# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_2
_database_code_depnum_ccdc_archive 'CCDC 911588'
#TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1358416028.new_COMB.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C68 H44 F40 N12 Pd Sn4), 5(C7 H8), C6 H6'
_chemical_formula_sum            'C177 H134 F80 N24 Pd2 Sn8'
_chemical_formula_weight         5279.40
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   21.8677(16)
_cell_length_b                   14.4922(10)
_cell_length_c                   58.575(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.258(1)
_cell_angle_gamma                90.00
_cell_volume                     18485(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    9972
_cell_measurement_theta_min      2.340
_cell_measurement_theta_max      25.181
_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10304
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6416
_exptl_absorpt_correction_T_max  0.8184
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            122656
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         25.50
_reflns_number_total             34041
_reflns_number_gt                27553
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       '<i>APEX2</i> (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         34041
_refine_ls_number_parameters     2343
_refine_ls_number_restraints     167
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1761
_refine_ls_wR_factor_gt          0.1658
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.77703(2) 0.76147(3) 0.552042(8) 0.01684(11) Uani 1 1 d . . .
Pd2 Pd 0.27003(2) 0.71079(3) 0.203249(8) 0.02141(12) Uani 1 1 d . . .
Sn1 Sn 0.684299(19) 0.69916(3) 0.526255(7) 0.01999(11) Uani 1 1 d . . .
Sn2 Sn 0.876085(19) 0.74804(3) 0.531785(8) 0.02127(11) Uani 1 1 d . . .
Sn3 Sn 0.792469(19) 0.67239(3) 0.590037(7) 0.01898(11) Uani 1 1 d . . .
Sn4 Sn 0.756853(18) 0.93078(3) 0.561679(7) 0.01803(11) Uani 1 1 d . . .
Sn5 Sn 0.204482(19) 0.56190(3) 0.199078(7) 0.02168(11) Uani 1 1 d . . .
Sn6 Sn 0.28432(2) 0.78258(3) 0.163664(8) 0.02334(11) Uani 1 1 d . . .
Sn7 Sn 0.37614(2) 0.66152(3) 0.222531(8) 0.02517(12) Uani 1 1 d . . .
Sn8 Sn 0.21792(2) 0.82691(3) 0.228769(8) 0.02854(12) Uani 1 1 d . . .
N11 N 0.6573(2) 0.7502(4) 0.49273(9) 0.0246(12) Uani 1 1 d . . .
N12 N 0.6006(2) 0.6277(4) 0.53342(9) 0.0247(12) Uani 1 1 d . . .
N13 N 0.6854(2) 0.5693(4) 0.50389(10) 0.0271(13) Uani 1 1 d . . .
N21 N 0.9559(2) 0.8373(4) 0.53199(9) 0.0228(12) Uani 1 1 d . . .
N22 N 0.9153(3) 0.6243(4) 0.51876(11) 0.0327(14) Uani 1 1 d . . .
N23 N 0.8807(2) 0.7815(4) 0.49355(9) 0.0260(12) Uani 1 1 d . . .
N31 N 0.7294(2) 0.6596(4) 0.61590(9) 0.0260(12) Uani 1 1 d . . .
N32 N 0.8526(3) 0.5570(4) 0.59838(10) 0.0272(13) Uani 1 1 d . . .
N33 N 0.8496(2) 0.7193(4) 0.62264(9) 0.0232(12) Uani 1 1 d . . .
N41 N 0.8180(2) 1.0067(3) 0.58542(9) 0.0224(12) Uani 1 1 d . . .
N42 N 0.7043(2) 1.0400(4) 0.54394(9) 0.0230(12) Uani 1 1 d . . .
N43 N 0.6936(2) 0.9803(3) 0.58841(9) 0.0207(11) Uani 1 1 d . . .
N51 N 0.1087(2) 0.5543(4) 0.18682(9) 0.0275(13) Uani 1 1 d . . .
N52 N 0.2178(3) 0.4288(4) 0.21549(10) 0.0306(13) Uani 1 1 d . . .
N53 N 0.2054(2) 0.4657(4) 0.16829(9) 0.0273(13) Uani 1 1 d . . .
N61 N 0.3000(3) 0.9208(4) 0.15030(9) 0.0283(13) Uani 1 1 d . . .
N62 N 0.3178(3) 0.7153(4) 0.13527(10) 0.0299(13) Uani 1 1 d . . .
N63 N 0.2040(3) 0.8033(4) 0.13546(9) 0.0284(13) Uani 1 1 d . . .
N71 N 0.3982(3) 0.6094(4) 0.25660(10) 0.0355(15) Uani 1 1 d . . .
N72 N 0.4596(2) 0.6194(4) 0.20800(10) 0.0304(13) Uani 1 1 d . . .
N73 N 0.4476(3) 0.7646(4) 0.23833(10) 0.0318(14) Uani 1 1 d . . .
N81 N 0.2579(3) 0.9579(4) 0.23831(10) 0.0369(15) Uani 1 1 d . . .
N82 N 0.1245(3) 0.8515(5) 0.23756(11) 0.0421(16) Uani 1 1 d . . .
N83 N 0.2264(3) 0.8199(5) 0.26776(11) 0.0418(16) Uani 1 1 d . . .
C1 C 0.7471(3) 0.5374(5) 0.49992(13) 0.0355(17) Uani 1 1 d . . .
H1A H 0.7440 0.4820 0.4903 0.053 Uiso 1 1 calc R . .
H1B H 0.7701 0.5228 0.5146 0.053 Uiso 1 1 calc R . .
H1C H 0.7686 0.5860 0.4922 0.053 Uiso 1 1 calc R . .
C2 C 0.8204(3) 0.7822(5) 0.47998(12) 0.0329(17) Uani 1 1 d . . .
H2A H 0.8260 0.7972 0.4640 0.049 Uiso 1 1 calc R . .
H2B H 0.7939 0.8287 0.4862 0.049 Uiso 1 1 calc R . .
H2C H 0.8013 0.7213 0.4807 0.049 Uiso 1 1 calc R . .
C3 C 0.8591(3) 0.8208(4) 0.62406(11) 0.0251(14) Uani 1 1 d . . .
H3A H 0.8838 0.8360 0.6384 0.038 Uiso 1 1 calc R . .
H3B H 0.8191 0.8518 0.6238 0.038 Uiso 1 1 calc R . .
H3C H 0.8804 0.8415 0.6110 0.038 Uiso 1 1 calc R . .
C4 C 0.6780(3) 0.9084(5) 0.60481(12) 0.0293(15) Uani 1 1 d . . .
H4A H 0.6510 0.9347 0.6156 0.044 Uiso 1 1 calc R . .
H4B H 0.7157 0.8857 0.6133 0.044 Uiso 1 1 calc R . .
H4C H 0.6570 0.8573 0.5964 0.044 Uiso 1 1 calc R . .
C5 C 0.2321(3) 0.5078(5) 0.14859(12) 0.0310(16) Uani 1 1 d . . .
H5A H 0.2311 0.4632 0.1360 0.047 Uiso 1 1 calc R . .
H5B H 0.2748 0.5257 0.1531 0.047 Uiso 1 1 calc R . .
H5C H 0.2083 0.5626 0.1436 0.047 Uiso 1 1 calc R . .
C6 C 0.1465(3) 0.7586(5) 0.14057(12) 0.0352(17) Uani 1 1 d . . .
H6A H 0.1147 0.7701 0.1280 0.053 Uiso 1 1 calc R . .
H6B H 0.1333 0.7840 0.1548 0.053 Uiso 1 1 calc R . .
H6C H 0.1532 0.6920 0.1423 0.053 Uiso 1 1 calc R . .
C7 C 0.4224(3) 0.8571(5) 0.24306(13) 0.0394(18) Uani 1 1 d . . .
H7A H 0.4555 0.8970 0.2497 0.059 Uiso 1 1 calc R . .
H7B H 0.3909 0.8510 0.2538 0.059 Uiso 1 1 calc R . .
H7C H 0.4040 0.8843 0.2287 0.059 Uiso 1 1 calc R . .
C8 C 0.2757(4) 0.7569(7) 0.27744(15) 0.056(2) Uani 1 1 d . . .
H8A H 0.2768 0.7569 0.2942 0.084 Uiso 1 1 calc R . .
H8B H 0.3153 0.7780 0.2729 0.084 Uiso 1 1 calc R . .
H8C H 0.2674 0.6943 0.2716 0.084 Uiso 1 1 calc R . .
C11 C 0.6504(3) 0.5908(5) 0.48184(12) 0.0309(16) Uani 1 1 d . . .
H11A H 0.6058 0.5865 0.4836 0.037 Uiso 1 1 calc R . .
H11B H 0.6603 0.5451 0.4702 0.037 Uiso 1 1 calc R . .
C12 C 0.6652(3) 0.6858(5) 0.47389(12) 0.0293(16) Uani 1 1 d . . .
H12A H 0.7080 0.6880 0.4697 0.035 Uiso 1 1 calc R . .
H12B H 0.6374 0.7027 0.4602 0.035 Uiso 1 1 calc R . .
C13 C 0.6412(3) 0.8402(5) 0.48712(12) 0.0297(16) Uani 1 1 d . . .
C14 C 0.6084(3) 0.8924(5) 0.50192(12) 0.0303(16) Uani 1 1 d . . .
C15 C 0.5879(3) 0.9800(5) 0.49716(13) 0.0349(17) Uani 1 1 d . . .
C16 C 0.5985(4) 1.0220(5) 0.47677(14) 0.0400(19) Uani 1 1 d . . .
C17 C 0.6317(4) 0.9753(6) 0.46195(13) 0.0411(19) Uani 1 1 d . . .
C18 C 0.6533(3) 0.8874(5) 0.46712(12) 0.0329(17) Uani 1 1 d . . .
C21 C 0.6546(3) 0.4991(4) 0.51752(12) 0.0284(15) Uani 1 1 d . . .
H21A H 0.6808 0.4852 0.5318 0.034 Uiso 1 1 calc R . .
H21B H 0.6487 0.4413 0.5086 0.034 Uiso 1 1 calc R . .
C22 C 0.5931(3) 0.5352(5) 0.52334(12) 0.0309(16) Uani 1 1 d . . .
H22A H 0.5644 0.5380 0.5093 0.037 Uiso 1 1 calc R . .
H22B H 0.5757 0.4930 0.5343 0.037 Uiso 1 1 calc R . .
C23 C 0.5529(3) 0.6619(4) 0.54465(11) 0.0237(14) Uani 1 1 d . . .
C24 C 0.4917(3) 0.6323(5) 0.54236(11) 0.0258(14) Uani 1 1 d . . .
C25 C 0.4465(3) 0.6688(5) 0.55483(12) 0.0323(17) Uani 1 1 d . . .
C26 C 0.4588(3) 0.7402(5) 0.56985(14) 0.0383(18) Uani 1 1 d . . .
C27 C 0.5175(3) 0.7741(5) 0.57252(12) 0.0319(16) Uani 1 1 d . . .
C28 C 0.5621(3) 0.7348(5) 0.56052(12) 0.0273(15) Uani 1 1 d . . .
C31 C 0.9068(3) 0.8760(5) 0.49397(12) 0.0284(15) Uani 1 1 d . . .
H31A H 0.8769 0.9201 0.4995 0.034 Uiso 1 1 calc R . .
H31B H 0.9151 0.8944 0.4783 0.034 Uiso 1 1 calc R . .
C32 C 0.9662(3) 0.8792(5) 0.50974(11) 0.0289(15) Uani 1 1 d . . .
H32A H 0.9988 0.8450 0.5027 0.035 Uiso 1 1 calc R . .
H32B H 0.9798 0.9439 0.5120 0.035 Uiso 1 1 calc R . .
C33 C 0.9989(3) 0.8554(4) 0.54990(12) 0.0246(14) Uani 1 1 d . . .
C34 C 1.0601(3) 0.8863(5) 0.54837(13) 0.0318(16) Uani 1 1 d . . .
C35 C 1.1000(3) 0.9086(5) 0.56705(13) 0.0298(16) Uani 1 1 d . . .
C36 C 1.0832(3) 0.8973(4) 0.58870(11) 0.0244(14) Uani 1 1 d . . .
C37 C 1.0254(3) 0.8635(5) 0.59137(12) 0.0279(15) Uani 1 1 d . . .
C38 C 0.9861(3) 0.8436(4) 0.57264(11) 0.0225(14) Uani 1 1 d . . .
C41 C 0.9227(3) 0.7119(5) 0.48426(12) 0.0318(16) Uani 1 1 d . . .
H41A H 0.9660 0.7292 0.4887 0.038 Uiso 1 1 calc R . .
H41B H 0.9163 0.7111 0.4673 0.038 Uiso 1 1 calc R . .
C42 C 0.9102(3) 0.6166(5) 0.49360(12) 0.0332(17) Uani 1 1 d . . .
H42A H 0.8685 0.5956 0.4878 0.040 Uiso 1 1 calc R . .
H42B H 0.9404 0.5715 0.4887 0.040 Uiso 1 1 calc R . .
C43 C 0.9307(3) 0.5460(5) 0.53112(15) 0.040(2) Uani 1 1 d . . .
C44 C 0.9612(3) 0.5537(5) 0.55303(16) 0.040(2) Uani 1 1 d . . .
C45 C 0.9825(4) 0.4809(6) 0.56649(17) 0.053(2) Uani 1 1 d . . .
C46 C 0.9723(4) 0.3906(6) 0.55733(17) 0.053(2) Uani 1 1 d U . .
C47 C 0.9434(4) 0.3804(6) 0.53693(18) 0.056(2) Uani 1 1 d U . .
C48 C 0.9212(4) 0.4548(5) 0.52357(19) 0.053(2) Uani 1 1 d . . .
C51 C 0.8177(3) 0.6879(5) 0.64246(11) 0.0278(15) Uani 1 1 d . . .
H51A H 0.8333 0.7229 0.6563 0.033 Uiso 1 1 calc R . .
H51B H 0.8266 0.6217 0.6453 0.033 Uiso 1 1 calc R . .
C52 C 0.7498(3) 0.7013(5) 0.63827(12) 0.0298(16) Uani 1 1 d . . .
H52A H 0.7288 0.6714 0.6506 0.036 Uiso 1 1 calc R . .
H52B H 0.7398 0.7679 0.6381 0.036 Uiso 1 1 calc R . .
C53 C 0.6699(3) 0.6314(4) 0.61201(11) 0.0249(14) Uani 1 1 d . . .
C54 C 0.6532(3) 0.5653(5) 0.59484(12) 0.0286(15) Uani 1 1 d . . .
C55 C 0.5960(3) 0.5288(5) 0.59091(12) 0.0317(16) Uani 1 1 d . . .
C56 C 0.5480(3) 0.5592(5) 0.60289(13) 0.0332(17) Uani 1 1 d . . .
C57 C 0.5611(3) 0.6260(5) 0.61937(14) 0.0365(18) Uani 1 1 d . . .
C58 C 0.6192(3) 0.6632(5) 0.62325(13) 0.0344(17) Uani 1 1 d . . .
C61 C 0.9096(3) 0.6728(5) 0.62155(12) 0.0270(15) Uani 1 1 d . . .
H61A H 0.9357 0.6835 0.6360 0.032 Uiso 1 1 calc R . .
H61B H 0.9308 0.6992 0.6088 0.032 Uiso 1 1 calc R . .
C62 C 0.9005(3) 0.5711(5) 0.61787(13) 0.0332(17) Uani 1 1 d . . .
H62A H 0.9396 0.5421 0.6144 0.040 Uiso 1 1 calc R . .
H62B H 0.8874 0.5422 0.6319 0.040 Uiso 1 1 calc R . .
C63 C 0.8458(3) 0.4679(4) 0.58954(13) 0.0306(16) Uani 1 1 d . . .
C64 C 0.8171(3) 0.4533(4) 0.56770(14) 0.0314(17) Uani 1 1 d . . .
C65 C 0.8070(3) 0.3681(5) 0.55789(15) 0.0372(18) Uani 1 1 d . . .
C66 C 0.8258(4) 0.2896(5) 0.57022(16) 0.0431(19) Uani 1 1 d U . .
C67 C 0.8549(4) 0.2999(5) 0.59125(18) 0.051(2) Uani 1 1 d . . .
C68 C 0.8644(3) 0.3876(5) 0.60109(14) 0.0379(18) Uani 1 1 d . . .
C71 C 0.7250(3) 1.0596(4) 0.60072(11) 0.0236(14) Uani 1 1 d . . .
H71A H 0.7057 1.0720 0.6150 0.028 Uiso 1 1 calc R . .
H71B H 0.7206 1.1155 0.5910 0.028 Uiso 1 1 calc R . .
C72 C 0.7926(3) 1.0381(4) 0.60636(11) 0.0234(14) Uani 1 1 d . . .
H72A H 0.8146 1.0941 0.6123 0.028 Uiso 1 1 calc R . .
H72B H 0.7976 0.9895 0.6182 0.028 Uiso 1 1 calc R . .
C73 C 0.8775(3) 1.0286(4) 0.58216(11) 0.0199(13) Uani 1 1 d . . .
C74 C 0.8949(3) 1.0417(4) 0.56001(11) 0.0224(14) Uani 1 1 d . . .
C75 C 0.9509(3) 1.0737(4) 0.55529(12) 0.0257(15) Uani 1 1 d . . .
C76 C 0.9961(3) 1.0933(5) 0.57243(13) 0.0309(16) Uani 1 1 d . . .
C77 C 0.9822(3) 1.0757(5) 0.59477(12) 0.0293(16) Uani 1 1 d . . .
C78 C 0.9258(3) 1.0439(4) 0.59955(11) 0.0251(14) Uani 1 1 d . . .
C81 C 0.6373(3) 1.0119(5) 0.57404(12) 0.0286(15) Uani 1 1 d . . .
H81A H 0.6088 1.0419 0.5839 0.034 Uiso 1 1 calc R . .
H81B H 0.6161 0.9579 0.5666 0.034 Uiso 1 1 calc R . .
C82 C 0.6539(3) 1.0786(5) 0.55608(11) 0.0277(15) Uani 1 1 d . . .
H82A H 0.6177 1.0903 0.5450 0.033 Uiso 1 1 calc R . .
H82B H 0.6669 1.1380 0.5633 0.033 Uiso 1 1 calc R . .
C83 C 0.7153(3) 1.0814(4) 0.52354(11) 0.0235(14) Uani 1 1 d . . .
C84 C 0.6993(3) 1.1709(5) 0.51644(13) 0.0329(16) Uani 1 1 d . . .
C85 C 0.7092(4) 1.2053(5) 0.49521(14) 0.0356(18) Uani 1 1 d . . .
C86 C 0.7370(4) 1.1538(5) 0.47975(13) 0.042(2) Uani 1 1 d . . .
C87 C 0.7552(3) 1.0660(5) 0.48625(13) 0.0348(17) Uani 1 1 d . . .
C88 C 0.7448(3) 1.0319(5) 0.50712(11) 0.0255(14) Uani 1 1 d . . .
C91 C 0.1405(3) 0.4368(5) 0.16170(13) 0.0338(17) Uani 1 1 d . . .
H91A H 0.1295 0.3860 0.1718 0.041 Uiso 1 1 calc R . .
H91B H 0.1369 0.4134 0.1457 0.041 Uiso 1 1 calc R . .
C92 C 0.0970(3) 0.5158(5) 0.16356(12) 0.0311(16) Uani 1 1 d . . .
H92A H 0.1039 0.5635 0.1520 0.037 Uiso 1 1 calc R . .
H92B H 0.0540 0.4941 0.1610 0.037 Uiso 1 1 calc R . .
C93 C 0.0633(3) 0.6023(5) 0.19615(12) 0.0278(15) Uani 1 1 d . . .
C94 C 0.0132(3) 0.6469(6) 0.18450(13) 0.0398(19) Uani 1 1 d . . .
C95 C -0.0317(3) 0.6903(7) 0.19575(16) 0.052(2) Uani 1 1 d . . .
C96 C -0.0278(3) 0.6965(6) 0.21875(16) 0.049(2) Uani 1 1 d . . .
C97 C 0.0204(3) 0.6567(6) 0.23117(12) 0.0374(18) Uani 1 1 d . . .
C98 C 0.0648(3) 0.6111(5) 0.21988(13) 0.0329(17) Uani 1 1 d . . .
C101 C 0.2441(3) 0.3849(5) 0.17706(13) 0.0359(17) Uani 1 1 d . . .
H10A H 0.2402 0.3342 0.1657 0.043 Uiso 1 1 calc R . .
H10B H 0.2878 0.4035 0.1792 0.043 Uiso 1 1 calc R . .
C102 C 0.2238(3) 0.3519(5) 0.19942(13) 0.0352(17) Uani 1 1 d . . .
H10C H 0.1837 0.3201 0.1966 0.042 Uiso 1 1 calc R . .
H10D H 0.2540 0.3069 0.2064 0.042 Uiso 1 1 calc R . .
C103 C 0.2117(3) 0.4064(5) 0.23805(14) 0.0352(18) Uani 1 1 d . . .
C104 C 0.2025(3) 0.3164(6) 0.24710(16) 0.047(2) Uani 1 1 d . . .
C105 C 0.1996(4) 0.3025(6) 0.27058(16) 0.048(2) Uani 1 1 d U . .
C106 C 0.2032(4) 0.3698(7) 0.28500(14) 0.048(2) Uani 1 1 d U . .
C107 C 0.2119(3) 0.4608(7) 0.27804(15) 0.048(2) Uani 1 1 d . . .
C108 C 0.2164(3) 0.4741(6) 0.25488(13) 0.0378(19) Uani 1 1 d . . .
C111 C 0.1951(3) 0.9041(5) 0.13440(13) 0.0389(19) Uani 1 1 d . . .
H11C H 0.1779 0.9253 0.1486 0.047 Uiso 1 1 calc R . .
H11D H 0.1652 0.9195 0.1212 0.047 Uiso 1 1 calc R . .
C112 C 0.2541(3) 0.9537(5) 0.13192(13) 0.0373(18) Uani 1 1 d . . .
H11E H 0.2685 0.9408 0.1167 0.045 Uiso 1 1 calc R . .
H11F H 0.2481 1.0211 0.1333 0.045 Uiso 1 1 calc R . .
C113 C 0.3544(3) 0.9676(4) 0.15355(11) 0.0266(15) Uani 1 1 d . . .
C114 C 0.3790(4) 1.0279(5) 0.13822(13) 0.0373(18) Uani 1 1 d . . .
C115 C 0.4346(4) 1.0747(5) 0.14352(13) 0.0380(18) Uani 1 1 d . . .
C116 C 0.4692(3) 1.0615(5) 0.16367(14) 0.0399(19) Uani 1 1 d . . .
C117 C 0.4466(3) 1.0020(5) 0.17926(12) 0.0331(17) Uani 1 1 d . . .
C118 C 0.3922(3) 0.9581(5) 0.17424(12) 0.0300(16) Uani 1 1 d . . .
C121 C 0.2236(3) 0.7627(5) 0.11380(12) 0.0335(17) Uani 1 1 d . . .
H12C H 0.2074 0.8014 0.1007 0.040 Uiso 1 1 calc R . .
H12D H 0.2054 0.7004 0.1116 0.040 Uiso 1 1 calc R . .
C122 C 0.2929(4) 0.7551(6) 0.11364(13) 0.0391(18) Uani 1 1 d . . .
H12E H 0.3031 0.7155 0.1008 0.047 Uiso 1 1 calc R . .
H12F H 0.3108 0.8170 0.1116 0.047 Uiso 1 1 calc R . .
C123 C 0.3724(3) 0.6673(5) 0.13498(12) 0.0308(16) Uani 1 1 d . . .
C124 C 0.3786(4) 0.5904(5) 0.12146(14) 0.043(2) Uani 1 1 d . . .
C125 C 0.4340(5) 0.5446(6) 0.12096(15) 0.053(2) Uani 1 1 d . . .
C126 C 0.4845(4) 0.5714(6) 0.13350(16) 0.052(2) Uani 1 1 d . . .
C127 C 0.4813(4) 0.6458(6) 0.14729(14) 0.043(2) Uani 1 1 d . . .
C128 C 0.4258(3) 0.6930(5) 0.14800(13) 0.0319(16) Uani 1 1 d . . .
C131 C 0.4777(3) 0.7230(5) 0.25997(13) 0.0398(19) Uani 1 1 d . . .
H13A H 0.4968 0.7725 0.2699 0.048 Uiso 1 1 calc R . .
H13B H 0.5106 0.6802 0.2562 0.048 Uiso 1 1 calc R . .
C132 C 0.4319(3) 0.6716(6) 0.27279(13) 0.0400(19) Uani 1 1 d . . .
H13C H 0.4533 0.6360 0.2856 0.048 Uiso 1 1 calc R . .
H13D H 0.4033 0.7154 0.2792 0.048 Uiso 1 1 calc R . .
C133 C 0.3800(3) 0.5255(5) 0.26481(13) 0.0339(17) Uani 1 1 d . . .
C134 C 0.3710(3) 0.4488(5) 0.25033(14) 0.0374(18) Uani 1 1 d . . .
C135 C 0.3562(3) 0.3621(6) 0.25745(17) 0.047(2) Uani 1 1 d . . .
C136 C 0.3509(3) 0.3461(7) 0.28040(19) 0.061(3) Uani 1 1 d . . .
C137 C 0.3561(4) 0.4176(7) 0.29451(16) 0.050(2) Uani 1 1 d U . .
C138 C 0.3684(3) 0.5061(7) 0.28757(14) 0.049(2) Uani 1 1 d . . .
C141 C 0.4920(4) 0.7714(5) 0.22058(15) 0.044(2) Uani 1 1 d . . .
H14A H 0.5278 0.8087 0.2266 0.053 Uiso 1 1 calc R . .
H14B H 0.4721 0.8033 0.2069 0.053 Uiso 1 1 calc R . .
C142 C 0.5135(3) 0.6781(6) 0.21374(14) 0.0398(19) Uani 1 1 d . . .
H14C H 0.5377 0.6837 0.2003 0.048 Uiso 1 1 calc R . .
H14D H 0.5401 0.6503 0.2265 0.048 Uiso 1 1 calc R . .
C143 C 0.4685(3) 0.5372(5) 0.19705(12) 0.0290(16) Uani 1 1 d . . .
C144 C 0.4217(3) 0.4969(5) 0.18264(12) 0.0310(16) Uani 1 1 d . . .
C145 C 0.4271(4) 0.4176(6) 0.17063(14) 0.043(2) Uani 1 1 d . . .
C146 C 0.4827(4) 0.3714(6) 0.17230(16) 0.052(2) Uani 1 1 d . . .
C147 C 0.5305(4) 0.4069(6) 0.18628(15) 0.047(2) Uani 1 1 d . . .
C148 C 0.5239(3) 0.4862(6) 0.19802(13) 0.0405(19) Uani 1 1 d . . .
C151 C 0.2380(4) 0.9175(6) 0.27628(14) 0.051(2) Uani 1 1 d . . .
H15A H 0.1983 0.9506 0.2758 0.061 Uiso 1 1 calc R . .
H15B H 0.2557 0.9154 0.2924 0.061 Uiso 1 1 calc R . .
C152 C 0.2796(4) 0.9687(6) 0.26277(14) 0.054(2) Uani 1 1 d . . .
H15C H 0.3219 0.9445 0.2657 0.064 Uiso 1 1 calc R . .
