#------------------------------------------------------------------------------
#$Date: 2016-04-05 21:08:15 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181743 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/72/7037271.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_7037271
loop_
_publ_author_name
'Thiele, G.'
'Donsbach, C.'
'Riedel, R.'
'Marsch, M.'
'Harms, K.'
'Dehnen, S.'
_publ_section_title
;
 Smallest molecular chalcogenidometalate anions of the heaviest metals:
 syntheses, structures, and their interconversion.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5958
_journal_page_last               5967
_journal_paper_doi               10.1039/c5dt03996g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C2 H10 K4 N2 O Pb Se4'
_chemical_formula_sum            'C2 H10 K4 N2 O Pb Se4'
_chemical_formula_weight         757.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-12 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                92.602(2)
_cell_angle_beta                 102.770(2)
_cell_angle_gamma                93.193(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0377(5)
_cell_length_b                   8.1958(5)
_cell_length_c                   12.6944(7)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.49
_cell_volume                     812.87(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34849
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.158
_diffrn_reflns_theta_min         2.493
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.333
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.2086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1606 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.2798.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.095
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+1.6923P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3464
_reflns_number_total             3613
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt03996g2.cif
_cod_data_source_block           Compound9
_cod_depositor_comments
'Adding full bibliography for 7037263--7037272.cif.'
_cod_database_code               7037271
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Others
 Uiso(H1A)=Uiso(H1B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C1(H1E,H1F), C2(H2C,H2D)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
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
Pb Pb 0.77327(2) 0.84305(2) 0.76186(2) 0.00518(4) Uani 1 1 d .
Se1 Se 0.96029(4) 0.59783(4) 0.81543(3) 0.00789(8) Uani 1 1 d .
Se2 Se 0.49367(4) 0.74571(4) 0.61903(3) 0.00779(8) Uani 1 1 d .
Se3 Se 0.94237(4) 1.07188(4) 0.68575(3) 0.00730(7) Uani 1 1 d .
Se4 Se 0.68608(4) 0.95340(4) 0.93570(3) 0.00834(8) Uani 1 1 d .
K1 K 0.98950(10) 0.24762(9) 0.93358(6) 0.01093(16) Uani 1 1 d .
K2 K 0.65941(10) 0.37293(10) 0.64391(6) 0.01213(16) Uani 1 1 d .
K3 K 0.27353(10) 0.08258(10) 0.55396(6) 0.01047(15) Uani 1 1 d .
K4 K 0.28022(9) -0.11353(10) 0.81338(6) 0.01041(15) Uani 1 1 d .
O1 O 0.4624(4) 0.1952(4) 0.7587(2) 0.0144(6) Uani 1 1 d .
N1 N 0.3925(5) 0.4985(4) 0.8534(3) 0.0153(7) Uani 1 1 d .
H1C H 0.460(6) 0.566(6) 0.832(4) 0.018 Uiso 1 1 d R
H1D H 0.288(6) 0.526(6) 0.818(4) 0.018 Uiso 1 1 d R
N2 N 0.1788(4) 0.3988(4) 0.5956(3) 0.0139(7) Uani 1 1 d .
H2A H 0.1412 0.4063 0.6581 0.017 Uiso 1 1 calc R
H2B H 0.2672 0.4748 0.5995 0.017 Uiso 1 1 calc R
C1 C 0.4159(5) 0.5289(5) 0.9711(3) 0.0143(8) Uani 1 1 d .
H1E H 0.3217 0.4704 0.9958 0.017 Uiso 1 1 calc R
H1F H 0.4124 0.6475 0.9885 0.017 Uiso 1 1 calc R
C2 C 0.0401(5) 0.4178(4) 0.5009(3) 0.0128(8) Uani 1 1 d .
H2C H -0.0505 0.3297 0.4980 0.015 Uiso 1 1 calc R
H2D H 0.0853 0.4027 0.4348 0.015 Uiso 1 1 calc R
H1A H 0.538(6) 0.160(6) 0.803(4) 0.021(9) Uiso 1 1 d .
