 
data_e92
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
;
C27 H60 Cl3.76 N3 Zn, Cl11 Pb3, 6(C9 H20 N), Cl2.67 Zn
;
_chemical_formula_sum
 'C81 H180 Cl18 N9 Pb3 Zn2' 
_chemical_formula_weight          2670.74

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'
 'Zn'  'Zn'   0.2839   1.4301
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            159
_space_group_name_H-M_alt         'P 3 1 c'
_space_group_name_Hall            'P 3 -2c'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, z+1/2'
 'x-y, -y, z+1/2'
 '-x, -x+y, z+1/2'
 
_cell_length_a                    14.8386(5)
_cell_length_b                    14.8386(5)
_cell_length_c                    30.6974(11)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      5853.5(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     43632
_cell_measurement_theta_min       1.560 
_cell_measurement_theta_max       23.200
 
_exptl_crystal_description        sphere
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.441          
_exptl_crystal_F_000              2682
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_rad           0.5
_exptl_crystal_size_max           0.5
_exptl_crystal_size_mid           0.5
_exptl_crystal_size_min           0.45
_exptl_absorpt_coefficient_mu     4.924
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.5782
_exptl_absorpt_correction_T_max   0.7453
_exptl_absorpt_process_details  
;
SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004
; 
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type  'Bruker PHOTON2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             43632
_diffrn_reflns_av_unetI/netI      0.0395
_diffrn_reflns_av_R_equivalents   0.0783
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -34
_diffrn_reflns_limit_l_max        34
_diffrn_reflns_theta_min          1.560
_diffrn_reflns_theta_max          23.200
_diffrn_reflns_theta_full         23.200
_diffrn_measured_fraction_theta_max   0.996
_diffrn_measured_fraction_theta_full  0.997
_diffrn_reflns_Laue_measured_fraction_max    0.996
_diffrn_reflns_Laue_measured_fraction_full   0.997
_diffrn_reflns_point_group_measured_fraction_max   0.996
_diffrn_reflns_point_group_measured_fraction_full  0.997
_reflns_number_total              5669
_reflns_number_gt                 4376
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.995
_reflns_Friedel_fraction_max      0.996
_reflns_Friedel_fraction_full     0.997
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'APEX2 (Bruker, 2003-2008)' 
_computing_cell_refinement        'APEX2 (Bruker, 2003-2008)' 
_computing_data_reduction         'SAINT (Bruker, 2009)' 
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'DIAMOND (Brandenburg, 2005)' 
_computing_publication_material   'publCIF (Westrip, 2009)' 
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1521P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refU
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.0013(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.50(3)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          5669
_refine_ls_number_parameters      92
_refine_ls_number_restraints      13
_refine_ls_R_factor_all           0.0938
_refine_ls_R_factor_gt            0.0735
_refine_ls_wR_factor_ref          0.2310
_refine_ls_wR_factor_gt           0.2113
_refine_ls_goodness_of_fit_ref    1.116
_refine_ls_restrained_S_all       1.119
_refine_ls_shift/su_max           0.010
_refine_ls_shift/su_mean          0.001
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pb Pb 0.75829(17) 0.51667(5) 0.72654(13) 0.0702(4) Uani 1 1 d . . . . .
Cl1 Cl 0.6667 0.3333 0.7921(4) 0.056(3) Uani 1 3 d S T P . .
Cl2 Cl 0.6667 0.3333 0.6690(5) 0.092(6) Uani 1 3 d S T P . .
Cl3 Cl 0.5419(15) 0.4691(16) 0.7308(5) 0.113(3) Uani 1 1 d . . . . .
Cl4 Cl 0.830(2) 0.6660(17) 0.7907(5) 0.207(8) Uani 1 1 d . . . . .
Cl5 Cl 0.8278(11) 0.6599(9) 0.6612(4) 0.123(4) Uani 1 1 d . . . . .