H15D H 0.2798 1.0348 0.2671 0.064 Uiso 1 1 calc R . .
C153 C 0.2770(3) 1.0195(5) 0.22269(13) 0.0320(17) Uani 1 1 d . . .
C154 C 0.2403(3) 1.0377(5) 0.20262(14) 0.0384(18) Uani 1 1 d . . .
C155 C 0.2551(4) 1.0974(5) 0.18614(13) 0.0375(18) Uani 1 1 d . . .
C156 C 0.3091(4) 1.1439(5) 0.18845(15) 0.044(2) Uani 1 1 d . . .
C157 C 0.3476(3) 1.1295(5) 0.20827(15) 0.042(2) Uani 1 1 d . . .
C158 C 0.3325(3) 1.0701(5) 0.22476(14) 0.0394(19) Uani 1 1 d . . .
C161 C 0.1666(4) 0.7853(6) 0.27343(15) 0.050(2) Uani 1 1 d . . .
H16A H 0.1646 0.7878 0.2902 0.060 Uiso 1 1 calc R . .
H16B H 0.1617 0.7202 0.2685 0.060 Uiso 1 1 calc R . .
C162 C 0.1147(4) 0.8426(7) 0.26163(14) 0.051(2) Uani 1 1 d . . .
H16C H 0.0748 0.8122 0.2632 0.062 Uiso 1 1 calc R . .
H16D H 0.1140 0.9044 0.2688 0.062 Uiso 1 1 calc R . .
C163 C 0.0763(3) 0.8843(6) 0.22301(13) 0.0387(18) Uani 1 1 d . . .
C164 C 0.0231(4) 0.9310(7) 0.22918(16) 0.053(2) Uani 1 1 d . . .
C165 C -0.0238(4) 0.9576(7) 0.21355(18) 0.061(3) Uani 1 1 d . . .
C166 C -0.0229(4) 0.9411(7) 0.19096(17) 0.058(2) Uani 1 1 d U . .
C167 C 0.0275(4) 0.8965(7) 0.18370(15) 0.053(2) Uani 1 1 d U . .
C168 C 0.0741(3) 0.8705(6) 0.19958(14) 0.046(2) Uani 1 1 d . . .
F14 F 0.59557(18) 0.8541(3) 0.52200(7) 0.0350(9) Uani 1 1 d . . .
F15 F 0.5551(2) 1.0248(3) 0.51223(8) 0.0469(12) Uani 1 1 d . . .
F16 F 0.5772(2) 1.1079(3) 0.47163(9) 0.0617(14) Uani 1 1 d . . .
F17 F 0.6448(2) 1.0150(3) 0.44231(8) 0.0589(14) Uani 1 1 d . . .
F18 F 0.6883(2) 0.8469(3) 0.45228(7) 0.0440(11) Uani 1 1 d . . .
F24 F 0.47259(17) 0.5648(3) 0.52736(7) 0.0335(9) Uani 1 1 d . . .
F25 F 0.38912(18) 0.6347(3) 0.55130(8) 0.0500(12) Uani 1 1 d . . .
F26 F 0.4149(2) 0.7770(4) 0.58180(9) 0.0605(15) Uani 1 1 d . . .
F27 F 0.5323(2) 0.8423(3) 0.58740(8) 0.0511(13) Uani 1 1 d . . .
F28 F 0.62021(17) 0.7686(3) 0.56433(7) 0.0330(9) Uani 1 1 d . . .
F34 F 1.08306(18) 0.8952(3) 0.52761(7) 0.0463(12) Uani 1 1 d . . .
F35 F 1.15618(18) 0.9393(3) 0.56409(8) 0.0482(12) Uani 1 1 d . . .
F36 F 1.12190(18) 0.9225(3) 0.60730(7) 0.0361(10) Uani 1 1 d . . .
F37 F 1.00697(18) 0.8531(3) 0.61261(7) 0.0392(10) Uani 1 1 d . . .
F38 F 0.92877(16) 0.8141(3) 0.57604(6) 0.0303(9) Uani 1 1 d . . .
F44 F 0.9723(2) 0.6397(3) 0.56205(8) 0.0496(12) Uani 1 1 d . . .
F45 F 1.0124(3) 0.4940(4) 0.58703(11) 0.0742(18) Uani 1 1 d . . .
F46 F 0.9933(3) 0.3182(4) 0.57096(11) 0.0758(17) Uani 1 1 d U . .
F47 F 0.9302(3) 0.2940(4) 0.52900(10) 0.0728(16) Uani 1 1 d U . .
F48 F 0.8889(2) 0.4373(3) 0.50369(11) 0.0653(16) Uani 1 1 d . . .
F54 F 0.69840(17) 0.5326(3) 0.58258(7) 0.0316(9) Uani 1 1 d . . .
F55 F 0.58431(19) 0.4642(3) 0.57452(7) 0.0415(11) Uani 1 1 d . . .
F56 F 0.49138(18) 0.5256(3) 0.59834(9) 0.0496(12) Uani 1 1 d . . .
F57 F 0.5157(2) 0.6582(4) 0.63072(9) 0.0598(14) Uani 1 1 d . . .
F58 F 0.62729(19) 0.7323(3) 0.63869(8) 0.0466(12) Uani 1 1 d . . .
F64 F 0.79816(19) 0.5277(3) 0.55513(7) 0.0343(9) Uani 1 1 d . . .
F65 F 0.7795(2) 0.3612(3) 0.53652(9) 0.0500(12) Uani 1 1 d . . .
F66 F 0.8154(2) 0.2056(3) 0.56036(9) 0.0611(14) Uani 1 1 d U . .
F67 F 0.8745(3) 0.2261(4) 0.60367(10) 0.0653(14) Uani 1 1 d U . .
F68 F 0.8907(3) 0.3865(3) 0.62291(9) 0.0614(14) Uani 1 1 d . . .
F74 F 0.85227(16) 1.0283(3) 0.54196(6) 0.0281(8) Uani 1 1 d . . .
F75 F 0.96317(18) 1.0886(3) 0.53343(7) 0.0349(10) Uani 1 1 d . . .
F76 F 1.05128(18) 1.1231(3) 0.56800(8) 0.0442(11) Uani 1 1 d . . .
F77 F 1.02596(18) 1.0896(3) 0.61231(8) 0.0453(11) Uani 1 1 d . . .
F78 F 0.91585(17) 1.0295(3) 0.62160(6) 0.0320(9) Uani 1 1 d . . .
F84 F 0.6743(2) 1.2302(3) 0.53098(7) 0.0413(11) Uani 1 1 d . . .
F85 F 0.6926(2) 1.2921(3) 0.48993(9) 0.0568(13) Uani 1 1 d U . .
F86 F 0.7455(2) 1.1852(4) 0.45870(9) 0.0613(14) Uani 1 1 d U . .
F87 F 0.7815(2) 1.0098(3) 0.47135(7) 0.0421(11) Uani 1 1 d . . .
F88 F 0.76167(17) 0.9438(2) 0.51213(6) 0.0272(8) Uani 1 1 d . . .
F94 F 0.0069(2) 0.6489(4) 0.16114(8) 0.0615(15) Uani 1 1 d . . .
F95 F -0.0791(3) 0.7317(4) 0.18275(10) 0.0709(16) Uani 1 1 d U . .
F96 F -0.0699(3) 0.7431(4) 0.22985(10) 0.0679(15) Uani 1 1 d U . .
F97 F 0.0260(2) 0.6593(4) 0.25416(8) 0.0595(14) Uani 1 1 d . . .
F98 F 0.11148(19) 0.5709(3) 0.23290(7) 0.0454(12) Uani 1 1 d . . .
F104 F 0.1975(3) 0.2407(4) 0.23383(10) 0.0683(16) Uani 1 1 d . . .
F105 F 0.1942(3) 0.2141(4) 0.27769(10) 0.0704(15) Uani 1 1 d U . .
F106 F 0.1996(3) 0.3566(4) 0.30790(11) 0.0789(17) Uani 1 1 d U . .
F107 F 0.2163(2) 0.5332(4) 0.29194(9) 0.0613(14) Uani 1 1 d U . .
F108 F 0.22872(18) 0.5630(3) 0.24817(7) 0.0380(10) Uani 1 1 d . . .
F114 F 0.3519(2) 1.0426(3) 0.11705(7) 0.0515(13) Uani 1 1 d . . .
F115 F 0.4546(2) 1.1326(3) 0.12794(8) 0.0542(13) Uani 1 1 d . . .
F116 F 0.5227(2) 1.1056(3) 0.16892(9) 0.0575(14) Uani 1 1 d . . .
F117 F 0.4784(2) 0.9888(3) 0.20001(8) 0.0518(13) Uani 1 1 d . . .
F118 F 0.37145(19) 0.9012(3) 0.19042(7) 0.0386(10) Uani 1 1 d . . .
F124 F 0.3284(2) 0.5578(3) 0.10868(8) 0.0566(13) Uani 1 1 d . . .
F125 F 0.4347(3) 0.4680(4) 0.10737(11) 0.0810(17) Uani 1 1 d U . .
F126 F 0.5377(3) 0.5252(4) 0.13265(10) 0.0703(15) Uani 1 1 d U . .
F127 F 0.5320(2) 0.6758(4) 0.16043(9) 0.0608(15) Uani 1 1 d . . .
F128 F 0.4257(2) 0.7677(3) 0.16197(8) 0.0423(11) Uani 1 1 d . . .
F134 F 0.3776(2) 0.4602(3) 0.22784(8) 0.0460(11) Uani 1 1 d . . .
F135 F 0.3505(2) 0.2925(3) 0.24252(11) 0.0683(16) Uani 1 1 d . . .
F136 F 0.3370(3) 0.2622(4) 0.28774(10) 0.0722(16) Uani 1 1 d U . .
F137 F 0.3465(3) 0.4070(4) 0.31739(11) 0.0799(17) Uani 1 1 d U . .
F138 F 0.3682(2) 0.5750(5) 0.30281(8) 0.0739(18) Uani 1 1 d . . .
F144 F 0.36667(17) 0.5403(3) 0.18048(7) 0.0349(10) Uani 1 1 d . . .
F145 F 0.3797(2) 0.3858(3) 0.15657(9) 0.0563(13) Uani 1 1 d . . .
F146 F 0.4890(3) 0.2928(4) 0.16002(10) 0.0737(16) Uani 1 1 d U . .
F147 F 0.5850(2) 0.3628(4) 0.18833(10) 0.0710(16) Uani 1 1 d . . .
F148 F 0.57327(19) 0.5133(4) 0.21238(8) 0.0532(13) Uani 1 1 d . . .
F154 F 0.1858(2) 0.9924(3) 0.19896(8) 0.0507(12) Uani 1 1 d . . .
F155 F 0.2164(2) 1.1131(3) 0.16716(8) 0.0548(13) Uani 1 1 d . . .
F156 F 0.3261(2) 1.2039(3) 0.17255(9) 0.0540(13) Uani 1 1 d . . .
F157 F 0.4026(2) 1.1735(3) 0.21086(9) 0.0580(14) Uani 1 1 d . . .
F158 F 0.3732(2) 1.0583(3) 0.24312(8) 0.0544(13) Uani 1 1 d . . .
F164 F 0.0180(2) 0.9552(4) 0.25142(9) 0.0702(17) Uani 1 1 d . . .
F165 F -0.0739(3) 0.9989(4) 0.22125(10) 0.0713(15) Uani 1 1 d U . .
F166 F -0.0695(3) 0.9666(4) 0.17567(11) 0.0803(17) Uani 1 1 d U . .
F167 F 0.0311(3) 0.8803(4) 0.16108(10) 0.0727(16) Uani 1 1 d U . .
F168 F 0.1231(2) 0.8254(3) 0.19130(8) 0.0511(13) Uani 1 1 d . . .
C171 C 0.4999(2) 0.2363(3) 0.03906(7) 0.0381(18) Uiso 1 1 d GD . .
C172 C 0.4837(2) 0.1636(2) 0.05274(9) 0.0421(19) Uiso 1 1 d G . .
H17A H 0.4861 0.1019 0.0474 0.051 Uiso 1 1 calc R . .
C173 C 0.4640(2) 0.1811(3) 0.07422(8) 0.047(2) Uiso 1 1 d G . .
H17B H 0.4529 0.1314 0.0836 0.056 Uiso 1 1 calc R . .
C174 C 0.4605(3) 0.2714(4) 0.08200(7) 0.047(2) Uiso 1 1 d G . .
H17C H 0.4470 0.2834 0.0967 0.057 Uiso 1 1 calc R . .
C175 C 0.4767(2) 0.3441(3) 0.06832(8) 0.047(2) Uiso 1 1 d G . .
H17D H 0.4743 0.4058 0.0736 0.056 Uiso 1 1 calc R . .
C176 C 0.4964(2) 0.3266(3) 0.04685(8) 0.0363(17) Uiso 1 1 d G . .
H17E H 0.5075 0.3763 0.0375 0.044 Uiso 1 1 calc R . .
C177 C 0.5188(4) 0.2199(6) 0.01514(16) 0.055(2) Uiso 1 1 d D . .
H17F H 0.5192 0.1535 0.0120 0.083 Uiso 1 1 calc R . .
H17G H 0.5600 0.2454 0.0140 0.083 Uiso 1 1 calc R . .
H17H H 0.4895 0.2503 0.0039 0.083 Uiso 1 1 calc R . .
C191 C 0.1758(2) 0.5783(4) 0.55608(11) 0.057(2) Uiso 1 1 d GD . .
C192 C 0.2393(2) 0.5851(3) 0.56021(10) 0.047(2) Uiso 1 1 d G . .
H19A H 0.2593 0.6420 0.5577 0.056 Uiso 1 1 calc R . .
C193 C 0.27355(19) 0.5088(4) 0.56803(10) 0.050(2) Uiso 1 1 d G . .
H19B H 0.3169 0.5134 0.5709 0.060 Uiso 1 1 calc R . .
C194 C 0.2444(3) 0.4256(3) 0.57171(11) 0.071(3) Uiso 1 1 d G . .
H19C H 0.2678 0.3734 0.5770 0.085 Uiso 1 1 calc R . .
C195 C 0.1809(3) 0.4188(3) 0.56758(12) 0.077(3) Uiso 1 1 d G . .
H19D H 0.1609 0.3620 0.5701 0.093 Uiso 1 1 calc R . .
C196 C 0.14665(19) 0.4951(4) 0.55976(12) 0.069(3) Uiso 1 1 d G . .
H19E H 0.1033 0.4905 0.5569 0.083 Uiso 1 1 calc R . .
C197 C 0.1381(6) 0.6603(9) 0.5477(2) 0.103(4) Uiso 1 1 d D . .
H19F H 0.1652 0.7132 0.5460 0.154 Uiso 1 1 calc R . .
H19G H 0.1087 0.6753 0.5588 0.154 Uiso 1 1 calc R . .
H19H H 0.1158 0.6458 0.5328 0.154 Uiso 1 1 calc R . .
C181 C 0.1892(2) 0.2665(4) 0.11204(12) 0.084(3) Uiso 1 1 d GD . .
C182 C 0.1860(2) 0.3391(4) 0.09647(11) 0.063(3) Uiso 1 1 d G . .
H18A H 0.1472 0.3612 0.0901 0.076 Uiso 1 1 calc R . .
C183 C 0.2396(3) 0.3795(4) 0.09017(10) 0.058(2) Uiso 1 1 d G . .
H18B H 0.2374 0.4291 0.0795 0.070 Uiso 1 1 calc R . .
C184 C 0.2964(2) 0.3473(4) 0.09944(11) 0.070(3) Uiso 1 1 d G . .
H18C H 0.3331 0.3749 0.0951 0.084 Uiso 1 1 calc R . .
C185 C 0.2996(2) 0.2747(4) 0.11501(11) 0.074(3) Uiso 1 1 d G . .
H18D H 0.3384 0.2527 0.1213 0.089 Uiso 1 1 calc R . .
C186 C 0.2460(3) 0.2343(4) 0.12131(10) 0.057(2) Uiso 1 1 d G . .
H18E H 0.2482 0.1847 0.1320 0.068 Uiso 1 1 calc R . .
C187 C 0.1343(8) 0.2210(12) 0.1195(3) 0.156(7) Uiso 1 1 d D . .
H18F H 0.0974 0.2494 0.1118 0.233 Uiso 1 1 calc R . .
H18G H 0.1338 0.2281 0.1361 0.233 Uiso 1 1 calc R . .
H18H H 0.1352 0.1553 0.1157 0.233 Uiso 1 1 calc R . .
C201 C 0.7285(3) 0.5305(4) 0.17045(13) 0.074(3) Uiso 1 1 d GD . .
C202 C 0.7144(2) 0.4416(5) 0.16279(12) 0.062(3) Uiso 1 1 d G . .
H20A H 0.6727 0.4236 0.1595 0.075 Uiso 1 1 calc R . .
C203 C 0.7612(3) 0.3789(4) 0.15994(13) 0.084(3) Uiso 1 1 d G . .
H20B H 0.7515 0.3182 0.1547 0.101 Uiso 1 1 calc R . .
C204 C 0.8221(3) 0.4052(5) 0.16475(14) 0.101(4) Uiso 1 1 d G . .
H20C H 0.8541 0.3624 0.1628 0.121 Uiso 1 1 calc R . .
C205 C 0.8363(2) 0.4941(5) 0.17241(13) 0.082(3) Uiso 1 1 d G . .
H20D H 0.8779 0.5121 0.1757 0.098 Uiso 1 1 calc R . .
C206 C 0.7894(3) 0.5568(4) 0.17526(12) 0.066(3) Uiso 1 1 d G . .
H20E H 0.7991 0.6176 0.1805 0.079 Uiso 1 1 calc R . .
C207 C 0.6833(7) 0.5917(10) 0.1737(3) 0.124(5) Uiso 1 1 d D . .
H20F H 0.6433 0.5629 0.1695 0.186 Uiso 1 1 calc R . .
H20G H 0.6878 0.6462 0.1641 0.186 Uiso 1 1 calc R . .
H20H H 0.6860 0.6101 0.1898 0.186 Uiso 1 1 calc R . .
C221 C 0.6950(3) 0.3584(4) 0.63574(10) 0.070(3) Uiso 1 1 d GD . .
C222 C 0.6423(3) 0.3151(5) 0.64205(9) 0.088(4) Uiso 1 1 d G . .
H22C H 0.6322 0.3185 0.6575 0.105 Uiso 1 1 calc R . .
C223 C 0.6045(3) 0.2669(5) 0.62582(12) 0.075(3) Uiso 1 1 d G . .
H22D H 0.5686 0.2374 0.6301 0.090 Uiso 1 1 calc R . .
C224 C 0.6193(3) 0.2619(4) 0.60327(11) 0.068(3) Uiso 1 1 d G . .
H22E H 0.5935 0.2290 0.5922 0.081 Uiso 1 1 calc R . .
C225 C 0.6720(3) 0.3052(4) 0.59696(9) 0.062(3) Uiso 1 1 d G . .
H22F H 0.6821 0.3018 0.5816 0.075 Uiso 1 1 calc R . .
C226 C 0.7098(2) 0.3534(4) 0.61319(11) 0.058(2) Uiso 1 1 d G . .
H22G H 0.7458 0.3830 0.6089 0.070 Uiso 1 1 calc R . .
C227 C 0.7378(7) 0.4101(10) 0.6526(3) 0.125(5) Uiso 1 1 d D . .
H22H H 0.7224 0.4077 0.6678 0.188 Uiso 1 1 calc R . .
H22I H 0.7404 0.4746 0.6477 0.188 Uiso 1 1 calc R . .
H22J H 0.7787 0.3819 0.6534 0.188 Uiso 1 1 calc R . .
C211 C 0.9610(5) 0.6810(7) 0.32957(19) 0.177(8) Uiso 1 1 d G . .
H21C H 0.9520 0.6273 0.3379 0.212 Uiso 1 1 calc R . .
C212 C 0.9982(5) 0.7496(9) 0.34000(14) 0.130(6) Uiso 1 1 d G . .
H21D H 1.0147 0.7428 0.3555 0.157 Uiso 1 1 calc R . .
C213 C 1.0113(4) 0.8283(7) 0.3278(2) 0.133(6) Uiso 1 1 d G . .
H21E H 1.0367 0.8752 0.3349 0.159 Uiso 1 1 calc R . .
C214 C 0.9872(5) 0.8383(6) 0.30510(19) 0.142(6) Uiso 1 1 d G . .
H21F H 0.9962 0.8920 0.2967 0.171 Uiso 1 1 calc R . .
C215 C 0.9500(5) 0.7697(8) 0.29468(14) 0.123(5) Uiso 1 1 d G . .
H21G H 0.9335 0.7766 0.2792 0.147 Uiso 1 1 calc R . .
C216 C 0.9369(4) 0.6911(7) 0.3069(2) 0.111(5) Uiso 1 1 d G . .