H1B H 0.443(6) 0.266(6) 0.788(4) 0.021(9) Uiso 1 1 d .
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'
K K 0.2009 0.2494 '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'
Se Se -0.0929 2.2259 '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
Se1 Pb Se2 110.589(12) . .
Se1 Pb K1 54.701(14) . 2_767
Se1 Pb K1 110.025(14) . 1_565
Se1 Pb K2 54.045(14) . .
Se1 Pb K3 110.163(14) . 2_666
Se1 Pb K4 125.149(14) . 1_565
Se1 Pb K4 57.870(14) . 1_665
Se2 Pb K1 139.291(14) . 1_565
Se2 Pb K1 138.819(14) . 2_767
Se2 Pb K2 56.544(14) . .
Se2 Pb K3 58.785(13) . 2_666
Se2 Pb K4 56.200(14) . 1_565
Se2 Pb K4 143.810(14) . 1_665
Se3 Pb Se1 110.939(12) . .
Se3 Pb Se2 109.942(12) . .
Se3 Pb K1 56.398(14) . 1_565
Se3 Pb K1 111.208(14) . 2_767
Se3 Pb K2 127.591(14) . .
Se3 Pb K3 55.034(13) . 2_666
Se3 Pb K4 123.733(14) . 1_565
Se3 Pb K4 56.158(14) . 1_665
Se4 Pb Se1 107.019(12) . .
Se4 Pb Se2 107.961(12) . .
Se4 Pb Se3 110.308(12) . .
Se4 Pb K1 55.223(14) . 2_767
Se4 Pb K1 56.488(14) . 1_565
Se4 Pb K2 122.083(15) . .
Se4 Pb K3 142.814(14) . 2_666
Se4 Pb K4 51.815(13) . 1_565
Se4 Pb K4 108.229(14) . 1_665
K1 Pb K1 67.708(19) 1_565 2_767
K1 Pb K2 163.915(16) 1_565 .
K1 Pb K2 97.947(16) 2_767 .
K1 Pb K3 108.603(17) 1_565 2_666
K1 Pb K4 65.492(16) 1_565 1_665
K1 Pb K4 98.241(16) 2_767 1_565
K1 Pb K4 97.109(16) 1_565 1_565
K2 Pb K4 92.016(16) . 1_565
K3 Pb K1 157.373(16) 2_666 2_767
K3 Pb K2 81.690(16) 2_666 .
K3 Pb K4 104.384(16) 2_666 1_565
K4 Pb K1 66.621(16) 1_665 2_767
K4 Pb K2 102.804(16) 1_665 .
K4 Pb K3 91.280(16) 1_665 2_666
K4 Pb K4 159.91(2) 1_665 1_565
Pb Se1 K1 85.327(17) . 2_767
Pb Se1 K1 145.923(19) . .
Pb Se1 K2 86.092(17) . .
Pb Se1 K4 81.748(17) . 1_665
K1 Se1 K1 83.06(2) . 2_767
K1 Se1 K4 81.99(2) 2_767 1_665
K1 Se1 K4 127.76(2) . 1_665
K2 Se1 K1 135.50(2) . 2_767
K2 Se1 K1 80.15(2) . .
K2 Se1 K4 139.39(2) . 1_665
Pb Se2 K2 83.533(16) . .
Pb Se2 K2 143.264(19) . 2_666
Pb Se2 K3 107.124(18) . 1_565
Pb Se2 K3 81.206(16) . 2_666
Pb Se2 K4 85.306(16) . 1_565
K2 Se2 K2 86.20(2) 2_666 .
K2 Se2 K3 84.01(2) 2_666 1_565
K2 Se2 K3 100.20(2) . 2_666
K2 Se2 K3 66.07(2) 2_666 2_666
K2 Se2 K4 130.04(2) 2_666 1_565
K2 Se2 K4 118.63(2) . 1_565
K3 Se2 K2 169.17(2) 1_565 .