Zn1 Zn 0.3333 0.6667 0.5280(4) 0.141(4) Uani 1 3 d DS T P . .
Zn2 Zn 0.3333 0.6667 0.9305(3) 0.105(3) Uani 1 3 d DS T P . .
Cl6 Cl 0.260(2) 0.748(2) 0.9660(9) 0.174(13) Uiso 0.74(7) 1 d . . . . .
Cl71 Cl 0.499(2) 0.727(5) 0.4998(11) 0.100(17) Uiso 0.37(13) 1 d . . . . .
Cl72 Cl 0.5009(17) 0.765(4) 0.5033(10) 0.112(12) Uiso 0.55(13) 1 d . . . . .
Cl8 Cl 0.3333 0.6667 0.5960(5) 0.219(12) Uiso 1 3 d DS . P . .
Cl9 Cl 0.3333 0.6667 0.8622(5) 0.219(12) Uiso 0.45(7) 3 d DS . . . .
N11 N 0.170(4) 0.841(4) 0.7202(14) 0.43(3) Uiso 1 1 d G U . . .
C11 C 0.156(8) 0.681(4) 0.723(2) 0.43(3) Uiso 1 1 d G U . . .
C21 C 0.094(4) 0.730(4) 0.7231(17) 0.43(3) Uiso 1 1 d G U . . .
C31 C 0.228(3) 0.885(3) 0.7612(16) 0.43(3) Uiso 1 1 d G U . . .
C41 C 0.163(3) 0.875(3) 0.7989(15) 0.43(3) Uiso 1 1 d G U . . .
C51 C 0.226(5) 0.914(5) 0.8387(17) 0.43(3) Uiso 1 1 d G U . . .
C61 C 0.163(6) 0.907(6) 0.8764(17) 0.43(3) Uiso 1 1 d G U . . .
C71 C 0.253(6) 0.751(7) 0.698(2) 0.43(3) Uiso 1 1 d G U . . .
C81 C 0.242(5) 0.844(5) 0.6870(17) 0.43(3) Uiso 1 1 d G U . . .
C91 C 0.122(7) 0.901(6) 0.7057(18) 0.43(3) Uiso 1 1 d G U . . .
H11 H 0.1739 0.6731 0.7524 0.43(3) Uiso 1 1 d G U . . .
H21 H 0.1326 0.9482 0.8718 0.43(3) Uiso 1 1 d G U . . .
H31 H 0.2564 0.7172 0.6721 0.43(3) Uiso 1 1 d G U . . .
H41 H 0.2755 0.9562 0.7566 0.43(3) Uiso 1 1 d G U . . .
H51 H 0.1120 0.8044 0.8027 0.43(3) Uiso 1 1 d G U . . .
H61 H 0.2781 0.9837 0.8346 0.43(3) Uiso 1 1 d G U . . .
H71 H 0.2589 0.8744 0.8441 0.43(3) Uiso 1 1 d G U . . .
H81 H 0.2049 0.9300 0.9013 0.43(3) Uiso 1 1 d G U . . .
H91 H 0.1103 0.8376 0.8805 0.43(3) Uiso 1 1 d G U . . .
H101 H 0.1288 0.9132 0.7938 0.43(3) Uiso 1 1 d G U . . .
H111 H 0.2663 0.8517 0.7677 0.43(3) Uiso 1 1 d G U . . .
H121 H 0.2147 0.8383 0.6587 0.43(3) Uiso 1 1 d G U . . .
H131 H 0.3071 0.9062 0.6889 0.43(3) Uiso 1 1 d G U . . .
H141 H 0.1710 0.9718 0.7073 0.43(3) Uiso 1 1 d G U . . .
H151 H 0.0652 0.8857 0.7235 0.43(3) Uiso 1 1 d G U . . .
H161 H 0.0996 0.8831 0.6768 0.43(3) Uiso 1 1 d G U . . .
H171 H 0.0542 0.7152 0.7489 0.43(3) Uiso 1 1 d G U . . .
