# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2b
_database_code_depnum_ccdc_archive 'CCDC 1530479'
_audit_update_record             
;
2017-01-31 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H49 N3 Sn'
_chemical_formula_weight         678.50

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   10.2651(16)
_cell_length_b                   22.732(3)
_cell_length_c                   15.116(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.724(6)
_cell_angle_gamma                90
_cell_volume                     3465.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    16085
_cell_measurement_theta_min      1.792
_cell_measurement_theta_max      27.444

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.767
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6636
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16085
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.792
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7845
_reflns_number_gt                6498
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_max     0.978
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0207P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2672 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7845
_refine_ls_number_parameters     403
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.0719
_refine_ls_wR_factor_gt          0.0672
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.977
_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_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
Sn1 Sn -0.89133(4) 1.05514(2) 0.06880(3) 0.01922(9) Uani 1 1 d . . . . .
N1 N -0.8349(4) 1.1295(2) 0.1484(3) 0.0199(11) Uani 1 1 d . . . . .
N2 N -1.0607(4) 1.07097(19) 0.1239(3) 0.0176(11) Uani 1 1 d . . . . .
N3 N -0.8971(5) 0.9644(2) 0.1677(3) 0.0210(11) Uani 1 1 d . . . . .
H3 H -0.825(6) 0.975(2) 0.211(4) 0.024(17) Uiso 1 1 d . . . . .
C1 C -0.9344(6) 1.1523(2) 0.1916(4) 0.0173(12) Uani 1 1 d . . . . .
C2 C -1.0527(5) 1.1226(2) 0.1796(3) 0.0111(11) Uani 1 1 d . . . . .
C3 C -1.1551(6) 1.1406(3) 0.2215(4) 0.0233(14) Uani 1 1 d . . . . .
H3A H -1.2354 1.1188 0.2142 0.028 Uiso 1 1 calc R U . . .
C4 C -1.1385(6) 1.1912(3) 0.2745(4) 0.0256(14) Uani 1 1 d . . . . .
H4A H -1.2079 1.2042 0.3035 0.031 Uiso 1 1 calc R U . . .
C5 C -1.0218(6) 1.2224(3) 0.2849(4) 0.0240(14) Uani 1 1 d . . . . .
H5A H -1.0117 1.2573 0.3202 0.029 Uiso 1 1 calc R U . . .
C6 C -0.9193(6) 1.2035(3) 0.2444(4) 0.0216(13) Uani 1 1 d . . . . .
H6A H -0.8388 1.2251 0.2523 0.026 Uiso 1 1 calc R U . . .
C7 C -0.7131(5) 1.1611(2) 0.1580(4) 0.0191(13) Uani 1 1 d . . . . .
C8 C -0.7051(6) 1.2107(2) 0.1030(4) 0.0222(13) Uani 1 1 d . . . . .
C9 C -0.5893(8) 1.2428(3) 0.1157(6) 0.028(2) Uani 1 1 d . . . . .
H9A H -0.5821 1.2755 0.0779 0.034 Uiso 1 1 calc R U . . .
C10 C -0.4827(6) 1.2278(3) 0.1833(5) 0.0316(16) Uani 1 1 d . . . . .
H10A H -0.4050 1.2514 0.1935 0.038 Uiso 1 1 calc R U . . .
C11 C -0.4906(6) 1.1784(3) 0.2354(4) 0.0266(15) Uani 1 1 d . . . . .
H11A H -0.4166 1.1681 0.2805 0.032 Uiso 1 1 calc R U . . .
C12 C -0.6037(6) 1.1435(2) 0.2238(4) 0.0208(13) Uani 1 1 d . . . . .
C13 C -0.6083(6) 1.0890(3) 0.2820(4) 0.0265(14) Uani 1 1 d . . . . .
H13A H -0.6694 1.0602 0.2454 0.032 Uiso 1 1 calc R U . . .
C14 C -0.6658(7) 1.1031(3) 0.3661(4) 0.0390(18) Uani 1 1 d . . . . .
H14A H -0.7536 1.1209 0.3482 0.059 Uiso 1 1 calc R U . . .
H14B H -0.6069 1.1306 0.4044 0.059 Uiso 1 1 calc R U . . .
H14C H -0.6734 1.0668 0.3996 0.059 Uiso 1 1 calc R U . . .
C15 C -0.4740(6) 1.0590(3) 0.3090(5) 0.0389(17) Uani 1 1 d . . . . .
H15A H -0.4376 1.0503 0.2549 0.058 Uiso 1 1 calc R U . . .
H15B H -0.4848 1.0223 0.3408 0.058 Uiso 1 1 calc R U . . .
H15C H -0.4132 1.0851 0.3485 0.058 Uiso 1 1 calc R U . . .
C16 C -0.8182(6) 1.2270(3) 0.0272(4) 0.0289(15) Uani 1 1 d . . . . .
H16A H -0.9001 1.2078 0.0406 0.035 Uiso 1 1 calc R U . . .
C17 C -0.7951(8) 1.2023(3) -0.0623(5) 0.048(2) Uani 1 1 d . . . . .
H17A H -0.7857 1.1595 -0.0578 0.072 Uiso 1 1 calc R U . . .
H17B H -0.7141 1.2195 -0.0769 0.072 Uiso 1 1 calc R U . . .
H17C H -0.8707 1.2122 -0.1098 0.072 Uiso 1 1 calc R U . . .
C18 C -0.8443(7) 1.2932(3) 0.0214(6) 0.056(2) Uani 1 1 d . . . . .
H18A H -0.8650 1.3072 0.0785 0.084 Uiso 1 1 calc R U . . .
H18B H -0.9194 1.3013 -0.0274 0.084 Uiso 1 1 calc R U . . .
H18C H -0.7653 1.3136 0.0093 0.084 Uiso 1 1 calc R U . . .
C19 C -1.1675(6) 1.0300(2) 0.1186(4) 0.0187(13) Uani 1 1 d . . . . .
C20 C -1.1443(6) 0.9752(2) 0.1641(4) 0.0229(13) Uani 1 1 d . . . . .
C21 C -1.2519(7) 0.9365(3) 0.1577(4) 0.0323(16) Uani 1 1 d . . . . .
H21A H -1.2395 0.8998 0.1881 0.039 Uiso 1 1 calc R U . . .
C22 C -1.3746(7) 0.9501(3) 0.1087(4) 0.0366(17) Uani 1 1 d . . . . .
H22A H -1.4462 0.9233 0.1065 0.044 Uiso 1 1 calc R U . . .
C23 C -1.3934(12) 1.0023(2) 0.0632(8) 0.0322(15) Uani 1 1 d . . . . .
H23A H -1.4780 1.0110 0.0281 0.039 Uiso 1 1 calc R U . . .
C24 C -1.2912(6) 1.0431(2) 0.0671(4) 0.0231(14) Uani 1 1 d . . . . .
C25 C -1.3126(6) 1.0999(3) 0.0102(4) 0.0253(14) Uani 1 1 d . . . . .
H25A H -1.2550 1.1311 0.0436 0.030 Uiso 1 1 calc R U . . .
C26 C -1.2685(7) 1.0905(3) -0.0798(4) 0.0381(17) Uani 1 1 d . . . . .
H26A H -1.2756 1.1276 -0.1132 0.057 Uiso 1 1 calc R U . . .
H26B H -1.3252 1.0608 -0.1149 0.057 Uiso 1 1 calc R U . . .
H26C H -1.1762 1.0769 -0.0690 0.057 Uiso 1 1 calc R U . . .
C27 C -1.4551(6) 1.1220(3) -0.0053(5) 0.0370(17) Uani 1 1 d . . . . .
H27A H -1.4599 1.1607 -0.0342 0.055 Uiso 1 1 calc R U . . .
H27B H -1.4845 1.1252 0.0526 0.055 Uiso 1 1 calc R U . . .
H27C H -1.5125 1.0944 -0.0443 0.055 Uiso 1 1 calc R U . . .
C28 C -1.0106(6) 0.9582(2) 0.2206(4) 0.0237(14) Uani 1 1 d . . . . .
C29 C -1.0085(7) 0.8952(3) 0.2580(4) 0.0353(17) Uani 1 1 d . . . . .
H29A H -1.0374 0.8676 0.2085 0.053 Uiso 1 1 calc R U . . .
H29B H -1.0686 0.8926 0.3012 0.053 Uiso 1 1 calc R U . . .
H29C H -0.9183 0.8852 0.2882 0.053 Uiso 1 1 calc R U . . .
C30 C -0.9758(7) 0.9998(3) 0.3021(4) 0.0325(16) Uani 1 1 d . . . . .
H30A H -1.0495 1.0008 0.3350 0.049 Uiso 1 1 calc R U . . .
H30B H -0.9600 1.0395 0.2811 0.049 Uiso 1 1 calc R U . . .
H30C H -0.8957 0.9856 0.3421 0.049 Uiso 1 1 calc R U . . .
C31 C -0.8510(7) 0.9121(3) 0.1258(4) 0.0219(14) Uani 1 1 d . . . . .
C32 C -0.9227(6) 0.8894(3) 0.0457(4) 0.0214(15) Uani 1 1 d . . . . .
C33 C -0.8753(6) 0.8398(3) 0.0078(4) 0.0266(14) Uani 1 1 d . . . . .
H33A H -0.9243 0.8243 -0.0468 0.032 Uiso 1 1 calc R U . . .
C34 C -0.7580(7) 0.8122(3) 0.0478(4) 0.0302(16) Uani 1 1 d . . . . .
C35 C -0.6866(6) 0.8366(3) 0.1259(5) 0.0322(16) Uani 1 1 d . . . . .
H35A H -0.6051 0.8189 0.1530 0.039 Uiso 1 1 calc R U . . .
C36 C -0.7297(7) 0.8862(3) 0.1661(4) 0.0273(16) Uani 1 1 d . . . . .
C37 C -0.6453(7) 0.9105(3) 0.2507(5) 0.0405(18) Uani 1 1 d . . . . .
H37A H -0.5692 0.8846 0.2702 0.061 Uiso 1 1 calc R U . . .
H37B H -0.6982 0.9130 0.2983 0.061 Uiso 1 1 calc R U . . .
H37C H -0.6138 0.9499 0.2385 0.061 Uiso 1 1 calc R U . . .
C38 C -1.0533(6) 0.9144(3) -0.0042(4) 0.0237(15) Uani 1 1 d . . . . .
H38A H -1.0494 0.9575 -0.0027 0.036 Uiso 1 1 calc R U . . .
H38B H -1.1257 0.9010 0.0248 0.036 Uiso 1 1 calc R U . . .
H38C H -1.0690 0.9010 -0.0669 0.036 Uiso 1 1 calc R U . . .
C39 C -0.7112(10) 0.7573(4) 0.0061(6) 0.044(3) Uani 1 1 d . . . . .
H39A H -0.6456 0.7368 0.0510 0.066 Uiso 1 1 calc R U . . .
H39B H -0.6707 0.7683 -0.0453 0.066 Uiso 1 1 calc R U . . .
H39C H -0.7869 0.7313 -0.0143 0.066 Uiso 1 1 calc R 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
Sn1 N1 2.093(5) . ?
Sn1 N2 2.094(5) . ?
Sn1 N3 2.555(5) . ?
N1 C1 1.409(7) . ?
N1 C7 1.426(7) . ?
N2 C19 1.430(7) . ?
N2 C2 1.438(6) . ?
N3 C31 1.465(8) . ?
N3 C28 1.537(7) . ?
C1 C2 1.371(7) . ?
C1 C6 1.405(8) . ?
C2 C3 1.387(7) . ?
C3 C4 1.394(8) . ?
C4 C5 1.376(8) . ?
C5 C6 1.380(8) . ?
C7 C12 1.413(8) . ?
C7 C8 1.414(8) . ?
C8 C9 1.377(9) . ?
C8 C16 1.517(8) . ?
C9 C10 1.393(10) . ?
C10 C11 1.383(8) . ?
C11 C12 1.391(8) . ?
C12 C13 1.524(8) . ?
C13 C15 1.525(8) . ?
C13 C14 1.532(8) . ?
C16 C17 1.523(9) . ?
C16 C18 1.529(8) . ?
C19 C24 1.393(8) . ?
C19 C20 1.422(8) . ?
C20 C21 1.399(8) . ?
C20 C28 1.526(8) . ?
C21 C22 1.372(9) . ?
C22 C23 1.368(10) . ?
C23 C24 1.393(11) . ?
C24 C25 1.544(8) . ?
C25 C27 1.523(8) . ?
C25 C26 1.527(8) . ?
C28 C29 1.538(8) . ?
C28 C30 1.542(8) . ?
C31 C32 1.394(8) . ?
C31 C36 1.411(9) . ?
C32 C33 1.393(8) . ?
C32 C38 1.522(8) . ?
C33 C34 1.392(9) . ?
C34 C35 1.385(9) . ?
C34 C39 1.515(10) . ?
C35 C36 1.391(9) . ?
C36 C37 1.509(9) . ?