K3 Se2 K3 80.01(2) 1_565 2_666
K3 Se2 K4 137.00(2) 2_666 1_565
K3 Se2 K4 65.359(19) 1_565 1_565
Pb Se3 K1 83.101(17) . 1_565
Pb Se3 K2 102.489(17) . 1_565
Pb Se3 K3 135.033(18) . 1_665
Pb Se3 K3 84.874(17) . 2_666
Pb Se3 K4 83.323(17) . 1_665
K1 Se3 K2 77.57(2) 1_565 1_565
K1 Se3 K3 121.28(2) 1_565 1_665
K2 Se3 K3 118.57(2) 1_565 1_665
K3 Se3 K1 155.62(2) 2_666 1_565
K3 Se3 K2 84.47(2) 2_666 1_565
K3 Se3 K3 81.81(2) 2_666 1_665
K3 Se3 K4 119.07(2) 2_666 1_665
K4 Se3 K1 80.45(2) 1_665 1_565
K4 Se3 K2 156.34(2) 1_665 1_565
K4 Se3 K3 66.70(2) 1_665 1_665
Pb Se4 K1 83.044(17) . 1_565
Pb Se4 K1 84.899(17) . 2_767
Pb Se4 K4 160.246(18) . 2_667
Pb Se4 K4 89.839(17) . 1_565
K1 Se4 K1 84.04(2) 2_767 1_565
K1 Se4 K4 80.32(2) 2_767 2_667
K4 Se4 K1 139.90(2) 1_565 2_767
K4 Se4 K1 134.76(2) 1_565 1_565
K4 Se4 K1 82.46(2) 2_667 1_565
K4 Se4 K4 109.905(18) 1_565 2_667
Pb K1 Pb 112.293(19) 1_545 2_767
Pb K1 K1 55.479(16) 2_767 2_757
Pb K1 K1 155.80(3) 1_545 2_767
Pb K1 K1 84.12(2) 2_767 2_767
Pb K1 K1 56.814(17) 1_545 2_757
Pb K1 K2 168.27(2) 2_767 .
Pb K1 K2 70.255(17) 1_545 .
Pb K1 K4 57.258(15) 1_545 1_655
Pb K1 K4 88.472(18) 1_545 2_657
Pb K1 K4 56.012(14) 2_767 2_657
Pb K1 K4 89.072(18) 2_767 1_655
Se1 K1 Pb 118.44(2) . 1_545
Se1 K1 Pb 39.971(11) 2_767 2_767
Se1 K1 Pb 129.26(2) . 2_767
Se1 K1 Pb 137.12(2) 2_767 1_545
Se1 K1 Se1 96.94(2) . 2_767
Se1 K1 Se3 86.15(2) . 1_545
Se1 K1 Se3 176.90(3) 2_767 1_545
Se1 K1 Se4 129.57(3) . 1_545
Se1 K1 Se4 134.20(3) . 2_767
Se1 K1 Se4 98.68(2) 2_767 1_545
Se1 K1 Se4 78.125(18) 2_767 2_767
Se1 K1 K1 175.20(3) . 2_757
Se1 K1 K1 87.67(2) 2_767 2_757
Se1 K1 K1 48.360(16) 2_767 2_767
Se1 K1 K1 48.578(17) . 2_767
Se1 K1 K2 130.32(3) 2_767 .
Se1 K1 K2 49.836(16) . .
Se1 K1 K4 117.20(2) . 1_655
Se1 K1 K4 128.05(2) 2_767 1_655
Se1 K1 K4 124.34(2) . 2_657
Se1 K1 K4 49.945(16) 2_767 2_657
Se3 K1 Pb 137.24(2) 1_545 2_767
Se3 K1 Pb 40.500(11) 1_545 1_545
Se3 K1 Se4 79.493(19) 1_545 1_545
Se3 K1 K1 134.72(3) 1_545 2_767
Se3 K1 K1 89.25(2) 1_545 2_757
Se3 K1 K2 52.205(16) 1_545 .
