#------------------------------------------------------------------------------
#$Date: 2020-10-06 13:13:42 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257772 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/95/7059577.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_7059577
loop_
_publ_author_name
'Nisa, Zaib ul'
'Tashi, Lobzang'
'Sen, Charanjeet'
'Ashashi, Nargis Akhter'
'Sahoo, Subash Chandra'
'Sheikh, Haq Nawaz'
_publ_section_title
;
 Synthesis of eight isostructural 2D lanthanide coordination polymers
 assembled by rigid furan-2,5-dicarboxylic acid and flexible adipic acid
 as linkers and exploration of luminescent Eu/Tb polymers as efficient and
 sensitive sensors for nitroaromatic compounds
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8125
_journal_page_last               8137
_journal_paper_doi               10.1039/D0NJ01018A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C29 H21 N3 O9 Pb2, 0.5(C6 H15 N)'
_chemical_formula_sum            'C32 H28.5 N3.5 O9 Pb2'
_chemical_formula_weight         1020.46
_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
_audit_block_doi                 10.5517/ccdc.csd.cc23701f
_audit_creation_date             2019-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.	2020-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.181(2)
_cell_angle_beta                 97.698(2)
_cell_angle_gamma                94.222(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2850(3)
_cell_length_b                   13.3070(3)
_cell_length_c                   13.3260(3)
_cell_measurement_reflns_used    11400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5140
_cell_measurement_theta_min      1.9870
_cell_volume                     1756.90(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  19.00   0.50   12.00    --   -6.40  77.00 -30.00   82
  2  ω     29.00  55.00   0.50   12.00    --   -6.40  77.00 -30.00   52
  3  ω     37.00  67.00   0.50   12.00    --   -6.40  77.00-120.00   60
  4  ω     26.00  58.00   0.50   12.00    --    7.80  77.00-150.00   64
  5  ω      3.00  61.00   0.50   12.00    --    7.80  77.00 -60.00  116
  6  ω    -18.00  12.00   0.50   12.00    --    7.80  77.00-150.00   60
  7  ω    -31.00  22.00   0.50   12.00    --   -6.40  77.00-120.00  106
  8  ω    -21.00  73.00   0.50   12.00    --    7.80  77.00  60.00  188
  9  ω      4.00  74.00   0.50   12.00    --    7.80  77.00 150.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0195265000
_diffrn_orient_matrix_UB_12      -0.0495548000
_diffrn_orient_matrix_UB_13      -0.0193035000
_diffrn_orient_matrix_UB_21      0.0150404000
_diffrn_orient_matrix_UB_22      -0.0067474000
_diffrn_orient_matrix_UB_23      0.0515280000
_diffrn_orient_matrix_UB_31      -0.0654953000
_diffrn_orient_matrix_UB_32      -0.0224854000
_diffrn_orient_matrix_UB_33      -0.0029502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.967
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.988
_refine_diff_density_min         -2.172
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0509P)²+10.7494P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5999
_reflns_number_total             6999
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj01018a2.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 7059575--7059582.cif.

 Adding full bibliography for 7059575--7059582.cif.
;
_cod_original_formula_sum        'C32 H28.50 N3.50 O9 Pb2'
_cod_database_code               7059577
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Pb C O N H'
_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_max   0.249
_shelx_estimated_absorpt_t_min   0.160
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C30 = N4-C32 = N4-C34
 1.463 with sigma of 0.001
 N4-C31 = N4-C33 = N4-C35
 2.532 with sigma of 0.002
 C30-C32 = C32-C34 = C34-C30
 2.416 with sigma of 0.002
 C30-C31 = C32-C33 = C34-C35
 1.439 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C35) = Uanis(N4) = Uanis(C30) = Uanis(C32) = Uanis(C34) = Uanis(C31) =
Uanis(C33)
4. Others
 Fixed Sof: N4(0.5) C30(0.5) H30A(0.5) H30B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C34(0.5) H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C16(H16), C12(H12), C20(H20), C13(H13), C5(H5), C11(H11),
 C18(H18), C25(H25), C23(H23), C24(H24), C26(H26), C10(H10), C27(H27)
5.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C31(H31A,H31B,
 H31C), C35(H35A,H35B,H35C)
;
_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 4.998
_oxdiff_exptl_absorpt_empirical_full_min 0.462
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
Pb1 Pb 1.00873(2) 1.33726(2) 0.04530(2) 0.01219(2) Uani 1 1 d . . . . .
