#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/97/4109747.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_4109747
loop_
_publ_author_name
'Zhong-Ming Sun'
'Hai Xiao'
'Jun Li'
'Lai-Sheng Wang'
_publ_section_title
;
 Pd2@Sn184-: Fusion of Two Endohedral Stannaspherenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9560
_journal_page_last               9561
_journal_paper_doi               10.1021/ja0728674
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C78 H168 K4 N14 O24 Pd2 Sn18'
_chemical_formula_weight         4191.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.71(3)
_cell_angle_beta                 98.62(3)
_cell_angle_gamma                100.53(3)
_cell_formula_units_Z            1
_cell_length_a                   14.913(3)
_cell_length_b                   15.930(3)
_cell_length_c                   16.270(3)
_cell_measurement_reflns_used    621
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      39.00
_cell_measurement_theta_min      3.12
_cell_volume                     3307.3(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Brucker Proteum Diffractometer'
_diffrn_measurement_method       'narrow frame method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10371
_diffrn_reflns_theta_full        39.00
_diffrn_reflns_theta_max         39.00
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    30.225
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            gray
_exptl_crystal_density_diffrn    2.105
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             1994
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         3605
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0752P)²+22.6913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                2803
_reflns_number_total             3605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0728674si20070424_060610.cif
_cod_data_source_block           1
_cod_original_cell_volume        3307.3(12)
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               4109747
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.59591(12) 1.00948(12) 0.57873(12) 0.0432(6) Uani 1 1 d .
Sn1 Sn 0.58739(12) 1.17957(11) 0.74166(11) 0.0531(6) Uani 1 1 d .
Sn2 Sn 0.26298(12) 0.96286(12) 0.52023(12) 0.0566(6) Uani 1 1 d .
Sn3 Sn 0.44040(12) 0.98512(12) 0.66238(12) 0.0565(6) Uani 1 1 d .
Sn4 Sn 0.55100(13) 0.82948(11) 0.58306(12) 0.0554(6) Uani 1 1 d .
Sn5 Sn 0.41210(12) 1.15758(12) 0.59625(12) 0.0553(6) Uani 1 1 d .
Sn6 Sn 0.62155(12) 1.18144(12) 0.55641(12) 0.0552(6) Uani 1 1 d .
Sn7 Sn 0.77569(12) 1.14879(12) 0.69697(12) 0.0608(7) Uani 1 1 d .
Sn8 Sn 0.75388(12) 0.93384(12) 0.60264(13) 0.0587(7) Uani 1 1 d .
Sn9 Sn 0.66112(13) 1.02091(12) 0.76165(12) 0.0605(7) Uani 1 1 d .
K1 K -0.1642(4) 0.4320(3) 0.2888(3) 0.0461(16) Uani 1 1 d .
K2 K -0.2430(4) 0.6999(3) -0.0525(3) 0.0455(16) Uani 1 1 d .
N1 N -0.145(2) 0.6218(17) 0.284(2) 0.071(7) Uani 1 1 d .
N2 N -0.174(2) 0.2445(15) 0.297(2) 0.072(8) Uani 1 1 d .
N3 N -0.376(2) 0.5220(18) -0.2212(19) 0.077(8) Uani 1 1 d .
N4 N -0.1130(19) 0.8764(17) 0.1151(15) 0.064(7) Uani 1 1 d .
N5 N 0.0048(19) 0.9240(19) 0.554(2) 0.144(11) Uani 1 1 d D
H5C H -0.0131 0.8689 0.5031 0.173 Uiso 1 1 calc R
H5D H 0.0180 0.9263 0.6080 0.173 Uiso 1 1 calc R
N6 N -0.490(3) 0.798(3) -0.172(3) 0.30(3) Uani 1 1 d .
H6C H -0.5484 0.7729 -0.1782 0.359 Uiso 1 1 calc R
H6D H -0.4675 0.7808 -0.2208 0.359 Uiso 1 1 calc R
N7 N -0.430(3) 0.932(3) 0.064(3) 0.205(17) Uani 1 1 d .
H7C H -0.3713 0.9511 0.0678 0.246 Uiso 1 1 calc R
H7D H -0.4492 0.9484 0.1149 0.246 Uiso 1 1 calc R
O1 O 0.0162(14) 0.5723(16) 0.3683(12) 0.072(7) Uani 1 1 d .
O2 O 0.0061(15) 0.387(2) 0.3415(14) 0.078(6) Uani 1 1 d .
O3 O -0.2002(13) 0.4303(17) 0.1062(12) 0.063(5) Uani 1 1 d .
O4 O -0.2436(13) 0.2558(14) 0.1199(14) 0.075(6) Uani 1 1 d .
O5 O -0.2790(15) 0.5508(17) 0.3742(13) 0.083(6) Uani 1 1 d .
O6 O -0.2687(11) 0.3936(15) 0.4088(12) 0.062(5) Uani 1 1 d .