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
N1 Sn1 N2 78.11(18) . . ?
N1 Sn1 N3 110.49(17) . . ?
N2 Sn1 N3 78.15(17) . . ?
C1 N1 C7 117.7(4) . . ?
C1 N1 Sn1 114.6(3) . . ?
C7 N1 Sn1 127.5(4) . . ?
C19 N2 C2 121.6(4) . . ?
C19 N2 Sn1 123.4(3) . . ?
C2 N2 Sn1 114.3(3) . . ?
C31 N3 C28 119.1(5) . . ?
C31 N3 Sn1 110.9(3) . . ?
C28 N3 Sn1 118.8(3) . . ?
C2 C1 C6 119.0(5) . . ?
C2 C1 N1 117.3(5) . . ?
C6 C1 N1 123.8(5) . . ?
C1 C2 C3 121.5(5) . . ?
C1 C2 N2 115.6(5) . . ?
C3 C2 N2 122.9(5) . . ?
C2 C3 C4 118.9(5) . . ?
C5 C4 C3 120.1(6) . . ?
C4 C5 C6 120.5(5) . . ?
C5 C6 C1 119.9(6) . . ?
C12 C7 C8 121.0(5) . . ?
C12 C7 N1 119.8(5) . . ?
C8 C7 N1 119.2(5) . . ?
C9 C8 C7 118.9(6) . . ?
C9 C8 C16 119.8(6) . . ?
C7 C8 C16 121.2(5) . . ?
C8 C9 C10 120.9(7) . . ?
C11 C10 C9 119.7(6) . . ?
C10 C11 C12 121.8(6) . . ?
C11 C12 C7 117.6(5) . . ?
C11 C12 C13 120.4(5) . . ?
C7 C12 C13 122.0(5) . . ?
C12 C13 C15 113.2(5) . . ?
C12 C13 C14 111.5(5) . . ?
C15 C13 C14 109.9(5) . . ?
C8 C16 C17 110.9(6) . . ?
C8 C16 C18 112.6(5) . . ?
C17 C16 C18 111.4(6) . . ?
C24 C19 C20 120.7(5) . . ?
C24 C19 N2 120.1(5) . . ?
C20 C19 N2 119.1(5) . . ?
C21 C20 C19 117.2(6) . . ?
C21 C20 C28 119.7(5) . . ?
C19 C20 C28 123.0(5) . . ?
C22 C21 C20 122.0(6) . . ?
C23 C22 C21 119.7(7) . . ?
C22 C23 C24 121.5(10) . . ?
C19 C24 C23 118.8(7) . . ?
C19 C24 C25 120.7(5) . . ?
C23 C24 C25 120.3(7) . . ?
C27 C25 C26 110.2(5) . . ?
C27 C25 C24 113.3(5) . . ?
C26 C25 C24 110.2(5) . . ?
C20 C28 N3 112.1(5) . . ?
C20 C28 C29 113.0(5) . . ?
N3 C28 C29 108.5(5) . . ?
C20 C28 C30 110.0(5) . . ?
N3 C28 C30 105.9(5) . . ?
C29 C28 C30 107.0(5) . . ?
C32 C31 C36 120.1(6) . . ?
C32 C31 N3 121.0(6) . . ?
C36 C31 N3 118.9(6) . . ?
C33 C32 C31 119.3(5) . . ?
C33 C32 C38 116.3(5) . . ?
C31 C32 C38 124.4(6) . . ?
C34 C33 C32 121.8(6) . . ?
C35 C34 C33 117.8(6) . . ?
C35 C34 C39 121.8(7) . . ?
C33 C34 C39 120.4(7) . . ?
C34 C35 C36 122.5(6) . . ?
C35 C36 C31 118.5(6) . . ?
C35 C36 C37 119.2(6) . . ?
C31 C36 C37 122.3(6) . . ?