O6 O 1.38878(12) 1.44849(10) 0.90144(10) 0.0130(4) Uani 1 1 d . . . . .
O7 O 0.90867(12) 1.44737(10) 0.89718(10) 0.0130(4) Uani 1 1 d . . . . .
O2 O 0.75526(13) 1.34154(10) 0.05217(11) 0.0173(4) Uani 1 1 d . . . . .
O3 O 0.28189(13) 1.36170(10) 0.09384(11) 0.0179(4) Uani 1 1 d . . . . .
O8 O 0.76962(13) 1.38931(12) 0.75078(11) 0.0188(4) Uani 1 1 d . . . . .
O4 O 0.16492(14) 1.21216(11) 0.08158(13) 0.0247(4) Uani 1 1 d . . . . .
O1 O 0.84999(13) 1.19961(11) 0.06871(12) 0.0178(4) Uani 1 1 d . . . . .
O5 O 1.46920(13) 1.46084(12) 0.75806(11) 0.0197(4) Uani 1 1 d . . . . .
N2 N 1.03111(16) 1.35789(14) 0.24749(13) 0.0169(5) Uani 1 1 d . . . . .
C1 C 0.75176(18) 1.25238(15) 0.06991(15) 0.0146(5) Uani 1 1 d . . . . .
N1 N 0.45188(17) 0.74867(14) 0.16666(14) 0.0202(5) Uani 1 1 d . . . . .
O9 O 0.98416(18) 1.20651(13) -0.13315(14) 0.0357(5) Uani 1 1 d . . . . .
C3 C 0.51743(18) 1.26223(15) 0.09585(16) 0.0143(5) Uani 1 1 d . . . . .
H3 H 0.5246 1.3298 0.0870 0.017 Uiso 1 1 calc R . . . .
C8 C 0.27279(19) 1.26728(15) 0.09447(16) 0.0157(5) Uani 1 1 d . . . . .
C21 C 0.88599(19) 1.41251(14) 0.80063(15) 0.0131(5) Uani 1 1 d . . . . .
C15 C 1.23502(18) 1.42548(15) 0.74608(15) 0.0127(5) Uani 1 1 d . . . . .
C2 C 0.62727(18) 1.20762(15) 0.09633(15) 0.0138(5) Uani 1 1 d . . . . .
C14 C 1.37251(18) 1.44674(15) 0.80479(15) 0.0137(5) Uani 1 1 d . . . . .
C4 C 0.39588(19) 1.21605(15) 0.10861(16) 0.0149(5) Uani 1 1 d . . . . .
C7 C 0.61807(19) 1.10933(15) 0.11719(16) 0.0159(5) Uani 1 1 d . . . . .
H7 H 0.6924 1.0736 0.1189 0.019 Uiso 1 1 calc R . . . .
C17 C 1.00050(18) 1.40447(15) 0.74303(16) 0.0144(5) Uani 1 1 d . . . . .
C16 C 1.12876(19) 1.42413(15) 0.79800(16) 0.0154(5) Uani 1 1 d . . . . .
H16 H 1.1420 1.4363 0.8701 0.018 Uiso 1 1 calc R . . . .
C12 C 0.5668(2) 0.79096(16) 0.14895(17) 0.0200(6) Uani 1 1 d . . . . .
H12 H 0.6351 0.7494 0.1406 0.024 Uiso 1 1 calc R . . . .
C20 C 1.21650(19) 1.40804(16) 0.63804(16) 0.0179(6) Uani 1 1 d . . . . .
H20 H 1.2891 1.4097 0.6035 0.021 Uiso 1 1 calc R . . . .
C13 C 0.5888(2) 0.89187(15) 0.14247(16) 0.0173(5) Uani 1 1 d . . . . .