Se3 K1 K4 128.26(2) 1_545 2_657
Se3 K1 K4 49.668(16) 1_545 1_655
Se4 K1 Pb 90.436(18) 1_545 2_767
Se4 K1 Pb 40.469(11) 1_545 1_545
Se4 K1 Pb 39.878(10) 2_767 2_767
Se4 K1 Pb 91.663(19) 2_767 1_545
Se4 K1 Se3 99.52(2) 2_767 1_545
Se4 K1 Se4 95.96(2) 2_767 1_545
Se4 K1 K1 48.065(16) 2_767 2_757
Se4 K1 K1 47.891(16) 1_545 2_757
Se4 K1 K1 111.68(3) 2_767 2_767
Se4 K1 K1 126.41(3) 1_545 2_767
Se4 K1 K2 151.25(3) 2_767 .
Se4 K1 K2 84.69(2) 1_545 .
Se4 K1 K4 49.932(16) 2_767 1_655
Se4 K1 K4 88.76(2) 1_545 1_655
Se4 K1 K4 48.770(16) 1_545 2_657
Se4 K1 K4 87.20(2) 2_767 2_657
K1 K1 K1 136.01(4) 2_767 2_757
K1 K1 K4 86.48(2) 2_767 2_657
K2 K1 K1 125.79(3) . 2_757
K2 K1 K1 90.19(3) . 2_767
K2 K1 K4 113.52(2) . 2_657
K2 K1 K4 101.46(2) . 1_655
K4 K1 K1 58.04(2) 2_657 2_757
K4 K1 K1 144.07(3) 1_655 2_767
K4 K1 K1 60.25(2) 1_655 2_757
K4 K1 K4 118.28(2) 1_655 2_657
Pb K2 K1 85.775(18) . .
Pb K2 K2 81.60(2) . 2_666
Pb K2 K3 154.50(2) . 2_656
Pb K2 H1A 112.3(9) . .
Pb K2 H1B 99.1(10) . .
Se1 K2 Pb 39.863(11) . .
Se1 K2 Se2 144.60(3) . 2_666
Se1 K2 Se2 79.79(2) . .
Se1 K2 Se3 84.76(2) . 1_545
Se1 K2 K1 50.010(16) . .
Se1 K2 K2 117.61(3) . 2_666
Se1 K2 K3 157.02(3) . .
Se1 K2 K3 126.91(2) . 2_656
Se1 K2 H1A 98.5(9) . .
Se1 K2 H1B 100.6(10) . .
Se2 K2 Pb 39.923(11) . .
Se2 K2 Pb 124.98(2) 2_666 .
Se2 K2 Se2 93.80(2) 2_666 .
Se2 K2 Se3 93.70(2) 2_666 1_545
Se2 K2 Se3 162.20(3) . 1_545
Se2 K2 K1 121.92(2) . .
Se2 K2 K1 143.67(3) 2_666 .
Se2 K2 K2 47.177(16) 2_666 2_666
Se2 K2 K2 46.625(16) . 2_666
Se2 K2 K3 58.374(18) 2_666 .
Se2 K2 K3 141.82(2) . 2_656
Se2 K2 K3 48.249(15) 2_666 2_656
Se2 K2 K3 102.99(2) . .
Se2 K2 H1A 115.4(9) 2_666 .
Se2 K2 H1A 115.5(10) . .
Se2 K2 H1B 114.6(10) 2_666 .
Se2 K2 H1B 93.2(10) . .
Se3 K2 Pb 124.07(2) 1_545 .
Se3 K2 K1 50.224(16) 1_545 .