_refine_diff_density_max         0.794
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.082

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1530482'
_audit_update_record             
;
2017-01-31 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H38 F3 N2 O3 S Sn'
_chemical_formula_weight         694.38

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-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                   30.2756(12)
_cell_length_b                   11.6808(5)
_cell_length_c                   17.9498(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.9769(18)
_cell_angle_gamma                90
_cell_volume                     6323.9(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    28694
_cell_measurement_theta_min      1.870
_cell_measurement_theta_max      27.688

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_F_000             2840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.925
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28694
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.870
_diffrn_reflns_theta_max         27.688
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7288
_reflns_number_gt                5709
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0199P)²+7.3197P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7288
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0697
_refine_ls_wR_factor_gt          0.0634
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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_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
Sn1 Sn 0.11138(2) 0.42548(2) 0.06314(2) 0.02098(6) Uani 1 1 d . . . . .
O1 O 0.13453(6) 0.24505(15) 0.07132(9) 0.0306(4) Uani 1 1 d . . . . .
O2 O 0.17729(8) 0.10292(19) 0.14488(12) 0.0501(6) Uani 1 1 d . . . . .
O3 O 0.15101(8) 0.2787(2) 0.20266(11) 0.0571(7) Uani 1 1 d . . . . .
N1 N 0.10351(7) 0.40097(17) -0.05670(10) 0.0214(5) Uani 1 1 d . . . . .
N2 N 0.17345(7) 0.48306(17) 0.02551(10) 0.0184(4) Uani 1 1 d . . . . .
C1 C 0.13843(8) 0.4316(2) -0.09342(12) 0.0202(5) Uani 1 1 d . . . . .
C2 C 0.17689(8) 0.4754(2) -0.04848(12) 0.0186(5) Uani 1 1 d . . . . .
C3 C 0.21413(9) 0.5121(2) -0.08515(13) 0.0244(6) Uani 1 1 d . . . . .
H3B H 0.239359 0.542590 -0.056757 0.029 Uiso 1 1 calc R U . . .
C4 C 0.21381(9) 0.5037(2) -0.16109(13) 0.0269(6) Uani 1 1 d . . . . .
H4A H 0.239314 0.525869 -0.184860 0.032 Uiso 1 1 calc R U . . .
C5 C 0.17599(9) 0.4624(2) -0.20488(13) 0.0274(6) Uani 1 1 d . . . . .
H5A H 0.176315 0.458469 -0.257691 0.033 Uiso 1 1 calc R U . . .
C6 C 0.13946(8) 0.4285(2) -0.17271(12) 0.0255(6) Uani 1 1 d . . . . .
H6A H 0.114233 0.402400 -0.203135 0.031 Uiso 1 1 calc R U . . .
C7 C 0.06029(8) 0.3894(2) -0.09729(12) 0.0244(6) Uani 1 1 d . . . . .
C8 C 0.04259(9) 0.2805(3) -0.11292(13) 0.0291(6) Uani 1 1 d . . . . .
C9 C -0.00011(10) 0.2744(3) -0.14924(14) 0.0368(7) Uani 1 1 d . . . . .
H9A H -0.013142 0.201729 -0.160285 0.044 Uiso 1 1 calc R U . . .
C10 C -0.02356(10) 0.3724(3) -0.16924(15) 0.0410(8) Uani 1 1 d . . . . .
H10A H -0.052463 0.366421 -0.194147 0.049 Uiso 1 1 calc R U . . .
C11 C -0.00555(9) 0.4788(3) -0.15352(14) 0.0356(7) Uani 1 1 d . . . . .
H11A H -0.022222 0.545453 -0.167491 0.043 Uiso 1 1 calc R U . . .
C12 C 0.03683(9) 0.4898(3) -0.11737(13) 0.0283(6) Uani 1 1 d . . . . .
C13 C 0.05516(10) 0.6088(2) -0.09928(14) 0.0312(6) Uani 1 1 d . . . . .
H13A H 0.085907 0.599271 -0.074883 0.037 Uiso 1 1 calc R U . . .
C14 C 0.02791(11) 0.6704(3) -0.04362(16) 0.0467(8) Uani 1 1 d . . . . .
H14A H 0.040423 0.746589 -0.032983 0.070 Uiso 1 1 calc R U . . .
H14B H -0.002839 0.677838 -0.065057 0.070 Uiso 1 1 calc R U . . .
H14C H 0.028697 0.626074 0.002852 0.070 Uiso 1 1 calc R U . . .
C15 C 0.05832(12) 0.6813(3) -0.16973(17) 0.0507(9) Uani 1 1 d . . . . .
H15A H 0.070237 0.756980 -0.155609 0.076 Uiso 1 1 calc R U . . .
H15B H 0.077988 0.643452 -0.202654 0.076 Uiso 1 1 calc R U . . .
H15C H 0.028745 0.689800 -0.195984 0.076 Uiso 1 1 calc R U . . .
C16 C 0.06839(11) 0.1721(3) -0.09418(17) 0.0374(7) Uani 1 1 d . . . . .
C17 C 0.0418(7) 0.0739(18) -0.0664(12) 0.072(4) Uani 0.661(11) 1 d . . P A 1
H17A H 0.061325 0.007797 -0.055841 0.108 Uiso 0.661(11) 1 calc R U P A 1
H17B H 0.028764 0.096877 -0.020668 0.108 Uiso 0.661(11) 1 calc R U P A 1
H17C H 0.018175 0.053160 -0.104818 0.108 Uiso 0.661(11) 1 calc R U P A 1
C18 C 0.0903(6) 0.1372(9) -0.1632(10) 0.052(2) Uani 0.661(11) 1 d . . P A 1
H18A H 0.107396 0.201744 -0.180507 0.078 Uiso 0.661(11) 1 calc R U P A 1
H18B H 0.110207 0.072322 -0.151229 0.078 Uiso 0.661(11) 1 calc R U P A 1
H18C H 0.067552 0.114836 -0.202705 0.078 Uiso 0.661(11) 1 calc R U P A 1
C17A C 0.0398(17) 0.091(4) -0.048(2) 0.064(7) Uani 0.339(11) 1 d . . P A 2
H17D H 0.056334 0.019972 -0.035582 0.097 Uiso 0.339(11) 1 calc R U P A 2
H17E H 0.033077 0.128949 -0.001670 0.097 Uiso 0.339(11) 1 calc R U P A 2
H17F H 0.012009 0.071779 -0.077632 0.097 Uiso 0.339(11) 1 calc R U P A 2
C18A C 0.0848(13) 0.1032(19) -0.161(2) 0.052(2) Uani 0.339(11) 1 d . . P A 2
H18D H 0.100980 0.035063 -0.142079 0.078 Uiso 0.339(11) 1 calc R U P A 2
H18E H 0.059221 0.079727 -0.194883 0.078 Uiso 0.339(11) 1 calc R U P A 2
H18F H 0.104431 0.151438 -0.188265 0.078 Uiso 0.339(11) 1 calc R U P A 2
C19 C 0.20538(8) 0.5490(2) 0.07259(12) 0.0199(5) Uani 1 1 d . . . . .
C20 C 0.24414(8) 0.4974(2) 0.10488(12) 0.0218(5) Uani 1 1 d . . . . .
C21 C 0.27349(9) 0.5651(2) 0.14999(13) 0.0284(6) Uani 1 1 d . . . . .
H21A H 0.300167 0.532082 0.172090 0.034 Uiso 1 1 calc R U . . .
C22 C 0.26466(9) 0.6787(2) 0.16325(14) 0.0307(6) Uani 1 1 d . . . . .
H22A H 0.285341 0.723815 0.193339 0.037 Uiso 1 1 calc R U . . .
C23 C 0.22568(9) 0.7263(2) 0.13255(14) 0.0300(6) Uani 1 1 d . . . . .
H23A H 0.219459 0.804031 0.143110 0.036 Uiso 1 1 calc R U . . .
C24 C 0.19521(9) 0.6644(2) 0.08673(13) 0.0240(6) Uani 1 1 d . . . . .
C25 C 0.15281(10) 0.7216(2) 0.05472(15) 0.0306(6) Uani 1 1 d . . . . .
C26 C 0.1299(10) 0.786(2) 0.115(2) 0.054(3) Uani 0.661(11) 1 d . . P A 1
H26A H 0.126168 0.734769 0.157566 0.080 Uiso 0.661(11) 1 calc R U P A 1
H26B H 0.148082 0.851946 0.132873 0.080 Uiso 0.661(11) 1 calc R U P A 1
H26C H 0.100724 0.813276 0.094590 0.080 Uiso 0.661(11) 1 calc R U P A 1
C27 C 0.1598(4) 0.7940(10) -0.0120(7) 0.057(3) Uani 0.661(11) 1 d . . P A 1
H27A H 0.131660 0.829223 -0.030780 0.085 Uiso 0.661(11) 1 calc R U P A 1
H27B H 0.181528 0.854035 0.002334 0.085 Uiso 0.661(11) 1 calc R U P A 1
H27C H 0.170878 0.746137 -0.051171 0.085 Uiso 0.661(11) 1 calc R U P A 1
C26A C 0.125(2) 0.763(5) 0.112(4) 0.054(3) Uani 0.339(11) 1 d . . P A 2
H26D H 0.098053 0.799177 0.087982 0.080 Uiso 0.339(11) 1 calc R U P A 2
H26E H 0.116376 0.698743 0.142906 0.080 Uiso 0.339(11) 1 calc R U P A 2
H26F H 0.141370 0.819534 0.144074 0.080 Uiso 0.339(11) 1 calc R U P A 2
C27A C 0.1652(10) 0.830(2) 0.0058(16) 0.057(3) Uani 0.339(11) 1 d . . P A 2
H27D H 0.183913 0.804835 -0.033072 0.085 Uiso 0.339(11) 1 calc R U P A 2
H27E H 0.138025 0.864565 -0.017598 0.085 Uiso 0.339(11) 1 calc R U P A 2
H27F H 0.181376 0.886115 0.038202 0.085 Uiso 0.339(11) 1 calc R U P A 2
C28 C 0.25482(9) 0.3723(2) 0.09352(14) 0.0272(6) Uani 1 1 d . . . . .
H28A H 0.228369 0.335728 0.065958 0.033 Uiso 1 1 calc R U . . .
C29 C 0.29420(10) 0.3567(3) 0.04689(15) 0.0399(7) Uani 1 1 d . . . . .
H29A H 0.300007 0.274845 0.040865 0.060 Uiso 1 1 calc R U . . .
H29B H 0.287446 0.391758 -0.002385 0.060 Uiso 1 1 calc R U . . .
H29C H 0.320442 0.393512 0.072254 0.060 Uiso 1 1 calc R U . . .
C30 C 0.26352(11) 0.3115(3) 0.16886(16) 0.0418(8) Uani 1 1 d . . . . .
H30A H 0.270364 0.230787 0.160475 0.063 Uiso 1 1 calc R U . . .
H30B H 0.288652 0.347867 0.197787 0.063 Uiso 1 1 calc R U . . .
H30C H 0.237099 0.316964 0.196590 0.063 Uiso 1 1 calc R U . . .
S1 S 0.14564(3) 0.19277(6) 0.14574(4) 0.03371(17) Uani 1 1 d . . . . .
C31 C 0.09408(14) 0.1226(4) 0.1628(2) 0.0634(11) Uani 1 1 d . . . . .
F1 F 0.0576(4) 0.198(2) 0.1559(14) 0.067(2) Uani 0.661(11) 1 d . . P A 1
F2 F 0.0825(3) 0.0451(6) 0.1229(5) 0.0761(17) Uani 0.661(11) 1 d . . P A 1
F3 F 0.0985(3) 0.0898(7) 0.2395(4) 0.091(2) Uani 0.661(11) 1 d . . P A 1
F1A F 0.0672(9) 0.196(4) 0.166(3) 0.067(2) Uani 0.339(11) 1 d . . P A 2
F2A F 0.0883(6) 0.0314(13) 0.0946(11) 0.0761(17) Uani 0.339(11) 1 d . . P A 2
F3A F 0.0947(7) 0.0529(13) 0.2107(8) 0.091(2) Uani 0.339(11) 1 d . . P A 2
H25A H 0.1335(10) 0.668(2) 0.0314(15) 0.036(8) Uiso 1 1 d . . . . .
H16A H 0.0908(10) 0.189(2) -0.0604(15) 0.034(8) Uiso 1 1 d . . . . .