H13 H 0.6708 0.9172 0.1308 0.021 Uiso 1 1 calc R . . . .
C6 C 0.50005(19) 1.06315(15) 0.13562(16) 0.0143(5) Uani 1 1 d . . . . .
C5 C 0.38861(19) 1.11709(15) 0.12739(15) 0.0149(5) Uani 1 1 d . . . . .
H5 H 0.3076 1.0858 0.1347 0.018 Uiso 1 1 calc R . . . .
C19 C 1.08829(19) 1.38797(17) 0.58104(16) 0.0191(6) Uani 1 1 d . . . . .
C11 C 0.3577(2) 0.81128(17) 0.18413(19) 0.0247(6) Uani 1 1 d . . . . .
H11 H 0.2793 0.7846 0.2008 0.030 Uiso 1 1 calc R . . . .
C18 C 0.98143(19) 1.38476(16) 0.63489(16) 0.0156(5) Uani 1 1 d . . . . .
H18 H 0.8963 1.3693 0.5982 0.019 Uiso 1 1 calc R . . . .
C9 C 0.48834(19) 0.95749(15) 0.15335(16) 0.0160(5) Uani 1 1 d . . . . .
C25 C 1.1524(2) 1.37909(19) 0.30662(17) 0.0260(6) Uani 1 1 d . . . . .
H25 H 1.2252 1.3886 0.2738 0.031 Uiso 1 1 calc R . . . .
C23 C 0.9442(2) 1.35271(19) 0.40549(17) 0.0259(7) Uani 1 1 d . . . . .
H23 H 0.8699 1.3427 0.4365 0.031 Uiso 1 1 calc R . . . .
C24 C 0.9315(2) 1.34583(19) 0.30018(17) 0.0260(7) Uani 1 1 d . . . . .
H24 H 0.8467 1.3316 0.2626 0.031 Uiso 1 1 calc R . . . .
C22 C 1.0691(2) 1.37474(17) 0.46567(16) 0.0176(6) Uani 1 1 d . . . . .
C26 C 1.1736(2) 1.38735(19) 0.41307(16) 0.0231(6) Uani 1 1 d . . . . .
H26 H 1.2591 1.4015 0.4493 0.028 Uiso 1 1 calc R . . . .
C10 C 0.3716(2) 0.91318(16) 0.17861(18) 0.0228(6) Uani 1 1 d . . . . .
H10 H 0.3031 0.9536 0.1917 0.027 Uiso 1 1 calc R . . . .
N3 N 0.9909(3) 1.0442(2) -0.2226(2) 0.0575(9) Uani 1 1 d . . . . .
C27 C 0.9931(3) 1.1154(2) -0.1362(2) 0.0451(9) Uani 1 1 d . . . . .
H27 H 1.0020 1.0943 -0.0737 0.054 Uiso 1 1 calc R . . . .
C29 C 0.9928(4) 0.9337(2) -0.2252(3) 0.0673(13) Uani 1 1 d . . . . .
H29A H 1.0096 0.9238 -0.1555 0.101 Uiso 1 1 calc GR . . . .
H29B H 1.0611 0.9074 -0.2627 0.101 Uiso 1 1 calc GR . . . .
H29C H 0.9090 0.8975 -0.2591 0.101 Uiso 1 1 calc GR . . . .
C28 C 0.9883(6) 1.0784(5) -0.3213(5) 0.1411(5) Uani 1 1 d . U . . .
H28A H 0.9016 1.0607 -0.3612 0.212 Uiso 1 1 calc GR . . . .
H28B H 1.0513 1.0448 -0.3600 0.212 Uiso 1 1 calc GR . . . .
H28C H 1.0101 1.1519 -0.3068 0.212 Uiso 1 1 calc GR . . . .
Pb2 Pb 1.64432(2) 1.44598(2) 0.90239(2) 0.01035(2) Uani 1 1 d . . . . .
N4 N 1.52765(3) 1.81688(3) 0.49726(2) 0.0873(12) Uani 0.5 1 d D . P . .
C30 C 1.43407(3) 1.72445(3) 0.45657(3) 0.0873(12) Uani 0.5 1 d D . P . .