Se3 K2 K2 138.32(3) 1_545 2_666
Se3 K2 K3 46.645(15) 1_545 2_656
Se3 K2 K3 94.69(2) 1_545 .
Se3 K2 H1A 75.4(10) 1_545 .
Se3 K2 H1B 98.3(10) 1_545 .
K1 K2 K2 167.31(3) . 2_666
K1 K2 K3 95.53(2) . 2_656
K1 K2 H1A 57.8(10) . .
K1 K2 H1B 73.1(10) . .
K2 K2 H1A 128.9(10) 2_666 .
K2 K2 H1B 110.2(10) 2_666 .
K3 K2 Pb 138.39(3) . .
K3 K2 K1 113.36(3) . .
K3 K2 K2 95.32(2) 2_656 2_666
K3 K2 K2 77.48(2) . 2_666
K3 K2 K3 63.85(2) . 2_656
K3 K2 H1A 59.4(9) . .
K3 K2 H1A 89.4(9) 2_656 .
K3 K2 H1B 56.7(10) . .
K3 K2 H1B 105.6(11) 2_656 .
O1 K2 Pb 113.00(7) . .
O1 K2 Se1 109.05(7) . .
O1 K2 Se2 105.64(7) . .
O1 K2 Se2 106.22(6) . 2_666
O1 K2 Se3 87.67(6) . 1_545
O1 K2 K1 72.58(6) . .
O1 K2 K2 113.68(7) . 2_666
O1 K2 K3 48.04(6) . .
O1 K2 K3 91.51(7) . 2_656
O1 K2 H1A 15.3(10) . .
O1 K2 H1B 14.2(10) . .
H1A K2 H1B 22.9(13) . .
Pb K3 K3 70.104(19) 2_666 2_656
Pb K3 K3 82.81(2) 2_666 2_556
Se2 K3 Pb 40.008(10) 2_666 2_666
Se2 K3 Pb 109.98(2) 1_545 2_666
Se2 K3 Se2 99.99(2) 1_545 2_666
Se2 K3 Se3 107.12(2) 1_545 1_445
Se2 K3 K2 55.556(18) 2_666 .
Se2 K3 K2 93.86(2) 1_545 .
Se2 K3 K3 50.812(17) 1_545 2_656
Se2 K3 K3 122.44(3) 2_666 2_556
Se2 K3 K3 49.174(16) 2_666 2_656
Se2 K3 K3 107.43(3) 1_545 2_556
Se2 K3 K4 147.64(3) 2_666 .
Se2 K3 K4 58.550(18) 1_545 .
Se2 K3 C2 176.58(7) 1_545 .
Se3 K3 Pb 125.07(2) 1_445 2_666
Se3 K3 Pb 40.092(11) 2_666 2_666
Se3 K3 Se2 152.88(3) 1_445 2_666
Se3 K3 Se2 77.935(19) 2_666 2_666
Se3 K3 Se2 95.40(2) 2_666 1_545
Se3 K3 Se3 98.19(2) 2_666 1_445
Se3 K3 K2 133.48(3) 2_666 .
Se3 K3 K2 122.13(3) 1_445 .
Se3 K3 K3 50.403(16) 2_666 2_556
Se3 K3 K3 47.784(16) 1_445 2_556
Se3 K3 K3 157.91(3) 1_445 2_656
Se3 K3 K3 84.71(2) 2_666 2_656
Se3 K3 K4 124.46(3) 2_666 .
Se3 K3 K4 55.129(17) 1_445 .
Se3 K3 C2 86.04(6) 2_666 .
K2 K3 Pb 94.22(2) . 2_666
K2 K3 K3 66.84(2) . 2_656
K2 K3 K3 158.25(3) . 2_556
K3 K3 K3 130.72(4) 2_656 2_556
K4 K3 Pb 162.92(3) . 2_666
K4 K3 K2 98.99(2) . .