_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 2.159(2) . ?
Sn1 N1 2.1625(18) . ?
Sn1 O1 2.2219(18) . ?
O1 S1 1.4807(18) . ?
O2 S1 1.422(2) . ?
O3 S1 1.431(2) . ?
N1 C1 1.342(3) . ?
N1 C7 1.448(3) . ?
N2 C2 1.344(3) . ?
N2 C19 1.449(3) . ?
C1 C6 1.427(3) . ?
C1 C2 1.451(3) . ?
C2 C3 1.420(3) . ?
C3 C4 1.366(3) . ?
C4 C5 1.416(4) . ?
C5 C6 1.350(4) . ?
C7 C8 1.399(4) . ?
C7 C12 1.402(4) . ?
C8 C9 1.398(4) . ?
C8 C16 1.511(4) . ?
C9 C10 1.377(4) . ?
C10 C11 1.377(5) . ?
C11 C12 1.392(4) . ?
C12 C13 1.521(4) . ?
C13 C14 1.529(4) . ?
C13 C15 1.532(4) . ?
C16 C17 1.51(2) . ?
C16 C18 1.512(17) . ?
C16 C18A 1.56(3) . ?
C16 C17A 1.57(5) . ?
C19 C20 1.399(3) . ?
C19 C24 1.411(3) . ?
C20 C21 1.395(3) . ?
C20 C28 1.514(4) . ?
C21 C22 1.379(4) . ?
C22 C23 1.376(4) . ?
C23 C24 1.385(3) . ?
C24 C25 1.516(4) . ?
C25 C26A 1.47(7) . ?
C25 C27 1.496(14) . ?
C25 C26 1.54(3) . ?
C25 C27A 1.60(3) . ?
C28 C29 1.526(4) . ?
C28 C30 1.530(4) . ?
S1 C31 1.813(4) . ?
C31 F3A 1.182(13) . ?
C31 F2 1.188(9) . ?
C31 F1A 1.19(4) . ?
C31 F1 1.409(17) . ?
C31 F3 1.423(8) . ?
C31 F2A 1.621(15) . ?

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 N1 75.75(7) . . ?
N2 Sn1 O1 92.18(7) . . ?
N1 Sn1 O1 86.97(7) . . ?
S1 O1 Sn1 119.77(10) . . ?
C1 N1 C7 119.59(19) . . ?
C1 N1 Sn1 115.46(15) . . ?
C7 N1 Sn1 121.98(15) . . ?
C2 N2 C19 120.4(2) . . ?
C2 N2 Sn1 115.62(15) . . ?
C19 N2 Sn1 122.54(14) . . ?
N1 C1 C6 124.7(2) . . ?
N1 C1 C2 116.69(19) . . ?
C6 C1 C2 118.5(2) . . ?
N2 C2 C3 124.8(2) . . ?
N2 C2 C1 116.5(2) . . ?
C3 C2 C1 118.7(2) . . ?
C4 C3 C2 120.2(2) . . ?
C3 C4 C5 120.9(2) . . ?
C6 C5 C4 121.0(2) . . ?
C5 C6 C1 120.6(2) . . ?
C8 C7 C12 122.2(2) . . ?
C8 C7 N1 120.0(2) . . ?
C12 C7 N1 117.8(2) . . ?
C9 C8 C7 117.5(3) . . ?
C9 C8 C16 120.0(3) . . ?
C7 C8 C16 122.4(2) . . ?
C10 C9 C8 120.9(3) . . ?
C11 C10 C9 120.7(3) . . ?
C10 C11 C12 120.8(3) . . ?
C11 C12 C7 117.9(3) . . ?
C11 C12 C13 119.2(3) . . ?
C7 C12 C13 122.8(2) . . ?
C12 C13 C14 111.2(2) . . ?
C12 C13 C15 112.1(2) . . ?
C14 C13 C15 110.8(3) . . ?
C17 C16 C8 115.5(9) . . ?
C17 C16 C18 110.5(7) . . ?
C8 C16 C18 107.4(6) . . ?
C8 C16 C18A 117.0(13) . . ?
C8 C16 C17A 109.1(17) . . ?
C18A C16 C17A 108.7(14) . . ?
C20 C19 C24 121.7(2) . . ?
C20 C19 N2 120.4(2) . . ?
C24 C19 N2 117.9(2) . . ?
C21 C20 C19 117.8(2) . . ?
C21 C20 C28 119.5(2) . . ?
C19 C20 C28 122.7(2) . . ?
C22 C21 C20 121.5(3) . . ?
C23 C22 C21 119.5(2) . . ?
C22 C23 C24 122.1(3) . . ?
C23 C24 C19 117.5(2) . . ?
C23 C24 C25 119.6(2) . . ?
C19 C24 C25 123.0(2) . . ?
C26A C25 C24 114(3) . . ?
C27 C25 C24 112.2(6) . . ?
C27 C25 C26 113.2(14) . . ?
C24 C25 C26 111.5(13) . . ?
C26A C25 C27A 107(3) . . ?
C24 C25 C27A 108.9(11) . . ?
C20 C28 C29 112.0(2) . . ?
C20 C28 C30 110.6(2) . . ?
C29 C28 C30 110.3(2) . . ?
O2 S1 O3 119.36(14) . . ?
O2 S1 O1 113.28(12) . . ?
O3 S1 O1 110.96(13) . . ?
O2 S1 C31 105.00(17) . . ?
O3 S1 C31 104.03(19) . . ?
O1 S1 C31 101.98(16) . . ?
F3A C31 F1A 116(3) . . ?
F2 C31 F1 103.5(11) . . ?
F2 C31 F3 112.1(6) . . ?
F1 C31 F3 105.1(11) . . ?
F3A C31 F2A 95.2(9) . . ?
F1A C31 F2A 119(2) . . ?
F3A C31 S1 118.3(11) . . ?
F2 C31 S1 117.2(4) . . ?
F1A C31 S1 106(2) . . ?
F1 C31 S1 112.5(9) . . ?
F3 C31 S1 106.0(5) . . ?
F2A C31 S1 102.0(6) . . ?

