#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:30:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179483 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/80/4338034.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_4338034
loop_
_publ_author_name
'Chang, Lixian'
'Wang, Li'
'Su, Xin'
'Pan, Shilie'
'Hailili, Reshalaiti'
'Yu, Hongwei'
'Yang, Zhihua'
_publ_section_title
;
 A Nitrate Nonlinear Optical Crystal Pb16(OH)16(NO3)16 with a Large
 Second-Harmonic Generation Response.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3320
_journal_paper_doi               10.1021/ic402404a
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'H16 N16 O64 Pb16'
_chemical_formula_weight         4579.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 133.54
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.4814(12)
_cell_length_b                   17.1832(8)
_cell_length_c                   18.1746(9)
_cell_measurement_temperature    120(2)
_cell_volume                     5768.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21767
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    46.652
_exptl_absorpt_correction_T_max  0.4555
_exptl_absorpt_correction_T_min  0.1662
_exptl_crystal_density_diffrn    5.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7808
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.488
_refine_diff_density_min         -3.853
_refine_diff_density_rms         0.566
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_coef       0.000053(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         9192
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+596.6030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                8176
_reflns_number_total             9192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402404a_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments          'Adding full bibliography for 4338034.cif.'
_cod_original_cell_volume        5768.7(5)
_cod_database_code               4338034
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pb1 Pb 0.65885(6) 0.58270(6) 0.95859(8) 0.0121(2) Uani 1 1 d .
Pb2 Pb 0.68314(6) 0.56925(6) 0.77327(8) 0.0111(2) Uani 1 1 d .
Pb3 Pb 0.50985(6) 0.49915(7) 0.68735(8) 0.0131(2) Uani 1 1 d .
Pb4 Pb 0.67903(6) 0.38773(6) 0.89151(8) 0.0131(2) Uani 1 1 d .
Pb5 Pb 0.01067(5) 0.46576(6) 0.65196(7) 0.0110(2) Uani 1 1 d .
Pb6 Pb 0.08387(6) 0.56016(6) 0.89805(7) 0.0108(2) Uani 1 1 d .
Pb7 Pb 0.19925(6) 0.41899(6) 0.90721(8) 0.0125(2) Uani 1 1 d .
Pb8 Pb 0.15863(6) 0.61553(6) 0.78364(8) 0.0128(2) Uani 1 1 d .
Pb9 Pb 0.45770(6) 0.65481(6) 0.90161(8) 0.0126(2) Uani 1 1 d .
Pb10 Pb 0.40856(6) 0.85585(6) 0.77501(8) 0.0113(2) Uani 1 1 d .
Pb11 Pb 0.35026(6) 0.79751(6) 0.91004(8) 0.0127(2) Uani 1 1 d .
Pb12 Pb 0.26887(6) 0.69854(6) 0.65910(8) 0.0125(2) Uani 1 1 d .
Pb13 Pb 0.40568(6) 0.34242(6) 0.95857(8) 0.0125(2) Uani 1 1 d .
Pb14 Pb 0.41383(6) 0.14658(6) 0.87709(8) 0.0124(2) Uani 1 1 d .
Pb15 Pb 0.43373(6) 0.32978(6) 0.77825(8) 0.0114(2) Uani 1 1 d .
Pb16 Pb 0.25286(6) 0.27418(7) 0.68319(8) 0.0141(2) Uani 1 1 d .