H21H H 0.9115 0.6442 0.2998 0.133 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0192(2) 0.0153(2) 0.0165(3) -0.00024(18) 0.00420(19) -0.00044(18)
Pd2 0.0215(2) 0.0261(3) 0.0167(3) -0.00129(19) 0.00252(19) 0.0007(2)
Sn1 0.0217(2) 0.0208(2) 0.0179(2) -0.00378(17) 0.00394(17) -0.00247(17)
Sn2 0.0220(2) 0.0189(2) 0.0243(3) 0.00041(17) 0.00928(18) -0.00052(17)
Sn3 0.0227(2) 0.0165(2) 0.0181(2) 0.00201(16) 0.00435(17) 0.00050(17)
Sn4 0.0217(2) 0.0158(2) 0.0168(2) -0.00108(16) 0.00281(17) 0.00054(16)
Sn5 0.0206(2) 0.0267(3) 0.0182(2) 0.00170(17) 0.00370(17) 0.00018(18)
Sn6 0.0273(2) 0.0239(2) 0.0191(2) 0.00015(18) 0.00383(18) -0.00134(18)
Sn7 0.0218(2) 0.0320(3) 0.0212(3) 0.00057(19) -0.00070(18) 0.00107(19)
Sn8 0.0302(2) 0.0351(3) 0.0204(3) -0.00795(19) 0.00259(19) 0.0037(2)
N11 0.028(3) 0.029(3) 0.017(3) -0.003(2) 0.002(2) -0.003(2)
N12 0.027(3) 0.021(3) 0.027(3) -0.005(2) 0.010(2) -0.006(2)
N13 0.027(3) 0.027(3) 0.029(3) -0.007(2) 0.011(2) -0.003(2)
N21 0.025(3) 0.026(3) 0.018(3) 0.001(2) 0.006(2) -0.006(2)
N22 0.034(3) 0.024(3) 0.042(4) -0.008(3) 0.012(3) 0.004(3)
N23 0.026(3) 0.030(3) 0.023(3) -0.005(2) 0.006(2) -0.001(2)
N31 0.032(3) 0.032(3) 0.015(3) -0.003(2) 0.008(2) -0.004(2)
N32 0.033(3) 0.019(3) 0.029(3) 0.006(2) 0.001(2) 0.007(2)
N33 0.027(3) 0.022(3) 0.020(3) 0.008(2) 0.002(2) -0.002(2)
N41 0.023(3) 0.018(3) 0.025(3) -0.003(2) 0.001(2) -0.003(2)
N42 0.028(3) 0.020(3) 0.021(3) 0.001(2) 0.003(2) 0.004(2)
N43 0.026(3) 0.021(3) 0.015(3) -0.001(2) 0.004(2) -0.004(2)
N51 0.025(3) 0.038(3) 0.020(3) 0.002(2) 0.005(2) -0.002(2)
N52 0.029(3) 0.031(3) 0.032(4) 0.007(3) 0.005(3) 0.002(3)
N53 0.028(3) 0.030(3) 0.025(3) -0.001(2) 0.005(2) -0.002(2)
N61 0.037(3) 0.027(3) 0.019(3) 0.007(2) -0.005(2) -0.004(3)
N62 0.034(3) 0.033(3) 0.023(3) 0.004(2) 0.006(3) 0.006(3)
N63 0.033(3) 0.034(3) 0.017(3) -0.006(2) 0.002(2) -0.003(3)
N71 0.036(3) 0.049(4) 0.020(3) -0.002(3) -0.005(3) 0.003(3)
N72 0.024(3) 0.035(3) 0.033(4) 0.000(3) 0.003(2) -0.002(3)
N73 0.027(3) 0.036(3) 0.031(4) -0.001(3) -0.006(3) 0.000(3)
N81 0.053(4) 0.040(4) 0.016(3) -0.011(3) -0.003(3) -0.002(3)
N82 0.034(3) 0.053(4) 0.040(4) -0.015(3) 0.006(3) 0.006(3)
N83 0.048(4) 0.053(4) 0.025(4) -0.007(3) 0.005(3) 0.013(3)
C1 0.034(4) 0.031(4) 0.043(5) -0.010(3) 0.014(3) 0.000(3)
C2 0.031(4) 0.045(5) 0.024(4) -0.001(3) 0.008(3) 0.000(3)
C3 0.030(3) 0.022(3) 0.023(4) -0.002(3) 0.005(3) -0.002(3)
C4 0.029(4) 0.033(4) 0.026(4) 0.002(3) 0.009(3) -0.007(3)
C5 0.035(4) 0.037(4) 0.023(4) -0.003(3) 0.007(3) -0.008(3)
C6 0.034(4) 0.049(5) 0.023(4) -0.005(3) 0.004(3) -0.006(3)
C7 0.043(4) 0.039(4) 0.036(5) -0.012(3) -0.002(3) -0.002(4)
C8 0.058(6) 0.072(7) 0.037(5) 0.004(4) 0.000(4) 0.016(5)
C11 0.027(3) 0.040(4) 0.026(4) -0.017(3) 0.006(3) -0.008(3)
C12 0.028(3) 0.036(4) 0.025(4) -0.005(3) 0.011(3) -0.009(3)
C13 0.029(4) 0.034(4) 0.024(4) -0.006(3) -0.007(3) -0.003(3)
C14 0.029(3) 0.040(4) 0.022(4) 0.000(3) 0.001(3) -0.003(3)
C15 0.033(4) 0.036(4) 0.034(4) -0.007(3) -0.006(3) 0.003(3)
C16 0.041(4) 0.037(4) 0.040(5) 0.008(4) -0.009(4) -0.004(4)
C17 0.051(5) 0.047(5) 0.023(4) 0.013(3) -0.007(4) -0.009(4)
C18 0.035(4) 0.047(5) 0.016(4) -0.003(3) -0.001(3) -0.006(3)
C21 0.037(4) 0.021(3) 0.028(4) -0.010(3) 0.010(3) -0.005(3)
C22 0.038(4) 0.028(4) 0.028(4) -0.010(3) 0.010(3) -0.013(3)
C23 0.025(3) 0.025(4) 0.022(4) 0.002(3) 0.008(3) -0.003(3)
C24 0.027(3) 0.029(4) 0.022(4) -0.003(3) 0.007(3) -0.006(3)
C25 0.024(3) 0.046(5) 0.027(4) 0.000(3) 0.008(3) -0.006(3)
C26 0.035(4) 0.040(5) 0.043(5) -0.008(4) 0.020(4) 0.003(3)
C27 0.031(4) 0.038(4) 0.027(4) -0.006(3) 0.007(3) -0.002(3)
C28 0.028(4) 0.031(4) 0.024(4) -0.004(3) 0.007(3) -0.005(3)
C31 0.034(4) 0.026(4) 0.028(4) -0.001(3) 0.018(3) -0.006(3)
C32 0.040(4) 0.025(4) 0.024(4) 0.006(3) 0.011(3) -0.009(3)
C33 0.024(3) 0.020(3) 0.031(4) -0.002(3) 0.009(3) 0.000(3)
C34 0.036(4) 0.028(4) 0.034(4) -0.001(3) 0.015(3) -0.004(3)
C35 0.019(3) 0.025(4) 0.045(5) 0.005(3) 0.003(3) -0.007(3)
C36 0.021(3) 0.028(4) 0.024(4) 0.001(3) 0.001(3) 0.001(3)
C37 0.027(3) 0.033(4) 0.025(4) 0.008(3) 0.009(3) 0.004(3)
C38 0.021(3) 0.020(3) 0.028(4) 0.002(3) 0.006(3) -0.003(3)
C41 0.039(4) 0.033(4) 0.027(4) -0.004(3) 0.016(3) 0.004(3)
C42 0.037(4) 0.030(4) 0.035(4) -0.013(3) 0.017(3) 0.001(3)
C43 0.034(4) 0.023(4) 0.066(6) 0.001(4) 0.030(4) 0.006(3)
C44 0.037(4) 0.024(4) 0.066(6) 0.011(4) 0.034(4) 0.008(3)
C45 0.042(5) 0.061(6) 0.059(6) 0.026(5) 0.022(4) 0.017(4)
C46 0.051(4) 0.041(4) 0.070(4) 0.022(3) 0.025(3) 0.014(3)
C47 0.054(4) 0.041(4) 0.076(5) -0.003(3) 0.029(4) 0.002(3)
C48 0.053(5) 0.025(4) 0.088(8) 0.002(4) 0.040(5) 0.001(4)
C51 0.038(4) 0.032(4) 0.014(4) 0.003(3) 0.006(3) -0.006(3)
C52 0.036(4) 0.031(4) 0.024(4) 0.002(3) 0.010(3) -0.009(3)
C53 0.029(3) 0.020(3) 0.026(4) 0.007(3) 0.004(3) -0.004(3)
C54 0.027(3) 0.030(4) 0.031(4) 0.005(3) 0.011(3) -0.003(3)
C55 0.038(4) 0.029(4) 0.026(4) 0.003(3) -0.006(3) -0.004(3)
C56 0.024(3) 0.034(4) 0.042(5) 0.007(3) 0.001(3) -0.008(3)
C57 0.029(4) 0.038(4) 0.045(5) 0.001(4) 0.020(3) 0.002(3)
C58 0.035(4) 0.030(4) 0.039(5) -0.010(3) 0.006(3) 0.000(3)
C61 0.026(3) 0.032(4) 0.023(4) 0.004(3) 0.003(3) 0.000(3)
C62 0.028(4) 0.036(4) 0.035(4) 0.006(3) -0.001(3) 0.008(3)
C63 0.030(4) 0.018(3) 0.047(5) 0.001(3) 0.020(3) 0.002(3)
C64 0.033(4) 0.011(3) 0.051(5) 0.005(3) 0.012(3) 0.002(3)
C65 0.028(4) 0.028(4) 0.056(6) -0.002(4) 0.006(4) 0.001(3)
C66 0.043(3) 0.023(3) 0.064(4) -0.005(3) 0.009(3) -0.001(3)
C67 0.044(5) 0.008(4) 0.101(8) 0.015(4) 0.011(5) 0.007(3)
C68 0.043(4) 0.025(4) 0.046(5) 0.004(3) 0.007(4) 0.006(3)
C71 0.027(3) 0.023(3) 0.021(4) -0.004(3) 0.005(3) 0.003(3)
C72 0.030(3) 0.019(3) 0.020(4) -0.003(3) 0.001(3) -0.003(3)
C73 0.022(3) 0.010(3) 0.028(4) 0.000(2) 0.003(3) 0.005(2)
C74 0.022(3) 0.017(3) 0.027(4) -0.001(3) -0.002(3) 0.004(3)
C75 0.026(3) 0.021(3) 0.030(4) -0.001(3) 0.006(3) -0.003(3)
C76 0.024(3) 0.023(4) 0.047(5) -0.005(3) 0.007(3) 0.001(3)
C77 0.031(4) 0.025(4) 0.031(4) -0.005(3) -0.002(3) 0.001(3)
C78 0.029(3) 0.021(3) 0.024(4) -0.002(3) -0.002(3) 0.003(3)
C81 0.018(3) 0.037(4) 0.031(4) -0.005(3) 0.002(3) 0.006(3)
C82 0.025(3) 0.032(4) 0.025(4) -0.004(3) -0.002(3) 0.009(3)
C83 0.019(3) 0.021(3) 0.029(4) 0.000(3) -0.005(3) 0.001(3)
C84 0.042(4) 0.025(4) 0.031(4) -0.003(3) 0.001(3) 0.003(3)
C85 0.047(4) 0.017(4) 0.042(5) 0.011(3) 0.000(4) 0.007(3)
C86 0.067(5) 0.032(4) 0.026(4) 0.020(3) 0.004(4) -0.004(4)
C87 0.038(4) 0.037(4) 0.030(4) 0.002(3) 0.009(3) -0.007(3)
C88 0.023(3) 0.030(4) 0.023(4) 0.001(3) 0.003(3) 0.006(3)
C91 0.026(4) 0.040(4) 0.035(4) -0.007(3) 0.000(3) -0.006(3)
C92 0.022(3) 0.048(5) 0.024(4) -0.005(3) 0.003(3) -0.011(3)
C93 0.020(3) 0.028(4) 0.036(4) 0.002(3) 0.004(3) 0.000(3)
C94 0.029(4) 0.056(5) 0.034(5) -0.004(4) -0.001(3) 0.005(4)
C95 0.024(4) 0.077(7) 0.053(6) -0.006(5) -0.007(4) 0.021(4)
C96 0.023(4) 0.065(6) 0.061(6) -0.015(5) 0.014(4) 0.016(4)
C97 0.037(4) 0.061(5) 0.016(4) -0.004(3) 0.010(3) -0.001(4)
C98 0.021(3) 0.041(4) 0.036(5) -0.002(3) -0.002(3) 0.002(3)
C101 0.033(4) 0.028(4) 0.046(5) -0.001(3) 0.006(3) 0.001(3)
C102 0.039(4) 0.027(4) 0.040(5) 0.006(3) 0.008(3) 0.004(3)
C103 0.022(3) 0.045(5) 0.039(5) 0.018(4) 0.006(3) 0.004(3)
C104 0.030(4) 0.055(6) 0.056(6) 0.025(5) 0.002(4) 0.004(4)
C105 0.040(3) 0.049(4) 0.055(4) 0.026(3) 0.006(3) -0.003(3)
C106 0.040(3) 0.070(4) 0.033(4) 0.021(3) 0.004(3) -0.002(3)
C107 0.027(4) 0.072(6) 0.046(5) 0.011(5) 0.008(4) 0.008(4)
C108 0.021(3) 0.066(6) 0.027(4) 0.023(4) 0.009(3) 0.007(3)
C111 0.044(4) 0.035(4) 0.034(5) -0.004(3) -0.014(3) 0.010(3)
C112 0.046(4) 0.027(4) 0.037(5) 0.003(3) -0.010(4) 0.000(3)
C113 0.040(4) 0.022(3) 0.017(4) -0.004(3) 0.000(3) -0.001(3)
C114 0.052(5) 0.034(4) 0.025(4) 0.005(3) -0.001(3) -0.010(4)
C115 0.051(5) 0.030(4) 0.034(5) 0.001(3) 0.005(4) -0.014(3)
C116 0.039(4) 0.035(4) 0.046(5) 0.005(4) 0.005(4) -0.011(3)
C117 0.042(4) 0.030(4) 0.026(4) 0.000(3) -0.005(3) -0.003(3)
C118 0.042(4) 0.022(4) 0.025(4) 0.001(3) 0.003(3) -0.004(3)
C121 0.038(4) 0.042(4) 0.020(4) -0.005(3) 0.002(3) -0.004(3)
C122 0.048(5) 0.048(5) 0.024(4) 0.004(3) 0.014(3) 0.001(4)
C123 0.043(4) 0.030(4) 0.023(4) 0.004(3) 0.020(3) -0.007(3)
C124 0.053(5) 0.040(5) 0.039(5) -0.006(4) 0.021(4) -0.002(4)
C125 0.081(7) 0.038(5) 0.044(5) -0.010(4) 0.033(5) 0.013(5)
C126 0.051(5) 0.056(6) 0.053(6) 0.021(5) 0.037(5) 0.029(4)
C127 0.044(5) 0.047(5) 0.041(5) 0.018(4) 0.022(4) 0.000(4)
C128 0.037(4) 0.028(4) 0.033(4) 0.006(3) 0.017(3) 0.001(3)
C131 0.039(4) 0.046(5) 0.032(5) 0.000(3) -0.009(3) -0.007(4)
C132 0.035(4) 0.054(5) 0.029(4) 0.003(4) -0.012(3) 0.005(4)
C133 0.021(3) 0.046(5) 0.036(4) 0.014(3) 0.005(3) 0.006(3)
C134 0.031(4) 0.044(5) 0.038(5) 0.013(4) 0.009(3) 0.006(3)
C135 0.025(4) 0.044(5) 0.072(7) 0.019(5) 0.007(4) 0.004(4)
C136 0.024(4) 0.067(7) 0.094(8) 0.055(6) 0.012(4) 0.001(4)
C137 0.042(4) 0.067(4) 0.042(4) 0.024(3) 0.008(3) -0.002(3)
C138 0.029(4) 0.086(7) 0.030(5) 0.013(5) -0.006(3) 0.000(4)
C141 0.036(4) 0.043(5) 0.054(6) -0.001(4) 0.000(4) -0.013(4)
C142 0.020(3) 0.057(5) 0.043(5) -0.003(4) 0.003(3) -0.003(3)
C143 0.034(4) 0.034(4) 0.021(4) 0.013(3) 0.013(3) 0.003(3)
C144 0.032(4) 0.026(4) 0.036(4) 0.003(3) 0.009(3) 0.003(3)
C145 0.054(5) 0.041(5) 0.037(5) 0.002(4) 0.016(4) -0.003(4)
C146 0.068(6) 0.027(4) 0.064(6) -0.005(4) 0.027(5) -0.001(4)
C147 0.051(5) 0.043(5) 0.052(6) 0.011(4) 0.024(4) 0.020(4)
C148 0.040(4) 0.050(5) 0.032(4) 0.010(4) 0.005(3) 0.016(4)
C151 0.063(6) 0.057(6) 0.032(5) -0.014(4) 0.005(4) -0.001(5)
C152 0.072(6) 0.048(5) 0.038(5) -0.013(4) -0.007(4) -0.003(5)
C153 0.029(4) 0.030(4) 0.036(4) -0.012(3) -0.002(3) 0.006(3)
C154 0.035(4) 0.036(4) 0.042(5) -0.009(4) -0.006(3) 0.004(3)
C155 0.044(4) 0.034(4) 0.032(5) -0.007(3) -0.009(3) 0.008(3)
C156 0.053(5) 0.029(4) 0.050(5) -0.003(4) 0.002(4) 0.013(4)
C157 0.036(4) 0.036(4) 0.054(6) -0.016(4) -0.003(4) 0.006(3)
C158 0.041(4) 0.026(4) 0.048(5) -0.008(3) -0.017(4) 0.002(3)
C161 0.058(5) 0.064(6) 0.032(5) -0.001(4) 0.015(4) 0.004(4)
C162 0.047(5) 0.078(7) 0.032(5) -0.006(4) 0.017(4) 0.013(4)
C163 0.029(4) 0.050(5) 0.038(5) -0.010(4) 0.011(3) -0.004(3)
C164 0.035(4) 0.075(7) 0.049(6) -0.023(5) 0.010(4) 0.004(4)
C165 0.027(4) 0.080(7) 0.077(7) -0.041(6) 0.002(4) 0.019(4)
C166 0.040(4) 0.075(4) 0.055(4) -0.008(4) -0.012(3) 0.010(3)
C167 0.048(4) 0.069(4) 0.040(4) -0.018(3) 0.002(3) 0.006(3)
C168 0.030(4) 0.065(6) 0.042(5) -0.026(4) -0.005(3) 0.005(4)
F14 0.042(2) 0.039(2) 0.025(2) -0.0030(18) 0.0103(18) 0.0053(19)
F15 0.044(3) 0.044(3) 0.050(3) -0.014(2) -0.005(2) 0.014(2)
F16 0.072(3) 0.041(3) 0.068(4) 0.008(2) -0.015(3) 0.012(3)
F17 0.077(3) 0.059(3) 0.039(3) 0.023(2) -0.005(2) -0.006(3)
F18 0.051(3) 0.051(3) 0.032(3) 0.002(2) 0.016(2) -0.002(2)
F24 0.030(2) 0.036(2) 0.035(2) -0.0093(18) 0.0052(17) -0.0095(17)
F25 0.027(2) 0.065(3) 0.060(3) -0.012(2) 0.014(2) -0.014(2)
F26 0.036(3) 0.071(4) 0.080(4) -0.025(3) 0.033(3) -0.005(2)
F27 0.046(3) 0.056(3) 0.054(3) -0.032(2) 0.023(2) -0.005(2)
F28 0.027(2) 0.032(2) 0.041(3) -0.0161(18) 0.0099(18) -0.0089(17)
F34 0.033(2) 0.077(3) 0.031(3) -0.003(2) 0.0157(19) -0.017(2)
F35 0.027(2) 0.075(3) 0.044(3) -0.002(2) 0.0104(19) -0.021(2)
F36 0.032(2) 0.044(3) 0.031(2) 0.0037(19) -0.0015(18) -0.0034(18)
F37 0.038(2) 0.056(3) 0.025(2) 0.0084(19) 0.0055(18) -0.010(2)
F38 0.0248(19) 0.042(2) 0.025(2) 0.0036(17) 0.0066(16) -0.0132(17)
F44 0.057(3) 0.043(3) 0.050(3) 0.011(2) 0.010(2) 0.008(2)
F45 0.073(4) 0.069(4) 0.086(5) 0.038(3) 0.035(3) 0.036(3)
F46 0.0756(18) 0.0741(18) 0.0781(19) 0.0039(10) 0.0101(10) 0.0031(10)
F47 0.0730(18) 0.0703(18) 0.0758(18) -0.0005(10) 0.0104(10) 0.0007(10)
F48 0.063(3) 0.032(3) 0.104(5) -0.019(3) 0.025(3) -0.007(2)
F54 0.033(2) 0.033(2) 0.030(2) -0.0076(17) 0.0123(17) -0.0055(17)
F55 0.046(2) 0.036(2) 0.043(3) -0.009(2) 0.005(2) -0.014(2)
F56 0.027(2) 0.045(3) 0.076(4) -0.005(2) 0.002(2) -0.011(2)
F57 0.035(3) 0.065(3) 0.084(4) -0.024(3) 0.032(3) -0.006(2)
F58 0.037(2) 0.044(3) 0.062(3) -0.022(2) 0.020(2) -0.006(2)
F64 0.051(2) 0.022(2) 0.029(2) 0.0014(17) 0.0035(19) 0.0037(18)
F65 0.053(3) 0.026(2) 0.070(4) -0.018(2) -0.001(2) 0.001(2)
F66 0.0621(16) 0.0575(16) 0.0636(16) -0.0012(10) 0.0045(10) 0.0006(10)
F67 0.0669(17) 0.0617(17) 0.0671(17) 0.0014(10) 0.0045(10) 0.0013(10)
F68 0.096(4) 0.027(3) 0.058(3) 0.015(2) -0.007(3) 0.007(2)
F74 0.029(2) 0.038(2) 0.017(2) -0.0015(16) 0.0016(15) -0.0038(17)
F75 0.036(2) 0.037(2) 0.033(2) 0.0007(18) 0.0139(18) -0.0066(18)
F76 0.029(2) 0.048(3) 0.057(3) 0.001(2) 0.007(2) -0.0124(19)
F77 0.030(2) 0.058(3) 0.046(3) -0.007(2) -0.010(2) -0.009(2)
F78 0.031(2) 0.040(2) 0.024(2) 0.0008(17) -0.0017(17) 0.0006(18)
F84 0.060(3) 0.023(2) 0.040(3) -0.0015(18) 0.004(2) 0.012(2)
F85 0.0598(15) 0.0542(15) 0.0563(16) 0.0031(10) 0.0048(10) 0.0018(10)
F86 0.0638(16) 0.0605(16) 0.0599(16) 0.0040(10) 0.0072(10) 0.0008(10)
F87 0.061(3) 0.043(3) 0.026(2) 0.0068(19) 0.021(2) 0.008(2)
F88 0.037(2) 0.024(2) 0.021(2) 0.0048(15) 0.0064(16) 0.0067(16)
F94 0.058(3) 0.090(4) 0.035(3) 0.003(3) -0.007(2) 0.034(3)
F95 0.0691(18) 0.0725(18) 0.0706(18) -0.0003(10) 0.0044(10) 0.0051(10)
F96 0.0660(17) 0.0695(17) 0.0683(17) -0.0023(10) 0.0074(10) 0.0040(10)
F97 0.054(3) 0.091(4) 0.036(3) -0.006(3) 0.013(2) 0.021(3)
F98 0.037(2) 0.077(3) 0.022(2) 0.002(2) 0.0018(18) 0.025(2)
F104 0.078(4) 0.045(3) 0.082(4) 0.031(3) 0.009(3) -0.008(3)
F105 0.0695(17) 0.0710(18) 0.0706(18) 0.0063(10) 0.0061(10) -0.0019(10)
F106 0.0785(19) 0.0814(19) 0.0771(19) 0.0043(10) 0.0085(10) -0.0012(10)
F107 0.0607(16) 0.0645(16) 0.0587(16) 0.0009(10) 0.0061(10) -0.0002(10)
F108 0.038(2) 0.051(3) 0.025(2) 0.0011(19) 0.0047(18) 0.001(2)
F114 0.073(3) 0.051(3) 0.028(3) 0.013(2) -0.010(2) -0.023(2)
F115 0.073(3) 0.045(3) 0.045(3) 0.012(2) 0.008(2) -0.027(2)
F116 0.052(3) 0.055(3) 0.063(3) 0.014(3) -0.007(2) -0.023(2)
F117 0.054(3) 0.053(3) 0.045(3) 0.016(2) -0.017(2) -0.019(2)
F118 0.045(2) 0.039(2) 0.031(2) 0.0092(19) -0.0019(19) -0.015(2)
F124 0.074(3) 0.055(3) 0.042(3) -0.018(2) 0.010(3) -0.007(3)
F125 0.0827(19) 0.0803(19) 0.0804(19) -0.0028(10) 0.0098(10) 0.0030(10)
F126 0.0695(17) 0.0711(17) 0.0709(18) 0.0018(10) 0.0099(10) 0.0039(10)
F127 0.032(2) 0.083(4) 0.068(4) 0.030(3) 0.006(2) 0.005(2)
F128 0.042(2) 0.039(3) 0.046(3) -0.003(2) 0.005(2) -0.005(2)
F134 0.054(3) 0.046(3) 0.041(3) 0.000(2) 0.019(2) -0.010(2)
F135 0.064(3) 0.036(3) 0.109(5) 0.010(3) 0.029(3) 0.002(3)
F136 0.0710(18) 0.0723(18) 0.0735(18) 0.0053(10) 0.0069(10) 0.0001(10)
F137 0.0793(19) 0.0825(19) 0.0780(19) 0.0043(10) 0.0079(10) -0.0012(10)
F138 0.066(4) 0.133(5) 0.022(3) 0.000(3) 0.001(2) -0.021(3)
F144 0.027(2) 0.034(2) 0.044(3) -0.0064(19) 0.0025(18) 0.0015(17)
F145 0.053(3) 0.050(3) 0.069(4) -0.026(3) 0.023(3) -0.016(2)
F146 0.0743(18) 0.0724(18) 0.0749(18) -0.0024(10) 0.0103(10) 0.0010(10)
F147 0.061(3) 0.075(4) 0.079(4) 0.008(3) 0.021(3) 0.038(3)
F148 0.031(2) 0.084(4) 0.043(3) 0.002(3) -0.003(2) 0.017(2)
F154 0.039(2) 0.055(3) 0.056(3) 0.002(2) -0.011(2) -0.006(2)
F155 0.053(3) 0.059(3) 0.049(3) 0.013(2) -0.014(2) 0.002(2)
F156 0.058(3) 0.040(3) 0.064(4) 0.008(2) 0.007(3) 0.003(2)
F157 0.047(3) 0.044(3) 0.079(4) -0.002(3) -0.014(3) -0.012(2)
F158 0.056(3) 0.056(3) 0.046(3) -0.002(2) -0.028(2) -0.006(2)
F164 0.054(3) 0.113(5) 0.045(3) -0.028(3) 0.013(2) 0.031(3)
F165 0.0689(17) 0.0735(18) 0.0716(18) -0.0032(10) 0.0073(10) 0.0027(10)
F166 0.0780(19) 0.0830(19) 0.0795(19) -0.0029(10) 0.0046(10) 0.0033(10)
F167 0.0711(18) 0.0752(18) 0.0714(18) -0.0037(10) 0.0046(10) 0.0032(10)
F168 0.039(2) 0.077(3) 0.037(3) -0.024(2) 0.001(2) 0.019(2)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pd1 Sn4 2.5651(6) . ?
Pd1 Sn3 2.5682(6) . ?
Pd1 Sn2 2.5707(6) . ?
Pd1 Sn1 2.5783(6) . ?
Pd2 Sn8 2.5840(7) . ?
Pd2 Sn6 2.5862(7) . ?
Pd2 Sn7 2.5863(6) . ?
Pd2 Sn5 2.5896(7) . ?
Sn1 N11 2.131(5) . ?
Sn1 N12 2.177(5) . ?
Sn1 N13 2.295(5) . ?
Sn2 N22 2.157(5) . ?
Sn2 N21 2.171(5) . ?
Sn2 N23 2.303(6) . ?
Sn3 N31 2.148(5) . ?
Sn3 N32 2.156(5) . ?
Sn3 N33 2.288(5) . ?
Sn4 N41 2.143(5) . ?
Sn4 N42 2.165(5) . ?
Sn4 N43 2.297(5) . ?
Sn5 N51 2.153(5) . ?
Sn5 N52 2.163(6) . ?
Sn5 N53 2.281(6) . ?
Sn6 N62 2.115(6) . ?
Sn6 N61 2.189(5) . ?
Sn6 N63 2.318(5) . ?
Sn7 N71 2.147(6) . ?
Sn7 N72 2.170(6) . ?
Sn7 N73 2.294(6) . ?
Sn8 N81 2.143(6) . ?
Sn8 N82 2.181(6) . ?
Sn8 N83 2.276(6) . ?
N11 C13 1.382(9) . ?
N11 C12 1.468(8) . ?
N12 C23 1.375(8) . ?
N12 C22 1.467(8) . ?
N13 C1 1.466(8) . ?
N13 C11 1.474(9) . ?
N13 C21 1.491(8) . ?
N21 C33 1.368(8) . ?
N21 C32 1.474(8) . ?
N22 C43 1.371(9) . ?
N22 C42 1.472(9) . ?
N23 C2 1.476(8) . ?
N23 C31 1.483(8) . ?
N23 C41 1.501(8) . ?
N31 C53 1.363(8) . ?
N31 C52 1.474(8) . ?
N32 C63 1.394(8) . ?
N32 C62 1.491(9) . ?
N33 C51 1.480(8) . ?
N33 C61 1.481(8) . ?
N33 C3 1.487(8) . ?
N41 C73 1.369(8) . ?
N41 C72 1.464(8) . ?
N42 C83 1.378(8) . ?
N42 C82 1.475(8) . ?
N43 C4 1.478(8) . ?
N43 C71 1.491(8) . ?
N43 C81 1.499(8) . ?
N51 C93 1.366(8) . ?
N51 C92 1.473(8) . ?
N52 C103 1.379(9) . ?
N52 C102 1.472(9) . ?
N53 C5 1.473(8) . ?
N53 C91 1.496(8) . ?
N53 C101 1.507(9) . ?
N61 C113 1.367(9) . ?
N61 C112 1.481(8) . ?
N62 C123 1.384(9) . ?
N62 C122 1.452(9) . ?
N63 C6 1.467(9) . ?
N63 C111 1.475(9) . ?
N63 C121 1.497(9) . ?
N71 C133 1.379(9) . ?
N71 C132 1.459(9) . ?
N72 C143 1.376(9) . ?
N72 C142 1.468(9) . ?
N73 C7 1.486(9) . ?
N73 C141 1.489(10) . ?
N73 C131 1.500(9) . ?
N81 C153 1.372(10) . ?
N81 C152 1.475(10) . ?
N82 C163 1.378(10) . ?
N82 C162 1.451(10) . ?
N83 C161 1.468(11) . ?
N83 C8 1.484(10) . ?
N83 C151 1.513(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C11 C12 1.498(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.397(10) . ?
C13 C18 1.403(10) . ?
C14 F14 1.354(8) . ?
C14 C15 1.367(10) . ?
C15 F15 1.353(8) . ?
C15 C16 1.380(11) . ?
C16 F16 1.354(9) . ?
C16 C17 1.361(12) . ?
C17 F17 1.341(9) . ?
C17 C18 1.383(11) . ?
C18 F18 1.345(8) . ?
C21 C22 1.511(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.401(9) . ?
C23 C28 1.408(9) . ?
C24 F24 1.356(7) . ?
C24 C25 1.387(9) . ?
C25 F25 1.346(8) . ?
C25 C26 1.369(10) . ?
C26 F26 1.349(8) . ?
C26 C27 1.369(10) . ?
C27 F27 1.338(8) . ?
C27 C28 1.377(10) . ?
C28 F28 1.361(7) . ?
C31 C32 1.524(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C38 1.396(9) . ?
C33 C34 1.423(9) . ?
C34 F34 1.364(8) . ?
C34 C35 1.373(10) . ?
C35 F35 1.333(7) . ?
C35 C36 1.362(10) . ?
C36 F36 1.367(7) . ?
C36 C37 1.378(9) . ?
C37 F37 1.350(7) . ?
C37 C38 1.361(9) . ?
C38 F38 1.357(7) . ?
C41 C42 1.520(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.396(12) . ?
C43 C48 1.403(11) . ?
C44 F44 1.367(9) . ?
C44 C45 1.372(11) . ?
C45 F45 1.329(11) . ?
C45 C46 1.424(13) . ?
C46 C47 1.308(13) . ?
C46 F46 1.373(10) . ?
C47 F47 1.356(10) . ?
C47 C48 1.393(13) . ?
C48 F48 1.330(12) . ?
C51 C52 1.494(9) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.413(9) . ?
C53 C58 1.418(10) . ?
C54 F54 1.359(8) . ?
C54 C55 1.359(9) . ?
C55 F55 1.349(8) . ?
C55 C56 1.387(10) . ?
C56 F56 1.334(7) . ?
C56 C57 1.379(10) . ?
C57 F57 1.329(8) . ?
C57 C58 1.379(10) . ?
C58 F58 1.350(8) . ?
C61 C62 1.500(9) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.389(10) . ?
C63 C68 1.388(10) . ?
C64 F64 1.348(7) . ?