O7 O -0.3016(15) 0.7049(16) -0.2242(13) 0.067(5) Uani 1 1 d .
O8 O -0.1563(14) 0.8603(15) -0.0764(18) 0.077(6) Uani 1 1 d .
O9 O -0.1778(15) 0.5358(13) -0.1398(13) 0.058(5) Uani 1 1 d .
O10 O -0.0662(13) 0.6915(16) 0.0341(14) 0.067(6) Uani 1 1 d .
O11 O -0.4168(13) 0.6000(16) -0.0326(18) 0.070(5) Uani 1 1 d .
O12 O -0.3023(17) 0.7841(17) 0.1146(14) 0.067(6) Uani 1 1 d .
C1 C -0.159(2) 0.598(3) 0.183(3) 0.078(10) Uani 1 1 d .
H1A H -0.1718 0.6524 0.1773 0.093 Uiso 1 1 calc R
H1B H -0.0993 0.5915 0.1676 0.093 Uiso 1 1 calc R
C2 C -0.231(2) 0.512(3) 0.114(2) 0.081(11) Uani 1 1 d .
H2A H -0.2894 0.5106 0.1333 0.097 Uiso 1 1 calc R
H2B H -0.2416 0.5122 0.0539 0.097 Uiso 1 1 calc R
C3 C -0.269(2) 0.342(3) 0.034(2) 0.080(10) Uani 1 1 d .
H3A H -0.2722 0.3391 -0.0271 0.096 Uiso 1 1 calc R
H3B H -0.3303 0.3409 0.0465 0.096 Uiso 1 1 calc R
C4 C -0.239(2) 0.260(2) 0.035(2) 0.081(10) Uani 1 1 d .
H4A H -0.2798 0.2007 -0.0181 0.098 Uiso 1 1 calc R
H4B H -0.1751 0.2658 0.0289 0.098 Uiso 1 1 calc R
C5 C -0.227(2) 0.170(2) 0.118(3) 0.103(12) Uani 1 1 d .
H5A H -0.1627 0.1695 0.1142 0.124 Uiso 1 1 calc R
H5B H -0.2698 0.1137 0.0627 0.124 Uiso 1 1 calc R
C6 C -0.243(2) 0.168(2) 0.209(3) 0.105(12) Uani 1 1 d .
H6A H -0.3056 0.1741 0.2141 0.126 Uiso 1 1 calc R
H6B H -0.2404 0.1054 0.2037 0.126 Uiso 1 1 calc R
C7 C -0.051(4) 0.686(2) 0.346(2) 0.099(13) Uani 1 1 d .
H7A H -0.0360 0.7384 0.3303 0.119 Uiso 1 1 calc R
H7B H -0.0563 0.7145 0.4102 0.119 Uiso 1 1 calc R
C8 C 0.029(2) 0.644(3) 0.342(2) 0.084(12) Uani 1 1 d .
H8A H 0.0369 0.6177 0.2787 0.101 Uiso 1 1 calc R
H8B H 0.0857 0.6952 0.3843 0.101 Uiso 1 1 calc R
C9 C 0.096(2) 0.533(3) 0.360(3) 0.105(14) Uani 1 1 d .
H9A H 0.1549 0.5840 0.3970 0.126 Uiso 1 1 calc R
H9B H 0.0988 0.5005 0.2949 0.126 Uiso 1 1 calc R
C10 C 0.081(3) 0.462(3) 0.398(3) 0.091(11) Uani 1 1 d .
H10A H 0.1367 0.4394 0.4035 0.109 Uiso 1 1 calc R
H10B H 0.0712 0.4942 0.4610 0.109 Uiso 1 1 calc R
C11 C -0.005(2) 0.317(3) 0.374(2) 0.085(10) Uani 1 1 d .
H11A H -0.0189 0.3447 0.4345 0.102 Uiso 1 1 calc R
H11B H 0.0544 0.3006 0.3819 0.102 Uiso 1 1 calc R
C12 C -0.082(3) 0.226(2) 0.306(3) 0.098(12) Uani 1 1 d .
H12A H -0.0688 0.2000 0.2443 0.117 Uiso 1 1 calc R
H12B H -0.0826 0.1784 0.3276 0.117 Uiso 1 1 calc R
C13 C -0.223(3) 0.662(2) 0.321(3) 0.099(12) Uani 1 1 d .
H13A H -0.2811 0.6286 0.2708 0.119 Uiso 1 1 calc R
H13B H -0.2083 0.7298 0.3378 0.119 Uiso 1 1 calc R
C14 C -0.241(3) 0.652(3) 0.406(2) 0.108(13) Uani 1 1 d .
H14A H -0.1830 0.6774 0.4556 0.129 Uiso 1 1 calc R
H14B H -0.2859 0.6868 0.4317 0.129 Uiso 1 1 calc R
C15 C -0.318(2) 0.537(2) 0.444(2) 0.093(11) Uani 1 1 d .