H30A H 1.3738 1.7388 0.4000 0.105 Uiso 0.5 1 calc R . P . .
H30B H 1.4838 1.6699 0.4260 0.105 Uiso 0.5 1 calc R . P . .
C32 C 1.59105(4) 1.82039(4) 0.60312(2) 0.0873(12) Uani 0.5 1 d D . P . .
H32A H 1.5231 1.8296 0.6472 0.105 Uiso 0.5 1 calc R . P . .
H32B H 1.6196 1.7526 0.6037 0.105 Uiso 0.5 1 calc R . P . .
C33 C 1.70142(4) 1.89516(4) 0.65284(6) 0.0873(12) Uani 0.5 1 d D . P . .
H33A H 1.7791 1.8754 0.6244 0.131 Uiso 0.5 1 calc GR . P . .
H33B H 1.7152 1.8980 0.7261 0.131 Uiso 0.5 1 calc GR . P . .
H33C H 1.6836 1.9619 0.6412 0.131 Uiso 0.5 1 calc GR . P . .
C31 C 1.35476(4) 1.68230(4) 0.52200(3) 0.0873(12) Uani 0.5 1 d D . P . .
H31A H 1.2763 1.6437 0.4803 0.131 Uiso 0.5 1 calc GR . P . .
H31B H 1.3309 1.7376 0.5729 0.131 Uiso 0.5 1 calc GR . P . .
H31C H 1.4041 1.6375 0.5564 0.131 Uiso 0.5 1 calc GR . P . .
C34 C 1.62521(3) 1.82557(2) 0.42830(2) 0.0873(12) Uani 0.5 1 d D . P . .
H34A H 1.7039 1.7989 0.4567 0.105 Uiso 0.5 1 calc R . P . .
H34B H 1.5913 1.7789 0.3621 0.105 Uiso 0.5 1 calc R . P . .
C35 C 1.66676(8) 1.92334(2) 0.40648(4) 0.0873(12) Uani 0.5 1 d D . P . .
H35A H 1.6418 1.9207 0.3339 0.131 Uiso 0.5 1 calc GR . P . .
H35B H 1.7609 1.9375 0.4244 0.131 Uiso 0.5 1 calc GR . P . .
H35C H 1.6254 1.9770 0.4466 0.131 Uiso 0.5 1 calc GR . 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'
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_
_citation_id
_citation_doi
_citation_year
1 10.1021/acs.inorgchem.9b02697 2019
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 N2 84.89(5) . . ?
O4 Pb1 O2 132.56(5) 1_655 . ?
O4 Pb1 N2 76.33(6) 1_655 . ?
O4 Pb1 O9 77.56(5) 1_655 . ?
O1 Pb1 O2 51.78(5) . . ?
O1 Pb1 O4 81.22(5) . 1_655 ?
O1 Pb1 N2 75.40(5) . . ?
O1 Pb1 O9 78.29(5) . . ?
O9 Pb1 O2 96.35(5) . . ?
O9 Pb1 N2 145.24(6) . . ?
C14 O6 Pb2 90.11(11) . . ?
C21 O7 Pb2 90.07(11) . 1_455 ?
C1 O2 Pb1 88.67(11) . . ?
C8 O3 Pb2 167.51(13) . 2_786 ?
C21 O8 Pb2 98.00(12) . 1_455 ?
C8 O4 Pb1 100.60(13) . 1_455 ?
C1 O1 Pb1 95.91(12) . . ?
C14 O5 Pb2 96.12(12) . . ?
C25 N2 Pb1 119.85(14) . . ?
C24 N2 Pb1 125.42(13) . . ?
C24 N2 C25 114.68(19) . . ?
O2 C1 O1 123.32(19) . . ?
O2 C1 C2 118.16(18) . . ?
O1 C1 C2 118.50(19) . . ?
C12 N1 Pb2 125.50(14) . 2_776 ?
C11 N1 C12 117.10(19) . . ?
C11 N1 Pb2 112.40(13) . 2_776 ?
C27 O9 Pb1 119.93(18) . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.26(19) . . ?
C4 C3 H3 119.9 . . ?