N1 N 0.7831(14) 0.7135(14) 0.9950(18) 0.014(2) Uani 1 1 d U
N2 N 0.3324(13) 0.5098(14) 0.9228(18) 0.012(5) Uani 1 1 d U
N3 N 0.5023(13) 0.3080(14) 0.6426(18) 0.012(2) Uani 1 1 d U
N4 N 0.1497(14) 0.7848(15) 0.6708(19) 0.016(2) Uani 1 1 d U
N5 N 0.8387(14) 0.4875(15) 0.9000(19) 0.015(5) Uani 1 1 d U
N6 N 0.0504(16) 0.9536(17) 0.019(2) 0.023(2) Uani 1 1 d U
N7 N 0.3119(14) 0.3046(15) 0.5377(19) 0.016(2) Uani 1 1 d U
N8 N 0.2050(15) 0.4942(16) 1.126(2) 0.020(5) Uani 1 1 d U
N9 N 0.2567(13) 0.9447(14) 0.1490(18) 0.013(4) Uani 1 1 d U
N10 N 0.5372(14) 0.9717(15) 1.0134(19) 0.016(5) Uani 1 1 d U
N11 N 0.5816(14) 0.7564(15) 0.9063(19) 0.015(5) Uani 1 1 d U
N12 N 0.4601(15) 0.2177(16) 1.135(2) 0.022(6) Uani 1 1 d U
N13 N 0.1514(16) 0.2897(17) 0.731(2) 0.024(6) Uani 1 1 d U
N14 N 0.5816(14) 0.2434(15) 0.8949(19) 0.015(5) Uani 1 1 d U
N15 N 0.8842(15) 0.4467(16) 0.153(2) 0.020(5) Uani 1 1 d U
N16 N 0.8956(10) 0.9680(10) 0.2129(11) 0.022(6) Uani 1 1 d DU
O1 O 0.7245(11) 0.5156(11) 0.9319(14) 0.009(4) Uani 1 1 d U
H1 H 0.7755 0.5193 0.9879 0.014 Uiso 1 1 d R
O2 O 0.6185(12) 0.4558(13) 0.7381(17) 0.0195(12) Uani 1 1 d U
H2 H 0.6108 0.4240 0.6882 0.029 Uiso 1 1 d R
O3 O 0.5965(10) 0.6011(11) 0.7858(13) 0.008(4) Uani 1 1 d U
H3 H 0.5760 0.6519 0.7606 0.012 Uiso 1 1 d R
O4 O 0.5896(11) 0.4670(12) 0.8609(15) 0.013(4) Uani 1 1 d U
H4 H 0.5663 0.4431 0.8795 0.020 Uiso 1 1 d R
O5 O 0.1426(12) 0.4819(13) 0.7576(17) 0.0195(12) Uani 1 1 d U
H5 H 0.1567 0.4628 0.7241 0.029 Uiso 1 1 d R
O6 O 0.1878(12) 0.5511(13) 0.9234(17) 0.019(5) Uani 1 1 d U
H6 H 0.2298 0.5727 0.9866 0.029 Uiso 1 1 d R
O7 O 0.0745(12) 0.4445(13) 0.8222(17) 0.0195(12) Uani 1 1 d U
H7 H 0.0550 0.4027 0.8318 0.029 Uiso 1 1 d R
O8 O 0.0450(11) 0.5834(11) 0.7356(15) 0.012(4) Uani 1 1 d U
H8 H 0.0094 0.6234 0.6967 0.019 Uiso 1 1 d R
O9 O 0.3005(10) 0.8186(11) 0.7408(14) 0.009(4) Uani 1 1 d U
H9 H 0.2632 0.8570 0.7040 0.014 Uiso 1 1 d R
O10 O 0.3373(11) 0.6852(12) 0.8321(15) 0.012(4) Uani 1 1 d U
H10 H 0.3196 0.6432 0.8444 0.018 Uiso 1 1 d R
O11 O 0.4465(12) 0.7857(13) 0.9189(17) 0.0195(12) Uani 1 1 d U
H11 H 0.4901 0.8071 0.9804 0.029 Uiso 1 1 d R
O12 O 0.3934(11) 0.7237(11) 0.7494(15) 0.012(4) Uani 1 1 d U
H12 H 0.4049 0.7059 0.7120 0.018 Uiso 1 1 d R
O13 O 0.3311(11) 0.2323(12) 0.8528(15) 0.014(4) Uani 1 1 d U
H13 H 0.3062 0.2095 0.8694 0.021 Uiso 1 1 d R
O14 O 0.3621(10) 0.2203(11) 0.7350(14) 0.010(3) Uani 1 1 d U
H14 H 0.3528 0.1901 0.6828 0.014 Uiso 1 1 d R
O15 O 0.4692(10) 0.2718(11) 0.9309(14) 0.010(4) Uani 1 1 d U
H15 H 0.5201 0.2706 0.9882 0.015 Uiso 1 1 d R
O16 O 0.3442(10) 0.3644(11) 0.7865(14) 0.010(3) Uani 1 1 d U
H16 H 0.3272 0.4170 0.7657 0.014 Uiso 1 1 d R
O17 O 0.7553(11) 0.6905(12) 0.9112(15) 0.014(2) Uani 1 1 d U
O18 O 0.8130(11) 0.7822(12) 1.0253(15) 0.014(2) Uani 1 1 d U
O19 O 0.7795(11) 0.6777(12) 1.0540(15) 0.014(2) Uani 1 1 d U