H181 H 0.0487 0.7084 0.6988 0.43(3) Uiso 1 1 d G U . . .
H191 H 0.1199 0.6140 0.7104 0.43(3) Uiso 1 1 d G U . . .
H201 H 0.3133 0.7703 0.7146 0.43(3) Uiso 1 1 d G U . . .
N12 N -0.028(3) 0.286(4) 1.047(2) 0.78(7) Uiso 1 1 d G U . . .
C12 C 0.076(5) 0.217(3) 1.060(3) 0.78(7) Uiso 1 1 d G U . . .
C22 C -0.018(5) 0.212(4) 1.075(3) 0.78(7) Uiso 1 1 d G U . . .
C32 C 0.046(4) 0.396(4) 1.058(2) 0.78(7) Uiso 1 1 d G U . . .
C42 C 0.039(6) 0.427(6) 1.103(2) 0.78(7) Uiso 1 1 d G U . . .
C52 C 0.121(8) 0.534(6) 1.112(3) 0.78(7) Uiso 1 1 d G U . . .
C62 C 0.113(10) 0.567(8) 1.156(3) 0.78(7) Uiso 1 1 d G U . . .
C72 C 0.086(5) 0.245(4) 1.013(3) 0.78(7) Uiso 1 1 d G U . . .
C82 C -0.004(5) 0.263(4) 1.004(3) 0.78(7) Uiso 1 1 d G U . . .
C92 C -0.134(4) 0.269(7) 1.048(3) 0.78(7) Uiso 1 1 d G U . . .
H12 H 0.1341 0.2680 1.0759 0.78(7) Uiso 1 1 d G U . . .
H22 H 0.0494 0.5646 1.1591 0.78(7) Uiso 1 1 d G U . . .
H32 H 0.0806 0.1899 0.9951 0.78(7) Uiso 1 1 d G U . . .
H42 H 0.0351 0.4388 1.0388 0.78(7) Uiso 1 1 d G U . . .
H52 H 0.0454 0.3813 1.1226 0.78(7) Uiso 1 1 d G U . . .
H62 H 0.1153 0.5790 1.0914 0.78(7) Uiso 1 1 d G U . . .
H72 H 0.1866 0.5396 1.1080 0.78(7) Uiso 1 1 d G U . . .
H82 H 0.1676 0.6348 1.1605 0.78(7) Uiso 1 1 d G U . . .
H92 H 0.1176 0.5220 1.1760 0.78(7) Uiso 1 1 d G U . . .
H102 H -0.0269 0.4205 1.1071 0.78(7) Uiso 1 1 d G U . . .
H112 H 0.1142 0.4081 1.0535 0.78(7) Uiso 1 1 d G U . . .
H122 H -0.0614 0.2030 0.9921 0.78(7) Uiso 1 1 d G U . . .
H132 H 0.0157 0.3196 0.9849 0.78(7) Uiso 1 1 d G U . . .
H142 H -0.1366 0.3219 1.0326 0.78(7) Uiso 1 1 d G U . . .
H152 H -0.1552 0.2678 1.0768 0.78(7) Uiso 1 1 d G U . . .
H162 H -0.1792 0.2046 1.0347 0.78(7) Uiso 1 1 d G U . . .
H172 H -0.0133 0.2313 1.1047 0.78(7) Uiso 1 1 d G U . . .
H182 H -0.0762 0.1443 1.0715 0.78(7) Uiso 1 1 d G U . . .
H192 H 0.0724 0.1519 1.0639 0.78(7) Uiso 1 1 d G U . . .
H202 H 0.1499 0.3057 1.0068 0.78(7) Uiso 1 1 d G U . . .
N13 N 0.587(3) 1.066(3) 0.9177(17) 0.48(3) Uiso 1 1 d G U . . .
C13 C 0.474(4) 1.124(3) 0.9346(19) 0.48(3) Uiso 1 1 d G U . . .