_refine_diff_density_max         0.364
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.076

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1a
_database_code_depnum_ccdc_archive 'CCDC 1530480'
_audit_update_record             
;
2017-01-31 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H38 N2 Pb'
_chemical_formula_weight         633.81

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   10.9016(7)
_cell_length_b                   21.6336(17)
_cell_length_c                   11.6083(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2737.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    24612
_cell_measurement_theta_min      1.883
_cell_measurement_theta_max      29.353

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_F_000             1256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    6.181
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6198
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24612
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.883
_diffrn_reflns_theta_max         29.353
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3219
_reflns_number_gt                2615
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0287P)²+3.0234P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3219
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0614
_refine_ls_wR_factor_gt          0.0571
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.002
_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_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
Pb1 Pb 0.23208(2) 0.2500 0.67729(2) 0.01858(7) Uani 1 2 d S T P . .
N1 N 0.0893(2) 0.31182(14) 0.6267(3) 0.0136(6) Uani 1 1 d . . . . .
C1 C -0.0127(3) 0.28285(16) 0.5946(3) 0.0133(7) Uani 1 1 d . . . . .
C2 C -0.1130(3) 0.31414(18) 0.5586(3) 0.0204(8) Uani 1 1 d . . . . .
H2A H -0.1142 0.3580 0.5578 0.024 Uiso 1 1 calc R U . . .
C3 C -0.2106(3) 0.28149(18) 0.5243(4) 0.0239(9) Uani 1 1 d . . . . .
H3A H -0.2819 0.3028 0.4992 0.029 Uiso 1 1 calc R U . . .
C4 C 0.1031(3) 0.37642(16) 0.6034(3) 0.0136(7) Uani 1 1 d . . . . .
C5 C 0.0794(3) 0.41968(17) 0.6961(3) 0.0175(8) Uani 1 1 d . . . . .
C6 C 0.1010(3) 0.48171(18) 0.6716(4) 0.0223(8) Uani 1 1 d . . . . .
H6A H 0.0881 0.5118 0.7300 0.027 Uiso 1 1 calc R U . . .
C7 C 0.1424(3) 0.50104(18) 0.5595(3) 0.0262(10) Uani 1 1 d . . . . .
H7A H 0.1575 0.5437 0.5460 0.031 Uiso 1 1 calc R U . . .
C8 C 0.1613(3) 0.45806(18) 0.4683(4) 0.0233(9) Uani 1 1 d . . . . .
H8A H 0.1867 0.4722 0.3946 0.028 Uiso 1 1 calc R U . . .
C9 C 0.1424(3) 0.39559(18) 0.4873(3) 0.0169(8) Uani 1 1 d . . . . .
C10 C 0.1631(3) 0.3498(2) 0.3838(3) 0.0232(9) Uani 1 1 d . . . . .
H10A H 0.1304 0.3086 0.4076 0.028 Uiso 0.68(4) 1 calc R U P A 1
H10B H 0.1617 0.3068 0.4155 0.028 Uiso 0.32(4) 1 calc R U P A 2
C11 C 0.0970(16) 0.3684(8) 0.2664(12) 0.049(3) Uani 0.68(4) 1 d . . P A 1
H11A H 0.0091 0.3742 0.2804 0.073 Uiso 0.68(4) 1 calc R U P A 1
H11B H 0.1324 0.4069 0.2371 0.073 Uiso 0.68(4) 1 calc R U P A 1
H11C H 0.1088 0.3354 0.2095 0.073 Uiso 0.68(4) 1 calc R U P A 1
C11A C 0.073(2) 0.3526(13) 0.289(2) 0.033(6) Uiso 0.32(4) 1 d . . P A 2
H11D H -0.0098 0.3475 0.3197 0.049 Uiso 0.32(4) 1 calc R U P A 2
H11E H 0.0796 0.3926 0.2497 0.049 Uiso 0.32(4) 1 calc R U P A 2
H11F H 0.0902 0.3193 0.2335 0.049 Uiso 0.32(4) 1 calc R U P A 2
C12 C 0.2917(7) 0.3420(6) 0.3575(15) 0.037(3) Uani 0.68(4) 1 d . . P A 1
H12A H 0.3006 0.3132 0.2927 0.055 Uiso 0.68(4) 1 calc R U P A 1
H12B H 0.3274 0.3820 0.3367 0.055 Uiso 0.68(4) 1 calc R U P A 1
H12C H 0.3343 0.3253 0.4250 0.055 Uiso 0.68(4) 1 calc R U P A 1
C12A C 0.2830(18) 0.3582(13) 0.321(2) 0.033(5) Uiso 0.32(4) 1 d . . P A 2
H12D H 0.3506 0.3571 0.3770 0.050 Uiso 0.32(4) 1 calc R U P A 2
H12E H 0.2935 0.3248 0.2652 0.050 Uiso 0.32(4) 1 calc R U P A 2
H12F H 0.2829 0.3981 0.2813 0.050 Uiso 0.32(4) 1 calc R U P A 2
C13 C 0.0282(3) 0.40079(18) 0.8185(3) 0.0214(8) Uani 1 1 d . . . . .
H13A H 0.0232 0.3547 0.8214 0.026 Uiso 1 1 calc R U . . .
C14 C -0.0946(4) 0.4250(3) 0.8303(4) 0.0421(13) Uani 1 1 d . . . . .
H14A H -0.1472 0.4074 0.7703 0.063 Uiso 1 1 calc R U . . .
H14B H -0.0928 0.4701 0.8223 0.063 Uiso 1 1 calc R U . . .
H14C H -0.1272 0.4140 0.9063 0.063 Uiso 1 1 calc R U . . .
C15 C 0.1013(4) 0.4229(2) 0.9255(4) 0.0327(11) Uani 1 1 d . . . . .
H15A H 0.1869 0.4096 0.9187 0.049 Uiso 1 1 calc R U . . .
H15B H 0.0651 0.4051 0.9952 0.049 Uiso 1 1 calc R U . . .
H15C H 0.0980 0.4681 0.9301 0.049 Uiso 1 1 calc R 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
Pb1 N1 2.134(3) 7_565 ?
Pb1 N1 2.134(3) . ?
N1 C1 1.330(4) . ?
N1 C4 1.431(4) . ?
C1 C2 1.353(5) . ?
C1 C1 1.422(7) 7_565 ?
C2 C3 1.337(5) . ?
C3 C3 1.362(8) 7_565 ?
C4 C5 1.449(5) . ?
C4 C9 1.474(5) . ?
C5 C6 1.392(5) . ?
C5 C13 1.580(5) . ?
C6 C7 1.440(5) . ?
C7 C8 1.424(6) . ?
C8 C9 1.385(5) . ?
C9 C10 1.573(5) . ?
C10 C12 1.444(8) . ?
C10 C11A 1.48(3) . ?
C10 C12A 1.51(2) . ?
C10 C11 1.593(12) . ?
C13 C14 1.444(5) . ?
C13 C15 1.552(5) . ?

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
N1 Pb1 N1 77.60(16) 7_565 . ?
C1 N1 C4 119.7(3) . . ?
C1 N1 Pb1 113.1(2) . . ?
C4 N1 Pb1 126.0(2) . . ?
N1 C1 C2 121.8(3) . . ?
N1 C1 C1 118.1(2) . 7_565 ?
C2 C1 C1 120.0(2) . 7_565 ?
C3 C2 C1 118.1(4) . . ?
C2 C3 C3 121.9(2) . 7_565 ?
N1 C4 C5 118.1(3) . . ?
N1 C4 C9 118.5(3) . . ?
C5 C4 C9 123.3(3) . . ?
C6 C5 C4 116.2(3) . . ?
C6 C5 C13 119.5(3) . . ?
C4 C5 C13 124.3(3) . . ?
C5 C6 C7 121.2(4) . . ?
C8 C7 C6 121.9(4) . . ?
C9 C8 C7 119.8(4) . . ?
C8 C9 C4 117.6(3) . . ?
C8 C9 C10 118.1(3) . . ?
C4 C9 C10 124.3(3) . . ?
C11A C10 C12A 102.2(11) . . ?
C12 C10 C9 112.0(5) . . ?
C11A C10 C9 116.8(11) . . ?
C12A C10 C9 114.6(8) . . ?
C12 C10 C11 106.7(6) . . ?
C9 C10 C11 115.4(5) . . ?
C14 C13 C15 106.7(3) . . ?
C14 C13 C5 108.6(3) . . ?
C15 C13 C5 117.3(3) . . ?