O20 O 0.3110(12) 0.4515(13) 0.9350(17) 0.0195(12) Uani 1 1 d U
O21 O 0.3834(13) 0.5109(14) 0.9271(17) 0.022(5) Uani 1 1 d U
O22 O 0.3007(12) 0.5767(13) 0.9048(17) 0.0195(12) Uani 1 1 d U
O23 O 0.5106(11) 0.2347(12) 0.6384(15) 0.012(2) Uani 1 1 d U
O24 O 0.4607(11) 0.3439(12) 0.5572(15) 0.012(2) Uani 1 1 d U
O25 O 0.5292(11) 0.3409(11) 0.7227(15) 0.012(2) Uani 1 1 d U
O26 O 0.1909(12) 0.7900(12) 0.7646(16) 0.016(2) Uani 1 1 d U
O27 O 0.1027(12) 0.8419(12) 0.6130(16) 0.016(2) Uani 1 1 d U
O28 O 0.1526(11) 0.7349(13) 0.6277(16) 0.016(2) Uani 1 1 d U
O29 O 0.7793(12) 0.4468(12) 0.8447(16) 0.016(4) Uani 1 1 d U
O30 O 0.8392(12) 0.5567(13) 0.9235(16) 0.017(4) Uani 1 1 d U
O31 O 0.8921(13) 0.4505(13) 0.9270(17) 0.022(5) Uani 1 1 d U
O32 O 0.0058(13) 0.9520(14) -0.0735(18) 0.023(2) Uani 1 1 d U
O33 O 0.0399(13) 0.9250(14) 0.0710(18) 0.023(2) Uani 1 1 d U
O34 O 0.1071(13) 1.0006(14) 0.0645(18) 0.023(2) Uani 1 1 d U
O35 O 0.3754(12) 0.2688(12) 0.5973(16) 0.016(2) Uani 1 1 d U
O36 O 0.2975(12) 0.3441(12) 0.5790(16) 0.016(2) Uani 1 1 d U
O37 O 0.2642(11) 0.2882(12) 0.4448(16) 0.016(2) Uani 1 1 d U
O38 O 0.2316(12) 0.4646(13) 1.2062(17) 0.0195(12) Uani 1 1 d U
O39 O 0.2069(12) 0.5611(13) 1.1118(17) 0.0195(12) Uani 1 1 d U
O40 O 0.1742(12) 0.4529(13) 1.0476(17) 0.0195(12) Uani 1 1 d U
O41 O 0.2803(14) 0.9063(15) 0.2252(19) 0.028(5) Uani 1 1 d U
O42 O 0.2072(13) 0.9171(14) 0.0622(18) 0.024(4) Uani 1 1 d U
O43 O 0.2769(14) 1.0157(14) 0.1567(19) 0.025(5) Uani 1 1 d U
O44 O 0.5460(11) 0.9162(12) 1.0659(15) 0.014(4) Uani 1 1 d U
O45 O 0.5076(11) 0.9569(11) 0.9236(15) 0.011(4) Uani 1 1 d U
O46 O 0.5533(12) 1.0383(13) 1.0383(17) 0.0195(12) Uani 1 1 d U
O47 O 0.5486(11) 0.8167(12) 0.8888(16) 0.015(4) Uani 1 1 d U
O48 O 0.5548(11) 0.6958(11) 0.8969(15) 0.012(4) Uani 1 1 d U
O49 O 0.6403(12) 0.7582(13) 0.9313(16) 0.016(4) Uani 1 1 d U
O50 O 0.4627(10) 0.2112(11) 1.0698(14) 0.009(4) Uani 1 1 d U
O51 O 0.4743(13) 0.2838(14) 1.1752(18) 0.023(5) Uani 1 1 d U
O52 O 0.4507(13) 0.1665(14) 1.1681(18) 0.024(5) Uani 1 1 d U
O53 O 0.1344(12) 0.2351(13) 0.6734(17) 0.0195(12) Uani 1 1 d U
O54 O 0.1172(12) 0.3120(13) 0.7550(17) 0.021(5) Uani 1 1 d U
O55 O 0.2037(13) 0.3315(14) 0.7643(18) 0.025(5) Uani 1 1 d U
O56 O 0.5888(12) 0.3121(13) 0.9277(17) 0.0195(12) Uani 1 1 d U
O57 O 0.6354(14) 0.2104(15) 0.9210(19) 0.028(5) Uani 1 1 d U
O58 O 0.5194(12) 0.2153(12) 0.8355(16) 0.017(4) Uani 1 1 d U
O59 O 0.8342(12) 0.3895(13) 0.0939(17) 0.019(4) Uani 1 1 d U
O60 O 0.9254(11) 0.4362(12) 0.2423(15) 0.014(4) Uani 1 1 d U
O61 O 0.8857(14) 0.4944(15) 0.1062(19) 0.029(5) Uani 1 1 d U
O62 O 0.8558(12) 0.9453(14) 0.2254(18) 0.026(5) Uani 1 1 d DU
O63 O 0.9517(11) 0.9274(12) 0.2582(16) 0.0195(12) Uani 1 1 d DU
O64 O 0.8870(12) 1.0227(12) 0.1639(15) 0.0195(12) Uani 1 1 d DU
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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_3
O1 Pb1 O3 73.3(6) .