C23 C 0.584(3) 1.158(3) 0.9322(18) 0.48(3) Uiso 1 1 d G U . . .
C33 C 0.556(3) 0.986(3) 0.9518(18) 0.48(3) Uiso 1 1 d G U . . .
C43 C 0.619(3) 1.019(3) 0.9913(18) 0.48(3) Uiso 1 1 d G U . . .
C53 C 0.578(4) 0.937(4) 1.025(2) 0.48(3) Uiso 1 1 d G U . . .
C63 C 0.642(4) 0.969(5) 1.064(2) 0.48(3) Uiso 1 1 d G U . . .
C73 C 0.423(4) 1.040(4) 0.9006(18) 0.48(3) Uiso 1 1 d G U . . .
C83 C 0.509(4) 1.026(3) 0.8827(17) 0.48(3) Uiso 1 1 d G U . . .
C93 C 0.689(4) 1.093(3) 0.9003(19) 0.48(3) Uiso 1 1 d G U . . .
H13 H 0.4480 1.0974 0.9626 0.48(3) Uiso 1 1 d G U . . .
H23 H 0.7095 0.9826 1.0569 0.48(3) Uiso 1 1 d G U . . .
H33 H 0.3932 1.0613 0.8783 0.48(3) Uiso 1 1 d G U . . .
H43 H 0.5591 0.9286 0.9398 0.48(3) Uiso 1 1 d G U . . .
H53 H 0.6204 1.0792 1.0026 0.48(3) Uiso 1 1 d G U . . .
H63 H 0.5757 0.8771 1.0129 0.48(3) Uiso 1 1 d G U . . .
H73 H 0.5099 0.9206 1.0319 0.48(3) Uiso 1 1 d G U . . .
H83 H 0.6129 0.9158 1.0845 0.48(3) Uiso 1 1 d G U . . .
H93 H 0.6461 1.0293 1.0753 0.48(3) Uiso 1 1 d G U . . .
H103 H 0.6884 1.0374 0.9844 0.48(3) Uiso 1 1 d G U . . .
H113 H 0.4860 0.9620 0.9595 0.48(3) Uiso 1 1 d G U . . .
H123 H 0.5368 1.0641 0.8567 0.48(3) Uiso 1 1 d G U . . .
H133 H 0.4862 0.9548 0.8772 0.48(3) Uiso 1 1 d G U . . .
H143 H 0.6906 1.0319 0.8943 0.48(3) Uiso 1 1 d G U . . .
H153 H 0.7401 1.1328 0.9209 0.48(3) Uiso 1 1 d G U . . .
H163 H 0.7010 1.1312 0.8746 0.48(3) Uiso 1 1 d G U . . .
H173 H 0.6160 1.1803 0.9599 0.48(3) Uiso 1 1 d G U . . .
H183 H 0.6183 1.2130 0.9121 0.48(3) Uiso 1 1 d G U . . .
H193 H 0.4629 1.1799 0.9287 0.48(3) Uiso 1 1 d G U . . .
H203 H 0.3701 0.9780 0.9131 0.48(3) Uiso 1 1 d G U . . .
 
 
_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
Pb Cl5 2.759(11) . ?
Pb Cl4 2.787(15) . ?
Pb Cl2 2.987(10) . ?
Pb Cl3 2.972(15) . ?
Pb Cl3 3.086(18) 3_665 ?
Cl2 Pb 2.987(10) 3_665 ?
Cl2 Pb 2.987(10) 2_655 ?
Cl3 Pb 3.086(18) 2_655 ?
Zn1 Cl8 2.113(13) . ?
Zn1 Cl72 2.33(2) 2_665 ?
Zn1 Cl72 2.33(2) . ?
Zn1 Cl72 2.33(2) 3_565 ?
Zn1 Cl71 2.36(3) 2_665 ?
Zn1 Cl71 2.36(3) 3_565 ?
Zn1 Cl71 2.36(3) . ?