K4 K3 K3 88.76(3) . 2_556
K4 K3 K3 105.30(3) . 2_656
O1 K3 Pb 141.65(7) . 2_666
O1 K3 Se2 81.35(6) . 1_545
O1 K3 Se2 103.06(6) . 2_666
O1 K3 Se3 82.36(6) . 1_445
O1 K3 Se3 176.71(7) . 2_666
O1 K3 K2 47.69(6) . .
O1 K3 K3 130.05(7) . 2_556
O1 K3 K3 93.57(7) . 2_656
O1 K3 K4 53.31(6) . .
O1 K3 N2 72.43(9) . .
O1 K3 C2 97.18(9) . .
N2 K3 Pb 91.76(7) . 2_666
N2 K3 Se2 153.76(7) . 1_545
N2 K3 Se2 87.13(7) . 2_666
N2 K3 Se3 68.96(7) . 1_445
N2 K3 Se3 110.81(7) . 2_666
N2 K3 K2 69.29(7) . .
N2 K3 K3 130.52(7) . 2_656
N2 K3 K3 89.22(7) . 2_556
N2 K3 K4 102.99(7) . .
N2 K3 C2 24.84(9) . .
C2 K3 Pb 73.08(6) . 2_666
C2 K3 Se2 83.34(7) . 2_666
C2 K3 Se3 69.58(7) . 1_445
C2 K3 K2 87.36(7) . .
C2 K3 K3 132.50(7) . 2_656
C2 K3 K3 71.13(7) . 2_556
C2 K3 K4 118.12(7) . .
Pb K4 Pb 159.90(2) 1_445 1_545
Pb K4 K1 138.92(2) 1_545 1_455
Pb K4 K1 57.250(14) 1_445 1_455
Pb K4 K1 135.79(2) 1_545 2_657
Pb K4 K1 57.368(14) 1_445 2_657
Pb K4 H1A 134.6(10) 1_445 .
Pb K4 H1A 53.1(10) 1_545 .
Se1 K4 Pb 40.381(10) 1_445 1_445
Se1 K4 Pb 131.07(2) 1_445 1_545
Se1 K4 Se2 106.44(2) 1_445 1_545
Se1 K4 K1 48.069(15) 1_445 2_657
Se1 K4 K1 89.20(2) 1_445 1_455
Se1 K4 K3 117.04(2) 1_445 .
Se1 K4 H1A 174.9(10) 1_445 .
Se2 K4 Pb 38.494(9) 1_545 1_545
Se2 K4 Pb 121.45(2) 1_545 1_445
Se2 K4 K1 150.46(3) 1_545 1_455
Se2 K4 K1 146.19(3) 1_545 2_657
Se2 K4 K3 56.090(18) 1_545 .
Se2 K4 H1A 75.3(9) 1_545 .
Se3 K4 Pb 40.518(10) 1_445 1_445
Se3 K4 Pb 133.52(2) 1_445 1_545
Se3 K4 Se1 79.165(18) 1_445 1_445
Se3 K4 Se2 107.63(2) 1_445 1_545
Se3 K4 Se4 99.55(2) 1_445 2_667
Se3 K4 K1 49.882(16) 1_445 1_455
Se3 K4 K1 90.47(2) 1_445 2_657
Se3 K4 K3 58.173(18) 1_445 .
Se3 K4 N1 137.60(7) 1_445 1_545
Se3 K4 H1A 95.7(10) 1_445 .
Se4 K4 Pb 91.524(18) 2_667 1_445
Se4 K4 Pb 161.42(3) 1_545 1_445
Se4 K4 Pb 38.346(11) 1_545 1_545
Se4 K4 Pb 108.440(19) 2_667 1_545
Se4 K4 Se1 96.81(2) 2_667 1_445
Se4 K4 Se1 136.40(3) 1_545 1_445
Se4 K4 Se2 76.809(18) 1_545 1_545
Se4 K4 Se2 146.88(2) 2_667 1_545
Se4 K4 Se3 142.67(3) 1_545 1_445
Se4 K4 Se4 70.096(18) 1_545 2_667
Se4 K4 K1 48.774(16) 2_667 2_657
Se4 K4 K1 106.02(2) 1_545 2_657
Se4 K4 K1 109.14(2) 1_545 1_455
Se4 K4 K1 49.749(15) 2_667 1_455
Se4 K4 K3 131.42(3) 2_667 .