O1 Pb1 O4 73.1(7) .
O3 Pb1 O4 69.8(7) .
O2 Pb2 O3 72.5(7) .
O2 Pb2 O1 70.2(7) .
O3 Pb2 O1 70.1(6) .
O2 Pb3 O4 72.9(8) .
O2 Pb3 O3 73.0(7) .
O4 Pb3 O3 70.7(7) .
O1 Pb4 O2 71.8(7) .
O1 Pb4 O4 74.0(7) .
O2 Pb4 O4 72.4(8) .
O1 Pb4 O42 77.5(7) 3_546
O2 Pb4 O42 134.5(8) 3_546
O4 Pb4 O42 67.3(7) 3_546
O8 Pb5 O7 70.2(8) .
O8 Pb5 O5 72.3(7) .
O7 Pb5 O5 69.8(8) .
O7 Pb6 O6 72.8(8) .
O7 Pb6 O8 68.3(7) .
O6 Pb6 O8 73.1(7) .
O7 Pb6 O40 71.8(7) .
O6 Pb6 O40 72.4(7) .
O8 Pb6 O40 133.1(7) .
O5 Pb7 O6 70.1(8) .
O5 Pb7 O7 71.4(8) .
O6 Pb7 O7 71.5(8) .
O5 Pb7 O20 80.7(8) .
O6 Pb7 O20 89.0(8) .
O7 Pb7 O20 150.0(7) .
O5 Pb7 O54 72.4(7) .
O6 Pb7 O54 135.1(7) .
O7 Pb7 O54 73.9(7) .
O20 Pb7 O54 108.4(7) .
O5 Pb8 O6 68.8(8) .
O5 Pb8 O8 72.8(8) .
O6 Pb8 O8 72.4(7) .
O5 Pb8 O22 82.7(7) .
O6 Pb8 O22 76.0(7) .
O8 Pb8 O22 145.3(7) .
O11 Pb9 O12 67.6(8) .
O11 Pb9 O10 68.5(7) .
O12 Pb9 O10 70.9(7) .
O11 Pb9 O48 87.2(7) .
O12 Pb9 O48 74.6(7) .
O10 Pb9 O48 143.3(6) .
O12 Pb10 O11 67.0(7) .
O12 Pb10 O9 71.8(7) .
O11 Pb10 O9 71.6(7) .
O12 Pb10 O47 81.8(7) .
O11 Pb10 O47 73.3(7) .
O9 Pb10 O47 142.1(6) .
O12 Pb10 O45 138.5(6) .
O11 Pb10 O45 80.5(7) .
O9 Pb10 O45 122.3(6) .
O47 Pb10 O45 64.0(6) .
O10 Pb11 O11 70.6(8) .
O10 Pb11 O9 67.1(7) .
O11 Pb11 O9 73.0(7) .
O10 Pb12 O9 67.6(7) .
O10 Pb12 O12 71.8(7) .
O9 Pb12 O12 72.1(7) .
O10 Pb12 O28 90.0(7) .
O9 Pb12 O28 77.1(7) .
O12 Pb12 O28 148.3(7) .
O15 Pb13 O16 74.1(7) .
O15 Pb13 O13 72.8(7) .
O16 Pb13 O13 68.5(7) .