H15A H -0.3734 0.5609 0.4492 0.112 Uiso 1 1 calc R
H15B H -0.2722 0.5730 0.5049 0.112 Uiso 1 1 calc R
C16 C -0.345(2) 0.433(2) 0.418(2) 0.077(9) Uiso 1 1 d .
H16A H -0.3715 0.4247 0.4657 0.093 Uiso 1 1 calc R
H16B H -0.3933 0.3976 0.3585 0.093 Uiso 1 1 calc R
C17 C -0.292(3) 0.297(3) 0.393(2) 0.104(12) Uani 1 1 d .
H17A H -0.3443 0.2578 0.3372 0.125 Uiso 1 1 calc R
H17B H -0.3119 0.2949 0.4463 0.125 Uiso 1 1 calc R
C18 C -0.211(3) 0.256(2) 0.380(3) 0.103(13) Uani 1 1 d .
H18A H -0.2285 0.1926 0.3765 0.123 Uiso 1 1 calc R
H18B H -0.1593 0.2966 0.4362 0.123 Uiso 1 1 calc R
C19 C 0.013(3) 1.015(2) 0.547(2) 0.163(18) Uiso 1 1 d D
H19A H -0.0291 1.0504 0.5786 0.195 Uiso 1 1 calc R
H19B H 0.0771 1.0571 0.5749 0.195 Uiso 1 1 calc R
C21 C -0.415(3) 0.550(3) -0.288(2) 0.105(13) Uani 1 1 d .
H21A H -0.4631 0.5807 -0.2649 0.126 Uiso 1 1 calc R
H21B H -0.4470 0.4913 -0.3466 0.126 Uiso 1 1 calc R
C22 C -0.354(3) 0.614(3) -0.311(2) 0.089(11) Uani 1 1 d .
H22A H -0.3924 0.6293 -0.3540 0.107 Uiso 1 1 calc R
H22B H -0.3106 0.5824 -0.3422 0.107 Uiso 1 1 calc R
C23 C -0.232(3) 0.768(3) -0.241(2) 0.098(12) Uani 1 1 d .
H23A H -0.2598 0.7728 -0.2965 0.118 Uiso 1 1 calc R
H23B H -0.1786 0.7421 -0.2526 0.118 Uiso 1 1 calc R
C24 C -0.201(3) 0.866(3) -0.157(3) 0.114(13) Uani 1 1 d .
H24A H -0.1571 0.9100 -0.1680 0.137 Uiso 1 1 calc R
H24B H -0.2550 0.8903 -0.1450 0.137 Uiso 1 1 calc R
C25 C -0.141(2) 0.952(3) 0.006(3) 0.102(11) Uani 1 1 d .
H25A H -0.1990 0.9589 0.0238 0.122 Uiso 1 1 calc R
H25B H -0.1156 1.0051 -0.0063 0.122 Uiso 1 1 calc R
C26 C -0.068(2) 0.951(2) 0.084(3) 0.106(12) Uani 1 1 d .
H26A H -0.0458 1.0155 0.1385 0.127 Uiso 1 1 calc R
H26B H -0.0140 0.9346 0.0612 0.127 Uiso 1 1 calc R
C27 C -0.453(2) 0.471(2) -0.193(2) 0.092(11) Uani 1 1 d .
H27A H -0.5044 0.4279 -0.2481 0.111 Uiso 1 1 calc R
H27B H -0.4274 0.4323 -0.1680 0.111 Uiso 1 1 calc R
C28 C -0.488(2) 0.541(2) -0.121(3) 0.104(12) Uani 1 1 d .
H28A H -0.5081 0.5832 -0.1445 0.125 Uiso 1 1 calc R
H28B H -0.5419 0.5068 -0.1113 0.125 Uiso 1 1 calc R
C29 C -0.448(2) 0.664(2) 0.044(2) 0.072(10) Uani 1 1 d .
H29A H -0.4969 0.6259 0.0566 0.087 Uiso 1 1 calc R
H29B H -0.4761 0.7051 0.0241 0.087 Uiso 1 1 calc R
C30 C -0.373(3) 0.726(3) 0.130(2) 0.081(10) Uani 1 1 d .
H30A H -0.3984 0.7662 0.1794 0.097 Uiso 1 1 calc R
H30B H -0.3454 0.6852 0.1513 0.097 Uiso 1 1 calc R
C31 C -0.236(3) 0.855(3) 0.197(2) 0.076(10) Uani 1 1 d .
H31A H -0.2036 0.8247 0.2272 0.091 Uiso 1 1 calc R
H31B H -0.2692 0.8935 0.2403 0.091 Uiso 1 1 calc R
C32 C -0.167(3) 0.9201(18) 0.181(2) 0.072(11) Uani 1 1 d .