Se4 K4 K3 100.99(2) 1_545 .
Se4 K4 N1 103.12(6) 2_667 1_545
Se4 K4 N1 79.27(6) 1_545 1_545
Se4 K4 H1A 83.6(9) 2_667 .
Se4 K4 H1A 48.5(10) 1_545 .
K1 K4 K1 61.72(2) 1_455 2_657
K1 K4 H1A 132.3(9) 2_657 .
K1 K4 H1A 87.2(10) 1_455 .
K3 K4 Pb 75.564(18) . 1_545
K3 K4 Pb 93.16(2) . 1_445
K3 K4 K1 148.62(3) . 2_657
K3 K4 K1 94.57(2) . 1_455
K3 K4 H1A 59.7(10) . .
O1 K4 Pb 120.69(6) . 1_445
O1 K4 Pb 63.32(6) . 1_545
O1 K4 Se1 159.81(6) . 1_445
O1 K4 Se2 76.54(6) . 1_545
O1 K4 Se3 80.92(6) . 1_445
O1 K4 Se4 63.76(6) . 1_545
O1 K4 Se4 89.74(6) . 2_667
O1 K4 K1 135.71(6) . 2_657
O1 K4 K1 80.48(6) . 1_455
O1 K4 K3 47.48(6) . .
O1 K4 N1 133.93(9) . 1_545
O1 K4 H1A 15.3(10) . .
N1 K4 Pb 70.66(6) 1_545 1_545
N1 K4 Pb 103.24(6) 1_545 1_445
N1 K4 Se1 63.02(6) 1_545 1_445
N1 K4 Se2 68.69(6) 1_545 1_545
N1 K4 K1 140.33(6) 1_545 1_455
N1 K4 K1 78.63(6) 1_545 2_657
N1 K4 K3 122.56(6) 1_545 .
N1 K4 H1A 121.9(10) 1_545 .
K2 O1 K3 84.26(8) . .
K2 O1 K4 154.37(12) . .
K2 O1 H1A 99(4) . .
K2 O1 H1B 94(4) . .
K3 O1 K4 79.21(8) . .
K3 O1 H1A 134(3) . .
K3 O1 H1B 123(4) . .
K4 O1 H1A 79(4) . .
K4 O1 H1B 111(4) . .
H1A O1 H1B 102(5) . .
K4 N1 H1C 61(3) 1_565 .
K4 N1 H1D 55(3) 1_565 .
H1C N1 H1D 103(4) . .
C1 N1 K4 90.6(2) . 1_565
C1 N1 H1C 108(3) . .
C1 N1 H1D 111(3) . .
K3 N2 H2A 111.4 . .
K3 N2 H2B 111.4 . .
H2A N2 H2B 109.2 . .
C2 N2 K3 101.9(2) . .
C2 N2 H2A 111.4 . .
C2 N2 H2B 111.4 . .
N1 C1 C1 110.3(4) . 2_667
N1 C1 H1E 109.6 . .
N1 C1 H1F 109.6 . .
C1 C1 H1E 109.6 2_667 .
C1 C1 H1F 109.6 2_667 .
H1E C1 H1F 108.1 . .
K3 C2 H2C 78.1 . .
K3 C2 H2D 77.8 . .
N2 C2 K3 53.24(17) . .
N2 C2 C2 114.9(4) . 2_566
N2 C2 H2C 108.6 . .
N2 C2 H2D 108.6 . .
C2 C2 K3 168.1(3) 2_566 .