Zn2 Cl9 2.119(14) . ?
Zn2 Cl6 2.30(3) . ?
Zn2 Cl6 2.30(3) 3_565 ?
Zn2 Cl6 2.30(3) 2_665 ?
Cl71 Cl72 0.56(4) . ?
Cl71 C92 2.1(5) 5_664 ?
N11 C21 1.4758 . ?
N11 C81 1.4824 . ?
N11 C91 1.4840 . ?
N11 C31 1.4945 . ?
C11 C21 1.4679 . ?
C11 C71 1.525(2) . ?
C11 H11 0.9576 . ?
C11 H191 0.9601 . ?
C21 H171 0.9585 . ?
C21 H181 0.9587 . ?
C31 C41 1.4807 . ?
C31 H41 0.9607 . ?
C31 H111 0.9605 . ?
C41 C51 1.4858 . ?
C41 H51 0.9607 . ?
C41 H101 0.9607 . ?
C51 C61 1.4785 . ?
C51 H61 0.9607 . ?
C51 H71 0.9606 . ?
C61 H21 0.9507 . ?
C61 H81 0.9485 . ?
C61 H91 0.9509 . ?
C71 C81 1.5311 . ?
C71 H31 0.9583 . ?
C71 H201 0.9596 . ?
C81 H121 0.9577 . ?
C81 H131 0.9606 . ?
C91 H141 0.9508 . ?
C91 H151 0.9497 . ?
C91 H161 0.9478 . ?
N12 C22 1.4726 . ?
N12 C82 1.4813 . ?
N12 C92 1.4847 . ?
N12 C32 1.4984(18) . ?
C12 C22 1.4666 . ?
C12 C72 1.5211 . ?
C12 H12 0.9597 . ?
C12 H192 0.9604 . ?
C22 H172 0.9588 . ?
C22 H182 0.9614 . ?
C32 C42 1.4799 . ?
C32 H42 0.9587 . ?
C32 H112 0.9606 . ?
C42 C52 1.489(3) . ?
C42 H52 0.9587 . ?
C42 H102 0.9608 . ?
C52 C62 1.4781 . ?
C52 H62 0.9585 . ?
C52 H72 0.9609 . ?
C62 H22 0.9508 . ?
C62 H82 0.9507 . ?
C62 H92 0.9489 . ?
C72 C82 1.5304 . ?
C72 H32 0.9601 . ?
C72 H202 0.9606 . ?
C82 H122 0.9602 . ?
C82 H132 0.9590 . ?
C92 Cl71 2.08(8) 5_565 ?
C92 H142 0.9494 . ?
C92 H152 0.9483 . ?
C92 H162 0.9504 . ?
N13 C23 1.4758 . ?
N13 C83 1.4826 . ?
N13 C93 1.4838 . ?
N13 C33 1.4945 . ?
C13 C23 1.4678 . ?
C13 C73 1.5252 . ?
C13 H13 0.9575 . ?
C13 H193 0.9603 . ?
C23 H173 0.9588 . ?
C23 H183 0.9583 . ?
C33 C43 1.4808 . ?
C33 H43 0.9606 . ?
C33 H113 0.9604 . ?
C43 C53 1.4855 . ?
C43 H53 0.9607 . ?
C43 H103 0.9606 . ?
C53 C63 1.4788 . ?
C53 H63 0.9607 . ?
C53 H73 0.9606 . ?
C63 H23 0.9507 . ?
C63 H83 0.9484 . ?
C63 H93 0.9506 . ?
C73 C83 1.5309 . ?
C73 H33 0.9584 . ?
C73 H203 0.9596 . ?
C83 H123 0.9577 . ?
C83 H133 0.9606 . ?
C93 H143 0.9508 . ?
C93 H153 0.9500 . ?
C93 H163 0.9479 . ?
 
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
Cl5 Pb Cl4 92.9(4) . . ?
Cl5 Pb Cl2 95.9(4) . . ?