H32A H -0.2001 0.9564 0.1584 0.086 Uiso 1 1 calc R
H32B H -0.1231 0.9665 0.2412 0.086 Uiso 1 1 calc R
C33 C -0.322(2) 0.458(2) -0.265(2) 0.068(9) Uani 1 1 d .
H33A H -0.2899 0.4804 -0.3024 0.081 Uiso 1 1 calc R
H33B H -0.3650 0.3939 -0.3081 0.081 Uiso 1 1 calc R
C34 C -0.250(2) 0.4474(18) -0.198(2) 0.054(9) Uani 1 1 d .
H34A H -0.2808 0.4274 -0.1584 0.065 Uiso 1 1 calc R
H34B H -0.2218 0.3973 -0.2334 0.065 Uiso 1 1 calc R
C35 C -0.104(2) 0.525(2) -0.084(2) 0.063(8) Uani 1 1 d .
H35A H -0.0772 0.4756 -0.1238 0.076 Uiso 1 1 calc R
H35B H -0.1269 0.5053 -0.0407 0.076 Uiso 1 1 calc R
C36 C -0.028(2) 0.623(3) -0.029(2) 0.072(9) Uani 1 1 d .
H36A H 0.0264 0.6160 0.0061 0.087 Uiso 1 1 calc R
H36B H -0.0079 0.6441 -0.0723 0.087 Uiso 1 1 calc R
C37 C 0.003(2) 0.782(3) 0.090(2) 0.086(10) Uani 1 1 d .
H37A H 0.0227 0.8085 0.0504 0.103 Uiso 1 1 calc R
H37B H 0.0575 0.7728 0.1225 0.103 Uiso 1 1 calc R
C38 C -0.039(2) 0.850(2) 0.162(2) 0.106(12) Uani 1 1 d .
H38A H -0.0662 0.8194 0.1958 0.127 Uiso 1 1 calc R
H38B H 0.0099 0.9085 0.2069 0.127 Uiso 1 1 calc R
C39 C -0.494(3) 0.875(4) -0.022(4) 0.24(4) Uani 1 1 d D
H39B H -0.5406 0.9063 -0.0341 0.292 Uiso 1 1 calc R
H39A H -0.5249 0.8118 -0.0307 0.292 Uiso 1 1 calc R
C40 C -0.429(5) 0.870(7) -0.078(4) 0.43(8) Uani 1 1 d D
H40A H -0.3767 0.8479 -0.0596 0.517 Uiso 1 1 calc R
H40B H -0.4039 0.9321 -0.0760 0.517 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn 0.0259 5.4591 '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
Sn4 Pd1 Sn6 173.29(8) . .
Sn4 Pd1 Sn8 64.67(7) . .
Sn6 Pd1 Sn8 120.21(8) . .
Sn4 Pd1 Sn1 116.97(8) . .
Sn6 Pd1 Sn1 65.92(6) . .
Sn8 Pd1 Sn1 116.51(8) . .
Sn4 Pd1 Sn7 117.78(8) . .
Sn6 Pd1 Sn7 68.88(7) . .
Sn8 Pd1 Sn7 62.79(6) . .
Sn1 Pd1 Sn7 64.16(7) . .
Sn4 Pd1 Sn5 65.94(6) . 2_676
Sn6 Pd1 Sn5 110.56(8) . 2_676
Sn8 Pd1 Sn5 69.65(7) . 2_676
Sn1 Pd1 Sn5 173.75(9) . 2_676
Sn7 Pd1 Sn5 120.09(9) . 2_676
Sn4 Pd1 Sn9 64.65(7) . .
Sn6 Pd1 Sn9 121.20(8) . .
Sn8 Pd1 Sn9 63.16(7) . .
Sn1 Pd1 Sn9 63.55(6) . .
Sn7 Pd1 Sn9 63.45(7) . .
Sn5 Pd1 Sn9 122.04(8) 2_676 .
Sn4 Pd1 Sn3 66.11(7) . .
Sn6 Pd1 Sn3 111.99(8) . .
Sn8 Pd1 Sn3 121.46(8) . .
Sn1 Pd1 Sn3 63.29(7) . .
Sn7 Pd1 Sn3 119.87(8) . .
Sn5 Pd1 Sn3 115.08(8) 2_676 .
Sn9 Pd1 Sn3 68.46(7) . .
Sn4 Pd1 Sn2 117.36(8) . 2_676
Sn6 Pd1 Sn2 63.87(7) . 2_676
Sn8 Pd1 Sn2 64.64(7) . 2_676
Sn1 Pd1 Sn2 117.16(8) . 2_676
Sn7 Pd1 Sn2 64.21(7) . 2_676
Sn5 Pd1 Sn2 63.71(7) 2_676 2_676
Sn9 Pd1 Sn2 117.87(8) . 2_676
Sn3 Pd1 Sn2 173.46(8) . 2_676
Pd1 Sn1 Sn3 58.57(6) . .
Pd1 Sn1 Sn9 58.37(6) . .