_refine_diff_density_max         0.753
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.122

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1530483'
_audit_update_record             
;
2017-01-31 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H49 N3 Pb'
_chemical_formula_weight         767.00

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.2497(8)
_cell_length_b                   22.1876(18)
_cell_length_c                   13.7655(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.600(3)
_cell_angle_gamma                90
_cell_volume                     3429.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    30953
_cell_measurement_theta_min      1.74
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_F_000             1544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    4.950
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6001
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30953
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.743
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7823
_reflns_number_gt                6203
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0236P)²+0.3818P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7823
_refine_ls_number_parameters     403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0535
_refine_ls_wR_factor_gt          0.0498
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.002
_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_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
Pb1 Pb 0.90294(2) 0.08925(2) 0.91124(2) 0.02081(4) Uani 1 1 d . . . . .
N1 N 1.0969(2) 0.10184(10) 0.90487(18) 0.0199(5) Uani 1 1 d . . . . .
N2 N 0.92551(19) 0.18489(10) 0.88173(17) 0.0176(5) Uani 1 1 d . . . . .
N3 N 0.8023(2) 0.11509(12) 0.72152(19) 0.0246(6) Uani 1 1 d . . . . .
H3A H 0.863(3) 0.1020(14) 0.697(2) 0.034(10) Uiso 1 1 d . . . . .
C1 C 1.1327(2) 0.16066(12) 0.8882(2) 0.0188(6) Uani 1 1 d . . . . .
C2 C 1.0411(2) 0.20491(13) 0.8773(2) 0.0189(6) Uani 1 1 d . . . . .
C3 C 1.0727(3) 0.26479(13) 0.8587(2) 0.0225(7) Uani 1 1 d . . . . .
H3B H 1.0122 0.2946 0.8512 0.027 Uiso 1 1 calc R U . . .
C4 C 1.1906(3) 0.28133(13) 0.8510(2) 0.0272(7) Uani 1 1 d . . . . .
H4A H 1.2102 0.3221 0.8386 0.033 Uiso 1 1 calc R U . . .
C5 C 1.2798(3) 0.23820(14) 0.8615(2) 0.0255(7) Uani 1 1 d . . . . .
H5A H 1.3606 0.2495 0.8564 0.031 Uiso 1 1 calc R U . . .
C6 C 1.2512(3) 0.17872(14) 0.8792(2) 0.0249(7) Uani 1 1 d . . . . .
H6A H 1.3129 0.1495 0.8855 0.030 Uiso 1 1 calc R U . . .
C7 C 1.1834(2) 0.05538(13) 0.9221(2) 0.0196(6) Uani 1 1 d . . . . .
C8 C 1.2566(2) 0.05514(13) 1.0087(2) 0.0207(6) Uani 1 1 d . . . . .
C9 C 1.3404(3) 0.00889(13) 1.0224(2) 0.0247(7) Uani 1 1 d . . . . .
H9A H 1.3922 0.0087 1.0796 0.030 Uiso 1 1 calc R U . . .
C10 C 1.3496(3) -0.03651(14) 0.9547(2) 0.0276(7) Uani 1 1 d . . . . .
H10A H 1.4066 -0.0677 0.9658 0.033 Uiso 1 1 calc R U . . .
C11 C 1.2763(3) -0.03648(13) 0.8713(2) 0.0254(7) Uani 1 1 d . . . . .
H11A H 1.2825 -0.0683 0.8256 0.030 Uiso 1 1 calc R U . . .
C12 C 1.1929(2) 0.00903(13) 0.8518(2) 0.0223(7) Uani 1 1 d . . . . .
C13 C 1.1182(3) 0.00947(13) 0.7561(2) 0.0256(7) Uani 1 1 d . . . . .
H13A H 1.0357 0.0215 0.7710 0.031 Uiso 1 1 calc R U . . .
C14 C 1.1089(3) -0.05193(15) 0.7055(2) 0.0351(8) Uani 1 1 d . . . . .
H14A H 1.0896 -0.0829 0.7528 0.053 Uiso 1 1 calc R U . . .
H14B H 1.1851 -0.0617 0.6785 0.053 Uiso 1 1 calc R U . . .
H14C H 1.0461 -0.0505 0.6529 0.053 Uiso 1 1 calc R U . . .
C15 C 1.1644(3) 0.05749(15) 0.6883(2) 0.0319(8) Uani 1 1 d . . . . .
H15A H 1.1662 0.0967 0.7213 0.048 Uiso 1 1 calc R U . . .
H15B H 1.1116 0.0598 0.6290 0.048 Uiso 1 1 calc R U . . .
H15C H 1.2450 0.0468 0.6712 0.048 Uiso 1 1 calc R U . . .
C16 C 1.2412(3) 0.10117(13) 1.0889(2) 0.0240(7) Uani 1 1 d . . . . .
H16A H 1.1957 0.1362 1.0600 0.029 Uiso 1 1 calc R U . . .
C17 C 1.1678(4) 0.07308(15) 1.1673(3) 0.0437(10) Uani 1 1 d . . . . .
H17A H 1.0897 0.0609 1.1383 0.066 Uiso 1 1 calc R U . . .
H17B H 1.1570 0.1027 1.2188 0.066 Uiso 1 1 calc R U . . .
H17C H 1.2096 0.0377 1.1951 0.066 Uiso 1 1 calc R U . . .
C18 C 1.3602(3) 0.12456(16) 1.1346(3) 0.0454(10) Uani 1 1 d . . . . .
H18A H 1.4075 0.1413 1.0837 0.068 Uiso 1 1 calc R U . . .
H18B H 1.4040 0.0913 1.1671 0.068 Uiso 1 1 calc R U . . .
H18C H 1.3452 0.1560 1.1823 0.068 Uiso 1 1 calc R U . . .
C19 C 0.8253(2) 0.22388(13) 0.8643(2) 0.0220(7) Uani 1 1 d . . . . .
C20 C 0.7597(3) 0.22179(13) 0.7737(2) 0.0253(7) Uani 1 1 d . . . . .
C21 C 0.6597(3) 0.25962(14) 0.7623(3) 0.0349(8) Uani 1 1 d . . . . .
H21A H 0.6145 0.2603 0.7016 0.042 Uiso 1 1 calc R U . . .
C22 C 0.6256(3) 0.29578(15) 0.8371(3) 0.0392(9) Uani 1 1 d . . . . .
H22A H 0.5572 0.3207 0.8273 0.047 Uiso 1 1 calc R U . . .
C23 C 0.6884(3) 0.29632(15) 0.9249(3) 0.0371(9) Uani 1 1 d . . . . .
H23A H 0.6634 0.3215 0.9756 0.045 Uiso 1 1 calc R U . . .
C24 C 0.7892(3) 0.26026(13) 0.9410(2) 0.0259(7) Uani 1 1 d . . . . .
C25 C 0.8546(3) 0.25759(15) 1.0407(2) 0.0340(8) Uani 1 1 d . . . . .
H25A H 0.9388 0.2454 1.0316 0.041 Uiso 1 1 calc R U . . .
C26 C 0.8574(3) 0.31714(17) 1.0951(3) 0.0504(10) Uani 1 1 d . . . . .