O3 C8 C4 118.91(17) . . ?
O4 C8 O3 123.59(19) . . ?
O4 C8 C4 117.48(18) . . ?
O7 C21 O8 122.40(19) . . ?
O7 C21 C17 117.95(16) . . ?
O8 C21 C17 119.55(17) . . ?
C16 C15 C14 120.43(18) . . ?
C16 C15 C20 120.43(17) . . ?
C20 C15 C14 119.14(18) . . ?
C3 C2 C1 119.85(19) . . ?
C3 C2 C7 119.50(19) . . ?
C7 C2 C1 120.59(18) . . ?
O6 C14 C15 118.30(18) . . ?
O5 C14 O6 121.53(17) . . ?
O5 C14 C15 120.16(18) . . ?
C3 C4 C8 121.38(19) . . ?
C5 C4 C3 119.04(19) . . ?
C5 C4 C8 119.41(18) . . ?
C2 C7 H7 119.2 . . ?
C2 C7 C6 121.61(19) . . ?
C6 C7 H7 119.2 . . ?
C16 C17 C21 119.69(18) . . ?
C18 C17 C21 120.64(17) . . ?
C18 C17 C16 119.52(19) . . ?
C15 C16 C17 120.32(19) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
N1 C12 H12 118.2 . . ?
N1 C12 C13 123.6(2) . . ?
C13 C12 H12 118.2 . . ?
C15 C20 H20 119.9 . . ?
C15 C20 C19 120.26(19) . . ?
C19 C20 H20 119.9 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C9 120.4(2) . . ?
C9 C13 H13 119.8 . . ?
C7 C6 C5 117.56(19) . . ?
C7 C6 C9 121.82(18) . . ?
C5 C6 C9 120.37(18) . . ?
C4 C5 C6 121.78(19) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C20 C19 C22 119.87(19) . . ?
C18 C19 C20 118.58(19) . . ?
C18 C19 C22 121.50(17) . . ?
N1 C11 H11 118.5 . . ?
N1 C11 C10 122.9(2) . . ?
C10 C11 H11 118.5 . . ?
C17 C18 C19 120.86(17) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C13 C9 C6 123.26(19) . . ?
C13 C9 C10 114.86(19) . . ?
C10 C9 C6 121.83(19) . . ?
N2 C25 H25 118.2 . . ?
N2 C25 C26 123.7(2) . . ?
C26 C25 H25 118.2 . . ?
C24 C23 H23 120.2 . . ?
C24 C23 C22 119.7(2) . . ?
C22 C23 H23 120.2 . . ?
N2 C24 C23 125.25(19) . . ?
N2 C24 H24 117.4 . . ?
C23 C24 H24 117.4 . . ?
C23 C22 C19 122.03(19) . . ?
C26 C22 C19 121.73(17) . . ?
C26 C22 C23 116.20(19) . . ?
C25 C26 H26 119.7 . . ?
C22 C26 C25 120.51(19) . . ?
C22 C26 H26 119.7 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C27 N3 C29 123.5(3) . . ?
C27 N3 C28 118.1(3) . . ?
C29 N3 C28 118.3(3) . . ?
O9 C27 N3 124.5(3) . . ?
O9 C27 H27 117.8 . . ?
N3 C27 H27 117.8 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O6 Pb2 O7 177.75(4) . 1_655 ?
O3 Pb2 O6 101.72(4) 2_786 . ?
O3 Pb2 O7 76.81(4) 2_786 1_655 ?
O3 Pb2 N1 161.02(5) 2_786 2_776 ?
O8 Pb2 O6 129.12(4) 1_655 . ?
O8 Pb2 O7 49.45(4) 1_655 1_655 ?
O8 Pb2 O3 89.64(5) 1_655 2_786 ?
O8 Pb2 N1 78.23(5) 1_655 2_776 ?
O5 Pb2 O6 51.01(5) . . ?
O5 Pb2 O7 126.93(5) . 1_655 ?
O5 Pb2 O3 84.58(5) . 2_786 ?
O5 Pb2 O8 81.72(5) . 1_655 ?