C64 C65 1.372(10) . ?
C65 F65 1.341(9) . ?
C65 C66 1.389(11) . ?
C66 C67 1.342(12) . ?
C66 F66 1.357(9) . ?
C67 F67 1.342(9) . ?
C67 C68 1.403(11) . ?
C68 F68 1.352(9) . ?
C71 C72 1.515(8) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.398(9) . ?
C73 C78 1.417(9) . ?
C74 F74 1.358(7) . ?
C74 C75 1.360(9) . ?
C75 F75 1.350(8) . ?
C75 C76 1.374(10) . ?
C76 F76 1.329(8) . ?
C76 C77 1.394(10) . ?
C77 F77 1.353(8) . ?
C77 C78 1.370(9) . ?
C78 F78 1.346(8) . ?
C81 C82 1.498(9) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 C84 1.397(9) . ?
C83 C88 1.402(9) . ?
C84 F84 1.359(8) . ?
C84 C85 1.375(10) . ?
C85 F85 1.339(8) . ?
C85 C86 1.358(11) . ?
C86 F86 1.343(8) . ?
C86 C87 1.378(10) . ?
C87 F87 1.359(8) . ?
C87 C88 1.357(10) . ?
C88 F88 1.354(7) . ?
C91 C92 1.500(10) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 C98 1.393(10) . ?
C93 C94 1.395(10) . ?
C94 F94 1.363(9) . ?
C94 C95 1.383(11) . ?
C95 C96 1.345(12) . ?
C95 F95 1.368(9) . ?
C96 C97 1.354(11) . ?
C96 F96 1.356(9) . ?
C97 F97 1.341(8) . ?
C97 C98 1.391(10) . ?
C98 F98 1.349(8) . ?
C101 C102 1.499(10) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C103 C108 1.388(11) . ?
C103 C104 1.429(11) . ?
C104 F104 1.343(11) . ?
C104 C105 1.397(12) . ?
C105 C106 1.288(12) . ?
C105 F105 1.356(9) . ?
C106 F106 1.364(10) . ?
C106 C107 1.398(12) . ?
C107 F107 1.327(10) . ?
C107 C108 1.382(11) . ?
C108 F108 1.380(9) . ?
C111 C112 1.496(11) . ?
C111 H11C 0.9900 . ?
C111 H11D 0.9900 . ?
C112 H11E 0.9900 . ?
C112 H11F 0.9900 . ?
C113 C114 1.396(10) . ?
C113 C118 1.410(9) . ?
C114 F114 1.341(8) . ?
C114 C115 1.402(10) . ?
C115 F115 1.343(8) . ?
C115 C116 1.356(11) . ?
C116 F116 1.343(8) . ?
C116 C117 1.380(10) . ?
C117 F117 1.357(8) . ?
C117 C118 1.358(10) . ?
C118 F118 1.364(8) . ?
C121 C122 1.519(10) . ?
C121 H12C 0.9900 . ?
C121 H12D 0.9900 . ?
C122 H12E 0.9900 . ?
C122 H12F 0.9900 . ?
C123 C124 1.381(10) . ?
C123 C128 1.385(10) . ?
C124 F124 1.355(9) . ?
C124 C125 1.383(12) . ?
C125 C126 1.328(13) . ?
C125 F125 1.367(10) . ?
C126 F126 1.348(9) . ?
C126 C127 1.353(12) . ?
C127 F127 1.361(10) . ?
C127 C128 1.398(10) . ?
C128 F128 1.358(8) . ?
C131 C132 1.503(11) . ?
C131 H13A 0.9900 . ?
C131 H13B 0.9900 . ?
C132 H13C 0.9900 . ?
C132 H13D 0.9900 . ?
C133 C134 1.402(11) . ?
C133 C138 1.408(11) . ?
C134 F134 1.349(9) . ?
C134 C135 1.372(11) . ?
C135 F135 1.334(10) . ?
C135 C136 1.379(13) . ?
C136 F136 1.333(10) . ?
C136 C137 1.325(14) . ?
C137 F137 1.384(10) . ?
C137 C138 1.379(12) . ?
C138 F138 1.339(11) . ?
C141 C142 1.499(11) . ?
C141 H14A 0.9900 . ?
C141 H14B 0.9900 . ?
C142 H14C 0.9900 . ?
C142 H14D 0.9900 . ?
C143 C144 1.394(10) . ?
C143 C148 1.415(10) . ?
C144 F144 1.355(8) . ?
C144 C145 1.358(10) . ?
C145 F145 1.345(9) . ?
C145 C146 1.385(12) . ?
C146 F146 1.360(9) . ?
C146 C147 1.368(13) . ?
C147 F147 1.348(9) . ?
C147 C148 1.353(11) . ?
C148 F148 1.365(9) . ?
C151 C152 1.462(12) . ?
C151 H15A 0.9900 . ?
C151 H15B 0.9900 . ?
C152 H15C 0.9900 . ?
C152 H15D 0.9900 . ?
C153 C154 1.387(10) . ?
C153 C158 1.413(10) . ?
C154 C155 1.357(11) . ?
C154 F154 1.360(8) . ?
C155 F155 1.353(8) . ?
C155 C156 1.356(11) . ?
C156 F156 1.351(9) . ?
C156 C157 1.386(11) . ?
C157 F157 1.357(9) . ?
C157 C158 1.357(11) . ?
C158 F158 1.343(8) . ?
C161 C162 1.519(12) . ?
C161 H16A 0.9900 . ?
C161 H16B 0.9900 . ?
C162 H16C 0.9900 . ?
C162 H16D 0.9900 . ?
C163 C168 1.383(11) . ?
C163 C164 1.422(11) . ?
C164 F164 1.363(10) . ?
C164 C165 1.366(12) . ?
C165 C166 1.346(13) . ?
C165 F165 1.361(9) . ?
C166 F166 1.344(10) . ?
C166 C167 1.378(12) . ?
C167 F167 1.355(10) . ?
C167 C168 1.369(11) . ?
C168 F168 1.380(9) . ?
C171 C172 1.3900 . ?
C171 C176 1.3900 . ?
C171 C177 1.516(10) . ?
C172 C173 1.3900 . ?
C172 H17A 0.9500 . ?
C173 C174 1.3900 . ?
C173 H17B 0.9500 . ?
C174 C175 1.3900 . ?
C174 H17C 0.9500 . ?
C175 C176 1.3900 . ?
C175 H17D 0.9500 . ?
C176 H17E 0.9500 . ?
C177 H17F 0.9800 . ?
C177 H17G 0.9800 . ?
C177 H17H 0.9800 . ?
C191 C192 1.3900 . ?
C191 C196 1.3900 . ?
C191 C197 1.503(13) . ?
C192 C193 1.3900 . ?
C192 H19A 0.9500 . ?
C193 C194 1.3900 . ?
C193 H19B 0.9500 . ?
C194 C195 1.3900 . ?
C194 H19C 0.9500 . ?
C195 C196 1.3900 . ?
C195 H19D 0.9500 . ?
C196 H19E 0.9500 . ?
C197 H19F 0.9800 . ?
C197 H19G 0.9800 . ?
C197 H19H 0.9800 . ?
C181 C182 1.3900 . ?
C181 C186 1.3900 . ?
C181 C187 1.472(18) . ?
C182 C183 1.3900 . ?
C182 H18A 0.9500 . ?
C183 C184 1.3900 . ?
C183 H18B 0.9500 . ?
C184 C185 1.3900 . ?
C184 H18C 0.9500 . ?
C185 C186 1.3900 . ?
C185 H18D 0.9500 . ?
C186 H18E 0.9500 . ?
C187 H18F 0.9800 . ?
C187 H18G 0.9800 . ?
C187 H18H 0.9800 . ?
C201 C207 1.354(14) . ?
C201 C202 1.3900 . ?
C201 C206 1.3900 . ?
C202 C203 1.3900 . ?
C202 H20A 0.9500 . ?
C203 C204 1.3900 . ?
C203 H20B 0.9500 . ?
C204 C205 1.3900 . ?
C204 H20C 0.9500 . ?
C205 C206 1.3900 . ?
C205 H20D 0.9500 . ?
C206 H20E 0.9500 . ?
C207 H20F 0.9800 . ?
C207 H20G 0.9800 . ?
C207 H20H 0.9800 . ?
C221 C222 1.3900 . ?
C221 C226 1.3900 . ?
C221 C227 1.499(15) . ?
C222 C223 1.3900 . ?
C222 H22C 0.9500 . ?
C223 C224 1.3900 . ?
C223 H22D 0.9500 . ?
C224 C225 1.3900 . ?
C224 H22E 0.9500 . ?
C225 C226 1.3900 . ?
C225 H22F 0.9500 . ?
C226 H22G 0.9500 . ?
C227 H22H 0.9800 . ?
C227 H22I 0.9800 . ?
C227 H22J 0.9800 . ?
C211 C212 1.3900 . ?
C211 C216 1.3900 . ?
C211 H21C 0.9500 . ?
C212 C213 1.3900 . ?
C212 H21D 0.9500 . ?
C213 C214 1.3900 . ?
C213 H21E 0.9500 . ?
C214 C215 1.3900 . ?
C214 H21F 0.9500 . ?
C215 C216 1.3900 . ?
C215 H21G 0.9500 . ?
C216 H21H 0.9500 . ?
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
Sn4 Pd1 Sn3 107.56(2) . . ?
Sn4 Pd1 Sn2 110.07(2) . . ?
Sn3 Pd1 Sn2 108.21(2) . . ?
Sn4 Pd1 Sn1 108.78(2) . . ?
Sn3 Pd1 Sn1 111.44(2) . . ?
Sn2 Pd1 Sn1 110.72(2) . . ?
Sn8 Pd2 Sn6 110.64(2) . . ?
Sn8 Pd2 Sn7 110.65(2) . . ?
Sn6 Pd2 Sn7 108.99(2) . . ?
Sn8 Pd2 Sn5 109.12(2) . . ?
Sn6 Pd2 Sn5 111.22(2) . . ?
Sn7 Pd2 Sn5 106.13(2) . . ?
N11 Sn1 N12 100.2(2) . . ?
N11 Sn1 N13 77.0(2) . . ?
N12 Sn1 N13 76.85(19) . . ?
N11 Sn1 Pd1 123.69(14) . . ?
N12 Sn1 Pd1 133.13(15) . . ?
N13 Sn1 Pd1 124.97(14) . . ?
N22 Sn2 N21 98.8(2) . . ?
N22 Sn2 N23 77.1(2) . . ?
N21 Sn2 N23 76.88(19) . . ?
N22 Sn2 Pd1 127.23(16) . . ?
N21 Sn2 Pd1 131.53(14) . . ?
N23 Sn2 Pd1 123.15(13) . . ?
N31 Sn3 N32 101.0(2) . . ?
N31 Sn3 N33 76.91(19) . . ?
N32 Sn3 N33 76.4(2) . . ?
N31 Sn3 Pd1 127.79(15) . . ?
N32 Sn3 Pd1 127.98(15) . . ?
N33 Sn3 Pd1 126.34(13) . . ?
N41 Sn4 N42 102.0(2) . . ?
N41 Sn4 N43 77.05(19) . . ?
N42 Sn4 N43 76.84(19) . . ?
N41 Sn4 Pd1 121.63(14) . . ?
N42 Sn4 Pd1 133.50(14) . . ?
N43 Sn4 Pd1 125.12(13) . . ?
N51 Sn5 N52 100.9(2) . . ?
N51 Sn5 N53 77.5(2) . . ?
N52 Sn5 N53 78.2(2) . . ?
N51 Sn5 Pd2 125.95(15) . . ?
N52 Sn5 Pd2 130.58(15) . . ?
N53 Sn5 Pd2 122.60(14) . . ?
N62 Sn6 N61 93.7(2) . . ?
N62 Sn6 N63 78.1(2) . . ?
N61 Sn6 N63 76.1(2) . . ?
N62 Sn6 Pd2 126.75(15) . . ?
N61 Sn6 Pd2 136.42(15) . . ?
N63 Sn6 Pd2 123.02(14) . . ?
N71 Sn7 N72 98.1(2) . . ?
N71 Sn7 N73 76.5(2) . . ?
N72 Sn7 N73 77.0(2) . . ?
N71 Sn7 Pd2 128.26(16) . . ?
N72 Sn7 Pd2 131.24(15) . . ?
N73 Sn7 Pd2 123.17(14) . . ?
N81 Sn8 N82 99.3(2) . . ?
N81 Sn8 N83 77.5(2) . . ?
N82 Sn8 N83 76.3(2) . . ?
N81 Sn8 Pd2 122.49(17) . . ?
N82 Sn8 Pd2 135.67(17) . . ?
N83 Sn8 Pd2 123.46(16) . . ?
C13 N11 C12 117.8(6) . . ?
C13 N11 Sn1 126.1(4) . . ?
C12 N11 Sn1 115.5(4) . . ?
C23 N12 C22 117.5(5) . . ?
C23 N12 Sn1 127.4(4) . . ?
C22 N12 Sn1 114.9(4) . . ?
C1 N13 C11 109.9(5) . . ?
C1 N13 C21 109.7(5) . . ?
C11 N13 C21 113.0(5) . . ?
C1 N13 Sn1 114.0(4) . . ?
C11 N13 Sn1 107.2(4) . . ?
C21 N13 Sn1 103.0(4) . . ?
C33 N21 C32 116.7(5) . . ?
C33 N21 Sn2 127.9(4) . . ?
C32 N21 Sn2 115.4(4) . . ?
C43 N22 C42 117.3(6) . . ?
C43 N22 Sn2 126.0(5) . . ?
C42 N22 Sn2 114.9(4) . . ?
C2 N23 C31 109.0(5) . . ?
C2 N23 C41 110.9(5) . . ?
C31 N23 C41 112.3(5) . . ?
C2 N23 Sn2 114.1(4) . . ?
C31 N23 Sn2 103.3(4) . . ?
C41 N23 Sn2 107.1(4) . . ?
C53 N31 C52 118.5(5) . . ?
C53 N31 Sn3 124.9(4) . . ?
C52 N31 Sn3 115.5(4) . . ?
C63 N32 C62 117.1(5) . . ?
C63 N32 Sn3 126.3(4) . . ?
C62 N32 Sn3 116.0(4) . . ?
C51 N33 C61 112.2(5) . . ?
C51 N33 C3 109.5(5) . . ?
C61 N33 C3 109.4(5) . . ?
C51 N33 Sn3 107.6(4) . . ?
C61 N33 Sn3 104.3(4) . . ?
C3 N33 Sn3 113.8(4) . . ?
C73 N41 C72 118.9(5) . . ?
C73 N41 Sn4 124.9(4) . . ?
C72 N41 Sn4 116.2(4) . . ?
C83 N42 C82 116.8(5) . . ?
C83 N42 Sn4 127.4(4) . . ?
C82 N42 Sn4 115.6(4) . . ?
C4 N43 C71 110.6(5) . . ?
C4 N43 C81 110.7(5) . . ?
C71 N43 C81 110.8(5) . . ?
C4 N43 Sn4 114.4(4) . . ?
C71 N43 Sn4 106.9(4) . . ?
C81 N43 Sn4 103.2(4) . . ?
C93 N51 C92 119.4(5) . . ?
C93 N51 Sn5 124.1(4) . . ?
C92 N51 Sn5 114.1(4) . . ?
C103 N52 C102 117.2(6) . . ?
C103 N52 Sn5 128.0(5) . . ?
C102 N52 Sn5 114.0(4) . . ?
C5 N53 C91 110.4(5) . . ?
C5 N53 C101 109.8(5) . . ?
C91 N53 C101 111.1(5) . . ?
C5 N53 Sn5 113.5(4) . . ?
C91 N53 Sn5 107.4(4) . . ?
C101 N53 Sn5 104.5(4) . . ?
C113 N61 C112 117.6(5) . . ?
C113 N61 Sn6 124.5(4) . . ?
C112 N61 Sn6 115.9(4) . . ?
C123 N62 C122 116.4(6) . . ?
C123 N62 Sn6 127.0(5) . . ?
C122 N62 Sn6 111.9(4) . . ?
C6 N63 C111 109.5(6) . . ?
C6 N63 C121 108.5(5) . . ?
C111 N63 C121 113.6(6) . . ?
C6 N63 Sn6 113.9(4) . . ?
C111 N63 Sn6 104.2(4) . . ?
C121 N63 Sn6 107.2(4) . . ?
C133 N71 C132 117.5(6) . . ?
C133 N71 Sn7 125.9(5) . . ?
C132 N71 Sn7 116.4(5) . . ?
C143 N72 C142 117.6(6) . . ?
C143 N72 Sn7 125.9(4) . . ?
C142 N72 Sn7 115.8(4) . . ?
C7 N73 C141 110.3(6) . . ?
C7 N73 C131 110.3(6) . . ?
C141 N73 C131 110.7(6) . . ?
C7 N73 Sn7 114.3(4) . . ?
C141 N73 Sn7 103.0(4) . . ?
C131 N73 Sn7 108.1(4) . . ?
C153 N81 C152 119.2(6) . . ?
C153 N81 Sn8 123.0(4) . . ?
C152 N81 Sn8 115.8(5) . . ?
C163 N82 C162 117.3(6) . . ?
C163 N82 Sn8 126.2(5) . . ?
C162 N82 Sn8 116.1(5) . . ?
C161 N83 C8 109.6(7) . . ?
C161 N83 C151 111.7(6) . . ?
C8 N83 C151 110.8(7) . . ?
C161 N83 Sn8 104.5(5) . . ?
C8 N83 Sn8 113.6(5) . . ?
C151 N83 Sn8 106.5(5) . . ?
N13 C1 H1A 109.5 . . ?
N13 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N13 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N23 C2 H2A 109.5 . . ?
N23 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N23 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N33 C3 H3A 109.5 . . ?
N33 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N33 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N43 C4 H4A 109.5 . . ?
N43 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N43 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N53 C5 H5A 109.5 . . ?
N53 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N53 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N63 C6 H6A 109.5 . . ?
N63 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N63 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N73 C7 H7A 109.5 . . ?
N73 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N73 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N83 C8 H8A 109.5 . . ?
N83 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N83 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N13 C11 C12 110.9(5) . . ?
N13 C11 H11A 109.5 . . ?
C12 C11 H11A 109.5 . . ?
N13 C11 H11B 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 108.0 . . ?
N11 C12 C11 107.9(5) . . ?
N11 C12 H12A 110.1 . . ?
C11 C12 H12A 110.1 . . ?
N11 C12 H12B 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
N11 C13 C14 119.9(6) . . ?
N11 C13 C18 126.5(7) . . ?
C14 C13 C18 113.6(7) . . ?
F14 C14 C15 117.9(6) . . ?
F14 C14 C13 118.4(6) . . ?
C15 C14 C13 123.7(7) . . ?
F15 C15 C14 119.8(7) . . ?
F15 C15 C16 119.6(7) . . ?
C14 C15 C16 120.5(7) . . ?
F16 C16 C17 120.6(7) . . ?
F16 C16 C15 121.1(8) . . ?
C17 C16 C15 118.3(7) . . ?
F17 C17 C16 120.1(7) . . ?
F17 C17 C18 119.2(8) . . ?
C16 C17 C18 120.7(7) . . ?
F18 C18 C17 117.6(7) . . ?
F18 C18 C13 119.3(7) . . ?
C17 C18 C13 123.1(7) . . ?
N13 C21 C22 109.8(5) . . ?
N13 C21 H21A 109.7 . . ?
C22 C21 H21A 109.7 . . ?
N13 C21 H21B 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
N12 C22 C21 109.8(5) . . ?
N12 C22 H22A 109.7 . . ?
C21 C22 H22A 109.7 . . ?
N12 C22 H22B 109.7 . . ?
C21 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
N12 C23 C24 127.1(6) . . ?
N12 C23 C28 121.2(6) . . ?
C24 C23 C28 111.7(6) . . ?
F24 C24 C25 115.1(6) . . ?
F24 C24 C23 121.2(6) . . ?
C25 C24 C23 123.7(6) . . ?
F25 C25 C26 120.2(6) . . ?
F25 C25 C24 118.6(6) . . ?
C26 C25 C24 121.2(6) . . ?
F26 C26 C27 120.2(7) . . ?
F26 C26 C25 121.6(7) . . ?
C27 C26 C25 118.2(7) . . ?
F27 C27 C26 120.5(6) . . ?
F27 C27 C28 119.8(6) . . ?
C26 C27 C28 119.6(7) . . ?
F28 C28 C27 117.5(6) . . ?
F28 C28 C23 116.9(6) . . ?
C27 C28 C23 125.6(6) . . ?
N23 C31 C32 110.1(5) . . ?
N23 C31 H31A 109.6 . . ?
C32 C31 H31A 109.6 . . ?
N23 C31 H31B 109.6 . . ?
C32 C31 H31B 109.6 . . ?
H31A C31 H31B 108.2 . . ?
N21 C32 C31 109.4(5) . . ?
N21 C32 H32A 109.8 . . ?
C31 C32 H32A 109.8 . . ?
N21 C32 H32B 109.8 . . ?
C31 C32 H32B 109.8 . . ?
H32A C32 H32B 108.2 . . ?
N21 C33 C38 121.7(6) . . ?
N21 C33 C34 126.7(6) . . ?
C38 C33 C34 111.7(6) . . ?
F34 C34 C35 115.4(6) . . ?
F34 C34 C33 120.7(6) . . ?
C35 C34 C33 123.8(7) . . ?
F35 C35 C36 119.4(6) . . ?
F35 C35 C34 120.0(7) . . ?
C36 C35 C34 120.6(6) . . ?
C35 C36 F36 120.7(6) . . ?
C35 C36 C37 118.5(6) . . ?
F36 C36 C37 120.8(6) . . ?
F37 C37 C38 120.0(6) . . ?
F37 C37 C36 119.9(6) . . ?
C38 C37 C36 120.1(6) . . ?
F38 C38 C37 118.2(6) . . ?
F38 C38 C33 116.5(5) . . ?
C37 C38 C33 125.3(6) . . ?
N23 C41 C42 110.1(5) . . ?
N23 C41 H41A 109.6 . . ?
C42 C41 H41A 109.6 . . ?
N23 C41 H41B 109.6 . . ?
C42 C41 H41B 109.6 . . ?
H41A C41 H41B 108.2 . . ?
N22 C42 C41 107.0(5) . . ?
N22 C42 H42A 110.3 . . ?
C41 C42 H42A 110.3 . . ?
N22 C42 H42B 110.3 . . ?
C41 C42 H42B 110.3 . . ?
H42A C42 H42B 108.6 . . ?
N22 C43 C44 119.6(7) . . ?
N22 C43 C48 126.2(9) . . ?
C44 C43 C48 114.1(8) . . ?
F44 C44 C45 116.1(8) . . ?
F44 C44 C43 118.7(6) . . ?
C45 C44 C43 125.2(8) . . ?
F45 C45 C44 121.5(9) . . ?
F45 C45 C46 121.3(8) . . ?
C44 C45 C46 117.1(9) . . ?
C47 C46 F46 123.5(9) . . ?
C47 C46 C45 119.7(8) . . ?
F46 C46 C45 116.8(9) . . ?
C46 C47 F47 119.2(9) . . ?
C46 C47 C48 122.6(9) . . ?
F47 C47 C48 118.0(9) . . ?
F48 C48 C47 118.3(8) . . ?
F48 C48 C43 120.5(8) . . ?
C47 C48 C43 121.2(10) . . ?
N33 C51 C52 111.3(5) . . ?
N33 C51 H51A 109.4 . . ?
C52 C51 H51A 109.4 . . ?
N33 C51 H51B 109.4 . . ?
C52 C51 H51B 109.4 . . ?
H51A C51 H51B 108.0 . . ?
N31 C52 C51 107.9(6) . . ?
N31 C52 H52A 110.1 . . ?
C51 C52 H52A 110.1 . . ?
N31 C52 H52B 110.1 . . ?
C51 C52 H52B 110.1 . . ?
H52A C52 H52B 108.4 . . ?
N31 C53 C54 120.2(6) . . ?
N31 C53 C58 126.9(6) . . ?
C54 C53 C58 112.8(6) . . ?
F54 C54 C55 118.5(6) . . ?
F54 C54 C53 117.4(6) . . ?
C55 C54 C53 124.0(6) . . ?
F55 C55 C54 120.1(7) . . ?
F55 C55 C56 118.5(6) . . ?
C54 C55 C56 121.3(7) . . ?
F56 C56 C57 121.8(7) . . ?
F56 C56 C55 121.0(7) . . ?
C57 C56 C55 117.2(6) . . ?
F57 C57 C56 118.6(7) . . ?
F57 C57 C58 119.9(7) . . ?
C56 C57 C58 121.4(6) . . ?
F58 C58 C57 117.6(6) . . ?
F58 C58 C53 119.4(6) . . ?
C57 C58 C53 123.0(6) . . ?
N33 C61 C62 110.2(5) . . ?
N33 C61 H61A 109.6 . . ?
C62 C61 H61A 109.6 . . ?
N33 C61 H61B 109.6 . . ?
C62 C61 H61B 109.6 . . ?
H61A C61 H61B 108.1 . . ?
N32 C62 C61 108.7(5) . . ?
N32 C62 H62A 110.0 . . ?
C61 C62 H62A 110.0 . . ?
N32 C62 H62B 110.0 . . ?
C61 C62 H62B 110.0 . . ?
H62A C62 H62B 108.3 . . ?
C64 C63 C68 114.2(6) . . ?
C64 C63 N32 120.4(6) . . ?
C68 C63 N32 125.4(7) . . ?
F64 C64 C65 117.5(7) . . ?
F64 C64 C63 118.2(6) . . ?
C65 C64 C63 124.3(7) . . ?
F65 C65 C64 119.9(7) . . ?
F65 C65 C66 120.7(7) . . ?
C64 C65 C66 119.4(8) . . ?
C67 C66 F66 122.5(7) . . ?
C67 C66 C65 118.6(7) . . ?
F66 C66 C65 118.9(8) . . ?
F67 C67 C66 120.7(7) . . ?
F67 C67 C68 118.1(8) . . ?
C66 C67 C68 121.2(7) . . ?
F68 C68 C63 123.4(7) . . ?
F68 C68 C67 114.3(7) . . ?
C63 C68 C67 122.2(8) . . ?
N43 C71 C72 110.1(5) . . ?
N43 C71 H71A 109.6 . . ?
C72 C71 H71A 109.6 . . ?
N43 C71 H71B 109.6 . . ?
C72 C71 H71B 109.6 . . ?
H71A C71 H71B 108.1 . . ?
N41 C72 C71 108.6(5) . . ?
N41 C72 H72A 110.0 . . ?
C71 C72 H72A 110.0 . . ?
N41 C72 H72B 110.0 . . ?
C71 C72 H72B 110.0 . . ?
H72A C72 H72B 108.4 . . ?
N41 C73 C74 120.3(6) . . ?
N41 C73 C78 126.3(6) . . ?
C74 C73 C78 113.4(6) . . ?
F74 C74 C75 117.1(6) . . ?
F74 C74 C73 118.5(5) . . ?
C75 C74 C73 124.2(6) . . ?
F75 C75 C74 120.6(6) . . ?
F75 C75 C76 117.9(6) . . ?
C74 C75 C76 121.5(7) . . ?
F76 C76 C75 122.0(7) . . ?
F76 C76 C77 121.5(6) . . ?