Cl4 Pb Cl2 171.1(6) . . ?
Cl5 Pb Cl3 99.4(4) . . ?
Cl4 Pb Cl3 95.6(6) . . ?
Cl2 Pb Cl3 81.9(3) . . ?
Cl5 Pb Cl3 102.1(4) . 3_665 ?
Cl4 Pb Cl3 99.2(5) . 3_665 ?
Cl2 Pb Cl3 80.0(3) . 3_665 ?
Cl3 Pb Cl3 153.1(2) . 3_665 ?
Pb Cl2 Pb 87.9(4) 3_665 2_655 ?
Pb Cl2 Pb 87.9(4) 3_665 . ?
Pb Cl2 Pb 87.9(4) 2_655 . ?
Pb Cl3 Pb 86.33(19) . 2_655 ?
Cl8 Zn1 Cl72 109.2(8) . 2_665 ?
Cl8 Zn1 Cl72 109.2(9) . . ?
Cl72 Zn1 Cl72 109.7(8) 2_665 . ?
Cl8 Zn1 Cl72 109.2(9) . 3_565 ?
Cl72 Zn1 Cl72 109.7(8) 2_665 3_565 ?
Cl72 Zn1 Cl72 109.7(8) . 3_565 ?
Cl8 Zn1 Cl71 111.8(9) . 2_665 ?
Cl72 Zn1 Cl71 13.7(9) 2_665 2_665 ?
Cl72 Zn1 Cl71 96.6(11) . 2_665 ?
Cl72 Zn1 Cl71 119.4(11) 3_565 2_665 ?
Cl8 Zn1 Cl71 111.8(9) . 3_565 ?
Cl72 Zn1 Cl71 96.6(11) 2_665 3_565 ?
Cl72 Zn1 Cl71 119.4(11) . 3_565 ?
Cl72 Zn1 Cl71 13.7(9) 3_565 3_565 ?
Cl71 Zn1 Cl71 107.1(10) 2_665 3_565 ?
Cl8 Zn1 Cl71 111.8(9) . . ?
Cl72 Zn1 Cl71 119.4(11) 2_665 . ?
Cl72 Zn1 Cl71 13.7(9) . . ?
Cl72 Zn1 Cl71 96.6(11) 3_565 . ?
Cl71 Zn1 Cl71 107.1(10) 2_665 . ?
Cl71 Zn1 Cl71 107.1(10) 3_565 . ?
Cl9 Zn2 Cl6 118.6(8) . . ?
Cl9 Zn2 Cl6 118.6(8) . 3_565 ?
Cl6 Zn2 Cl6 98.9(10) . 3_565 ?
Cl9 Zn2 Cl6 118.6(8) . 2_665 ?
Cl6 Zn2 Cl6 98.9(10) . 2_665 ?
Cl6 Zn2 Cl6 98.9(10) 3_565 2_665 ?
Cl72 Cl71 C92 99(10) . 5_664 ?
Cl72 Cl71 Zn1 80(5) . . ?
C92 Cl71 Zn1 110(9) 5_664 . ?
Cl71 Cl72 Zn1 87(4) . . ?
C21 N11 C81 102.9 . . ?
C21 N11 C91 111.39(13) . . ?
C81 N11 C91 109.9 . . ?
C21 N11 C31 113.7 . . ?
C81 N11 C31 109.02(6) . . ?
C91 N11 C31 109.7 . . ?
C21 C11 C71 105.9 . . ?
C21 C11 H11 110.5 . . ?
C71 C11 H11 110.4 . . ?
C21 C11 H191 110.6 . . ?
C71 C11 H191 110.7 . . ?
H11 C11 H191 108.7 . . ?
C11 C21 N11 103.92(8) . . ?
C11 C21 H171 111.0 . . ?
N11 C21 H171 111.1 . . ?
C11 C21 H181 111.0 . . ?
N11 C21 H181 111.1 . . ?
