na1 49.6(2) 7_575 . ?
O4 C7 Na1 49.6(2) . . ?
C8 C7 Na1 79.4(3) 7_575 . ?
C8 C7 Na1 79.4(3) . . ?
O4 C7 H7A 124.4 7_575 . ?
O4 C7 H7A 107.3 . . ?
C8 C7 H7A 93.1 7_575 . ?
C8 C7 H7A 120.0 . . ?
Na1 C7 H7A 84.2 . . ?
O4 C7 H7B 130.2 7_575 . ?
O4 C7 H7B 105.2 . . ?
C8 C7 H7B 76.7 7_575 . ?
C8 C7 H7B 114.0 . . ?
Na1 C7 H7B 154.7 . . ?
H7A C7 H7B 105.0 . . ?
O4 C7 H7A 107.3(3) 7_575 7_575 ?
O4 C7 H7A 124.4(3) . 7_575 ?
C8 C7 H7A 120.0(3) 7_575 7_575 ?
C8 C7 H7A 93.1(3) . 7_575 ?
Na1 C7 H7A 84.24(10) . 7_575 ?
H7A C7 H7A 27.6 . 7_575 ?
H7B C7 H7A 114.9 . 7_575 ?
O4 C7 H7B 105.2(3) 7_575 7_575 ?
O4 C7 H7B 130.2(3) . 7_575 ?
C8 C7 H7B 114.0(3) 7_575 7_575 ?
C8 C7 H7B 76.7(3) . 7_575 ?
Na1 C7 H7B 154.70(7) . 7_575 ?
H7A C7 H7B 114.9 . 7_575 ?
H7B C7 H7B 39.9 . 7_575 ?
H7A C7 H7B 105.0 7_575 7_575 ?
C6 C8 O4 109.2(10) 7_575 7_575 ?
C6 C8 O5 40.7(7) 7_575 . ?
O4 C8 O5 68.9(5) 7_575 . ?
C6 C8 C7 139.0(10) 7_575 . ?
O4 C8 C7 57.0(5) 7_575 . ?
O5 C8 C7 108.1(5) . . ?
C6 C8 H8A 72.4 7_575 . ?
O4 C8 H8A 159.6 7_575 . ?
O5 C8 H8A 107.9 . . ?
C7 C8 H8A 107.8 . . ?
C6 C8 H8B 106.2 7_575 . ?
O4 C8 H8B 91.4 7_575 . ?
O5 C8 H8B 112.8 . . ?
C7 C8 H8B 112.1 . . ?
H8A C8 H8B 107.9 . . ?
C5 C9 O3 114(7) 7_575 7_575 ?
C5 C9 O5 55(5) 7_575 . ?
O3 C9 O5 68.5(8) 7_575 . ?
C5 C9 C10 154(8) 7_575 . ?
O3 C9 C10 42.2(6) 7_575 . ?
O5 C9 C10 107.8(10) . . ?
C5 C9 C6 24(6) 7_575 7_575 ?
O3 C9 C6 99.6(10) 7_575 7_575 ?
O5 C9 C6 33.3(4) . 7_575 ?
C10 C9 C6 140.8(11) . 7_575 ?
C5 C9 H9A 66.2 7_575 . ?
O3 C9 H9A 109.7 7_575 . ?
O5 C9 H9A 110.5 . . ?
C10 C9 H9A 109.5 . . ?
C6 C9 H9A 89.2 7_575 . ?
C5 C9 H9B 91.7 7_575 . ?
O3 C9 H9B 140.6 7_575 . ?
O5 C9 H9B 108.0 . . ?
C10 C9 H9B 113.0 . . ?
C6 C9 H9B 91.8 7_575 . ?
H9A C9 H9B 108.1 . . ?
C5 C9 H5B 98(8) 7_575 7_575 ?
O3 C9 H5B 132(3) 7_575 7_575 ?
O5 C9 H5B 107(2) . 7_575 ?
C10 C9 H5B 106(2) . 7_575 ?
C6 C9 H5B 95.3(17) 7_575 7_575 ?
H9A C9 H5B 115.5 . 7_575 ?
H9B C9 H5B 8.2 . 7_575 ?
C4 C10 O3 116.2(18) 7_575 7_575 ?
C4 C10 O1 91.4(13) 7_575 . ?
O3 C10 O1 92.8(7) 7_575 . ?
C4 C10 C9 161.1(18) 7_575 . ?
O3 C10 C9 57.3(8) 7_575 . ?
O1 C10 C9 106.2(11) . . ?
C4 C10 C3 62.1(12) 7_575 7_575 ?
O3 C10 C3 123.9(7) 7_575 7_575 ?
O1 C10 C3 36.4(3) . 7_575 ?
C9 C10 C3 136.8(12) . 7_575 ?
C4 C10 C5 158.3(17) 7_575 7_575 ?
O3 C10 C5 53.5(6) 7_575 7_575 ?
O1 C10 C5 107.3(9) . 7_575 ?
C9 C10 C5 4.2(14) . 7_575 ?
C3 C10 C5 139.4(10) 7_575 7_575 ?
C4 C10 Na1 105.5(15) 7_575 . ?