C75 C76 C77 116.4(6) . . ?
F77 C77 C78 118.8(6) . . ?
F77 C77 C76 119.1(6) . . ?
C78 C77 C76 122.1(6) . . ?
F78 C78 C77 118.5(6) . . ?
F78 C78 C73 119.3(6) . . ?
C77 C78 C73 122.2(6) . . ?
N43 C81 C82 110.6(5) . . ?
N43 C81 H81A 109.5 . . ?
C82 C81 H81A 109.5 . . ?
N43 C81 H81B 109.5 . . ?
C82 C81 H81B 109.5 . . ?
H81A C81 H81B 108.1 . . ?
N42 C82 C81 109.5(5) . . ?
N42 C82 H82A 109.8 . . ?
C81 C82 H82A 109.8 . . ?
N42 C82 H82B 109.8 . . ?
C81 C82 H82B 109.8 . . ?
H82A C82 H82B 108.2 . . ?
N42 C83 C84 127.1(6) . . ?
N42 C83 C88 120.0(6) . . ?
C84 C83 C88 112.9(6) . . ?
F84 C84 C85 116.3(6) . . ?
F84 C84 C83 120.3(6) . . ?
C85 C84 C83 123.3(7) . . ?
F85 C85 C86 119.4(7) . . ?
F85 C85 C84 119.2(7) . . ?
C86 C85 C84 121.4(6) . . ?
F86 C86 C85 122.3(7) . . ?
F86 C86 C87 120.4(7) . . ?
C85 C86 C87 117.3(7) . . ?
F87 C87 C88 118.5(6) . . ?
F87 C87 C86 120.4(7) . . ?
C88 C87 C86 121.1(7) . . ?
F88 C88 C87 118.2(6) . . ?
F88 C88 C83 117.9(6) . . ?
C87 C88 C83 123.9(6) . . ?
N53 C91 C92 111.1(6) . . ?
N53 C91 H91A 109.4 . . ?
C92 C91 H91A 109.4 . . ?
N53 C91 H91B 109.4 . . ?
C92 C91 H91B 109.4 . . ?
H91A C91 H91B 108.0 . . ?
N51 C92 C91 107.4(6) . . ?
N51 C92 H92A 110.2 . . ?
C91 C92 H92A 110.2 . . ?
N51 C92 H92B 110.2 . . ?
C91 C92 H92B 110.2 . . ?
H92A C92 H92B 108.5 . . ?
N51 C93 C98 119.6(6) . . ?
N51 C93 C94 127.4(7) . . ?
C98 C93 C94 113.0(6) . . ?
F94 C94 C95 117.2(7) . . ?
F94 C94 C93 120.3(7) . . ?
C95 C94 C93 122.5(7) . . ?
C96 C95 F95 120.3(7) . . ?
C96 C95 C94 121.7(7) . . ?
F95 C95 C94 118.0(8) . . ?
C95 C96 C97 119.0(7) . . ?
C95 C96 F96 122.0(8) . . ?
C97 C96 F96 119.0(8) . . ?
F97 C97 C96 121.5(7) . . ?
F97 C97 C98 119.1(7) . . ?
C96 C97 C98 119.3(7) . . ?
F98 C98 C97 117.5(7) . . ?
F98 C98 C93 118.2(6) . . ?
C97 C98 C93 124.3(6) . . ?
C102 C101 N53 110.1(6) . . ?
C102 C101 H10A 109.6 . . ?
N53 C101 H10A 109.6 . . ?
C102 C101 H10B 109.6 . . ?
N53 C101 H10B 109.6 . . ?
H10A C101 H10B 108.2 . . ?
N52 C102 C101 111.6(6) . . ?
N52 C102 H10C 109.3 . . ?
C101 C102 H10C 109.3 . . ?
N52 C102 H10D 109.3 . . ?
C101 C102 H10D 109.3 . . ?
H10C C102 H10D 108.0 . . ?
N52 C103 C108 120.5(7) . . ?
N52 C103 C104 126.8(8) . . ?
C108 C103 C104 112.7(7) . . ?
F104 C104 C105 116.3(8) . . ?
F104 C104 C103 122.5(8) . . ?
C105 C104 C103 121.2(9) . . ?
C106 C105 F105 121.0(8) . . ?
C106 C105 C104 122.1(8) . . ?
F105 C105 C104 116.9(9) . . ?
C105 C106 F106 122.2(8) . . ?
C105 C106 C107 121.6(8) . . ?
F106 C106 C107 116.1(9) . . ?
F107 C107 C108 118.9(8) . . ?
F107 C107 C106 124.8(8) . . ?
C108 C107 C106 116.2(9) . . ?
C107 C108 F108 116.3(8) . . ?
C107 C108 C103 126.2(8) . . ?
F108 C108 C103 117.4(6) . . ?
N63 C111 C112 111.7(6) . . ?
N63 C111 H11C 109.3 . . ?
C112 C111 H11C 109.3 . . ?
N63 C111 H11D 109.3 . . ?
C112 C111 H11D 109.3 . . ?
H11C C111 H11D 107.9 . . ?
N61 C112 C111 107.9(6) . . ?
N61 C112 H11E 110.1 . . ?
C111 C112 H11E 110.1 . . ?
N61 C112 H11F 110.1 . . ?
C111 C112 H11F 110.1 . . ?
H11E C112 H11F 108.4 . . ?
N61 C113 C114 127.1(6) . . ?
N61 C113 C118 120.4(6) . . ?
C114 C113 C118 112.6(6) . . ?
F114 C114 C113 122.1(6) . . ?
F114 C114 C115 115.4(6) . . ?
C113 C114 C115 122.5(7) . . ?
F115 C115 C116 119.2(7) . . ?
F115 C115 C114 118.8(7) . . ?
C116 C115 C114 121.9(7) . . ?
F116 C116 C115 122.5(7) . . ?
F116 C116 C117 120.2(7) . . ?
C115 C116 C117 117.3(7) . . ?
F117 C117 C118 119.7(6) . . ?
F117 C117 C116 119.7(6) . . ?
C118 C117 C116 120.6(7) . . ?
C117 C118 F118 118.2(6) . . ?
C117 C118 C113 125.0(7) . . ?
F118 C118 C113 116.8(6) . . ?
N63 C121 C122 113.4(6) . . ?
N63 C121 H12C 108.9 . . ?
C122 C121 H12C 108.9 . . ?
N63 C121 H12D 108.9 . . ?
C122 C121 H12D 108.9 . . ?
H12C C121 H12D 107.7 . . ?
N62 C122 C121 108.5(6) . . ?
N62 C122 H12E 110.0 . . ?
C121 C122 H12E 110.0 . . ?
N62 C122 H12F 110.0 . . ?
C121 C122 H12F 110.0 . . ?
H12E C122 H12F 108.4 . . ?
C124 C123 N62 122.8(7) . . ?
C124 C123 C128 114.3(7) . . ?
N62 C123 C128 122.9(6) . . ?
F124 C124 C125 119.1(7) . . ?
F124 C124 C123 118.8(7) . . ?
C125 C124 C123 122.0(8) . . ?
C126 C125 F125 120.4(8) . . ?
C126 C125 C124 122.2(8) . . ?
F125 C125 C124 117.3(9) . . ?
C125 C126 F126 120.8(9) . . ?
C125 C126 C127 118.5(7) . . ?
F126 C126 C127 120.7(9) . . ?
C126 C127 F127 120.5(8) . . ?
C126 C127 C128 120.0(8) . . ?
F127 C127 C128 119.5(8) . . ?
F128 C128 C123 119.9(6) . . ?
F128 C128 C127 117.2(7) . . ?
C123 C128 C127 122.9(7) . . ?
N73 C131 C132 111.1(6) . . ?
N73 C131 H13A 109.4 . . ?
C132 C131 H13A 109.4 . . ?
N73 C131 H13B 109.4 . . ?
C132 C131 H13B 109.4 . . ?
H13A C131 H13B 108.0 . . ?
N71 C132 C131 107.6(6) . . ?
N71 C132 H13C 110.2 . . ?
C131 C132 H13C 110.2 . . ?
N71 C132 H13D 110.2 . . ?
C131 C132 H13D 110.2 . . ?
H13C C132 H13D 108.5 . . ?
N71 C133 C134 121.1(7) . . ?
N71 C133 C138 126.1(8) . . ?
C134 C133 C138 112.8(7) . . ?
F134 C134 C135 117.3(8) . . ?
F134 C134 C133 118.2(7) . . ?
C135 C134 C133 124.5(8) . . ?
F135 C135 C136 120.0(8) . . ?
F135 C135 C134 120.3(8) . . ?
C136 C135 C134 119.6(9) . . ?
F136 C136 C137 121.4(9) . . ?
F136 C136 C135 120.7(11) . . ?
C137 C136 C135 117.8(8) . . ?
C136 C137 F137 120.4(8) . . ?
C136 C137 C138 123.5(9) . . ?
F137 C137 C138 116.1(9) . . ?
F138 C138 C137 119.0(8) . . ?
F138 C138 C133 119.6(8) . . ?
C137 C138 C133 121.5(9) . . ?
N73 C141 C142 111.6(6) . . ?
N73 C141 H14A 109.3 . . ?
C142 C141 H14A 109.3 . . ?
N73 C141 H14B 109.3 . . ?
C142 C141 H14B 109.3 . . ?
H14A C141 H14B 108.0 . . ?
N72 C142 C141 108.5(6) . . ?
N72 C142 H14C 110.0 . . ?
C141 C142 H14C 110.0 . . ?
N72 C142 H14D 110.0 . . ?
C141 C142 H14D 110.0 . . ?
H14C C142 H14D 108.4 . . ?
N72 C143 C144 121.2(6) . . ?
N72 C143 C148 126.3(7) . . ?
C144 C143 C148 112.5(7) . . ?
F144 C144 C145 117.6(7) . . ?
F144 C144 C143 117.3(6) . . ?
C145 C144 C143 125.1(7) . . ?
F145 C145 C144 120.6(7) . . ?
F145 C145 C146 120.1(8) . . ?
C144 C145 C146 119.3(8) . . ?
F146 C146 C147 121.6(8) . . ?
F146 C146 C145 119.9(8) . . ?
C147 C146 C145 118.5(8) . . ?
F147 C147 C148 119.5(8) . . ?
F147 C147 C146 119.6(8) . . ?
C148 C147 C146 120.8(7) . . ?
C147 C148 F148 116.2(7) . . ?
C147 C148 C143 123.7(8) . . ?
F148 C148 C143 120.0(7) . . ?
C152 C151 N83 112.9(7) . . ?
C152 C151 H15A 109.0 . . ?
N83 C151 H15A 109.0 . . ?
C152 C151 H15B 109.0 . . ?
N83 C151 H15B 109.0 . . ?
H15A C151 H15B 107.8 . . ?
C151 C152 N81 108.1(7) . . ?
C151 C152 H15C 110.1 . . ?
N81 C152 H15C 110.1 . . ?
C151 C152 H15D 110.1 . . ?
N81 C152 H15D 110.1 . . ?
H15C C152 H15D 108.4 . . ?
N81 C153 C154 120.0(7) . . ?
N81 C153 C158 126.4(7) . . ?
C154 C153 C158 113.6(7) . . ?
C155 C154 F154 117.2(6) . . ?
C155 C154 C153 124.5(7) . . ?
F154 C154 C153 118.2(7) . . ?
F155 C155 C156 118.2(7) . . ?
F155 C155 C154 121.3(7) . . ?
C156 C155 C154 120.5(7) . . ?
F156 C156 C155 122.9(7) . . ?
F156 C156 C157 119.3(8) . . ?
C155 C156 C157 117.7(8) . . ?
F157 C157 C158 119.3(7) . . ?
F157 C157 C156 119.1(8) . . ?
C158 C157 C156 121.5(7) . . ?
F158 C158 C157 117.7(7) . . ?
F158 C158 C153 120.2(7) . . ?
C157 C158 C153 122.1(7) . . ?
N83 C161 C162 110.8(7) . . ?
N83 C161 H16A 109.5 . . ?
C162 C161 H16A 109.5 . . ?
N83 C161 H16B 109.5 . . ?
C162 C161 H16B 109.5 . . ?
H16A C161 H16B 108.1 . . ?
N82 C162 C161 108.7(6) . . ?
N82 C162 H16C 110.0 . . ?
C161 C162 H16C 110.0 . . ?
N82 C162 H16D 110.0 . . ?
C161 C162 H16D 110.0 . . ?
H16C C162 H16D 108.3 . . ?
N82 C163 C168 121.3(7) . . ?
N82 C163 C164 127.2(7) . . ?
C168 C163 C164 111.5(7) . . ?
F164 C164 C165 116.5(7) . . ?
F164 C164 C163 120.3(8) . . ?
C165 C164 C163 123.1(8) . . ?
C166 C165 F165 119.2(8) . . ?
C166 C165 C164 122.1(8) . . ?
F165 C165 C164 118.6(9) . . ?
F166 C166 C165 121.9(8) . . ?
F166 C166 C167 120.1(9) . . ?
C165 C166 C167 118.0(8) . . ?
F167 C167 C168 120.7(8) . . ?
F167 C167 C166 120.2(8) . . ?
C168 C167 C166 119.1(8) . . ?
C167 C168 F168 116.5(7) . . ?
C167 C168 C163 126.2(8) . . ?
F168 C168 C163 117.4(7) . . ?
C172 C171 C176 120.0 . . ?
C172 C171 C177 121.3(5) . . ?
C176 C171 C177 118.6(5) . . ?
C171 C172 C173 120.0 . . ?
C171 C172 H17A 120.0 . . ?
C173 C172 H17A 120.0 . . ?
C174 C173 C172 120.0 . . ?
C174 C173 H17B 120.0 . . ?
C172 C173 H17B 120.0 . . ?
C173 C174 C175 120.0 . . ?
C173 C174 H17C 120.0 . . ?
C175 C174 H17C 120.0 . . ?
C176 C175 C174 120.0 . . ?
C176 C175 H17D 120.0 . . ?
C174 C175 H17D 120.0 . . ?
C175 C176 C171 120.0 . . ?
C175 C176 H17E 120.0 . . ?
C171 C176 H17E 120.0 . . ?
C171 C177 H17F 109.5 . . ?
C171 C177 H17G 109.5 . . ?
H17F C177 H17G 109.5 . . ?
C171 C177 H17H 109.5 . . ?
H17F C177 H17H 109.5 . . ?
H17G C177 H17H 109.5 . . ?
C192 C191 C196 120.0 . . ?
C192 C191 C197 120.7(7) . . ?
C196 C191 C197 119.3(6) . . ?
C193 C192 C191 120.0 . . ?
C193 C192 H19A 120.0 . . ?
C191 C192 H19A 120.0 . . ?
C192 C193 C194 120.0 . . ?
C192 C193 H19B 120.0 . . ?
C194 C193 H19B 120.0 . . ?
C195 C194 C193 120.0 . . ?
C195 C194 H19C 120.0 . . ?
C193 C194 H19C 120.0 . . ?
C194 C195 C196 120.0 . . ?
C194 C195 H19D 120.0 . . ?
C196 C195 H19D 120.0 . . ?
C195 C196 C191 120.0 . . ?
C195 C196 H19E 120.0 . . ?
C191 C196 H19E 120.0 . . ?
C191 C197 H19F 109.5 . . ?
C191 C197 H19G 109.5 . . ?
H19F C197 H19G 109.5 . . ?
C191 C197 H19H 109.5 . . ?
H19F C197 H19H 109.5 . . ?
H19G C197 H19H 109.5 . . ?
C182 C181 C186 120.0 . . ?
C182 C181 C187 122.8(8) . . ?
C186 C181 C187 117.2(8) . . ?
C181 C182 C183 120.0 . . ?
C181 C182 H18A 120.0 . . ?
C183 C182 H18A 120.0 . . ?
C184 C183 C182 120.0 . . ?
C184 C183 H18B 120.0 . . ?
C182 C183 H18B 120.0 . . ?
C183 C184 C185 120.0 . . ?
C183 C184 H18C 120.0 . . ?
C185 C184 H18C 120.0 . . ?
C184 C185 C186 120.0 . . ?
C184 C185 H18D 120.0 . . ?
C186 C185 H18D 120.0 . . ?
C185 C186 C181 120.0 . . ?
C185 C186 H18E 120.0 . . ?
C181 C186 H18E 120.0 . . ?
C181 C187 H18F 109.5 . . ?
C181 C187 H18G 109.5 . . ?
H18F C187 H18G 109.5 . . ?
C181 C187 H18H 109.5 . . ?
H18F C187 H18H 109.5 . . ?
H18G C187 H18H 109.5 . . ?
C207 C201 C202 120.6(8) . . ?
C207 C201 C206 119.4(8) . . ?
C202 C201 C206 120.0 . . ?
C203 C202 C201 120.0 . . ?
C203 C202 H20A 120.0 . . ?
C201 C202 H20A 120.0 . . ?
C202 C203 C204 120.0 . . ?
C202 C203 H20B 120.0 . . ?
C204 C203 H20B 120.0 . . ?
C203 C204 C205 120.0 . . ?
C203 C204 H20C 120.0 . . ?
C205 C204 H20C 120.0 . . ?
C206 C205 C204 120.0 . . ?
C206 C205 H20D 120.0 . . ?
C204 C205 H20D 120.0 . . ?
C205 C206 C201 120.0 . . ?
C205 C206 H20E 120.0 . . ?
C201 C206 H20E 120.0 . . ?
C201 C207 H20F 109.5 . . ?
C201 C207 H20G 109.5 . . ?
H20F C207 H20G 109.5 . . ?
C201 C207 H20H 109.5 . . ?
H20F C207 H20H 109.5 . . ?
H20G C207 H20H 109.5 . . ?
C222 C221 C226 120.0 . . ?
C222 C221 C227 122.2(8) . . ?
C226 C221 C227 117.8(8) . . ?
C223 C222 C221 120.0 . . ?
C223 C222 H22C 120.0 . . ?
C221 C222 H22C 120.0 . . ?
C222 C223 C224 120.0 . . ?
C222 C223 H22D 120.0 . . ?
C224 C223 H22D 120.0 . . ?
C225 C224 C223 120.0 . . ?
C225 C224 H22E 120.0 . . ?
C223 C224 H22E 120.0 . . ?
C226 C225 C224 120.0 . . ?
C226 C225 H22F 120.0 . . ?
C224 C225 H22F 120.0 . . ?
C225 C226 C221 120.0 . . ?
C225 C226 H22G 120.0 . . ?
C221 C226 H22G 120.0 . . ?
C221 C227 H22H 109.5 . . ?
C221 C227 H22I 109.5 . . ?
H22H C227 H22I 109.5 . . ?
C221 C227 H22J 109.5 . . ?
H22H C227 H22J 109.5 . . ?
H22I C227 H22J 109.5 . . ?
C212 C211 C216 120.0 . . ?
C212 C211 H21C 120.0 . . ?
C216 C211 H21C 120.0 . . ?
C211 C212 C213 120.0 . . ?
C211 C212 H21D 120.0 . . ?
C213 C212 H21D 120.0 . . ?
C212 C213 C214 120.0 . . ?
C212 C213 H21E 120.0 . . ?
C214 C213 H21E 120.0 . . ?
C215 C214 C213 120.0 . . ?
C215 C214 H21F 120.0 . . ?
C213 C214 H21F 120.0 . . ?
C214 C215 C216 120.0 . . ?
C214 C215 H21G 120.0 . . ?
C216 C215 H21G 120.0 . . ?
C215 C216 C211 120.0 . . ?
C215 C216 H21H 120.0 . . ?
C211 C216 H21H 120.0 . . ?
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.896
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.149


data_ge2_5
_database_code_depnum_ccdc_archive 'CCDC 911589'
#TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1358416028.new_COMB.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H11 Cl2 F10 N3 Sn'
_chemical_formula_sum            'C17 H11 Cl2 F10 N3 Sn'
_chemical_formula_weight         636.88
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
Sn Sn 0.0259 5.4591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   12.0827(5)
_cell_length_b                   11.7253(4)
_cell_length_c                   16.1419(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.740(3)
_cell_angle_gamma                90.00
_cell_volume                     2124.22(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5342
_cell_measurement_theta_min      7.90
_cell_measurement_theta_max      68
_exptl_crystal_description       PRISM
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    12.826
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_absorpt_correction_T_min  0.2061
_exptl_absorpt_correction_T_max  0.3082
_exptl_special_details           
;
?
;
_diffrn_measurement_device_type  Stoe
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_voltage           50
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_monochromator  none
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_ambient_temperature      296
_diffrn_measurement_method       'rotation method'
_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2000)'
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5347
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.95
_diffrn_reflns_theta_max         68.00
_reflns_number_total             3837
_reflns_number_gt                2873
_reflns_threshold_expression     I>2\s(I)
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
All fluorine atoms were refined with restrained anisotropic displacement
parameters (DELU) due to their high thermal motion.
;
_iucr_refine_instruction_details 
;
TITL ge2 in P 21/n
CELL 1.54186 12.0827 11.7253 16.1419 90.000 111.740 90.000
ZERR 4 0.0005 0.0004 0.0006 0.000 0.003 0.000
LATT 1
SYMM 1/2-X,1/2+Y,1/2-Z
SFAC C H Cl F N Sn
UNIT 68 44 8 40 12 4
OMIT -2 136
acta
L.S. 14
BOND $H
FMAP 2
PLAN 20
size .18 .12 .12
WGHT 0.097200
EXTI 0.000486
FVAR 0.92911
MOLE 1
dfix 1.54 .006 c2 c3
delu .01 c7 f1 c8 f2 c9 f3 c10 f4 c11 f5
delu .01 c17 f6 c16 f7 c15 f8 c14 f9 c13 f10
SN1 6 0.539174 0.626746 0.206623 11.00000 0.04715 0.05309 =
0.04475 -0.00079 0.01852 -0.00597
CL1 3 0.529670 0.433809 0.237325 11.00000 0.09733 0.05195 =
0.10004 0.00830 0.03685 -0.00322
CL2 3 0.406494 0.616558 0.055939 11.00000 0.05838 0.08938 =
0.04835 -0.00593 0.01446 -0.00949
N1 5 0.672743 0.664487 0.350123 11.00000 0.06143 0.08575 =
0.04344 0.00234 0.02465 -0.00993
N2 5 0.445752 0.737046 0.249349 11.00000 0.06027 0.06532 =
0.06821 -0.01489 0.02982 -0.01058
N3 5 0.685224 0.671386 0.182952 11.00000 0.04877 0.09548 =
0.05003 0.00494 0.01847 -0.01481
F1 4 0.272698 0.573217 0.206640 11.00000 0.07303 0.06123 =
0.09354 0.00198 0.02188 -0.00747
F2 4 0.040431 0.617208 0.116666 11.00000 0.06002 0.12284 =
0.13925 -0.00995 0.02157 -0.02305
F3 4 -0.032879 0.832633 0.062421 11.00000 0.07621 0.14667 =
0.09366 -0.01002 0.00812 0.03587
F4 4 0.130247 1.003135 0.099175 11.00000 0.14161 0.08961 =
0.10303 0.02626 0.03655 0.04136
F5 4 0.363753 0.958218 0.188090 11.00000 0.11787 0.06652 =
0.12139 0.00361 0.05842 -0.01810
F6 4 0.811901 0.532619 0.111149 11.00000 0.07567 0.08100 =
0.15400 -0.01350 0.03978 0.01146
F7 4 0.821385 0.579430 -0.051262 11.00000 0.14417 0.25801 =
0.20394 -0.15762 0.13524 -0.09200
F8 4 0.696734 0.757169 -0.148641 11.00000 0.19970 0.29696 =
0.06225 -0.00871 0.05803 -0.13799
F9 4 0.566510 0.892637 -0.081655 11.00000 0.15122 0.18517 =
0.15598 0.11615 0.00612 -0.04256
F10 4 0.564761 0.850610 0.078458 11.00000 0.09401 0.07301 =
0.18049 0.00822 0.04598 0.01492
C1 1 0.716543 0.568209 0.411723 11.00000 0.15116 0.10924 =
0.06313 0.01736 -0.01497 0.01100
AFIX 137
H1A 2 0.755138 0.514098 0.386759 11.00000 -1.50000
H1B 2 0.650764 0.532122 0.421020 11.00000 -1.50000
H1C 2 0.772380 0.595421 0.467689 11.00000 -1.50000
AFIX 0
C2 1 0.610704 0.741287 0.390957 11.00000 0.11689 0.16557 =
0.06790 -0.03760 0.01803 0.01917
AFIX 23
H2A 2 0.668352 0.793563 0.430659 11.00000 -1.20000
H2B 2 0.577799 0.696215 0.426730 11.00000 -1.20000
AFIX 0
C3 1 0.510903 0.810060 0.323792 11.00000 0.06688 0.13450 =
0.09630 -0.06698 0.01099 0.00622
AFIX 23
H3A 2 0.457805 0.838916 0.351600 11.00000 -1.20000
H3B 2 0.543864 0.874527 0.303049 11.00000 -1.20000
AFIX 0
C4 1 0.771498 0.727788 0.336597 11.00000 0.08941 0.14956 =
0.06801 -0.03523 0.02403 -0.03978
AFIX 23
H4A 2 0.842487 0.723890 0.390437 11.00000 -1.20000
H4B 2 0.749578 0.807367 0.324405 11.00000 -1.20000
AFIX 0
C5 1 0.797003 0.677289 0.259993 11.00000 0.05430 0.14205 =
0.05247 -0.00105 0.01484 -0.02374
AFIX 23
H5A 2 0.853942 0.724409 0.246246 11.00000 -1.20000
H5B 2 0.830611 0.601545 0.275465 11.00000 -1.20000
AFIX 66
C6 1 0.323496 0.765191 0.201225 11.00000 0.05368 0.06674 =
0.05822 0.00369 0.03003 -0.00231
C7 1 0.240177 0.677623 0.181746 11.00000 0.05396 0.07342 =
0.05885 -0.00836 0.02207 -0.00234
C8 1 0.120237 0.700903 0.135275 11.00000 0.05801 0.09234 =
0.06452 -0.00430 0.02417 -0.00100
C9 1 0.083615 0.811750 0.108284 11.00000 0.06519 0.10968 =
0.05429 -0.00754 0.01777 0.01621
C10 1 0.166932 0.899319 0.127763 11.00000 0.09147 0.07531 =
0.06702 -0.00374 0.02000 0.02984
C11 1 0.286873 0.876041 0.174234 11.00000 0.08087 0.06963 =
0.07002 -0.00815 0.03976 0.00495
AFIX 66
C12 1 0.689402 0.691427 0.098906 11.00000 0.05449 0.06085 =
0.05253 0.00057 0.01665 -0.01360
C13 1 0.626284 0.782637 0.048246 11.00000 0.06719 0.07770 =
0.07533 0.01326 0.01937 -0.00972
C14 1 0.628970 0.802936 -0.035828 11.00000 0.10130 0.13179 =
0.07285 0.04184 0.01096 -0.04685
C15 1 0.694773 0.732026 -0.069243 11.00000 0.11748 0.19523 =
0.04346 -0.01393 0.02899 -0.08809
C16 1 0.757892 0.640816 -0.018584 11.00000 0.08497 0.15548 =
0.08306 -0.05392 0.05612 -0.05730
C17 1 0.755207 0.620515 0.065490 11.00000 0.05891 0.07776 =
0.07681 -0.02013 0.03369 -0.01348
HKLF 4
REM ge2 in P 21/n
REM R1 = 0.0515 for 2873 Fo > 4sig(Fo) and 0.0651 for all 3837 data
REM 276 parameters refined using 41 restraints
END
WGHT 0.0970 0.0000
REM Highest difference peak 1.067, deepest hole -0.738, 1-sigma level 0.140
Q1 1 0.5581 0.6274 0.2654 11.00000 0.05 1.07
Q2 1 0.5235 0.6270 0.1455 11.00000 0.05 0.95
Q3 1 0.6604 0.6279 0.3021 11.00000 0.05 0.69
Q4 1 0.6238 0.6204 0.2113 11.00000 0.05 0.66
Q5 1 0.5015 0.5336 0.2780 11.00000 0.05 0.58
Q6 1 0.4200 0.6208 0.1187 11.00000 0.05 0.56
Q7 1 0.4549 0.6255 0.2045 11.00000 0.05 0.53
Q8 1 0.1273 0.9371 0.2142 11.00000 0.05 0.50
Q9 1 0.7629 0.6266 0.3435 11.00000 0.05 0.49
Q10 1 0.4889 0.5971 0.0790 11.00000 0.05 0.48
Q11 1 0.5781 0.5222 0.1452 11.00000 0.05 0.47
Q12 1 0.3401 0.6608 0.1686 11.00000 0.05 0.47
Q13 1 0.5989 0.5677 0.3305 11.00000 0.05 0.46
Q14 1 0.1019 0.7581 0.0987 11.00000 0.05 0.46
Q15 1 0.6781 0.8637 0.2105 11.00000 0.05 0.45
Q16 1 0.6030 0.6469 0.3280 11.00000 0.05 0.44
Q17 1 0.3750 0.8172 0.2792 11.00000 0.05 0.44
Q18 1 0.4972 0.7543 0.3545 11.00000 0.05 0.44
Q19 1 0.4990 0.7186 0.2906 11.00000 0.05 0.42
Q20 1 0.6228 0.5687 0.2746 11.00000 0.05 0.42
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00049(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3837
_refine_ls_number_parameters     276
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1426
_refine_ls_wR_factor_gt          0.1321
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.53917(3) 0.62675(3) 0.20662(2) 0.04790(19) Uani 1 1 d . . .