H171 C21 H181 108.7 . . ?
C41 C31 N11 115.08(8) . . ?
C41 C31 H41 108.4 . . ?
N11 C31 H41 108.6 . . ?
C41 C31 H111 108.6 . . ?
N11 C31 H111 108.4 . . ?
H41 C31 H111 107.5 . . ?
C31 C41 C51 111.31(8) . . ?
C31 C41 H51 109.3 . . ?
C51 C41 H51 109.4 . . ?
C31 C41 H101 109.5 . . ?
C51 C41 H101 109.4 . . ?
H51 C41 H101 108.0 . . ?
C61 C51 C41 111.87(10) . . ?
C61 C51 H61 109.2 . . ?
C41 C51 H61 109.2 . . ?
C61 C51 H71 109.4 . . ?
C41 C51 H71 109.2 . . ?
H61 C51 H71 107.9 . . ?
C51 C61 H21 109.6 . . ?
C51 C61 H81 109.4 . . ?
H21 C61 H81 109.4 . . ?
C51 C61 H91 109.5 . . ?
H21 C61 H91 109.4 . . ?
H81 C61 H91 109.5 . . ?
C11 C71 C81 104.4 . . ?
C11 C71 H31 110.8 . . ?
C81 C71 H31 111.0 . . ?
C11 C71 H201 111.1 . . ?
C81 C71 H201 110.7 . . ?
H31 C71 H201 108.8 . . ?
N11 C81 C71 103.2 . . ?
N11 C81 H121 111.0 . . ?
C71 C81 H121 111.2 . . ?
N11 C81 H131 111.1 . . ?
C71 C81 H131 111.2 . . ?
H121 C81 H131 109.1 . . ?
N11 C91 H141 109.6 . . ?
N11 C91 H151 109.5 . . ?
H141 C91 H151 109.6 . . ?
N11 C91 H161 109.4 . . ?
H141 C91 H161 109.5 . . ?
H151 C91 H161 109.3 . . ?
C22 N12 C82 102.7 . . ?
C22 N12 C92 111.42(5) . . ?
C82 N12 C92 109.84(6) . . ?
C22 N12 C32 113.68(7) . . ?
C82 N12 C32 109.18(10) . . ?
C92 N12 C32 109.77(5) . . ?
C22 C12 C72 105.9 . . ?
C22 C12 H12 110.5 . . ?
C72 C12 H12 110.4 . . ?
C22 C12 H192 110.6 . . ?
C72 C12 H192 110.5 . . ?
H12 C12 H192 108.9 . . ?
C12 C22 N12 104.1 . . ?
C12 C22 H172 111.0 . . ?
N12 C22 H172 110.8 . . ?
C12 C22 H182 111.0 . . ?
N12 C22 H182 111.1 . . ?
H172 C22 H182 108.8 . . ?
C42 C32 N12 115.27(9) . . ?
C42 C32 H42 108.2 . . ?
N12 C32 H42 108.5 . . ?
C42 C32 H112 108.6 . . ?
N12 C32 H112 108.5 . . ?
H42 C32 H112 107.5 . . ?
C32 C42 C52 111.49(12) . . ?
C32 C42 H52 109.1 . . ?
C52 C42 H52 109.4 . . ?
C32 C42 H102 109.4 . . ?
C52 C42 H102 109.4 . . ?
H52 C42 H102 108.0 . . ?
C62 C52 C42 112.07(18) . . ?
C62 C52 H62 109.0 . . ?
C42 C52 H62 109.3 . . ?
C62 C52 H72 109.3 . . ?
C42 C52 H72 109.2 . . ?
H62 C52 H72 107.9 . . ?
C52 C62 H22 109.6 . . ?
C52 C62 H82 109.6 . . ?
H22 C62 H82 109.4 . . ?
C52 C62 H92 109.3 . . ?
H22 C62 H92 109.4 . . ?
H82 C62 H92 109.5 . . ?
C12 C72 C82 104.39(6) . . ?