O15 Pb13 O50 68.3(6) .
O16 Pb13 O50 130.4(6) .
O13 Pb13 O50 70.3(6) .
O14 Pb14 O13 72.5(7) .
O14 Pb14 O15 71.6(7) .
O13 Pb14 O15 73.2(7) .
O14 Pb14 O41 72.0(7) 2_565
O13 Pb14 O41 71.3(8) 2_565
O15 Pb14 O41 135.0(7) 2_565
O14 Pb15 O15 69.5(6) .
O14 Pb15 O16 71.0(7) .
O15 Pb15 O16 70.4(6) .
O14 Pb15 O58 76.7(7) .
O15 Pb15 O58 71.6(7) .
O16 Pb15 O58 136.6(7) .
O14 Pb15 O35 68.6(7) .
O15 Pb15 O35 132.7(6) .
O16 Pb15 O35 114.2(7) .
O58 Pb15 O35 78.4(7) .
O16 Pb16 O13 70.7(7) .
O16 Pb16 O14 72.3(7) .
O13 Pb16 O14 70.4(7) .
O16 Pb16 O55 84.1(7) .
O13 Pb16 O55 71.9(7) .
O14 Pb16 O55 140.3(7) .
O17 N1 O19 125(3) .
O17 N1 O18 119(2) .
O19 N1 O18 116(2) .
O20 N2 O21 125(3) .
O20 N2 O22 119(3) .
O21 N2 O22 116(2) .
O25 N3 O23 122(2) .
O25 N3 O24 122(2) .
O23 N3 O24 116(2) .
O28 N4 O26 125(3) .
O28 N4 O27 116(2) .
O26 N4 O27 119(3) .
O30 N5 O31 126(3) .
O30 N5 O29 120(2) .
O31 N5 O29 114(2) .
O32 N6 O33 124(3) .
O32 N6 O34 117(3) .
O33 N6 O34 119(3) .
O36 N7 O37 121(3) .
O36 N7 O35 118(2) .
O37 N7 O35 120(3) .
O39 N8 O38 127(3) .
O39 N8 O40 112(3) .
O38 N8 O40 121(3) .
O41 N9 O42 120(3) .
O41 N9 O43 122(3) .
O42 N9 O43 118(2) .
O46 N10 O44 127(3) .
O46 N10 O45 115(3) .
O44 N10 O45 118(2) .
O48 N11 O47 119(3) .
O48 N11 O49 120(3) .
O47 N11 O49 121(3) .
O52 N12 O50 126(3) .
O52 N12 O51 117(3) .
O50 N12 O51 117(3) .
O53 N13 O55 119(3) .
O53 N13 O54 126(3) .
O55 N13 O54 115(3) .
O57 N14 O58 125(3) .
O57 N14 O56 119(3) .
O58 N14 O56 117(3) .
O60 N15 O61 130(3) .
O60 N15 O59 116(3) .
O61 N15 O59 114(3) .
O64 N16 O62 128(2) .
O64 N16 O63 117(2) .
O62 N16 O63 114(2) .
Pb1 O1 Pb4 104.8(8) .
Pb1 O1 Pb2 105.5(7) .
Pb4 O1 Pb2 105.2(7) .
Pb1 O1 H1 113.0 .
Pb4 O1 H1 114.3 .
Pb2 O1 H1 113.2 .
Pb2 O2 Pb3 105.1(9) .
Pb2 O2 Pb4 109.0(9) .
Pb3 O2 Pb4 104.7(9) .
Pb2 O2 H2 112.4 .
Pb3 O2 H2 113.1 .
Pb4 O2 H2 112.1 .
Pb1 O3 Pb3 109.0(7) .
Pb1 O3 Pb2 105.7(7) .
Pb3 O3 Pb2 101.3(7) .
Pb1 O3 H3 113.7 .
Pb3 O3 H3 113.1 .
Pb2 O3 H3 113.0 .
Pb3 O4 Pb4 104.6(8) .
Pb3 O4 Pb1 108.0(8) .
Pb4 O4 Pb1 101.6(8) .
Pb3 O4 H4 113.7 .
Pb4 O4 H4 113.7 .
Pb1 O4 H4 114.2 .
Pb7 O5 Pb8 110.3(9) .
Pb7 O5 Pb5 106.0(9) .
Pb8 O5 Pb5 102.9(9) .
Pb7 O5 H5 112.9 .