H26A H 0.9078 0.3132 1.1555 0.076 Uiso 1 1 calc R U . . .
H26B H 0.7764 0.3281 1.1107 0.076 Uiso 1 1 calc R U . . .
H26C H 0.8899 0.3486 1.0543 0.076 Uiso 1 1 calc R U . . .
C27 C 0.7982(4) 0.20905(18) 1.1021(3) 0.0586(12) Uani 1 1 d . . . . .
H27A H 0.8446 0.2049 1.1644 0.088 Uiso 1 1 calc R U . . .
H27B H 0.7977 0.1705 1.0672 0.088 Uiso 1 1 calc R U . . .
H27C H 0.7163 0.2206 1.1139 0.088 Uiso 1 1 calc R U . . .
C28 C 0.7929(3) 0.18102(14) 0.6890(2) 0.0298(8) Uani 1 1 d . . . . .
C29 C 0.7038(3) 0.18588(16) 0.6006(2) 0.0421(9) Uani 1 1 d . . . . .
H29A H 0.7255 0.1573 0.5505 0.063 Uiso 1 1 calc R U . . .
H29B H 0.7051 0.2269 0.5745 0.063 Uiso 1 1 calc R U . . .
H29C H 0.6236 0.1766 0.6204 0.063 Uiso 1 1 calc R U . . .
C30 C 0.9156(3) 0.19858(16) 0.6543(2) 0.0388(9) Uani 1 1 d . . . . .
H30A H 0.9303 0.1763 0.5948 0.058 Uiso 1 1 calc R U . . .
H30B H 0.9775 0.1887 0.7051 0.058 Uiso 1 1 calc R U . . .
H30C H 0.9171 0.2419 0.6410 0.058 Uiso 1 1 calc R U . . .
C31 C 0.7095(3) 0.07246(13) 0.6922(2) 0.0235(7) Uani 1 1 d . . . . .
C32 C 0.7307(3) 0.02994(15) 0.6201(2) 0.0307(8) Uani 1 1 d . . . . .
C33 C 0.6457(3) -0.01510(15) 0.5978(2) 0.0344(8) Uani 1 1 d . . . . .
H33A H 0.6612 -0.0445 0.5501 0.041 Uiso 1 1 calc R U . . .
C34 C 0.5406(3) -0.01762(15) 0.6435(2) 0.0346(8) Uani 1 1 d . . . . .
C35 C 0.5210(3) 0.02548(14) 0.7137(2) 0.0311(8) Uani 1 1 d . . . . .
H35A H 0.4481 0.0244 0.7450 0.037 Uiso 1 1 calc R U . . .
C36 C 0.6029(3) 0.06995(14) 0.7399(2) 0.0263(7) Uani 1 1 d . . . . .
C37 C 0.5740(3) 0.11395(15) 0.8185(2) 0.0295(7) Uani 1 1 d . . . . .
H37A H 0.5116 0.0970 0.8570 0.044 Uiso 1 1 calc R U . . .
H37B H 0.5461 0.1519 0.7887 0.044 Uiso 1 1 calc R U . . .
H37C H 0.6456 0.1215 0.8611 0.044 Uiso 1 1 calc R U . . .
C38 C 0.8432(3) 0.03083(18) 0.5661(3) 0.0448(10) Uani 1 1 d . . . . .
H38A H 0.8518 0.0703 0.5353 0.067 Uiso 1 1 calc R U . . .
H38B H 0.8391 -0.0006 0.5159 0.067 Uiso 1 1 calc R U . . .
H38C H 0.9119 0.0234 0.6118 0.067 Uiso 1 1 calc R U . . .
C39 C 0.4515(3) -0.06731(17) 0.6201(3) 0.0490(10) Uani 1 1 d . . . . .
H39A H 0.4791 -0.0923 0.5673 0.073 Uiso 1 1 calc R U . . .
H39B H 0.3741 -0.0496 0.5999 0.073 Uiso 1 1 calc R U . . .
H39C H 0.4434 -0.0923 0.6781 0.073 Uiso 1 1 calc R 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
Pb1 N2 2.178(2) . ?
Pb1 N1 2.207(2) . ?
N1 C1 1.389(3) . ?
N1 C7 1.428(3) . ?
N2 C2 1.379(3) . ?
N2 C19 1.429(3) . ?
N3 C31 1.448(4) . ?
N3 C28 1.532(4) . ?
C1 C6 1.404(4) . ?
C1 C2 1.425(4) . ?
C2 C3 1.403(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.388(4) . ?
C5 C6 1.384(4) . ?
C7 C8 1.404(4) . ?
C7 C12 1.420(4) . ?
C8 C9 1.399(4) . ?
C8 C16 1.522(4) . ?
C9 C10 1.381(4) . ?
C10 C11 1.371(4) . ?
C11 C12 1.393(4) . ?
C12 C13 1.517(4) . ?
C13 C15 1.529(4) . ?
C13 C14 1.530(4) . ?
C16 C17 1.533(5) . ?
C16 C18 1.534(4) . ?
C19 C20 1.409(4) . ?
C19 C24 1.409(4) . ?
C20 C21 1.405(4) . ?
C20 C28 1.541(4) . ?
C21 C22 1.379(5) . ?
C22 C23 1.361(5) . ?
C23 C24 1.394(4) . ?
C24 C25 1.518(4) . ?
C25 C26 1.518(4) . ?
C25 C27 1.531(5) . ?
C28 C29 1.531(4) . ?
C28 C30 1.538(4) . ?
C31 C32 1.400(4) . ?
C31 C36 1.405(4) . ?
C32 C33 1.403(4) . ?
C32 C38 1.508(5) . ?
C33 C34 1.375(5) . ?
C34 C35 1.386(5) . ?
C34 C39 1.511(5) . ?
C35 C36 1.382(4) . ?
C36 C37 1.508(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pb1 N1 75.06(8) . . ?
C1 N1 C7 120.2(2) . . ?
C1 N1 Pb1 115.05(17) . . ?
C7 N1 Pb1 124.60(18) . . ?
C2 N2 C19 122.2(2) . . ?
C2 N2 Pb1 116.32(18) . . ?
C19 N2 Pb1 121.40(17) . . ?
C31 N3 C28 120.5(2) . . ?
N1 C1 C6 124.7(3) . . ?
N1 C1 C2 116.7(2) . . ?
C6 C1 C2 118.6(3) . . ?
N2 C2 C3 124.3(3) . . ?
N2 C2 C1 116.8(3) . . ?
C3 C2 C1 118.8(3) . . ?
C4 C3 C2 121.3(3) . . ?
C3 C4 C5 119.9(3) . . ?
C6 C5 C4 120.1(3) . . ?
C5 C6 C1 121.3(3) . . ?
C8 C7 C12 120.7(3) . . ?
C8 C7 N1 120.1(3) . . ?
C12 C7 N1 119.3(3) . . ?
C9 C8 C7 118.1(3) . . ?
C9 C8 C16 120.0(3) . . ?
C7 C8 C16 121.7(3) . . ?
C10 C9 C8 121.5(3) . . ?
C11 C10 C9 119.9(3) . . ?
C10 C11 C12 121.6(3) . . ?
C11 C12 C7 118.2(3) . . ?
C11 C12 C13 120.0(3) . . ?
C7 C12 C13 121.7(3) . . ?
C12 C13 C15 110.1(2) . . ?
C12 C13 C14 114.1(3) . . ?
C15 C13 C14 111.0(3) . . ?
C8 C16 C17 109.2(2) . . ?
C8 C16 C18 112.9(3) . . ?
C17 C16 C18 110.1(3) . . ?
C20 C19 C24 121.5(3) . . ?
C20 C19 N2 119.5(3) . . ?
C24 C19 N2 118.9(3) . . ?
C21 C20 C19 116.8(3) . . ?
C21 C20 C28 119.8(3) . . ?
C19 C20 C28 123.4(3) . . ?
C22 C21 C20 121.5(3) . . ?
C23 C22 C21 121.0(3) . . ?
C22 C23 C24 120.5(3) . . ?
C23 C24 C19 118.7(3) . . ?
C23 C24 C25 120.6(3) . . ?
C19 C24 C25 120.6(3) . . ?
C24 C25 C26 114.0(3) . . ?
C24 C25 C27 109.4(3) . . ?
C26 C25 C27 109.7(3) . . ?
C29 C28 N3 109.2(3) . . ?
C29 C28 C30 107.0(3) . . ?
N3 C28 C30 106.6(3) . . ?
C29 C28 C20 112.5(3) . . ?
N3 C28 C20 110.8(2) . . ?
C30 C28 C20 110.5(3) . . ?
C32 C31 C36 119.5(3) . . ?
C32 C31 N3 119.1(3) . . ?
C36 C31 N3 121.2(3) . . ?
C31 C32 C33 119.4(3) . . ?
C31 C32 C38 121.7(3) . . ?
C33 C32 C38 118.9(3) . . ?
C34 C33 C32 121.5(3) . . ?
C33 C34 C35 118.0(3) . . ?
C33 C34 C39 120.7(3) . . ?
C35 C34 C39 121.3(3) . . ?
C36 C35 C34 122.8(3) . . ?
C35 C36 C31 118.7(3) . . ?
C35 C36 C37 118.7(3) . . ?
C31 C36 C37 122.6(3) . . ?