Cl1 Cl 0.52967(19) 0.43381(15) 0.23732(15) 0.0830(5) Uani 1 1 d . . .
Cl2 Cl 0.40649(13) 0.61656(16) 0.05594(11) 0.0669(4) Uani 1 1 d . . .
N1 N 0.6727(5) 0.6645(6) 0.3501(3) 0.0620(13) Uani 1 1 d . . .
N2 N 0.4458(4) 0.7370(5) 0.2493(4) 0.0629(13) Uani 1 1 d . . .
N3 N 0.6852(4) 0.6714(6) 0.1830(3) 0.0647(14) Uani 1 1 d . . .
F1 F 0.2727(4) 0.5732(4) 0.2066(3) 0.0785(11) Uani 1 1 d U . .
F2 F 0.0404(4) 0.6172(5) 0.1167(4) 0.1118(19) Uani 1 1 d U . .
F3 F -0.0329(4) 0.8326(6) 0.0624(4) 0.1122(19) Uani 1 1 d U . .
F4 F 0.1302(6) 1.0031(5) 0.0992(4) 0.1139(18) Uani 1 1 d U . .
F5 F 0.3638(5) 0.9582(4) 0.1881(4) 0.0979(14) Uani 1 1 d U . .
F6 F 0.8119(4) 0.5326(4) 0.1111(4) 0.1043(16) Uani 1 1 d U . .
F7 F 0.8214(7) 0.5794(9) -0.0513(6) 0.182(4) Uani 1 1 d U . .
F8 F 0.6967(7) 0.7572(9) -0.1486(4) 0.184(4) Uani 1 1 d U . .
F9 F 0.5665(7) 0.8926(8) -0.0817(6) 0.179(4) Uani 1 1 d U . .
F10 F 0.5648(5) 0.8506(5) 0.0785(5) 0.117(2) Uani 1 1 d U . .
C1 C 0.7165(11) 0.5682(10) 0.4117(6) 0.123(4) Uani 1 1 d . . .
H1A H 0.7551 0.5141 0.3868 0.185 Uiso 1 1 calc R . .
H1B H 0.6508 0.5321 0.4210 0.185 Uiso 1 1 calc R . .
H1C H 0.7724 0.5954 0.4677 0.185 Uiso 1 1 calc R . .
C2 C 0.6107(9) 0.7413(11) 0.3910(6) 0.121(4) Uani 1 1 d D . .
H2A H 0.6684 0.7936 0.4307 0.146 Uiso 1 1 calc R . .
H2B H 0.5778 0.6962 0.4267 0.146 Uiso 1 1 calc R . .
C3 C 0.5109(7) 0.8101(9) 0.3238(6) 0.105(4) Uani 1 1 d D . .
H3A H 0.4578 0.8389 0.3516 0.126 Uiso 1 1 calc R . .
H3B H 0.5439 0.8745 0.3030 0.126 Uiso 1 1 calc R . .
C4 C 0.7715(8) 0.7278(11) 0.3366(6) 0.104(3) Uani 1 1 d . . .
H4A H 0.8425 0.7239 0.3904 0.125 Uiso 1 1 calc R . .
H4B H 0.7496 0.8074 0.3244 0.125 Uiso 1 1 calc R . .
C5 C 0.7970(6) 0.6773(9) 0.2600(5) 0.084(3) Uani 1 1 d . . .
H5A H 0.8539 0.7244 0.2462 0.101 Uiso 1 1 calc R . .
H5B H 0.8306 0.6015 0.2755 0.101 Uiso 1 1 calc R . .
C6 C 0.3235(3) 0.7652(4) 0.2012(3) 0.0569(15) Uani 1 1 d G . .
C7 C 0.2402(4) 0.6776(3) 0.1817(3) 0.0617(15) Uani 1 1 d GU . .
C8 C 0.1202(3) 0.7009(4) 0.1353(3) 0.0712(17) Uani 1 1 d GU . .
C9 C 0.0836(3) 0.8118(5) 0.1083(3) 0.0776(18) Uani 1 1 d GU . .
C10 C 0.1669(4) 0.8993(3) 0.1278(3) 0.081(2) Uani 1 1 d GU . .
C11 C 0.2869(4) 0.8760(3) 0.1742(3) 0.0701(17) Uani 1 1 d GU . .
C12 C 0.6894(4) 0.6914(4) 0.0989(2) 0.0569(14) Uani 1 1 d G . .
C13 C 0.6263(4) 0.7826(4) 0.0482(3) 0.0754(18) Uani 1 1 d GU . .
C14 C 0.6290(5) 0.8029(5) -0.0358(3) 0.108(2) Uani 1 1 d GU . .
C15 C 0.6948(6) 0.7320(6) -0.0692(3) 0.119(3) Uani 1 1 d GU . .
C16 C 0.7579(5) 0.6408(6) -0.0186(4) 0.101(2) Uani 1 1 d GU . .
C17 C 0.7552(4) 0.6205(4) 0.0655(3) 0.0687(17) Uani 1 1 d GU . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.0472(2) 0.0531(3) 0.0448(3) -0.00079(16) 0.01852(16) -0.00597(16)
Cl1 0.0973(12) 0.0520(8) 0.1000(14) 0.0083(9) 0.0368(11) -0.0032(9)
Cl2 0.0584(7) 0.0894(12) 0.0483(8) -0.0059(8) 0.0145(6) -0.0095(8)
N1 0.061(3) 0.086(4) 0.043(3) 0.002(3) 0.025(2) -0.010(3)
N2 0.060(3) 0.065(3) 0.068(3) -0.015(3) 0.030(2) -0.011(3)
N3 0.049(2) 0.095(4) 0.050(3) 0.005(3) 0.018(2) -0.015(3)
F1 0.073(2) 0.061(2) 0.094(3) 0.002(2) 0.022(2) -0.007(2)
F2 0.060(2) 0.123(4) 0.139(5) -0.010(3) 0.022(2) -0.023(3)
F3 0.076(2) 0.147(5) 0.094(4) -0.010(3) 0.008(2) 0.036(3)
F4 0.142(4) 0.090(3) 0.103(4) 0.026(3) 0.037(3) 0.041(3)
F5 0.118(3) 0.067(3) 0.121(4) 0.004(3) 0.058(3) -0.018(3)
F6 0.076(2) 0.081(3) 0.154(5) -0.014(3) 0.040(3) 0.011(2)
F7 0.144(5) 0.258(8) 0.204(7) -0.158(6) 0.135(5) -0.092(5)
F8 0.200(7) 0.297(11) 0.062(3) -0.009(4) 0.058(4) -0.138(7)
F9 0.151(5) 0.185(7) 0.156(7) 0.116(6) 0.006(5) -0.043(5)
F10 0.094(3) 0.073(3) 0.180(6) 0.008(3) 0.046(4) 0.015(3)
C1 0.151(9) 0.109(8) 0.063(6) 0.017(5) -0.015(6) 0.011(7)
C2 0.117(7) 0.166(11) 0.068(5) -0.038(6) 0.018(5) 0.019(8)
C3 0.067(4) 0.135(9) 0.096(6) -0.067(6) 0.011(4) 0.006(5)
C4 0.089(5) 0.150(9) 0.068(5) -0.035(6) 0.024(4) -0.040(6)
C5 0.054(3) 0.142(8) 0.052(4) -0.001(5) 0.015(3) -0.024(4)
C6 0.054(3) 0.067(4) 0.058(4) 0.004(3) 0.030(3) -0.002(3)
C7 0.054(3) 0.073(4) 0.059(4) -0.008(3) 0.022(3) -0.002(3)
C8 0.058(3) 0.092(4) 0.065(4) -0.004(4) 0.024(3) -0.001(3)
C9 0.065(3) 0.110(5) 0.054(4) -0.008(4) 0.018(3) 0.016(4)
C10 0.091(4) 0.075(4) 0.067(5) -0.004(4) 0.020(4) 0.030(3)
C11 0.081(4) 0.070(4) 0.070(5) -0.008(3) 0.040(3) 0.005(3)
C12 0.054(3) 0.061(4) 0.053(3) 0.001(3) 0.017(2) -0.014(3)
C13 0.067(3) 0.078(4) 0.075(4) 0.013(4) 0.019(3) -0.010(4)
C14 0.101(5) 0.132(7) 0.073(5) 0.042(5) 0.011(4) -0.047(5)
C15 0.117(6) 0.195(8) 0.043(4) -0.014(5) 0.029(4) -0.088(5)
C16 0.085(4) 0.155(7) 0.083(5) -0.054(4) 0.056(4) -0.057(4)
C17 0.059(3) 0.078(4) 0.077(4) -0.020(3) 0.034(3) -0.013(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Sn1 N2 2.000(5) . ?
Sn1 N3 2.008(5) . ?
Sn1 N1 2.323(5) . ?
Sn1 Cl1 2.3278(17) . ?
Sn1 Cl2 2.3689(15) . ?
N1 C1 1.467(11) . ?
N1 C2 1.474(11) . ?
N1 C4 1.488(10) . ?
N2 C6 1.430(6) . ?
N2 C3 1.448(9) . ?
N3 C12 1.396(6) . ?
N3 C5 1.460(7) . ?
F1 C7 1.303(5) . ?
F2 C8 1.330(6) . ?
F3 C9 1.348(5) . ?
F4 C10 1.319(6) . ?
F5 C11 1.299(6) . ?
F6 C17 1.304(7) . ?
F7 C16 1.298(8) . ?
F8 C15 1.324(6) . ?
F9 C14 1.345(8) . ?
F10 C13 1.302(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.520(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.502(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.3900 . ?
C6 C11 1.3900 . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C12 C13 1.3900 . ?
C12 C17 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
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
N2 Sn1 N3 123.0(2) . . ?
N2 Sn1 N1 78.8(2) . . ?
N3 Sn1 N1 78.77(19) . . ?
N2 Sn1 Cl1 118.45(17) . . ?
N3 Sn1 Cl1 114.2(2) . . ?
N1 Sn1 Cl1 92.50(17) . . ?
N2 Sn1 Cl2 97.64(16) . . ?
N3 Sn1 Cl2 97.23(15) . . ?
N1 Sn1 Cl2 171.65(16) . . ?
Cl1 Sn1 Cl2 95.83(7) . . ?
C1 N1 C2 106.4(8) . . ?
C1 N1 C4 112.1(8) . . ?
C2 N1 C4 109.2(8) . . ?
C1 N1 Sn1 118.2(6) . . ?
C2 N1 Sn1 106.4(4) . . ?
C4 N1 Sn1 104.3(4) . . ?
C6 N2 C3 116.7(5) . . ?
C6 N2 Sn1 124.3(4) . . ?
C3 N2 Sn1 117.8(4) . . ?
C12 N3 C5 117.7(5) . . ?
C12 N3 Sn1 125.4(3) . . ?
C5 N3 Sn1 116.8(4) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 113.9(7) . . ?
N1 C2 H2A 108.8 . . ?
C3 C2 H2A 108.8 . . ?
N1 C2 H2B 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N2 C3 C2 108.8(7) . . ?
N2 C3 H3A 109.9 . . ?
C2 C3 H3A 109.9 . . ?
N2 C3 H3B 109.9 . . ?
C2 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N1 C4 C5 110.1(7) . . ?
N1 C4 H4A 109.6 . . ?
C5 C4 H4A 109.6 . . ?
N1 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N3 C5 C4 108.2(6) . . ?
N3 C5 H5A 110.1 . . ?
C4 C5 H5A 110.1 . . ?
N3 C5 H5B 110.1 . . ?
C4 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
C7 C6 C11 120.0 . . ?
C7 C6 N2 117.9(4) . . ?
C11 C6 N2 122.1(4) . . ?
F1 C7 C6 120.9(3) . . ?
F1 C7 C8 119.1(3) . . ?
C6 C7 C8 120.0 . . ?
F2 C8 C9 119.9(4) . . ?
F2 C8 C7 120.1(4) . . ?
C9 C8 C7 120.0 . . ?
F3 C9 C8 119.2(5) . . ?
F3 C9 C10 120.8(5) . . ?
C8 C9 C10 120.0 . . ?
F4 C10 C11 121.2(4) . . ?
F4 C10 C9 118.8(4) . . ?
C11 C10 C9 120.0 . . ?
F5 C11 C10 118.9(4) . . ?
F5 C11 C6 121.0(4) . . ?
C10 C11 C6 120.0 . . ?
C13 C12 C17 120.0 . . ?
C13 C12 N3 119.5(4) . . ?
C17 C12 N3 120.5(4) . . ?
F10 C13 C12 121.0(5) . . ?
F10 C13 C14 119.0(5) . . ?
C12 C13 C14 120.0 . . ?
F9 C14 C15 122.6(7) . . ?
F9 C14 C13 117.4(7) . . ?
C15 C14 C13 120.0 . . ?
F8 C15 C14 117.4(7) . . ?
F8 C15 C16 122.6(7) . . ?
C14 C15 C16 120.0 . . ?
F7 C16 C17 122.2(7) . . ?
F7 C16 C15 117.8(7) . . ?
C17 C16 C15 120.0 . . ?
F6 C17 C16 119.3(5) . . ?
F6 C17 C12 120.6(5) . . ?
C16 C17 C12 120.0 . . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        68.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.140


data_8
_database_code_depnum_ccdc_archive 'CCDC 911590'
#TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1358416028.new_COMB.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H76 Ge4 N4 O8 Pd, C7 H8'
_chemical_formula_sum            'C75 H84 Ge4 N4 O8 Pd'
_chemical_formula_weight         1566.22
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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   15.2818(19)
_cell_length_b                   16.426(2)
_cell_length_c                   17.317(2)
_cell_angle_alpha                94.652(2)
_cell_angle_beta                 115.307(2)
_cell_angle_gamma                113.764(2)
_cell_volume                     3423.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6221
_cell_measurement_theta_min      3.353
_cell_measurement_theta_max      26.298
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    2.052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_T_max  0.8211
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27142
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         26.00
_reflns_number_total             13253
_reflns_number_gt                10275
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       '<i>APEX2</i> (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13253
_refine_ls_number_parameters     834
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0720
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.226893(19) 0.620621(16) 0.352866(14) 0.02275(6) Uani 1 1 d . . .
Ge1 Ge 0.33815(2) 0.69867(2) 0.50922(2) 0.02187(8) Uani 1 1 d . . .
Ge2 Ge 0.07332(3) 0.64411(2) 0.31679(2) 0.02552(8) Uani 1 1 d . . .
Ge3 Ge 0.30888(3) 0.68141(2) 0.26756(2) 0.02412(8) Uani 1 1 d . . .
Ge4 Ge 0.17238(3) 0.46023(2) 0.31126(2) 0.02614(8) Uani 1 1 d . . .
N1 N 0.39951(19) 0.84293(17) 0.56313(16) 0.0235(5) Uani 1 1 d . . .
N2 N -0.0442(2) 0.58479(19) 0.35761(16) 0.0310(6) Uani 1 1 d . . .
N3 N 0.2173(2) 0.64104(18) 0.12682(16) 0.0294(6) Uani 1 1 d . . .
N4 N 0.2708(2) 0.39350(18) 0.32922(17) 0.0285(6) Uani 1 1 d . . .
O11 O 0.26891(17) 0.68343(14) 0.57641(13) 0.0291(5) Uani 1 1 d . . .
O12 O 0.47984(16) 0.72504(13) 0.59175(13) 0.0249(5) Uani 1 1 d . . .
O21 O 0.09487(17) 0.75681(15) 0.37272(14) 0.0341(5) Uani 1 1 d . . .
O22 O -0.04921(16) 0.60268(15) 0.20523(13) 0.0314(5) Uani 1 1 d . . .
O31 O 0.39857(18) 0.64358(16) 0.24750(15) 0.0399(6) Uani 1 1 d . . .
O32 O 0.35818(17) 0.80097(14) 0.26018(13) 0.0290(5) Uani 1 1 d . . .
O41 O 0.10271(18) 0.39729(15) 0.19111(13) 0.0360(5) Uani 1 1 d . . .
O42 O 0.10521(16) 0.37210(15) 0.35550(14) 0.0302(5) Uani 1 1 d . . .
C11 C 0.3988(3) 0.8925(2) 0.4956(2) 0.0314(7) Uani 1 1 d . . .
H11A H 0.4251 0.9585 0.5225 0.047 Uiso 1 1 calc R . .
H11B H 0.3232 0.8644 0.4445 0.047 Uiso 1 1 calc R . .
H11C H 0.4475 0.8874 0.4750 0.047 Uiso 1 1 calc R . .
C12 C 0.2953(3) 0.7659(2) 0.6336(2) 0.0322(7) Uani 1 1 d . . .
H12A H 0.3602 0.7826 0.6930 0.039 Uiso 1 1 calc R . .
H12B H 0.2321 0.7562 0.6420 0.039 Uiso 1 1 calc R . .
C13 C 0.3213(3) 0.8442(2) 0.5926(2) 0.0305(7) Uani 1 1 d . . .
H13A H 0.2525 0.8351 0.5406 0.037 Uiso 1 1 calc R . .
H13B H 0.3555 0.9051 0.6373 0.037 Uiso 1 1 calc R . .
C14 C 0.5116(2) 0.8791(2) 0.64227(19) 0.0256(7) Uani 1 1 d . . .
H14A H 0.5062 0.8775 0.6971 0.031 Uiso 1 1 calc R . .
H14B H 0.5592 0.9448 0.6492 0.031 Uiso 1 1 calc R . .
C15 C 0.5648(2) 0.8193(2) 0.63097(19) 0.0237(7) Uani 1 1 d . . .
C16 C 0.6486(2) 0.8301(2) 0.72675(19) 0.0255(7) Uani 1 1 d . . .
C17 C 0.6058(3) 0.7889(2) 0.7787(2) 0.0344(8) Uani 1 1 d . . .
H17 H 0.5280 0.7508 0.7521 0.041 Uiso 1 1 calc R . .
C18 C 0.6738(3) 0.8024(3) 0.8677(2) 0.0452(9) Uani 1 1 d . . .
H18 H 0.6428 0.7745 0.9022 0.054 Uiso 1 1 calc R . .
C19 C 0.7871(3) 0.8564(3) 0.9067(2) 0.0473(10) Uani 1 1 d . . .
H19 H 0.8341 0.8673 0.9686 0.057 Uiso 1 1 calc R . .
C20 C 0.8313(3) 0.8940(3) 0.8565(2) 0.0445(9) Uani 1 1 d . . .
H20 H 0.9094 0.9293 0.8828 0.053 Uiso 1 1 calc R . .
C21 C 0.7624(3) 0.8809(2) 0.7664(2) 0.0351(8) Uani 1 1 d . . .
H21 H 0.7942 0.9073 0.7319 0.042 Uiso 1 1 calc R . .
C22 C 0.6151(2) 0.8507(2) 0.57215(19) 0.0233(7) Uani 1 1 d . . .
C23 C 0.6932(2) 0.9435(2) 0.5944(2) 0.0299(7) Uani 1 1 d . . .
H23 H 0.7199 0.9865 0.6496 0.036 Uiso 1 1 calc R . .
C24 C 0.7327(3) 0.9744(2) 0.5381(2) 0.0378(8) Uani 1 1 d . . .
H24 H 0.7882 1.0374 0.5557 0.045 Uiso 1 1 calc R . .
C25 C 0.6915(3) 0.9137(3) 0.4563(2) 0.0400(9) Uani 1 1 d . . .
H25 H 0.7168 0.9353 0.4167 0.048 Uiso 1 1 calc R . .
C26 C 0.6134(3) 0.8217(3) 0.4321(2) 0.0346(8) Uani 1 1 d . . .
H26 H 0.5846 0.7800 0.3755 0.042 Uiso 1 1 calc R . .
C27 C 0.5765(2) 0.7896(2) 0.4905(2) 0.0283(7) Uani 1 1 d . . .
H27 H 0.5247 0.7256 0.4743 0.034 Uiso 1 1 calc R . .
C31 C -0.0490(3) 0.4996(3) 0.3828(2) 0.0417(9) Uani 1 1 d . . .
H31A H -0.1004 0.4783 0.4057 0.063 Uiso 1 1 calc R . .
H31B H 0.0249 0.5138 0.4295 0.063 Uiso 1 1 calc R . .
H31C H -0.0749 0.4504 0.3300 0.063 Uiso 1 1 calc R . .
C32 C 0.0301(3) 0.7522(3) 0.4128(2) 0.0428(9) Uani 1 1 d . . .
H32A H -0.0367 0.7548 0.3707 0.051 Uiso 1 1 calc R . .
H32B H 0.0733 0.8060 0.4677 0.051 Uiso 1 1 calc R . .
C33 C -0.0037(3) 0.6618(3) 0.4361(2) 0.0410(9) Uani 1 1 d . . .
H33A H 0.0605 0.6655 0.4891 0.049 Uiso 1 1 calc R . .
H33B H -0.0628 0.6503 0.4506 0.049 Uiso 1 1 calc R . .
C34 C -0.1517(2) 0.5674(3) 0.2824(2) 0.0358(8) Uani 1 1 d . . .
H34A H -0.1620 0.6223 0.2924 0.043 Uiso 1 1 calc R . .
H34B H -0.2128 0.5127 0.2811 0.043 Uiso 1 1 calc R . .
C35 C -0.1566(2) 0.5489(2) 0.1916(2) 0.0301(7) Uani 1 1 d . . .
C36 C -0.2335(2) 0.5795(2) 0.1261(2) 0.0309(7) Uani 1 1 d . . .
C37 C -0.2119(3) 0.6127(2) 0.0617(2) 0.0323(7) Uani 1 1 d . . .
H37 H -0.1487 0.6179 0.0598 0.039 Uiso 1 1 calc R . .
C38 C -0.2815(3) 0.6384(2) 0.0002(2) 0.0425(9) Uani 1 1 d . . .
H38 H -0.2664 0.6601 -0.0442 0.051 Uiso 1 1 calc R . .
C39 C -0.3730(3) 0.6326(3) 0.0029(2) 0.0471(10) Uani 1 1 d . . .
H39 H -0.4209 0.6502 -0.0395 0.056 Uiso 1 1 calc R . .
C40 C -0.3938(3) 0.6013(3) 0.0672(3) 0.0484(10) Uani 1 1 d . . .
H40 H -0.4562 0.5974 0.0696 0.058 Uiso 1 1 calc R . .
C41 C -0.3251(3) 0.5753(3) 0.1285(2) 0.0423(9) Uani 1 1 d . . .
H41 H -0.3404 0.5541 0.1730 0.051 Uiso 1 1 calc R . .
C42 C -0.1991(3) 0.4442(2) 0.1528(2) 0.0344(8) Uani 1 1 d . . .
C43 C -0.3088(3) 0.3789(3) 0.1202(3) 0.0560(11) Uani 1 1 d . . .
H43 H -0.3598 0.3996 0.1162 0.067 Uiso 1 1 calc R . .
C44 C -0.3450(4) 0.2851(3) 0.0936(3) 0.0697(13) Uani 1 1 d . . .
H44 H -0.4208 0.2419 0.0709 0.084 Uiso 1 1 calc R . .
C45 C -0.2728(4) 0.2522(3) 0.0992(3) 0.0579(11) Uani 1 1 d . . .
H45 H -0.2980 0.1870 0.0810 0.070 Uiso 1 1 calc R . .
C46 C -0.1641(3) 0.3160(3) 0.1316(2) 0.0470(10) Uani 1 1 d . . .
H46 H -0.1130 0.2948 0.1370 0.056 Uiso 1 1 calc R . .
C47 C -0.1278(3) 0.4109(2) 0.1567(2) 0.0363(8) Uani 1 1 d . . .
H47 H -0.0527 0.4539 0.1769 0.044 Uiso 1 1 calc R . .
C51 C 0.0973(3) 0.6059(2) 0.0909(2) 0.0412(9) Uani 1 1 d . . .
H51A H 0.0593 0.5908 0.0254 0.062 Uiso 1 1 calc R . .
H51B H 0.0863 0.6541 0.1162 0.062 Uiso 1 1 calc R . .
H51C H 0.0668 0.5497 0.1073 0.062 Uiso 1 1 calc R . .
C52 C 0.2396(3) 0.5677(2) 0.0994(2) 0.0408(9) Uani 1 1 d . . .
H52A H 0.2193 0.5564 0.0356 0.049 Uiso 1 1 calc R . .
H52B H 0.1950 0.5086 0.1065 0.049 Uiso 1 1 calc R . .
C53 C 0.3617(3) 0.5997(3) 0.1579(2) 0.0460(10) Uani 1 1 d . . .
H53A H 0.3744 0.5453 0.1549 0.055 Uiso 1 1 calc R . .
H53B H 0.4042 0.6440 0.1356 0.055 Uiso 1 1 calc R . .
C54 C 0.2691(3) 0.7260(2) 0.1031(2) 0.0316(7) Uani 1 1 d . . .
H54A H 0.2140 0.7236 0.0444 0.038 Uiso 1 1 calc R . .
H54B H 0.3315 0.7273 0.0976 0.038 Uiso 1 1 calc R . .
C55 C 0.3118(3) 0.8155(2) 0.17528(19) 0.0279(7) Uani 1 1 d . . .