O3 C10 Na1 43.9(4) 7_575 . ?
O1 C10 Na1 49.3(4) . . ?
C9 C10 Na1 81.9(7) . . ?
C3 C10 Na1 80.8(4) 7_575 . ?
C5 C10 Na1 79.9(6) 7_575 . ?
C4 C10 H10A 78.0 7_575 . ?
O3 C10 H10A 157.0 7_575 . ?
O1 C10 H10A 105.4 . . ?
C9 C10 H10A 103.2 . . ?
C3 C10 H10A 78.3 7_575 . ?
C5 C10 H10A 106.6 7_575 . ?
Na1 C10 H10A 154.0 . . ?
C4 C10 H10B 47.6 7_575 . ?
O3 C10 H10B 74.6 7_575 . ?
O1 C10 H10B 116.5 . . ?
C9 C10 H10B 116.0 . . ?
C3 C10 H10B 103.8 7_575 . ?
C5 C10 H10B 112.2 7_575 . ?
Na1 C10 H10B 91.7 . . ?
H10A C10 H10B 108.2 . . ?
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 2.9662(3) 7_575 ?
Pb1 Br1 2.9662(3) . ?
Pb1 Br1 3.0568(3) 4_566 ?
Pb1 Br1 3.0568(3) 6_657 ?
Pb1 Br2 3.0643(5) 6_657 ?
Pb1 Br2 3.0922(5) . ?
Br2 Na1 2.9254(18) . ?
Na1 O5 2.327(4) 7_575 ?
Na1 O5 2.327(4) . ?
Na1 O1 2.385(5) 7_575 ?
Na1 O1 2.385(5) . ?
Na1 O2 2.412(5) 7_575 ?
Na1 O2 2.412(5) . ?
Na1 O3 2.421(4) . ?
Na1 O3 2.421(4) 7_575 ?
Na1 O4 2.444(5) 7_575 ?
Na1 O4 2.444(5) . ?
Na1 C10 3.053(9) . ?
O1 C3 1.003(7) 7_575 ?
O1 O2 1.379(6) 7_575 ?
O1 C10 1.418(9) . ?
O1 C1 1.422(8) . ?
O1 C4 1.577(9) 7_575 ?
O1 O3 1.790(6) 7_575 ?
O2 C1 0.802(7) 7_575 ?
O2 C2 1.366(6) . ?
O2 C3 1.427(7) . ?
O2 O2 1.654(10) 7_575 ?
O3 C10 1.026(10) 7_575 ?
O3 C9 1.285(17) 7_575 ?
O3 C5 1.433(13) . ?
O3 C4 1.442(8) . ?
O3 O5 1.533(6) 7_575 ?
O3 H10B 1.199(8) 7_575 ?
O4 C8 0.969(7) 7_575 ?
O4 C7 1.361(6) . ?
O4 O5 1.409(6) 7_575 ?
O4 C6 1.423(7) . ?
O4 O4 1.530(9) 7_575 ?
O5 C6 0.984(7) 7_575 ?
O5 C5 1.281(15) 7_575 ?
O5 C9 1.429(14) . ?
O5 C8 1.430(7) . ?
C1 C3 0.892(8) 7_575 ?
C1 C2 1.578(8) . ?
C1 H1A 0.9521 . ?
C1 H1B 0.9493 . ?
C2 H2A 0.9641 . ?
C2 H2B 0.9665 . ?
C2 H2A 0.9640 7_575 ?
C2 H2B 0.9665 7_575 ?
C3 C4 1.498(10) . ?
C3 C10 1.689(11) 7_575 ?
C3 H3A 0.9508 . ?
C3 H3B 0.9497 . ?
C4 C10 0.658(8) 7_575 ?
C4 H4A 0.9548 . ?
C4 H4B 0.9495 . ?
C4 H10B 0.701(16) 7_575 ?
C5 C9 0.30(3) 7_575 ?
C5 C6 1.516(13) . ?
C5 C10 1.783(15) 7_575 ?
C5 H5A 0.9555 . ?
C5 H5B 0.9489 . ?
C5 H9A 0.88(4) 7_575 ?
C5 H9B 1.01(5) 7_575 ?
C6 C8 0.771(7) 7_575 ?
C6 C9 1.787(15) 7_575 ?
C6 H6A 0.9507 . ?
C6 H6B 0.9490 . ?
C7 C8 1.619(8) 7_575 ?
C7 C8 1.619(8) . ?
C7 H7A 0.9681 . ?
C7 H7B 0.9798 . ?
C7 H7A 0.9680 7_575 ?
C7 H7B 0.9798 7_575 ?
C8 H8A 0.9519 . ?
C8 H8B 0.9492 . ?
C9 C10 1.505(13) . ?
C9 H9A 0.9538 . ?
C9 H9B 0.9492 . ?
C10 H10A 0.9523 . ?
C10 H10B 0.9495 . ?
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 2.62 3.413(10) 141.7 3_646 yes
C10 H10A Br1 0.95 3.03 3.886(10) 150.4 5_666 yes
C6 H6B Br1 0.95 2.96 3.865(7) 159.0 4_566 yes
C3 H3A Br1 0.95 2.88 3.636(7) 137.4 8_665 yes