Pb8 O5 H5 112.2 .
Pb5 O5 H5 112.0 .
Pb7 O6 Pb6 105.1(9) .
Pb7 O6 Pb8 107.0(9) .
Pb6 O6 Pb8 106.2(9) .
Pb7 O6 H6 113.4 .
Pb6 O6 H6 112.8 .
Pb8 O6 H6 111.8 .
Pb5 O7 Pb6 110.1(9) .
Pb5 O7 Pb7 106.5(9) .
Pb6 O7 Pb7 102.8(8) .
Pb5 O7 H7 112.7 .
Pb6 O7 H7 112.7 .
Pb7 O7 H7 111.4 .
Pb5 O8 Pb6 108.1(8) .
Pb5 O8 Pb8 104.6(8) .
Pb6 O8 Pb8 102.3(7) .
Pb5 O8 H8 114.0 .
Pb6 O8 H8 113.7 .
Pb8 O8 H8 113.0 .
Pb12 O9 Pb11 109.0(7) .
Pb12 O9 Pb10 103.1(8) .
Pb11 O9 Pb10 101.8(7) .
Pb12 O9 H9 115.1 .
Pb11 O9 H9 113.0 .
Pb10 O9 H9 113.5 .
Pb11 O10 Pb12 114.1(8) .
Pb11 O10 Pb9 105.5(8) .
Pb12 O10 Pb9 103.0(8) .
Pb11 O10 H10 112.6 .
Pb12 O10 H10 110.8 .
Pb9 O10 H10 110.2 .
Pb9 O11 Pb11 107.1(9) .
Pb9 O11 Pb10 109.6(9) .
Pb11 O11 Pb10 105.3(9) .
Pb9 O11 H11 112.4 .
Pb11 O11 H11 111.4 .
Pb10 O11 H11 110.7 .
Pb10 O12 Pb9 112.1(8) .
Pb10 O12 Pb12 105.9(8) .
Pb9 O12 Pb12 103.6(8) .
Pb10 O12 H12 111.7 .
Pb9 O12 H12 111.7 .
Pb12 O12 H12 111.3 .
Pb14 O13 Pb16 106.2(8) .
Pb14 O13 Pb13 103.3(8) .
Pb16 O13 Pb13 107.2(8) .
Pb14 O13 H13 112.8 .
Pb16 O13 H13 113.1 .
Pb13 O13 H13 113.6 .
Pb14 O14 Pb15 110.6(8) .
Pb14 O14 Pb16 105.2(8) .
Pb15 O14 Pb16 104.1(7) .
Pb14 O14 H14 111.9 .
Pb15 O14 H14 111.8 .
Pb16 O14 H14 112.8 .
Pb13 O15 Pb14 104.8(8) .
Pb13 O15 Pb15 105.1(7) .
Pb14 O15 Pb15 104.4(7) .
Pb13 O15 H15 113.5 .
Pb14 O15 H15 113.9 .
Pb15 O15 H15 114.0 .
Pb16 O16 Pb13 110.3(8) .
Pb16 O16 Pb15 104.2(7) .
Pb13 O16 Pb15 104.1(7) .
Pb16 O16 H16 112.6 .
Pb13 O16 H16 112.2 .
Pb15 O16 H16 112.9 .
N2 O20 Pb7 134.7(19) .
N2 O22 Pb8 131.6(17) .
N4 O28 Pb12 125.8(19) .
N7 O35 Pb15 98.7(16) .
N8 O40 Pb6 100.8(18) .
N9 O41 Pb14 129(2) 2_564
N9 O42 Pb4 139(2) 3_454
N10 O45 Pb10 137.3(18) .
N11 O47 Pb10 135.6(18) .
N11 O48 Pb9 133.5(19) .
N12 O50 Pb13 106.6(18) .
N13 O54 Pb7 108.8(19) .
N13 O55 Pb16 106(2) .
N14 O58 Pb15 105.9(17) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.34(2) .
Pb1 O3 2.369(18) .
Pb1 O4 2.43(2) .
Pb2 O2 2.34(2) .
Pb2 O3 2.432(19) .
Pb2 O1 2.467(19) .
Pb3 O2 2.36(2) .
Pb3 O4 2.36(2) .
Pb3 O3 2.388(19) .
Pb4 O1 2.353(19) .
Pb4 O2 2.37(2) .
Pb4 O4 2.37(2) .