O5 Pb2 N1 79.31(5) . 2_776 ?
N1 Pb2 O6 75.75(5) 2_776 . ?
N1 Pb2 O7 105.06(5) 2_776 1_655 ?
C30 N4 C32 111.60(3) . . ?
C30 N4 C34 111.44(2) . . ?
C32 N4 C34 111.40(3) . . ?
N4 C30 H30A 106.9 . . ?
N4 C30 H30B 106.9 . . ?
H30A C30 H30B 106.7 . . ?
C31 C30 N4 121.66(3) . . ?
C31 C30 H30A 106.9 . . ?
C31 C30 H30B 106.9 . . ?
N4 C32 H32A 107.0 . . ?
N4 C32 H32B 107.0 . . ?
H32A C32 H32B 106.7 . . ?
C33 C32 N4 121.33(5) . . ?
C33 C32 H32A 107.0 . . ?
C33 C32 H32B 107.0 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N4 C34 H34A 107.0 . . ?
N4 C34 H34B 107.0 . . ?
H34A C34 H34B 106.7 . . ?
C35 C34 N4 121.44(4) . . ?
C35 C34 H34A 107.0 . . ?
C35 C34 H34B 107.0 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 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
Pb1 O2 2.6251(14) . ?
Pb1 O4 2.4719(15) 1_655 ?
Pb1 O1 2.4607(14) . ?
Pb1 N2 2.6269(18) . ?
Pb1 O9 2.6027(16) . ?
O6 C14 1.271(2) . ?
O6 Pb2 2.6293(13) . ?
O7 C21 1.256(2) . ?
O7 Pb2 2.7278(13) 1_455 ?
O2 C1 1.257(3) . ?
O3 C8 1.255(3) . ?
O3 Pb2 2.6033(14) 2_786 ?
O8 C21 1.271(2) . ?
O8 Pb2 2.5513(14) 1_455 ?
O4 Pb1 2.4719(15) 1_455 ?
O4 C8 1.255(2) . ?
O1 C1 1.272(2) . ?
O5 C14 1.265(3) . ?
O5 Pb2 2.5035(14) . ?
N2 C25 1.359(3) . ?
N2 C24 1.336(3) . ?
C1 C2 1.488(3) . ?
N1 C12 1.342(3) . ?
N1 C11 1.335(3) . ?
N1 Pb2 2.6283(17) 2_776 ?
O9 C27 1.215(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.387(3) . ?
C3 C4 1.399(3) . ?
C8 C4 1.490(3) . ?
C21 C17 1.488(3) . ?
C15 C14 1.498(3) . ?
C15 C16 1.371(3) . ?
C15 C20 1.394(3) . ?
C2 C7 1.393(3) . ?
C4 C5 1.390(3) . ?
C7 H7 0.9300 . ?
C7 C6 1.395(3) . ?
C17 C16 1.398(3) . ?
C17 C18 1.393(3) . ?
C16 H16 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.368(3) . ?
C20 H20 0.9300 . ?
C20 C19 1.408(3) . ?
C13 H13 0.9300 . ?
C13 C9 1.403(3) . ?
C6 C5 1.401(3) . ?
C6 C9 1.473(3) . ?
C5 H5 0.9300 . ?
C19 C18 1.394(3) . ?
C19 C22 1.494(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.371(3) . ?
C18 H18 0.9300 . ?
C9 C10 1.411(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.386(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.375(3) . ?
C23 C22 1.396(3) . ?
C24 H24 0.9300 . ?
C22 C26 1.379(3) . ?
C26 H26 0.9300 . ?
C10 H10 0.9300 . ?
N3 C27 1.323(4) . ?
N3 C29 1.465(4) . ?
N3 C28 1.478(8) . ?
C27 H27 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Pb2 O7 2.7278(13) 1_655 ?
Pb2 O3 2.6034(14) 2_786 ?
Pb2 O8 2.5513(14) 1_655 ?
Pb2 N1 2.6283(17) 2_776 ?
N4 C30 1.4621(4) . ?
N4 C32 1.4625(4) . ?
N4 C34 1.4627(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.4386(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.4393(5) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.4391(5) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