Sn3 Sn1 Sn9 64.85(6) . .
Pd1 Sn1 Sn7 57.94(7) . .
Sn3 Sn1 Sn7 110.33(7) . .
Sn9 Sn1 Sn7 59.68(6) . .
Pd1 Sn1 Sn5 80.88(7) . .
Sn3 Sn1 Sn5 67.69(7) . .
Sn9 Sn1 Sn5 128.64(7) . .
Sn7 Sn1 Sn5 124.47(7) . .
Pd1 Sn1 Sn6 56.84(6) . .
Sn3 Sn1 Sn6 101.73(7) . .
Sn9 Sn1 Sn6 108.86(7) . .
Sn7 Sn1 Sn6 63.39(6) . .
Sn5 Sn1 Sn6 63.16(6) . .
Pd1 Sn2 Sn6 57.51(6) 2_676 2_676
Pd1 Sn2 Sn5 57.88(6) 2_676 .
Sn6 Sn2 Sn5 101.50(7) 2_676 .
Pd1 Sn2 Sn7 57.58(7) 2_676 2_676
Sn6 Sn2 Sn7 64.11(6) 2_676 2_676
Sn5 Sn2 Sn7 109.25(8) . 2_676
Pd1 Sn2 Sn3 81.31(7) 2_676 .
Sn6 Sn2 Sn3 63.40(6) 2_676 .
Sn5 Sn2 Sn3 67.50(7) . .
Sn7 Sn2 Sn3 125.12(8) 2_676 .
Pd1 Sn2 Sn8 57.18(6) 2_676 2_676
Sn6 Sn2 Sn8 108.26(7) 2_676 2_676
Sn5 Sn2 Sn8 64.72(6) . 2_676
Sn7 Sn2 Sn8 58.21(6) 2_676 2_676
Sn3 Sn2 Sn8 128.27(8) . 2_676
Pd1 Sn3 Sn1 58.15(6) . .
Pd1 Sn3 Sn2 105.09(7) . .
Sn1 Sn3 Sn2 112.88(8) . .
Pd1 Sn3 Sn4 56.17(6) . .
Sn1 Sn3 Sn4 104.78(7) . .
Sn2 Sn3 Sn4 115.67(7) . .
Pd1 Sn3 Sn6 71.78(7) . 2_676
Sn1 Sn3 Sn6 124.85(8) . 2_676
Sn2 Sn3 Sn6 57.86(6) . 2_676
Sn4 Sn3 Sn6 57.87(6) . 2_676
Pd1 Sn3 Sn9 55.71(6) . .
Sn1 Sn3 Sn9 57.71(6) . .
Sn2 Sn3 Sn9 160.72(8) . .
Sn4 Sn3 Sn9 57.37(6) . .
Sn6 Sn3 Sn9 111.56(8) 2_676 .
Pd1 Sn4 Sn8 58.10(6) . .
Pd1 Sn4 Sn9 58.42(6) . .
Sn8 Sn4 Sn9 59.05(7) . .
Pd1 Sn4 Sn6 74.73(7) . 2_676
Sn8 Sn4 Sn6 122.57(8) . 2_676
Sn9 Sn4 Sn6 121.43(8) . 2_676
Pd1 Sn4 Sn5 57.69(6) . 2_676
Sn8 Sn4 Sn5 64.33(7) . 2_676
Sn9 Sn4 Sn5 109.58(7) . 2_676
Sn6 Sn4 Sn5 63.45(6) 2_676 2_676
Pd1 Sn4 Sn3 57.73(6) . .
Sn8 Sn4 Sn3 108.76(7) . .
Sn9 Sn4 Sn3 63.35(6) . .
Sn6 Sn4 Sn3 62.59(6) 2_676 .
Sn5 Sn4 Sn3 102.63(7) 2_676 .
Pd1 Sn5 Sn2 58.41(7) 2_676 .
Pd1 Sn5 Sn1 105.32(8) 2_676 .
Sn2 Sn5 Sn1 111.91(8) . .
Pd1 Sn5 Sn4 56.37(6) 2_676 2_676
Sn2 Sn5 Sn4 105.34(8) . 2_676
Sn1 Sn5 Sn4 116.52(8) . 2_676
Pd1 Sn5 Sn6 71.38(7) 2_676 .
Sn2 Sn5 Sn6 124.60(7) . .
Sn1 Sn5 Sn6 58.98(6) . .
Sn4 Sn5 Sn6 57.62(6) 2_676 .
Pd1 Sn6 Sn2 58.62(6) . 2_676
Pd1 Sn6 Sn4 111.92(8) . 2_676
Sn2 Sn6 Sn4 118.22(7) 2_676 2_676
Pd1 Sn6 Sn1 57.24(6) . .
Sn2 Sn6 Sn1 105.99(7) 2_676 .
Sn4 Sn6 Sn1 116.72(7) 2_676 .