C56 C 0.4059(3) 0.8961(2) 0.17294(19) 0.0312(7) Uani 1 1 d . . .
C57 C 0.5035(3) 0.8923(3) 0.1997(2) 0.0411(9) Uani 1 1 d . . .
H57 H 0.5093 0.8412 0.2188 0.049 Uiso 1 1 calc R . .
C58 C 0.5922(3) 0.9614(3) 0.1989(2) 0.0489(10) Uani 1 1 d . . .
H58 H 0.6585 0.9579 0.2177 0.059 Uiso 1 1 calc R . .
C59 C 0.5843(3) 1.0356(3) 0.1707(3) 0.0541(11) Uani 1 1 d . . .
H59 H 0.6443 1.0825 0.1684 0.065 Uiso 1 1 calc R . .
C60 C 0.4896(3) 1.0415(3) 0.1461(2) 0.0498(10) Uani 1 1 d . . .
H60 H 0.4850 1.0935 0.1283 0.060 Uiso 1 1 calc R . .
C61 C 0.4004(3) 0.9720(2) 0.1469(2) 0.0375(8) Uani 1 1 d . . .
H61 H 0.3350 0.9766 0.1294 0.045 Uiso 1 1 calc R . .
C62 C 0.2151(3) 0.8329(2) 0.15986(19) 0.0283(7) Uani 1 1 d . . .
C63 C 0.1480(3) 0.8373(2) 0.0763(2) 0.0367(8) Uani 1 1 d . . .
H63 H 0.1654 0.8334 0.0301 0.044 Uiso 1 1 calc R . .
C64 C 0.0572(3) 0.8471(2) 0.0604(2) 0.0425(9) Uani 1 1 d . . .
H64 H 0.0128 0.8505 0.0035 0.051 Uiso 1 1 calc R . .
C65 C 0.0297(3) 0.8522(2) 0.1260(2) 0.0417(9) Uani 1 1 d . . .
H65 H -0.0334 0.8586 0.1146 0.050 Uiso 1 1 calc R . .
C66 C 0.0952(3) 0.8477(2) 0.2088(2) 0.0375(8) Uani 1 1 d . . .
H66 H 0.0768 0.8508 0.2545 0.045 Uiso 1 1 calc R . .
C67 C 0.1875(3) 0.8388(2) 0.2254(2) 0.0304(7) Uani 1 1 d . . .
H67 H 0.2324 0.8368 0.2829 0.036 Uiso 1 1 calc R . .
C71 C 0.3886(3) 0.4562(2) 0.3957(2) 0.0418(9) Uani 1 1 d . . .
H71A H 0.4314 0.4245 0.3970 0.063 Uiso 1 1 calc R . .
H71B H 0.3972 0.4725 0.4552 0.063 Uiso 1 1 calc R . .
H71C H 0.4157 0.5131 0.3793 0.063 Uiso 1 1 calc R . .
C72 C 0.1339(3) 0.3324(2) 0.1697(2) 0.0382(8) Uani 1 1 d . . .
H72A H 0.1237 0.3262 0.1087 0.046 Uiso 1 1 calc R . .
H72B H 0.0868 0.2704 0.1708 0.046 Uiso 1 1 calc R . .
C73 C 0.2539(3) 0.3663(2) 0.2376(2) 0.0394(8) Uani 1 1 d . . .
H73A H 0.2729 0.3161 0.2313 0.047 Uiso 1 1 calc R . .
H73B H 0.3024 0.4207 0.2275 0.047 Uiso 1 1 calc R . .
C74 C 0.2210(2) 0.3104(2) 0.3550(2) 0.0280(7) Uani 1 1 d . . .
H74A H 0.2795 0.2973 0.3952 0.034 Uiso 1 1 calc R . .
H74B H 0.1669 0.2554 0.3007 0.034 Uiso 1 1 calc R . .
C75 C 0.1624(2) 0.3270(2) 0.4033(2) 0.0278(7) Uani 1 1 d . . .
C76 C 0.0772(2) 0.2326(2) 0.3972(2) 0.0298(7) Uani 1 1 d . . .
C77 C 0.1058(3) 0.1650(3) 0.4246(3) 0.0517(10) Uani 1 1 d . . .
H77 H 0.1795 0.1766 0.4455 0.062 Uiso 1 1 calc R . .
C78 C 0.0289(3) 0.0817(3) 0.4219(3) 0.0585(11) Uani 1 1 d . . .
H78 H 0.0507 0.0376 0.4429 0.070 Uiso 1 1 calc R . .
C79 C -0.0786(3) 0.0622(3) 0.3891(3) 0.0484(10) Uani 1 1 d . . .
H79 H -0.1318 0.0046 0.3867 0.058 Uiso 1 1 calc R . .
C80 C -0.1077(3) 0.1267(3) 0.3601(3) 0.0483(10) Uani 1 1 d . . .
H80 H -0.1823 0.1134 0.3370 0.058 Uiso 1 1 calc R . .
C81 C -0.0315(3) 0.2110(2) 0.3634(2) 0.0358(8) Uani 1 1 d . . .
H81 H -0.0544 0.2545 0.3422 0.043 Uiso 1 1 calc R . .
C82 C 0.2456(2) 0.3871(2) 0.5026(2) 0.0267(7) Uani 1 1 d . . .
C83 C 0.3195(3) 0.3615(2) 0.5599(2) 0.0374(8) Uani 1 1 d . . .
H83 H 0.3182 0.3061 0.5372 0.045 Uiso 1 1 calc R . .
C84 C 0.3945(3) 0.4137(3) 0.6482(2) 0.0401(8) Uani 1 1 d . . .
H84 H 0.4429 0.3936 0.6859 0.048 Uiso 1 1 calc R . .
C85 C 0.3994(3) 0.4961(2) 0.6824(2) 0.0354(8) Uani 1 1 d . . .
H85 H 0.4518 0.5333 0.7431 0.042 Uiso 1 1 calc R . .
C86 C 0.3268(3) 0.5226(2) 0.6261(2) 0.0333(8) Uani 1 1 d . . .
H86 H 0.3290 0.5786 0.6485 0.040 Uiso 1 1 calc R . .
C87 C 0.2506(2) 0.4686(2) 0.5374(2) 0.0279(7) Uani 1 1 d . . .
H87 H 0.2010 0.4878 0.4999 0.033 Uiso 1 1 calc R . .
C91 C 0.8357(4) 0.9061(3) 0.1819(3) 0.0629(12) Uani 1 1 d . . .
C92 C 0.7278(4) 0.8788(4) 0.1178(3) 0.0736(14) Uani 1 1 d . . .
H92 H 0.6701 0.8196 0.1076 0.088 Uiso 1 1 calc R . .
C93 C 0.7026(6) 0.9349(5) 0.0692(4) 0.0927(17) Uani 1 1 d . . .
H93 H 0.6277 0.9152 0.0262 0.111 Uiso 1 1 calc R . .
C94 C 0.7843(7) 1.0195(5) 0.0817(4) 0.100(2) Uani 1 1 d . . .
H94 H 0.7663 1.0587 0.0477 0.121 Uiso 1 1 calc R . .
C95 C 0.8911(6) 1.0476(4) 0.1428(4) 0.097(2) Uani 1 1 d . . .
H95 H 0.9481 1.1059 0.1505 0.117 Uiso 1 1 calc R . .
C96 C 0.9182(5) 0.9911(4) 0.1949(4) 0.0780(14) Uani 1 1 d . . .
H96 H 0.9930 1.0116 0.2387 0.094 Uiso 1 1 calc R . .
C97 C 0.8602(5) 0.8449(4) 0.2355(4) 0.0916(17) Uani 1 1 d . . .
H97D H 0.9343 0.8813 0.2886 0.137 Uiso 1 1 calc R . .
H97A H 0.8575 0.7940 0.1992 0.137 Uiso 1 1 calc R . .
H97B H 0.8053 0.8189 0.2542 0.137 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.02723(13) 0.02140(13) 0.02179(12) 0.00729(10) 0.01325(10) 0.01257(11)
Ge1 0.02486(17) 0.02006(18) 0.02220(16) 0.00728(13) 0.01228(14) 0.01158(15)
Ge2 0.02500(18) 0.0288(2) 0.02333(17) 0.00877(14) 0.01253(14) 0.01305(16)
Ge3 0.02967(18) 0.02402(19) 0.02244(17) 0.00865(14) 0.01460(15) 0.01438(15)
Ge4 0.03110(19) 0.02146(18) 0.02628(17) 0.00719(14) 0.01455(15) 0.01306(16)
N1 0.0242(13) 0.0215(14) 0.0268(13) 0.0085(11) 0.0122(11) 0.0134(12)
N2 0.0261(14) 0.0404(17) 0.0245(14) 0.0122(12) 0.0133(12) 0.0134(13)
N3 0.0400(16) 0.0251(15) 0.0223(13) 0.0077(11) 0.0157(12) 0.0153(13)
N4 0.0281(14) 0.0250(15) 0.0373(15) 0.0110(12) 0.0198(13) 0.0133(13)
O11 0.0351(12) 0.0270(12) 0.0310(12) 0.0082(10) 0.0214(10) 0.0152(10)
O12 0.0251(11) 0.0185(11) 0.0286(11) 0.0063(9) 0.0108(9) 0.0117(10)
O21 0.0375(13) 0.0348(14) 0.0336(12) 0.0078(10) 0.0198(11) 0.0191(11)
O22 0.0236(11) 0.0423(14) 0.0245(11) 0.0124(10) 0.0132(10) 0.0111(11)
O31 0.0452(14) 0.0478(16) 0.0402(13) 0.0100(12) 0.0252(12) 0.0307(13)
O32 0.0358(12) 0.0245(12) 0.0209(11) 0.0072(9) 0.0122(10) 0.0120(10)
O41 0.0446(14) 0.0337(14) 0.0259(12) 0.0027(10) 0.0140(11) 0.0210(12)
O42 0.0276(12) 0.0301(13) 0.0419(13) 0.0182(10) 0.0203(10) 0.0176(10)
C11 0.0364(18) 0.0237(18) 0.0379(18) 0.0163(15) 0.0172(16) 0.0182(16)
C12 0.0379(19) 0.034(2) 0.0327(18) 0.0101(15) 0.0213(16) 0.0211(17)
C13 0.0308(18) 0.0276(19) 0.0340(18) 0.0044(14) 0.0151(15) 0.0174(16)
C14 0.0261(16) 0.0203(17) 0.0304(17) 0.0061(13) 0.0130(14) 0.0127(14)
C15 0.0231(16) 0.0218(17) 0.0242(16) 0.0062(13) 0.0093(13) 0.0121(14)
C16 0.0282(17) 0.0227(17) 0.0271(16) 0.0074(13) 0.0112(14) 0.0167(15)
C17 0.0335(19) 0.037(2) 0.0376(19) 0.0152(16) 0.0170(16) 0.0215(17)
C18 0.057(3) 0.059(3) 0.038(2) 0.0266(19) 0.028(2) 0.038(2)
C19 0.060(3) 0.057(3) 0.0269(19) 0.0140(18) 0.0110(19) 0.041(2)
C20 0.033(2) 0.043(2) 0.038(2) 0.0082(18) 0.0036(17) 0.0175(18)
C21 0.0331(19) 0.034(2) 0.0335(18) 0.0116(15) 0.0120(16) 0.0169(17)
C22 0.0233(16) 0.0241(17) 0.0262(16) 0.0110(13) 0.0098(13) 0.0169(14)
C23 0.0278(17) 0.0282(19) 0.0333(18) 0.0104(15) 0.0126(15) 0.0161(16)
C24 0.0341(19) 0.030(2) 0.056(2) 0.0237(18) 0.0243(18) 0.0188(17)
C25 0.045(2) 0.052(3) 0.050(2) 0.032(2) 0.0333(19) 0.033(2)
C26 0.0356(19) 0.048(2) 0.0341(18) 0.0159(17) 0.0196(16) 0.0300(19)
C27 0.0281(17) 0.0301(19) 0.0351(18) 0.0129(15) 0.0170(15) 0.0198(15)
C31 0.044(2) 0.051(2) 0.0343(19) 0.0219(18) 0.0233(17) 0.0202(19)
C32 0.041(2) 0.049(2) 0.043(2) 0.0059(18) 0.0210(18) 0.0276(19)
C33 0.037(2) 0.059(3) 0.0324(19) 0.0118(18) 0.0219(17) 0.0235(19)
C34 0.0245(17) 0.051(2) 0.0329(18) 0.0152(17) 0.0145(15) 0.0186(17)
C35 0.0257(17) 0.038(2) 0.0280(17) 0.0150(15) 0.0148(14) 0.0139(16)
C36 0.0252(17) 0.0261(19) 0.0307(17) 0.0058(14) 0.0095(15) 0.0089(15)
C37 0.0343(19) 0.0290(19) 0.0294(17) 0.0067(15) 0.0138(15) 0.0146(16)
C38 0.051(2) 0.037(2) 0.0340(19) 0.0163(17) 0.0165(18) 0.0213(19)
C39 0.034(2) 0.041(2) 0.048(2) 0.0193(19) 0.0067(18) 0.0171(19)
C40 0.0255(19) 0.045(2) 0.063(3) 0.017(2) 0.0145(19) 0.0160(18)
C41 0.0256(18) 0.045(2) 0.045(2) 0.0163(18) 0.0139(17) 0.0111(17)
C42 0.0367(19) 0.039(2) 0.0295(18) 0.0182(16) 0.0193(16) 0.0157(17)
C43 0.046(2) 0.040(3) 0.083(3) 0.027(2) 0.036(2) 0.017(2)
C44 0.056(3) 0.044(3) 0.100(4) 0.027(3) 0.045(3) 0.010(2)
C45 0.085(3) 0.035(2) 0.065(3) 0.024(2) 0.050(3) 0.025(2)
C46 0.069(3) 0.052(3) 0.033(2) 0.0175(18) 0.029(2) 0.036(2)
C47 0.039(2) 0.040(2) 0.0256(17) 0.0092(15) 0.0152(16) 0.0166(18)
C51 0.036(2) 0.032(2) 0.0325(19) 0.0027(16) 0.0092(16) 0.0069(17)
C52 0.064(3) 0.027(2) 0.0321(19) 0.0052(15) 0.0261(19) 0.0222(19)
C53 0.076(3) 0.044(2) 0.047(2) 0.0180(18) 0.042(2) 0.041(2)
C54 0.045(2) 0.0303(19) 0.0241(16) 0.0091(14) 0.0194(16) 0.0201(17)
C55 0.0376(18) 0.0237(18) 0.0193(15) 0.0084(13) 0.0133(14) 0.0130(15)
C56 0.042(2) 0.0267(19) 0.0209(16) 0.0055(14) 0.0174(15) 0.0122(16)
C57 0.051(2) 0.036(2) 0.040(2) 0.0168(17) 0.0259(18) 0.0201(19)
C58 0.046(2) 0.043(2) 0.054(2) 0.0096(19) 0.029(2) 0.014(2)
C59 0.060(3) 0.045(3) 0.053(2) 0.015(2) 0.040(2) 0.009(2)
C60 0.072(3) 0.032(2) 0.037(2) 0.0148(17) 0.029(2) 0.016(2)
C61 0.050(2) 0.030(2) 0.0295(18) 0.0124(15) 0.0209(17) 0.0153(18)
C62 0.0363(18) 0.0204(17) 0.0238(16) 0.0076(13) 0.0134(15) 0.0118(15)
C63 0.049(2) 0.039(2) 0.0239(17) 0.0132(15) 0.0174(16) 0.0234(18)
C64 0.047(2) 0.039(2) 0.0322(19) 0.0123(16) 0.0118(17) 0.0226(19)
C65 0.040(2) 0.041(2) 0.041(2) 0.0106(17) 0.0161(18) 0.0223(18)
C66 0.044(2) 0.033(2) 0.039(2) 0.0106(16) 0.0242(18) 0.0185(18)
C67 0.0341(18) 0.0248(18) 0.0272(17) 0.0076(14) 0.0135(15) 0.0121(15)
C71 0.0294(19) 0.042(2) 0.048(2) 0.0108(18) 0.0203(17) 0.0121(18)
C72 0.053(2) 0.0260(19) 0.0339(19) 0.0049(15) 0.0240(18) 0.0168(18)
C73 0.055(2) 0.035(2) 0.048(2) 0.0164(17) 0.038(2) 0.0259(19)
C74 0.0290(17) 0.0258(18) 0.0365(18) 0.0121(14) 0.0194(15) 0.0159(15)
C75 0.0239(16) 0.0257(18) 0.0390(18) 0.0158(15) 0.0173(15) 0.0138(15)
C76 0.0269(17) 0.0288(19) 0.0316(17) 0.0106(14) 0.0163(15) 0.0098(15)
C77 0.034(2) 0.034(2) 0.074(3) 0.028(2) 0.020(2) 0.0117(18)
C78 0.052(3) 0.038(2) 0.075(3) 0.032(2) 0.028(2) 0.015(2)
C79 0.054(3) 0.028(2) 0.061(3) 0.0119(19) 0.041(2) 0.0059(19)
C80 0.034(2) 0.037(2) 0.068(3) -0.0041(19) 0.034(2) 0.0071(18)
C81 0.0315(18) 0.029(2) 0.047(2) 0.0041(16) 0.0230(17) 0.0136(16)
C82 0.0258(16) 0.0255(18) 0.0354(18) 0.0123(14) 0.0199(15) 0.0127(15)
C83 0.040(2) 0.036(2) 0.045(2) 0.0127(17) 0.0206(18) 0.0263(18)
C84 0.038(2) 0.045(2) 0.040(2) 0.0152(18) 0.0175(17) 0.0240(19)
C85 0.0365(19) 0.035(2) 0.0344(19) 0.0127(16) 0.0209(16) 0.0138(17)
C86 0.041(2) 0.0272(19) 0.041(2) 0.0149(16) 0.0282(17) 0.0158(17)
C87 0.0287(17) 0.0261(18) 0.0394(19) 0.0174(15) 0.0219(15) 0.0158(15)
C91 0.086(4) 0.057(3) 0.071(3) 0.016(2) 0.053(3) 0.043(3)
C92 0.084(4) 0.073(4) 0.065(3) 0.008(3) 0.040(3) 0.040(3)
C93 0.125(5) 0.110(5) 0.065(3) 0.033(3) 0.052(4) 0.069(5)
C94 0.179(7) 0.088(5) 0.090(5) 0.047(4) 0.098(5) 0.076(5)
C95 0.124(5) 0.072(4) 0.100(5) 0.015(4) 0.081(5) 0.026(4)
C96 0.090(4) 0.064(4) 0.091(4) 0.016(3) 0.061(3) 0.032(3)
C97 0.124(5) 0.088(4) 0.106(4) 0.042(3) 0.070(4) 0.074(4)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pd1 Ge2 2.3584(5) . ?
Pd1 Ge3 2.3585(4) . ?
Pd1 Ge4 2.3588(5) . ?
Pd1 Ge1 2.3685(5) . ?
Ge1 O12 1.8484(19) . ?
Ge1 O11 1.8500(19) . ?
Ge1 N1 2.114(2) . ?
Ge2 O22 1.835(2) . ?
Ge2 O21 1.849(2) . ?
Ge2 N2 2.112(2) . ?
Ge3 O32 1.836(2) . ?
Ge3 O31 1.856(2) . ?
Ge3 N3 2.100(2) . ?
Ge4 O42 1.841(2) . ?
Ge4 O41 1.844(2) . ?
Ge4 N4 2.132(2) . ?
N1 C11 1.476(4) . ?
N1 C14 1.486(3) . ?
N1 C13 1.493(4) . ?
N2 C31 1.482(4) . ?
N2 C33 1.484(4) . ?
N2 C34 1.486(4) . ?
N3 C52 1.473(4) . ?
N3 C51 1.483(4) . ?
N3 C54 1.491(4) . ?
N4 C71 1.473(4) . ?
N4 C74 1.481(4) . ?
N4 C73 1.493(4) . ?
O11 C12 1.407(4) . ?
O12 C15 1.414(3) . ?
O21 C32 1.415(4) . ?
O22 C35 1.413(3) . ?
O31 C53 1.410(4) . ?
O32 C55 1.422(3) . ?
O41 C72 1.413(4) . ?
O42 C75 1.414(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.515(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.552(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C22 1.527(4) . ?
C15 C16 1.541(4) . ?
C16 C21 1.382(4) . ?
C16 C17 1.392(4) . ?
C17 C18 1.377(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.359(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.395(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C27 1.392(4) . ?
C22 C23 1.393(4) . ?
C23 C24 1.383(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.378(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.397(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.515(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.541(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.532(4) . ?
C35 C42 1.540(5) . ?
C36 C37 1.385(4) . ?
C36 C41 1.392(4) . ?
C37 C38 1.381(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.385(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.367(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.376(5) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C47 1.384(4) . ?
C42 C43 1.386(5) . ?
C43 C44 1.368(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.383(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.370(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.384(5) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.513(5) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.543(4) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.531(4) . ?
C55 C62 1.533(4) . ?
C56 C61 1.382(4) . ?
C56 C57 1.390(5) . ?
C57 C58 1.379(5) . ?
C57 H57 0.9500 . ?
C58 C59 1.380(5) . ?
C58 H58 0.9500 . ?
C59 C60 1.370(5) . ?
C59 H59 0.9500 . ?
C60 C61 1.389(5) . ?
C60 H60 0.9500 . ?
C61 H61 0.9500 . ?
C62 C67 1.380(4) . ?
C62 C63 1.400(4) . ?
C63 C64 1.374(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.376(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.382(4) . ?
C65 H65 0.9500 . ?
C66 C67 1.385(4) . ?
C66 H66 0.9500 . ?
C67 H67 0.9500 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 C73 1.511(5) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 C75 1.540(4) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 C76 1.530(4) . ?
C75 C82 1.547(4) . ?
C76 C81 1.374(4) . ?
C76 C77 1.395(4) . ?
C77 C78 1.378(5) . ?
C77 H77 0.9500 . ?
C78 C79 1.369(5) . ?
C78 H78 0.9500 . ?
C79 C80 1.359(5) . ?
C79 H79 0.9500 . ?
C80 C81 1.382(5) . ?
C80 H80 0.9500 . ?
C81 H81 0.9500 . ?
C82 C87 1.381(4) . ?
C82 C83 1.389(4) . ?
C83 C84 1.372(5) . ?
C83 H83 0.9500 . ?
C84 C85 1.391(5) . ?
C84 H84 0.9500 . ?
C85 C86 1.380(4) . ?
C85 H85 0.9500 . ?
C86 C87 1.386(4) . ?
C86 H86 0.9500 . ?
C87 H87 0.9500 . ?
C91 C96 1.370(6) . ?
C91 C92 1.382(6) . ?
C91 C97 1.472(6) . ?
C92 C93 1.358(7) . ?
C92 H92 0.9500 . ?
C93 C94 1.362(8) . ?
C93 H93 0.9500 . ?
C94 C95 1.355(8) . ?
C94 H94 0.9500 . ?
C95 C96 1.403(7) . ?
C95 H95 0.9500 . ?
C96 H96 0.9500 . ?
C97 H97D 0.9800 . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
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
Ge2 Pd1 Ge3 110.336(15) . . ?
Ge2 Pd1 Ge4 111.398(15) . . ?
Ge3 Pd1 Ge4 103.963(14) . . ?
Ge2 Pd1 Ge1 101.237(14) . . ?
Ge3 Pd1 Ge1 115.024(17) . . ?
Ge4 Pd1 Ge1 115.077(14) . . ?
O12 Ge1 O11 103.12(9) . . ?
O12 Ge1 N1 83.90(9) . . ?
O11 Ge1 N1 84.76(9) . . ?
O12 Ge1 Pd1 131.53(6) . . ?
O11 Ge1 Pd1 118.06(7) . . ?
N1 Ge1 Pd1 122.24(6) . . ?
O22 Ge2 O21 104.85(10) . . ?
O22 Ge2 N2 84.06(9) . . ?
O21 Ge2 N2 84.52(10) . . ?
O22 Ge2 Pd1 126.49(7) . . ?
O21 Ge2 Pd1 119.68(7) . . ?
N2 Ge2 Pd1 125.77(7) . . ?
O32 Ge3 O31 103.65(10) . . ?
O32 Ge3 N3 84.74(9) . . ?
O31 Ge3 N3 83.58(10) . . ?
O32 Ge3 Pd1 126.71(6) . . ?
O31 Ge3 Pd1 122.90(7) . . ?
N3 Ge3 Pd1 121.97(7) . . ?
O42 Ge4 O41 103.58(10) . . ?
O42 Ge4 N4 83.36(9) . . ?
O41 Ge4 N4 84.72(10) . . ?
O42 Ge4 Pd1 126.39(7) . . ?
O41 Ge4 Pd1 118.24(7) . . ?
N4 Ge4 Pd1 129.76(7) . . ?
C11 N1 C14 113.3(2) . . ?
C11 N1 C13 111.3(2) . . ?
C14 N1 C13 110.2(2) . . ?
C11 N1 Ge1 111.94(18) . . ?
C14 N1 Ge1 106.48(16) . . ?
C13 N1 Ge1 103.05(17) . . ?
C31 N2 C33 111.3(2) . . ?
C31 N2 C34 112.8(3) . . ?
C33 N2 C34 110.6(2) . . ?
C31 N2 Ge2 113.27(19) . . ?
C33 N2 Ge2 102.28(19) . . ?
C34 N2 Ge2 106.05(17) . . ?
C52 N3 C51 111.8(3) . . ?
C52 N3 C54 111.1(2) . . ?
C51 N3 C54 112.5(2) . . ?
C52 N3 Ge3 103.05(18) . . ?
C51 N3 Ge3 113.04(18) . . ?
C54 N3 Ge3 104.77(18) . . ?
C71 N4 C74 112.5(2) . . ?
C71 N4 C73 111.3(2) . . ?
C74 N4 C73 111.5(2) . . ?
C71 N4 Ge4 112.6(2) . . ?
C74 N4 Ge4 105.95(16) . . ?
C73 N4 Ge4 102.53(18) . . ?
C12 O11 Ge1 116.07(18) . . ?
C15 O12 Ge1 118.56(16) . . ?
C32 O21 Ge2 116.5(2) . . ?
C35 O22 Ge2 120.55(17) . . ?
C53 O31 Ge3 117.2(2) . . ?
C55 O32 Ge3 119.41(18) . . ?
C72 O41 Ge4 116.20(19) . . ?
C75 O42 Ge4 118.26(17) . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O11 C12 C13 109.3(2) . . ?
O11 C12 H12A 109.8 . . ?
C13 C12 H12A 109.8 . . ?
O11 C12 H12B 109.8 . . ?
C13 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
N1 C13 C12 107.9(2) . . ?
N1 C13 H13A 110.1 . . ?
C12 C13 H13A 110.1 . . ?
N1 C13 H13B 110.1 . . ?
C12 C13 H13B 110.1 . . ?
H13A C13 H13B 108.4 . . ?
N1 C14 C15 110.6(2) . . ?
N1 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
O12 C15 C22 111.7(2) . . ?
O12 C15 C16 107.7(2) . . ?
C22 C15 C16 114.5(2) . . ?
O12 C15 C14 107.0(2) . . ?
C22 C15 C14 109.6(2) . . ?
C16 C15 C14 105.9(2) . . ?
C21 C16 C17 117.5(3) . . ?
C21 C16 C15 125.3(3) . . ?