C2 C2 H2C 108.6 2_566 .
C2 C2 H2D 108.6 2_566 .
H2C C2 H2D 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb Se1 2.6019(4) .
Pb Se2 2.6157(4) .
Pb Se3 2.5999(4) .
Pb Se4 2.5985(4) .
Pb K1 4.0368(8) 2_767
Pb K1 3.9741(8) 1_565
Pb K2 4.0500(8) .
Pb K3 4.0208(8) 2_666
Pb K4 3.9745(8) 1_665
Pb K4 4.1883(8) 1_565
Se1 K1 3.2945(9) .
Se1 K1 3.3056(8) 2_767
Se1 K2 3.2860(9) .
Se1 K4 3.4010(8) 1_665
Se2 K2 3.4006(9) .
Se2 K2 3.3701(9) 2_666
Se2 K3 3.3972(9) 1_565
Se2 K3 3.4796(9) 2_666
Se2 K4 3.4921(9) 1_565
Se3 K1 3.3342(8) 1_565
Se3 K2 3.4282(9) 1_565
Se3 K3 3.3083(8) 2_666
Se3 K3 3.4420(8) 1_665
Se3 K4 3.3237(8) 1_665
Se4 K1 3.3289(8) 2_767
Se4 K1 3.3381(9) 1_565
Se4 K4 3.2921(8) 1_565
Se4 K4 3.3379(9) 2_667
K1 Pb 3.9742(8) 1_545
K1 Pb 4.0368(8) 2_767
K1 Se1 3.3056(8) 2_767
K1 Se3 3.3342(8) 1_545
K1 Se4 3.3289(8) 2_767
K1 Se4 3.3381(9) 1_545
K1 K1 4.3760(16) 2_767
K1 K1 4.4630(16) 2_757
K1 K2 4.2366(11) .
K1 K4 4.2996(11) 1_655
K1 K4 4.3999(11) 2_657
K2 Se2 3.3701(9) 2_666
K2 Se3 3.4281(9) 1_545
K2 K2 4.6262(16) 2_666
K2 K3 4.5287(11) 2_656
K2 K3 3.7352(11) .
K2 O1 2.776(3) .
K2 H1A 3.01(5) .
K2 H1B 2.92(5) .
K3 Pb 4.0208(8) 2_666
K3 Se2 3.3972(9) 1_545
K3 Se2 3.4797(8) 2_666
K3 Se3 3.4420(8) 1_445
K3 Se3 3.3083(8) 2_666
K3 K3 4.4214(15) 2_556
K3 K3 4.4214(15) 2_656
K3 K4 3.7207(11) .
K3 O1 2.792(3) .
K3 N2 2.801(3) .
K3 C2 3.421(4) .
K4 Pb 4.1883(8) 1_545
K4 Pb 3.9745(8) 1_445
K4 Se1 3.4010(8) 1_445
K4 Se2 3.4921(9) 1_545
K4 Se3 3.3237(8) 1_445
K4 Se4 3.2921(8) 1_545
K4 Se4 3.3379(9) 2_667
K4 K1 4.3999(11) 2_657
K4 K1 4.2995(11) 1_455
K4 O1 3.037(3) .
K4 N1 3.383(4) 1_545
K4 H1A 2.99(5) .
O1 H1A 0.80(5) .
O1 H1B 0.72(5) .
N1 K4 3.383(4) 1_565
N1 H1C 0.84(5) .
N1 H1D 0.91(5) .
N1 C1 1.471(5) .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
N2 C2 1.469(5) .
C1 C1 1.502(7) 2_667
C1 H1E 0.9900 .
C1 H1F 0.9900 .
C2 C2 1.525(7) 2_566
C2 H2C 0.9900 .
C2 H2D 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
K3 N2 C2 C2 -179.7(4) . 2_566
K4 N1 C1 C1 -131.6(4) 1_565 2_667