Pd1 Sn6 Sn3 79.41(7) . 2_676
Sn2 Sn6 Sn3 58.74(6) 2_676 2_676
Sn4 Sn6 Sn3 59.54(6) 2_676 2_676
Sn1 Sn6 Sn3 132.40(7) . 2_676
Pd1 Sn6 Sn7 55.77(6) . .
Sn2 Sn6 Sn7 58.28(6) 2_676 .
Sn4 Sn6 Sn7 167.64(7) 2_676 .
Sn1 Sn6 Sn7 57.30(6) . .
Sn3 Sn6 Sn7 115.08(7) 2_676 .
Pd1 Sn6 Sn5 78.26(7) . .
Sn2 Sn6 Sn5 132.77(7) 2_676 .
Sn4 Sn6 Sn5 58.93(6) 2_676 .
Sn1 Sn6 Sn5 57.87(6) . .
Sn3 Sn6 Sn5 97.64(7) 2_676 .
Sn7 Sn6 Sn5 113.52(7) . .
Pd1 Sn7 Sn8 58.42(6) . .
Pd1 Sn7 Sn9 58.40(6) . .
Sn8 Sn7 Sn9 60.02(6) . .
Pd1 Sn7 Sn1 57.90(6) . .
Sn8 Sn7 Sn1 107.68(8) . .
Sn9 Sn7 Sn1 59.80(6) . .
Pd1 Sn7 Sn2 58.21(7) . 2_676
Sn8 Sn7 Sn2 61.10(7) . 2_676
Sn9 Sn7 Sn2 108.60(7) . 2_676
Sn1 Sn7 Sn2 107.10(8) . 2_676
Pd1 Sn7 Sn6 55.35(6) . .
Sn8 Sn7 Sn6 105.45(8) . .
Sn9 Sn7 Sn6 105.80(7) . .
Sn1 Sn7 Sn6 59.31(6) . .
Sn2 Sn7 Sn6 57.61(6) 2_676 .
Pd1 Sn8 Sn7 58.80(7) . .
Pd1 Sn8 Sn9 58.73(6) . .
Sn7 Sn8 Sn9 60.62(7) . .
Pd1 Sn8 Sn4 57.23(6) . .
Sn7 Sn8 Sn4 108.16(8) . .
Sn9 Sn8 Sn4 60.63(7) . .
Pd1 Sn8 Sn2 58.18(6) . 2_676
Sn7 Sn8 Sn2 60.69(6) . 2_676
Sn9 Sn8 Sn2 108.75(7) . 2_676
Sn4 Sn8 Sn2 106.07(7) . 2_676
Pd1 Sn9 Sn8 58.11(6) . .
Pd1 Sn9 Sn7 58.15(7) . .
Sn8 Sn9 Sn7 59.36(6) . .
Pd1 Sn9 Sn1 58.08(6) . .
Sn8 Sn9 Sn1 107.74(8) . .
Sn7 Sn9 Sn1 60.52(6) . .
Pd1 Sn9 Sn4 56.94(6) . .
Sn8 Sn9 Sn4 60.32(6) . .
Sn7 Sn9 Sn4 106.93(7) . .
Sn1 Sn9 Sn4 106.14(7) . .
Pd1 Sn9 Sn3 55.83(6) . .
Sn8 Sn9 Sn3 106.57(7) . .
Sn7 Sn9 Sn3 105.24(7) . .
Sn1 Sn9 Sn3 57.44(6) . .
Sn4 Sn9 Sn3 59.28(6) . .
O4 K1 O5 120.7(6) . .
O4 K1 O1 133.8(6) . .
O5 K1 O1 100.3(7) . .
O4 K1 O6 99.8(6) . .
O5 K1 O6 59.2(7) . .
O1 K1 O6 120.3(5) . .
O4 K1 O2 95.7(7) . .
O5 K1 O2 139.5(6) . .
O1 K1 O2 57.8(7) . .
O6 K1 O2 100.2(6) . .
O4 K1 O3 59.4(7) . .
O5 K1 O3 98.9(6) . .
O1 K1 O3 96.3(6) . .
O6 K1 O3 138.9(5) . .
O2 K1 O3 115.9(6) . .
O4 K1 N1 119.6(8) . .
O5 K1 N1 61.2(8) . .
O1 K1 N1 61.1(7) . .
O6 K1 N1 119.3(7) . .
O2 K1 N1 117.8(8) . .
O3 K1 N1 60.9(7) . .
O4 K1 N2 61.9(7) . .
O5 K1 N2 120.3(9) . .
O1 K1 N2 116.4(8) . .
O6 K1 N2 61.8(7) . .
O2 K1 N2 59.6(8) . .
O3 K1 N2 120.1(7) . .
N1 K1 N2 177.4(8) . .
O9 K2 O12 134.4(6) . .
O9 K2 O7 93.0(5) . .
O12 K2 O7 128.4(5) . .