Pb4 O42 2.71(2) 3_546
Pb5 O8 2.31(2) .
Pb5 O7 2.33(2) .
Pb5 O5 2.48(2) .
Pb6 O7 2.34(2) .
Pb6 O6 2.36(2) .
Pb6 O8 2.42(2) .
Pb6 O40 2.73(2) .
Pb7 O5 2.29(2) .
Pb7 O6 2.33(2) .
Pb7 O7 2.43(2) .
Pb7 O20 2.59(2) .
Pb7 O54 2.73(2) .
Pb8 O5 2.32(2) .
Pb8 O6 2.37(2) .
Pb8 O8 2.44(2) .
Pb8 O22 2.72(2) .
Pb9 O11 2.32(2) .
Pb9 O12 2.34(2) .
Pb9 O10 2.44(2) .
Pb9 O48 2.63(2) .
Pb10 O12 2.30(2) .
Pb10 O11 2.40(2) .
Pb10 O9 2.45(2) .
Pb10 O47 2.70(2) .
Pb10 O45 2.70(2) .
Pb11 O10 2.28(2) .
Pb11 O11 2.35(2) .
Pb11 O9 2.414(19) .
Pb12 O10 2.329(19) .
Pb12 O9 2.337(19) .
Pb12 O12 2.40(2) .
Pb12 O28 2.68(2) .
Pb13 O15 2.34(2) .
Pb13 O16 2.372(19) .
Pb13 O13 2.42(2) .
Pb13 O50 2.690(19) .
Pb14 O14 2.306(19) .
Pb14 O13 2.35(2) .
Pb14 O15 2.382(19) .
Pb14 O41 2.66(3) 2_565
Pb15 O14 2.348(19) .
Pb15 O15 2.461(19) .
Pb15 O16 2.46(2) .
Pb15 O58 2.57(2) .
Pb15 O35 2.72(2) .
Pb16 O16 2.307(19) .
Pb16 O13 2.35(2) .
Pb16 O14 2.43(2) .
Pb16 O55 2.69(3) .
N1 O17 1.22(3) .
N1 O19 1.29(3) .
N1 O18 1.30(3) .
N2 O20 1.23(3) .
N2 O21 1.25(3) .
N2 O22 1.31(3) .
N3 O25 1.24(3) .
N3 O23 1.29(3) .
N3 O24 1.28(3) .
N4 O28 1.20(3) .
N4 O26 1.25(3) .
N4 O27 1.33(3) .
N5 O30 1.26(3) .
N5 O31 1.26(3) .
N5 O29 1.30(3) .
N6 O32 1.22(4) .
N6 O33 1.24(4) .
N6 O34 1.33(4) .
N7 O36 1.24(3) .
N7 O37 1.26(3) .
N7 O35 1.33(3) .
N8 O39 1.19(4) .
N8 O38 1.21(4) .
N8 O40 1.27(3) .
N9 O41 1.25(3) .
N9 O42 1.25(3) .
N9 O43 1.29(3) .
N10 O46 1.19(3) .
N10 O44 1.26(3) .
N10 O45 1.27(3) .
N11 O48 1.19(3) .
N11 O47 1.23(3) .
N11 O49 1.23(3) .
N12 O52 1.18(4) .
N12 O50 1.23(3) .
N12 O51 1.26(4) .
N13 O53 1.24(4) .
N13 O55 1.24(4) .
N13 O54 1.27(4) .
N14 O57 1.24(4) .
N14 O58 1.25(3) .
N14 O56 1.28(3) .
N15 O60 1.19(3) .
N15 O61 1.20(4) .
N15 O59 1.36(3) .
N16 O64 1.208(17) .
N16 O62 1.243(18) .
N16 O63 1.260(17) .
O1 H1 0.9524 .
O2 H2 0.9558 .
O3 H3 0.9568 .
O4 H4 0.9545 .
O5 H5 0.9546 .
O6 H6 0.9537 .
O7 H7 0.9556 .
O8 H8 0.9551 .
O9 H9 0.9550 .
O10 H10 0.9557 .
O11 H11 0.9537 .
O12 H12 0.9549 .
O13 H13 0.9545 .
O14 H14 0.9558 .
O15 H15 0.9524 .
O16 H16 0.9602 .
O41 Pb14 2.66(2) 2_564
O42 Pb4 2.71(2) 3_454