C17 C16 C15 117.1(3) . . ?
C18 C17 C16 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 119.8(3) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.3(3) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C16 C21 C20 120.9(3) . . ?
C16 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C27 C22 C23 118.0(3) . . ?
C27 C22 C15 120.8(3) . . ?
C23 C22 C15 121.0(3) . . ?
C24 C23 C22 121.5(3) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C25 C24 C23 119.9(3) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 119.9(3) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C27 120.2(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C22 C27 C26 120.5(3) . . ?
C22 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
N2 C31 H31A 109.5 . . ?
N2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O21 C32 C33 109.2(3) . . ?
O21 C32 H32A 109.8 . . ?
C33 C32 H32A 109.8 . . ?
O21 C32 H32B 109.8 . . ?
C33 C32 H32B 109.8 . . ?
H32A C32 H32B 108.3 . . ?
N2 C33 C32 108.1(3) . . ?
N2 C33 H33A 110.1 . . ?
C32 C33 H33A 110.1 . . ?
N2 C33 H33B 110.1 . . ?
C32 C33 H33B 110.1 . . ?
H33A C33 H33B 108.4 . . ?
N2 C34 C35 111.3(2) . . ?
N2 C34 H34A 109.4 . . ?
C35 C34 H34A 109.4 . . ?
N2 C34 H34B 109.4 . . ?
C35 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
O22 C35 C36 108.3(2) . . ?
O22 C35 C42 110.3(3) . . ?
C36 C35 C42 110.0(3) . . ?
O22 C35 C34 108.6(2) . . ?
C36 C35 C34 109.8(3) . . ?
C42 C35 C34 109.7(3) . . ?
C37 C36 C41 118.2(3) . . ?
C37 C36 C35 119.3(3) . . ?
C41 C36 C35 122.5(3) . . ?
C38 C37 C36 120.5(3) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
C37 C38 C39 120.5(3) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C40 C39 C38 119.2(3) . . ?
C40 C39 H39 120.4 . . ?
C38 C39 H39 120.4 . . ?
C39 C40 C41 120.6(3) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C40 C41 C36 120.9(3) . . ?
C40 C41 H41 119.5 . . ?
C36 C41 H41 119.5 . . ?
C47 C42 C43 117.4(3) . . ?
C47 C42 C35 121.5(3) . . ?
C43 C42 C35 120.9(3) . . ?
C44 C43 C42 121.4(4) . . ?
C44 C43 H43 119.3 . . ?
C42 C43 H43 119.3 . . ?
C43 C44 C45 121.0(4) . . ?
C43 C44 H44 119.5 . . ?
C45 C44 H44 119.5 . . ?
C46 C45 C44 118.3(4) . . ?
C46 C45 H45 120.9 . . ?
C44 C45 H45 120.9 . . ?
C45 C46 C47 120.9(4) . . ?
C45 C46 H46 119.6 . . ?
C47 C46 H46 119.6 . . ?
C42 C47 C46 121.1(3) . . ?
C42 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
N3 C51 H51A 109.5 . . ?
N3 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N3 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N3 C52 C53 108.4(3) . . ?
N3 C52 H52A 110.0 . . ?
C53 C52 H52A 110.0 . . ?
N3 C52 H52B 110.0 . . ?
C53 C52 H52B 110.0 . . ?
H52A C52 H52B 108.4 . . ?
O31 C53 C52 110.1(3) . . ?
O31 C53 H53A 109.6 . . ?
C52 C53 H53A 109.6 . . ?
O31 C53 H53B 109.6 . . ?
C52 C53 H53B 109.6 . . ?
H53A C53 H53B 108.2 . . ?
N3 C54 C55 110.9(2) . . ?
N3 C54 H54A 109.5 . . ?
C55 C54 H54A 109.5 . . ?
N3 C54 H54B 109.5 . . ?
C55 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
O32 C55 C56 107.3(2) . . ?
O32 C55 C62 110.4(2) . . ?
C56 C55 C62 113.7(3) . . ?
O32 C55 C54 107.3(2) . . ?
C56 C55 C54 108.5(2) . . ?
C62 C55 C54 109.5(2) . . ?
C61 C56 C57 118.2(3) . . ?
C61 C56 C55 124.5(3) . . ?
C57 C56 C55 117.3(3) . . ?
C58 C57 C56 121.3(3) . . ?
C58 C57 H57 119.4 . . ?
C56 C57 H57 119.4 . . ?
C57 C58 C59 119.7(4) . . ?
C57 C58 H58 120.1 . . ?
C59 C58 H58 120.1 . . ?
C60 C59 C58 119.8(4) . . ?
C60 C59 H59 120.1 . . ?
C58 C59 H59 120.1 . . ?
C59 C60 C61 120.4(4) . . ?
C59 C60 H60 119.8 . . ?
C61 C60 H60 119.8 . . ?
C56 C61 C60 120.5(3) . . ?
C56 C61 H61 119.7 . . ?
C60 C61 H61 119.7 . . ?
C67 C62 C63 118.0(3) . . ?
C67 C62 C55 121.4(3) . . ?
C63 C62 C55 120.5(3) . . ?
C64 C63 C62 120.7(3) . . ?
C64 C63 H63 119.7 . . ?
C62 C63 H63 119.7 . . ?
C63 C64 C65 120.8(3) . . ?
C63 C64 H64 119.6 . . ?
C65 C64 H64 119.6 . . ?
C64 C65 C66 119.1(3) . . ?
C64 C65 H65 120.5 . . ?
C66 C65 H65 120.5 . . ?
C65 C66 C67 120.3(3) . . ?
C65 C66 H66 119.9 . . ?
C67 C66 H66 119.9 . . ?
C62 C67 C66 121.1(3) . . ?
C62 C67 H67 119.5 . . ?
C66 C67 H67 119.5 . . ?
N4 C71 H71A 109.5 . . ?
N4 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
N4 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
O41 C72 C73 109.0(3) . . ?
O41 C72 H72A 109.9 . . ?
C73 C72 H72A 109.9 . . ?
O41 C72 H72B 109.9 . . ?
C73 C72 H72B 109.9 . . ?
H72A C72 H72B 108.3 . . ?
N4 C73 C72 108.3(2) . . ?
N4 C73 H73A 110.0 . . ?
C72 C73 H73A 110.0 . . ?
N4 C73 H73B 110.0 . . ?
C72 C73 H73B 110.0 . . ?
H73A C73 H73B 108.4 . . ?
N4 C74 C75 110.6(2) . . ?
N4 C74 H74A 109.5 . . ?
C75 C74 H74A 109.5 . . ?
N4 C74 H74B 109.5 . . ?
C75 C74 H74B 109.5 . . ?
H74A C74 H74B 108.1 . . ?
O42 C75 C76 108.3(2) . . ?
O42 C75 C74 106.5(2) . . ?
C76 C75 C74 109.1(2) . . ?
O42 C75 C82 110.9(2) . . ?
C76 C75 C82 110.2(2) . . ?
C74 C75 C82 111.7(2) . . ?
C81 C76 C77 117.5(3) . . ?
C81 C76 C75 120.6(3) . . ?
C77 C76 C75 121.9(3) . . ?
C78 C77 C76 121.1(3) . . ?
C78 C77 H77 119.5 . . ?
C76 C77 H77 119.5 . . ?
C79 C78 C77 120.4(4) . . ?
C79 C78 H78 119.8 . . ?
C77 C78 H78 119.8 . . ?
C80 C79 C78 118.8(3) . . ?
C80 C79 H79 120.6 . . ?
C78 C79 H79 120.6 . . ?
C79 C80 C81 121.6(3) . . ?
C79 C80 H80 119.2 . . ?
C81 C80 H80 119.2 . . ?
C76 C81 C80 120.5(3) . . ?
C76 C81 H81 119.7 . . ?
C80 C81 H81 119.7 . . ?
C87 C82 C83 117.5(3) . . ?
C87 C82 C75 121.6(3) . . ?
C83 C82 C75 120.9(3) . . ?
C84 C83 C82 122.1(3) . . ?
C84 C83 H83 119.0 . . ?
C82 C83 H83 119.0 . . ?
C83 C84 C85 120.0(3) . . ?
C83 C84 H84 120.0 . . ?
C85 C84 H84 120.0 . . ?
C86 C85 C84 118.6(3) . . ?
C86 C85 H85 120.7 . . ?
C84 C85 H85 120.7 . . ?
C85 C86 C87 120.8(3) . . ?
C85 C86 H86 119.6 . . ?
C87 C86 H86 119.6 . . ?
C82 C87 C86 121.1(3) . . ?
C82 C87 H87 119.5 . . ?
C86 C87 H87 119.5 . . ?
C96 C91 C92 118.6(5) . . ?
C96 C91 C97 121.2(5) . . ?
C92 C91 C97 120.1(5) . . ?
C93 C92 C91 121.3(6) . . ?
C93 C92 H92 119.3 . . ?
C91 C92 H92 119.3 . . ?
C92 C93 C94 120.2(6) . . ?
C92 C93 H93 119.9 . . ?
C94 C93 H93 119.9 . . ?
C95 C94 C93 119.9(6) . . ?
C95 C94 H94 120.0 . . ?
C93 C94 H94 120.0 . . ?
C94 C95 C96 120.5(6) . . ?
C94 C95 H95 119.8 . . ?
C96 C95 H95 119.8 . . ?
C91 C96 C95 119.4(5) . . ?
C91 C96 H96 120.3 . . ?
C95 C96 H96 120.3 . . ?
C91 C97 H97D 109.5 . . ?
C91 C97 H97A 109.5 . . ?
H97D C97 H97A 109.5 . . ?
C91 C97 H97B 109.5 . . ?
H97D C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.077


data_12
_database_code_depnum_ccdc_archive 'CCDC 911591'
#TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1358416028.new_COMB.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H40 N2 O4 Pd, 3(C6 H6)'
_chemical_formula_sum            'C52 H58 N2 O4 Pd'
_chemical_formula_weight         881.40
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
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'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   29.222(4)
_cell_length_b                   11.0428(14)
_cell_length_c                   14.8017(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.719(2)
_cell_angle_gamma                90.00
_cell_volume                     4467.5(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.312
_cell_measurement_theta_max      30.463
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8738
_exptl_absorpt_correction_T_max  0.9863
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            24132
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         29.00
_reflns_number_total             5924
_reflns_number_gt                4765
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       '<i>APEX2</i> (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The structure contains two disordered solvate benzene molecules, one of them
lies on the inversion centre. This molecule was refined with restrained C-C
distances (SADI).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+3.5423P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5924
_refine_ls_number_parameters     237
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0921
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.2500 0.2500 0.5000 0.02082(7) Uani 1 2 d S . .
N1 N 0.24818(6) 0.32152(14) 0.37022(10) 0.0265(3) Uani 1 1 d . . .
O1 O 0.29520(5) 0.38677(11) 0.55936(8) 0.0256(3) Uani 1 1 d . . .
O2 O 0.24344(8) 0.05302(16) 0.31213(14) 0.0560(5) Uani 1 1 d . . .
H2 H 0.2346(12) 0.061(3) 0.355(3) 0.070(10) Uiso 1 1 d . . .
C1 C 0.19646(8) 0.3254(2) 0.30132(14) 0.0368(4) Uani 1 1 d . . .
H1A H 0.1950 0.3704 0.2433 0.055 Uiso 1 1 calc R . .
H1B H 0.1759 0.3658 0.3321 0.055 Uiso 1 1 calc R . .
H1C H 0.1846 0.2427 0.2834 0.055 Uiso 1 1 calc R . .
C2 C 0.28610(9) 0.1235(2) 0.34394(18) 0.0444(5) Uani 1 1 d . . .
H2A H 0.3091 0.0918 0.3140 0.053 Uiso 1 1 calc R . .
H2B H 0.3018 0.1133 0.4147 0.053 Uiso 1 1 calc R . .
C3 C 0.27880(9) 0.25699(17) 0.32202(15) 0.0329(4) Uani 1 1 d . . .
H3A H 0.3113 0.2964 0.3421 0.040 Uiso 1 1 calc R . .
H3B H 0.2632 0.2673 0.2513 0.040 Uiso 1 1 calc R . .
C4 C 0.30816(7) 0.45638(16) 0.49192(12) 0.0247(3) Uani 1 1 d . . .
C5 C 0.26546(7) 0.44963(17) 0.39483(13) 0.0269(4) Uani 1 1 d . . .
H5A H 0.2380 0.4999 0.3980 0.032 Uiso 1 1 calc R . .
H5B H 0.2761 0.4828 0.3432 0.032 Uiso 1 1 calc R . .
C11 C 0.31658(7) 0.58799(17) 0.52774(13) 0.0272(4) Uani 1 1 d . . .
C12 C 0.30322(9) 0.68713(19) 0.46659(17) 0.0394(5) Uani 1 1 d . . .
H12 H 0.2871 0.6747 0.3992 0.047 Uiso 1 1 calc R . .
C13 C 0.31297(9) 0.8048(2) 0.5023(2) 0.0467(5) Uani 1 1 d . . .
H13 H 0.3031 0.8718 0.4596 0.056 Uiso 1 1 calc R . .
C14 C 0.33703(9) 0.8236(2) 0.5997(2) 0.0449(5) Uani 1 1 d . . .
H14 H 0.3445 0.9036 0.6241 0.054 Uiso 1 1 calc R . .
C15 C 0.35018(9) 0.7264(2) 0.66121(19) 0.0410(5) Uani 1 1 d . . .
H15 H 0.3663 0.7395 0.7285 0.049 Uiso 1 1 calc R . .
C16 C 0.34014(8) 0.60883(19) 0.62612(15) 0.0338(4) Uani 1 1 d . . .
H16 H 0.3494 0.5423 0.6695 0.041 Uiso 1 1 calc R . .
C21 C 0.35645(7) 0.41050(17) 0.48432(13) 0.0274(4) Uani 1 1 d . . .
C22 C 0.38117(8) 0.3134(2) 0.53922(15) 0.0360(4) Uani 1 1 d . . .
H22 H 0.3687 0.2760 0.5836 0.043 Uiso 1 1 calc R . .
C23 C 0.42406(10) 0.2698(2) 0.5302(2) 0.0492(6) Uani 1 1 d . . .
H23 H 0.4406 0.2031 0.5683 0.059 Uiso 1 1 calc R . .
C24 C 0.44271(9) 0.3233(3) 0.46593(19) 0.0504(6) Uani 1 1 d . . .
H24 H 0.4718 0.2931 0.4595 0.060 Uiso 1 1 calc R . .
C25 C 0.41853(9) 0.4215(2) 0.41102(18) 0.0444(5) Uani 1 1 d . . .
H25 H 0.4312 0.4589 0.3670 0.053 Uiso 1 1 calc R . .
C26 C 0.37586(8) 0.4647(2) 0.42054(15) 0.0353(4) Uani 1 1 d . . .
H26 H 0.3596 0.5323 0.3831 0.042 Uiso 1 1 calc R . .
C31 C 0.57436(18) -0.0128(2) 0.6464(4) 0.0887(19) Uiso 0.62 1 d PG A 1
H31 H 0.5763 -0.0986 0.6456 0.106 Uiso 0.62 1 calc PR A 1
C32 C 0.58789(15) 0.0556(4) 0.5811(3) 0.0789(16) Uiso 0.62 1 d PG A 1
H32 H 0.5991 0.0165 0.5356 0.095 Uiso 0.62 1 calc PR A 1
C33 C 0.58501(13) 0.1812(4) 0.5823(3) 0.0582(11) Uiso 0.62 1 d PG A 1
H33 H 0.5943 0.2279 0.5376 0.070 Uiso 0.62 1 calc PR A 1
C34 C 0.56861(14) 0.2384(2) 0.6488(3) 0.0550(12) Uiso 0.62 1 d PG A 1
H34 H 0.5666 0.3242 0.6496 0.066 Uiso 0.62 1 calc PR A 1
C35 C 0.55508(15) 0.1700(4) 0.7141(3) 0.0600(13) Uiso 0.62 1 d PG A 1
H35 H 0.5439 0.2091 0.7596 0.072 Uiso 0.62 1 calc PR A 1
C36 C 0.55796(16) 0.0444(4) 0.7129(3) 0.0718(15) Uiso 0.62 1 d PG A 1
H36 H 0.5487 -0.0023 0.7576 0.086 Uiso 0.62 1 calc PR A 1
C41 C 0.5772(3) 0.0105(5) 0.5932(4) 0.081(3) Uiso 0.38 1 d PG B 2
H41 H 0.5829 -0.0552 0.5571 0.098 Uiso 0.38 1 calc PR B 2
C42 C 0.5781(2) 0.1287(7) 0.5616(4) 0.067(2) Uiso 0.38 1 d PG B 2
H42 H 0.5844 0.1438 0.5039 0.080 Uiso 0.38 1 calc PR B 2
C43 C 0.5697(2) 0.2248(4) 0.6144(5) 0.0530(18) Uiso 0.38 1 d PG B 2
H43 H 0.5704 0.3056 0.5928 0.064 Uiso 0.38 1 calc PR B 2
C44 C 0.5605(3) 0.2027(5) 0.6988(5) 0.067(2) Uiso 0.38 1 d PG B 2
H44 H 0.5548 0.2684 0.7349 0.080 Uiso 0.38 1 calc PR B 2
C45 C 0.5596(3) 0.0845(7) 0.7304(4) 0.069(2) Uiso 0.38 1 d PG B 2
H45 H 0.5533 0.0694 0.7881 0.083 Uiso 0.38 1 calc PR B 2
C46 C 0.5679(3) -0.0116(4) 0.6776(5) 0.0581(18) Uiso 0.38 1 d PG B 2
H46 H 0.5673 -0.0924 0.6992 0.070 Uiso 0.38 1 calc PR B 2
C51 C 0.48297(12) 0.7296(3) 0.7041(2) 0.0511(8) Uiso 0.80 1 d PD . 3
H51 H 0.4712 0.8041 0.6722 0.061 Uiso 0.80 1 calc PR . 3
C52 C 0.46576(13) 0.6215(3) 0.6579(2) 0.0519(7) Uiso 0.80 1 d PD C 3
H52 H 0.4420 0.6213 0.5945 0.062 Uiso 0.80 1 calc PR C 3
C53 C 0.48316(12) 0.5142(3) 0.70407(19) 0.0594(9) Uiso 0.80 1 d PD . 3
H53 H 0.4718 0.4396 0.6720 0.071 Uiso 0.80 1 calc PR . 3
C61 C 0.5000 0.7443(13) 0.7500 0.0433(15) Uiso 0.20 2 d SPD . 4
H61 H 0.5000 0.8303 0.7500 0.052 Uiso 0.20 2 calc SPR . 4
C62 C 0.4680(4) 0.6821(9) 0.6728(7) 0.0433(15) Uiso 0.20 1 d PD D 4
H62 H 0.4459 0.7251 0.6197 0.052 Uiso 0.20 1 calc PR D 4
C63 C 0.4682(4) 0.5580(9) 0.6727(7) 0.0433(15) Uiso 0.20 1 d PD D 4
H63 H 0.4464 0.5144 0.6195 0.052 Uiso 0.20 1 calc PR D 4
C64 C 0.5000 0.4980(14) 0.7500 0.0433(15) Uiso 0.20 2 d SPD . 4
H64 H 0.5000 0.4120 0.7500 0.052 Uiso 0.20 2 calc SPR . 4
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.02693(10) 0.02234(10) 0.01513(10) -0.00028(6) 0.00984(7) -0.00237(7)
N1 0.0333(8) 0.0291(8) 0.0182(6) -0.0005(6) 0.0105(6) -0.0055(6)
O1 0.0334(6) 0.0273(6) 0.0184(5) -0.0007(5) 0.0119(5) -0.0068(5)
O2 0.0899(14) 0.0474(10) 0.0533(10) -0.0263(8) 0.0534(11) -0.0315(9)
C1 0.0386(11) 0.0403(11) 0.0245(9) 0.0062(8) 0.0025(8) -0.0083(9)
C2 0.0620(14) 0.0391(12) 0.0466(12) -0.0148(10) 0.0371(12) -0.0082(10)
C3 0.0441(11) 0.0385(11) 0.0236(9) -0.0084(7) 0.0211(8) -0.0120(8)
C4 0.0317(9) 0.0248(8) 0.0202(8) 0.0003(6) 0.0122(7) -0.0033(7)
C5 0.0339(9) 0.0271(9) 0.0203(8) 0.0020(7) 0.0103(7) -0.0034(7)
C11 0.0297(9) 0.0263(9) 0.0292(9) -0.0010(7) 0.0147(7) -0.0020(7)
C12 0.0493(12) 0.0293(11) 0.0399(11) 0.0032(9) 0.0162(10) -0.0027(9)
C13 0.0549(14) 0.0271(11) 0.0601(15) 0.0048(10) 0.0230(12) -0.0003(10)
C14 0.0464(12) 0.0286(10) 0.0677(16) -0.0151(11) 0.0299(12) -0.0056(9)
C15 0.0462(12) 0.0408(12) 0.0406(12) -0.0140(9) 0.0210(10) -0.0070(9)
C16 0.0401(10) 0.0327(10) 0.0304(9) -0.0044(8) 0.0145(8) -0.0058(8)
C21 0.0308(9) 0.0277(9) 0.0252(8) -0.0062(7) 0.0116(7) -0.0049(7)
C22 0.0400(11) 0.0375(11) 0.0333(10) 0.0006(8) 0.0164(8) 0.0035(9)
C23 0.0465(13) 0.0505(14) 0.0519(15) 0.0007(11) 0.0191(12) 0.0150(11)
C24 0.0419(12) 0.0594(16) 0.0567(15) -0.0133(12) 0.0258(11) 0.0053(11)
C25 0.0471(12) 0.0496(13) 0.0485(13) -0.0103(10) 0.0319(11) -0.0088(10)
C26 0.0399(10) 0.0350(10) 0.0367(10) -0.0029(8) 0.0205(9) -0.0057(8)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Pd1 O1 1.9941(12) 7_556 ?
Pd1 O1 1.9941(12) . ?
Pd1 N1 2.0602(14) 7_556 ?
Pd1 N1 2.0602(14) . ?
N1 C1 1.495(2) . ?
N1 C5 1.503(2) . ?
N1 C3 1.506(3) . ?
O1 C4 1.414(2) . ?
O2 C2 1.402(3) . ?
O2 H2 0.77(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.508(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.536(2) . ?
C4 C11 1.537(3) . ?
C4 C21 1.540(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C11 C12 1.386(3) . ?
C11 C16 1.392(3) . ?
C12 C13 1.393(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.372(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.385(3) . ?
C21 C26 1.397(3) . ?
C22 C23 1.392(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C31 H31 0.9500 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 C35 1.3900 . ?
C34 H34 0.9500 . ?
C35 C36 1.3900 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.3900 . ?
C41 C46 1.3900 . ?
C41 H41 0.9500 . ?
C42 C43 1.3900 . ?
C42 H42 0.9500 . ?
C43 C44 1.3900 . ?
C43 H43 0.9500 . ?
C44 C45 1.3900 . ?
C44 H44 0.9500 . ?
C45 C46 1.3900 . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C51 1.372(5) 2_656 ?
C51 C52 1.379(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.373(4) . ?
C52 H52 0.9500 . ?
C53 C53 1.368(5) 2_656 ?
C53 H53 0.9500 . ?
C61 C62 1.377(6) . ?
C61 C62 1.377(6) 2_656 ?
C61 H61 0.9500 . ?
C62 C63 1.370(6) . ?
C62 H62 0.9500 . ?
C63 C64 1.364(6) . ?
C63 H63 0.9500 . ?
C64 C63 1.364(6) 2_656 ?
C64 H64 0.9500 . ?
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
O1 Pd1 O1 180.00(8) 7_556 . ?
O1 Pd1 N1 85.13(5) 7_556 7_556 ?
O1 Pd1 N1 94.87(5) . 7_556 ?
O1 Pd1 N1 94.87(5) 7_556 . ?
O1 Pd1 N1 85.13(5) . . ?
N1 Pd1 N1 180.0 7_556 . ?
C1 N1 C5 108.07(15) . . ?
C1 N1 C3 108.48(16) . . ?
C5 N1 C3 110.80(14) . . ?
C1 N1 Pd1 109.48(11) . . ?
C5 N1 Pd1 103.84(10) . . ?
C3 N1 Pd1 115.88(12) . . ?
C4 O1 Pd1 113.70(10) . . ?
C2 O2 H2 100(3) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 C3 115.4(2) . . ?
O2 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
O2 C2 H2B 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
N1 C3 C2 115.02(16) . . ?
N1 C3 H3A 108.5 . . ?
C2 C3 H3A 108.5 . . ?
N1 C3 H3B 108.5 . . ?
C2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
O1 C4 C5 107.60(14) . . ?
O1 C4 C11 108.70(14) . . ?
C5 C4 C11 110.28(15) . . ?
O1 C4 C21 110.73(15) . . ?
C5 C4 C21 112.19(14) . . ?
C11 C4 C21 107.30(14) . . ?
N1 C5 C4 111.38(14) . . ?
N1 C5 H5A 109.4 . . ?
C4 C5 H5A 109.4 . . ?
N1 C5 H5B 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C12 C11 C16 118.25(18) . . ?
C12 C11 C4 123.23(17) . . ?
C16 C11 C4 118.48(17) . . ?
C11 C12 C13 121.1(2) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 119.8(2) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C15 C14 C13 119.8(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 120.7(2) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C11 120.4(2) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C22 C21 C26 118.45(18) . . ?
C22 C21 C4 120.88(16) . . ?
C26 C21 C4 120.66(17) . . ?
C21 C22 C23 120.8(2) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 119.5(2) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C26 C25 C24 119.9(2) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C21 121.0(2) . . ?
C25 C26 H26 119.5 . . ?
C21 C26 H26 119.5 . . ?
C32 C31 C36 120.0 . . ?
C32 C31 H31 120.0 . . ?
C36 C31 H31 120.0 . . ?
C31 C32 C33 120.0 . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
C42 C41 C46 120.0 . . ?
C42 C41 H41 120.0 . . ?
C46 C41 H41 120.0 . . ?
C43 C42 C41 120.0 . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 120.0 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C45 120.0 . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C46 120.0 . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C41 120.0 . . ?
C45 C46 H46 120.0 . . ?
C41 C46 H46 120.0 . . ?
C51 C51 C52 120.03(18) 2_656 . ?
C51 C51 H51 120.0 2_656 . ?
C52 C51 H51 120.0 . . ?
C53 C52 C51 119.7(3) . . ?
C53 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C53 C53 C52 120.27(19) 2_656 . ?
C53 C53 H53 119.9 2_656 . ?
C52 C53 H53 119.9 . . ?
C62 C61 C62 120.1(14) . 2_656 ?
C62 C61 H61 120.0 . . ?
C62 C61 H61 120.0 2_656 . ?
C63 C62 C61 120.0(11) . . ?
C63 C62 H62 120.0 . . ?
C61 C62 H62 120.0 . . ?
C64 C63 C62 119.1(12) . . ?
C64 C63 H63 120.5 . . ?
C62 C63 H63 120.5 . . ?
C63 C64 C63 121.9(15) 2_656 . ?
C63 C64 H64 119.1 2_656 . ?
C63 C64 H64 119.1 . . ?
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
O2 H2 O1 0.77(3) 1.87(4) 2.618(2) 166(4) 7_556
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.070