O9 K2 O10 59.5(6) . .
O12 K2 O10 96.4(6) . .
O7 K2 O10 130.3(6) . .
O9 K2 O8 113.8(6) . .
O12 K2 O8 104.7(7) . .
O7 K2 O8 59.2(7) . .
O10 K2 O8 92.7(6) . .
O9 K2 O11 96.9(6) . .
O12 K2 O11 59.3(7) . .
O7 K2 O11 103.7(7) . .
O10 K2 O11 119.0(6) . .
O8 K2 O11 144.5(5) . .
O9 K2 N4 119.0(7) . .
O12 K2 N4 60.7(7) . .
O7 K2 N4 119.7(7) . .
O10 K2 N4 60.2(7) . .
O8 K2 N4 61.2(7) . .
O11 K2 N4 119.3(7) . .
O9 K2 N3 61.3(7) . .
O12 K2 N3 118.9(8) . .
O7 K2 N3 60.4(8) . .
O10 K2 N3 120.1(8) . .
O8 K2 N3 118.9(9) . .
O11 K2 N3 60.3(7) . .
N4 K2 N3 179.6(8) . .
C7 N1 C1 115(3) . .
C7 N1 C13 112(3) . .
C1 N1 C13 110(3) . .
C7 N1 K1 106.7(17) . .
C1 N1 K1 106.0(15) . .
C13 N1 K1 107.1(17) . .
C12 N2 C6 112(3) . .
C12 N2 C18 112(3) . .
C6 N2 C18 110(3) . .
C12 N2 K1 111.3(18) . .
C6 N2 K1 105.7(16) . .
C18 N2 K1 105.5(17) . .
C33 N3 C21 107(3) . .
C33 N3 C27 110(3) . .
C21 N3 C27 111(3) . .
C33 N3 K2 108.3(17) . .
C21 N3 K2 108.4(19) . .
C27 N3 K2 111.4(17) . .
C32 N4 C38 109(2) . .
C32 N4 C26 109(3) . .
C38 N4 C26 111(3) . .
C32 N4 K2 108.5(16) . .
C38 N4 K2 110.2(16) . .
C26 N4 K2 110.0(17) . .
C8 O1 C9 109(3) . .
C8 O1 K1 116.9(18) . .
C9 O1 K1 115.4(17) . .
C10 O2 C11 111(3) . .
C10 O2 K1 116(2) . .
C11 O2 K1 115.4(17) . .
C2 O3 C3 110(2) . .
C2 O3 K1 110.2(14) . .
C3 O3 K1 111.6(15) . .
C5 O4 C4 113(3) . .
C5 O4 K1 118.2(17) . .
C4 O4 K1 115.9(16) . .
C14 O5 C15 110(2) . .
C14 O5 K1 115.4(19) . .
C15 O5 K1 118.0(17) . .
C16 O6 C17 113(3) . .
C16 O6 K1 113.7(16) . .
C17 O6 K1 116.1(17) . .
C23 O7 C22 113(3) . .
C23 O7 K2 114.7(16) . .
C22 O7 K2 119.9(16) . .
C24 O8 C25 108(3) . .
C24 O8 K2 116.9(17) . .
C25 O8 K2 112.7(17) . .
C35 O9 C34 113(2) . .
C35 O9 K2 117.4(14) . .
C34 O9 K2 114.8(14) . .
C37 O10 C36 111(2) . .
C37 O10 K2 115.5(15) . .
C36 O10 K2 114.0(14) . .
C29 O11 C28 116(2) . .
C29 O11 K2 111.8(16) . .
C28 O11 K2 112.7(17) . .
C31 O12 C30 113(3) . .
C31 O12 K2 119.0(17) . .
C30 O12 K2 118.5(18) . .
C2 C1 N1 118(2) . .
O3 C2 C1 108(3) . .
O3 C3 C4 108(3) . .
O4 C4 C3 112(3) . .
O4 C5 C6 109(2) . .
N2 C6 C5 115(3) . .
C8 C7 N1 119(3) . .
O1 C8 C7 112(3) . .
O1 C9 C10 105(3) . .
O2 C10 C9 110(3) . .
O2 C11 C12 112(3) . .
N2 C12 C11 112(2) . .
N1 C13 C14 115(3) . .
O5 C14 C13 106(2) . .
O5 C15 C16 110(3) . .
O6 C16 C15 113(3) . .
O6 C17 C18 111(3) . .
C17 C18 N2 118(3) . .
C19 C19 N5 104(4) 2_576 .
N3 C21 C22 120(3) . .
C21 C22 O7 110(3) . .
O7 C23 C24 108(3) . .
O8 C24 C23 111(3) . .
O8 C25 C26 105(3) . .
C25 C26 N4 111(2) . .
C28 C27 N3 111(2) . .
O11 C28 C27 112(3) . .
O11 C29 C30 113(3) . .
O12 C30 C29 110(3) . .