C12 C72 H32 110.8 . . ?
C82 C72 H32 110.9 . . ?
C12 C72 H202 110.9 . . ?
C82 C72 H202 110.8 . . ?
H32 C72 H202 109.0 . . ?
N12 C82 C72 103.2 . . ?
N12 C82 H122 111.1 . . ?
C72 C82 H122 111.1 . . ?
N12 C82 H132 110.9 . . ?
C72 C82 H132 111.1 . . ?
H122 C82 H132 109.3 . . ?
N12 C92 Cl71 132(4) . 5_565 ?
N12 C92 H142 109.5 . . ?
Cl71 C92 H142 45.8 5_565 . ?
N12 C92 H152 109.5 . . ?
Cl71 C92 H152 117.0 5_565 . ?
H142 C92 H152 109.4 . . ?
N12 C92 H162 109.5 . . ?
Cl71 C92 H162 64.6 5_565 . ?
H142 C92 H162 109.6 . . ?
H152 C92 H162 109.4 . . ?
C23 N13 C83 102.9 . . ?
C23 N13 C93 111.39(5) . . ?
C83 N13 C93 109.9 . . ?
C23 N13 C33 113.7 . . ?
C83 N13 C33 109.03(11) . . ?
C93 N13 C33 109.7 . . ?
C23 C13 C73 105.9 . . ?
C23 C13 H13 110.5 . . ?
C73 C13 H13 110.4 . . ?
C23 C13 H193 110.6 . . ?
C73 C13 H193 110.6 . . ?
H13 C13 H193 108.7 . . ?
C13 C23 N13 103.91(7) . . ?
C13 C23 H173 111.0 . . ?
N13 C23 H173 111.1 . . ?
C13 C23 H183 111.0 . . ?
N13 C23 H183 111.1 . . ?
H173 C23 H183 108.7 . . ?
C43 C33 N13 115.09(12) . . ?
C43 C33 H43 108.4 . . ?
N13 C33 H43 108.6 . . ?
C43 C33 H113 108.7 . . ?
N13 C33 H113 108.4 . . ?
H43 C33 H113 107.5 . . ?
C33 C43 C53 111.31(15) . . ?
C33 C43 H53 109.3 . . ?
C53 C43 H53 109.4 . . ?
C33 C43 H103 109.5 . . ?
C53 C43 H103 109.3 . . ?
H53 C43 H103 108.0 . . ?
C63 C53 C43 111.88(16) . . ?
C63 C53 H63 109.2 . . ?
C43 C53 H63 109.2 . . ?
C63 C53 H73 109.3 . . ?
C43 C53 H73 109.2 . . ?
H63 C53 H73 107.9 . . ?
C53 C63 H23 109.6 . . ?
C53 C63 H83 109.4 . . ?
H23 C63 H83 109.4 . . ?
C53 C63 H93 109.5 . . ?
H23 C63 H93 109.4 . . ?
H83 C63 H93 109.5 . . ?
C13 C73 C83 104.44(7) . . ?
C13 C73 H33 110.8 . . ?
C83 C73 H33 111.0 . . ?
C13 C73 H203 111.0 . . ?
C83 C73 H203 110.7 . . ?
H33 C73 H203 108.8 . . ?
N13 C83 C73 103.2 . . ?
N13 C83 H123 111.0 . . ?
C73 C83 H123 111.1 . . ?
N13 C83 H133 111.1 . . ?
C73 C83 H133 111.2 . . ?
H123 C83 H133 109.1 . . ?
N13 C93 H143 109.6 . . ?
N13 C93 H153 109.5 . . ?
H143 C93 H153 109.6 . . ?
N13 C93 H163 109.4 . . ?
H143 C93 H163 109.5 . . ?
H153 C93 H163 109.3 . . ?
 
_refine_diff_density_max    1.692
_refine_diff_density_min   -0.926
_refine_diff_density_rms    0.212