O12 C31 C32 113(3) . .
N4 C32 C31 117(2) . .
N3 C33 C34 115(3) . .
O9 C34 C33 112(2) . .
O9 C35 C36 108(2) . .
O10 C36 C35 109(2) . .
O10 C37 C38 109(3) . .
N4 C38 C37 111(2) . .
N7 C39 C40 97(4) . .
C39 C40 N6 100(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Sn4 2.857(2) .
Pd1 Sn6 2.882(2) .
Pd1 Sn8 2.885(3) .
Pd1 Sn1 2.895(3) .
Pd1 Sn7 2.896(3) .
Pd1 Sn5 2.900(3) 2_676
Pd1 Sn9 2.904(3) .
Pd1 Sn3 2.908(3) .
Pd1 Sn2 2.917(3) 2_676
Sn1 Sn3 3.044(3) .
Sn1 Sn9 3.054(3) .
Sn1 Sn7 3.076(3) .
Sn1 Sn5 3.106(3) .
Sn1 Sn6 3.143(3) .
Sn2 Pd1 2.917(3) 2_676
Sn2 Sn6 3.067(3) 2_676
Sn2 Sn5 3.070(3) .
Sn2 Sn7 3.090(3) 2_676
Sn2 Sn3 3.096(3) .
Sn2 Sn8 3.102(3) 2_676
Sn3 Sn4 3.145(3) .
Sn3 Sn6 3.239(3) 2_676
Sn3 Sn9 3.270(3) .
Sn4 Sn8 3.071(3) .
Sn4 Sn9 3.081(3) .
Sn4 Sn6 3.089(3) 2_676
Sn4 Sn5 3.133(3) 2_676
Sn5 Pd1 2.900(3) 2_676
Sn5 Sn4 3.133(3) 2_676
Sn5 Sn6 3.272(3) .
Sn6 Sn2 3.067(3) 2_676
Sn6 Sn4 3.089(3) 2_676
Sn6 Sn3 3.239(3) 2_676
Sn6 Sn7 3.268(3) .
Sn7 Sn8 3.012(3) .
Sn7 Sn9 3.050(3) .
Sn7 Sn2 3.090(3) 2_676
Sn8 Sn9 3.032(3) .
Sn8 Sn2 3.102(3) 2_676
K1 O4 2.820(18) .
K1 O5 2.838(19) .
K1 O1 2.856(18) .
K1 O6 2.867(16) .
K1 O2 2.88(2) .
K1 O3 2.925(17) .
K1 N1 3.02(2) .
K1 N2 3.03(2) .
K2 O9 2.815(17) .
K2 O12 2.823(19) .
K2 O7 2.837(17) .
K2 O10 2.852(17) .
K2 O8 2.855(19) .
K2 O11 2.925(17) .
K2 N4 2.98(2) .
K2 N3 3.01(2) .
N1 C7 1.47(4) .
N1 C1 1.48(3) .
N1 C13 1.51(3) .
N2 C12 1.45(3) .
N2 C6 1.48(4) .
N2 C18 1.48(4) .
N3 C33 1.43(3) .
N3 C21 1.44(4) .
N3 C27 1.53(3) .
N4 C32 1.45(4) .
N4 C38 1.46(3) .
N4 C26 1.57(4) .
N5 C19 1.490(11) .
N6 C40 1.47(7) .
N7 C39 1.37(5) .
O1 C8 1.38(4) .
O1 C9 1.45(3) .
O2 C10 1.34(4) .
O2 C11 1.41(3) .
O3 C2 1.42(3) .
O3 C3 1.44(3) .
O4 C5 1.42(3) .
O4 C4 1.42(3) .
O5 C14 1.42(3) .
O5 C15 1.43(3) .
O6 C16 1.39(3) .
O6 C17 1.41(3) .
O7 C23 1.45(3) .
O7 C22 1.48(3) .
O8 C24 1.42(3) .
O8 C25 1.44(3) .
O9 C35 1.41(3) .
O9 C34 1.42(3) .
O10 C37 1.41(3) .
O10 C36 1.42(3) .
O11 C29 1.43(3) .
O11 C28 1.44(3) .
O12 C31 1.39(3) .
O12 C30 1.40(3) .
C1 C2 1.43(3) .
C3 C4 1.46(3) .
C5 C6 1.56(4) .
C7 C8 1.46(4) .
C9 C10 1.51(4) .
C11 C12 1.50(4) .
C13 C14 1.52(4) .
C15 C16 1.48(3) .
C17 C18 1.48(4) .
C19 C19 1.35(6) 2_576
C21 C22 1.45(4) .
C23 C24 1.49(4) .
C25 C26 1.55(4) .
C27 C28 1.46(4) .
C29 C30 1.46(3) .
C31 C32 1.46(4) .
C33 C34 1.50(3) .
C35 C36 1.53(3) .
C37 C38 1.52(4) .
C39 C40 1.418(11) .