_refine_diff_density_max         0.852
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.101

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1530481'
_audit_update_record             
;
2017-01-31 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT201_3                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          4 Report
RESPONSE: The data quality is relatively poor and didn't allow for the anisotropic refinement of 4 atoms involved in the disordered portion. 
;
# Added during the CSD deposition process: Tuesday 31 January 2017 05:02 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H47 N3 O Pb'
_chemical_formula_weight         708.92

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.8076(12)
_cell_length_b                   26.177(2)
_cell_length_c                   20.3861(17)
_cell_angle_alpha                90
_cell_angle_beta                 92.810(4)
_cell_angle_gamma                90
_cell_volume                     7892.7(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    63320
_cell_measurement_theta_min      1.835
_cell_measurement_theta_max      26.000

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             2848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    4.298
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4961
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63320
_diffrn_reflns_av_unetI/netI     0.1814
_diffrn_reflns_av_R_equivalents  0.1686
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.835
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15512
_reflns_number_gt                7870
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0673P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15512
_refine_ls_number_parameters     691
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1590
_refine_ls_R_factor_gt           0.0663
_refine_ls_wR_factor_ref         0.1673
_refine_ls_wR_factor_gt          0.1341
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.006
_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_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
Pb1 Pb -0.17280(3) 0.85871(2) 0.70299(2) 0.03321(14) Uani 1 1 d . . . . .
O1 O -0.0271(5) 0.8319(3) 0.7436(4) 0.038(2) Uani 1 1 d . . . . .
N1 N -0.2206(6) 0.8785(4) 0.8007(5) 0.033(2) Uani 1 1 d . . . . .
N2 N -0.2332(6) 0.7872(3) 0.7384(4) 0.032(2) Uani 1 1 d . . . . .
N3 N 0.0519(6) 0.8391(4) 0.7105(5) 0.036(3) Uani 1 1 d . . . . .
N4 N 0.1039(6) 0.8648(3) 0.4642(4) 0.027(2) Uani 1 1 d . . . . .
N5 N 0.2178(6) 0.7877(3) 0.5013(5) 0.032(2) Uani 1 1 d . . . . .
C1 C -0.2607(8) 0.8388(4) 0.8329(6) 0.029(3) Uani 1 1 d . . . . .
C2 C -0.2703(8) 0.7906(5) 0.7995(5) 0.032(3) Uani 1 1 d . . . . .
C3 C -0.3139(8) 0.7510(5) 0.8298(6) 0.037(3) Uani 1 1 d . . . . .
H3A H -0.319063 0.718692 0.808797 0.044 Uiso 1 1 calc R U . . .
C4 C -0.3497(9) 0.7581(6) 0.8900(6) 0.048(4) Uani 1 1 d . . . . .
H4A H -0.381642 0.730782 0.908894 0.057 Uiso 1 1 calc R U . . .
C5 C -0.3410(9) 0.8039(6) 0.9241(6) 0.047(4) Uani 1 1 d . . . . .
H5A H -0.365442 0.807954 0.965981 0.057 Uiso 1 1 calc R U . . .
C6 C -0.2957(8) 0.8430(5) 0.8952(7) 0.043(3) Uani 1 1 d . . . . .
H6A H -0.287727 0.874261 0.918524 0.052 Uiso 1 1 calc R U . . .
C7 C 0.1249(9) 0.8108(7) 0.7463(8) 0.075(5) Uani 1 1 d . . . . .
H7A H 0.128460 0.821582 0.792403 0.113 Uiso 1 1 calc R U . . .
H7B H 0.182586 0.817957 0.726516 0.113 Uiso 1 1 calc R U . . .
H7C H 0.112297 0.774102 0.743788 0.113 Uiso 1 1 calc R U . . .
C8 C 0.0780(11) 0.8950(5) 0.7085(8) 0.068(5) Uani 1 1 d . . . . .
H8A H 0.089171 0.907657 0.753432 0.102 Uiso 1 1 calc R U . . .
H8B H 0.028676 0.914610 0.686807 0.102 Uiso 1 1 calc R U . . .
H8C H 0.132868 0.898900 0.684059 0.102 Uiso 1 1 calc R U . . .
C9 C 0.0412(9) 0.8208(5) 0.6398(6) 0.051(4) Uani 1 1 d . . . . .
H9A H 0.020169 0.785304 0.639014 0.076 Uiso 1 1 calc R U . . .
H9B H 0.099617 0.822928 0.619346 0.076 Uiso 1 1 calc R U . . .
H9C H -0.002977 0.842359 0.615543 0.076 Uiso 1 1 calc R U . . .
C10 C -0.2436(8) 0.9305(4) 0.8162(6) 0.034(3) Uani 1 1 d . . . . .
C12 C -0.2083(10) 1.0140(6) 0.8585(8) 0.070(5) Uani 1 1 d . . . . .
H12A H -0.165244 1.037184 0.877696 0.084 Uiso 1 1 calc R U . . .
C13 C -0.2949(9) 1.0310(5) 0.8441(7) 0.058(4) Uani 1 1 d . . . . .
H13A H -0.311629 1.065181 0.853492 0.069 Uiso 1 1 calc R U . . .
C14 C -0.3561(9) 0.9978(5) 0.8161(7) 0.053(4) Uani 1 1 d . . . . .
H14A H -0.416402 1.009086 0.807406 0.064 Uiso 1 1 calc R U . . .
C15 C -0.3339(8) 0.9481(5) 0.7998(7) 0.044(3) Uani 1 1 d . . . . .
C16 C -0.4044(9) 0.9132(5) 0.7644(7) 0.051(4) Uani 1 1 d . . . . .
H16A H -0.377019 0.878553 0.760141 0.061 Uiso 1 1 calc R U . . .
C17 C -0.4282(9) 0.9335(5) 0.6950(7) 0.066(5) Uani 1 1 d . . . . .
H17A H -0.372527 0.938555 0.671666 0.099 Uiso 1 1 calc R U . . .
H17B H -0.460091 0.966186 0.698010 0.099 Uiso 1 1 calc R U . . .
H17C H -0.467018 0.908842 0.671021 0.099 Uiso 1 1 calc R U . . .
C18 C -0.4888(9) 0.9081(6) 0.8053(10) 0.094(7) Uani 1 1 d . . . . .
H18A H -0.470152 0.899142 0.850599 0.140 Uiso 1 1 calc R U . . .
H18B H -0.528171 0.881254 0.786379 0.140 Uiso 1 1 calc R U . . .
H18C H -0.521568 0.940613 0.804776 0.140 Uiso 1 1 calc R U . . .
C11 C -0.1812(9) 0.9635(5) 0.8459(7) 0.052(4) Uani 1 1 d . . . . .
C19 C -0.0843(10) 0.9447(6) 0.8679(9) 0.071(5) Uani 1 1 d . . . . .
H19A H -0.068245 0.910345 0.850432 0.085 Uiso 1 1 calc R U . A 1
C20 C -0.012(2) 0.9930(13) 0.8471(16) 0.056(6) Uiso 0.52(3) 1 d . . P B 1
H20A H 0.049984 0.983430 0.859819 0.084 Uiso 0.52(3) 1 calc R U P B 1
H20B H -0.018016 0.998752 0.799592 0.084 Uiso 0.52(3) 1 calc R U P B 1
H20C H -0.028267 1.024410 0.870090 0.084 Uiso 0.52(3) 1 calc R U P B 1
C21 C -0.085(3) 0.9480(18) 0.957(2) 0.095(9) Uiso 0.52(3) 1 d . . P B 1
H21A H -0.026004 0.936741 0.975684 0.142 Uiso 0.52(3) 1 calc R U P B 1
H21B H -0.096174 0.983218 0.970160 0.142 Uiso 0.52(3) 1 calc R U P B 1
H21C H -0.132421 0.925678 0.972277 0.142 Uiso 0.52(3) 1 calc R U P B 1
C20A C -0.010(2) 0.9705(15) 0.8367(18) 0.056(6) Uiso 0.48(3) 1 d . . P B 2
H20D H -0.024276 0.973179 0.789318 0.084 Uiso 0.48(3) 1 calc R U P B 2
H20E H -0.002050 1.004781 0.855345 0.084 Uiso 0.48(3) 1 calc R U P B 2
H20F H 0.045726 0.950828 0.844342 0.084 Uiso 0.48(3) 1 calc R U P B 2
C21A C -0.065(3) 0.941(2) 0.934(2) 0.095(9) Uiso 0.48(3) 1 d . . P B 2
H21D H -0.114235 0.923638 0.954971 0.142 Uiso 0.48(3) 1 calc R U P B 2
H21E H -0.008695 0.921269 0.941681 0.142 Uiso 0.48(3) 1 calc R U P B 2
H21F H -0.056471 0.975221 0.952684 0.142 Uiso 0.48(3) 1 calc R U P B 2
C22 C -0.2531(7) 0.7437(4) 0.6969(5) 0.026(3) Uani 1 1 d . . . . .
C23 C -0.3287(8) 0.7456(4) 0.6545(5) 0.026(3) Uani 1 1 d . . . . .
C24 C -0.3448(9) 0.7037(5) 0.6147(6) 0.043(3) Uani 1 1 d . . . . .
H24A H -0.396139 0.704735 0.584859 0.051 Uiso 1 1 calc R U . . .
C25 C -0.2916(9) 0.6599(5) 0.6149(6) 0.044(4) Uani 1 1 d . . . . .
H25A H -0.304978 0.631827 0.586620 0.053 Uiso 1 1 calc R U . . .
C26 C -0.2178(8) 0.6602(5) 0.6592(6) 0.037(3) Uani 1 1 d . . . . .
H26A H -0.181339 0.630279 0.661306 0.045 Uiso 1 1 calc R U . . .
C27 C -0.1926(8) 0.6996(4) 0.7002(6) 0.031(3) Uani 1 1 d . . . . .
C28 C -0.1167(10) 0.6971(5) 0.7487(6) 0.049(4) Uani 1 1 d . . . . .
H28A H -0.109478 0.731284 0.770306 0.058 Uiso 1 1 calc R U . . .
C29 C -0.0300(9) 0.6841(6) 0.7165(7) 0.060(4) Uani 1 1 d . . . . .
H29A H -0.019502 0.708885 0.681727 0.091 Uiso 1 1 calc R U . . .
H29B H -0.034792 0.649717 0.697523 0.091 Uiso 1 1 calc R U . . .
H29C H 0.020525 0.685093 0.749377 0.091 Uiso 1 1 calc R U . . .
C30 C -0.1320(9) 0.6575(5) 0.8011(6) 0.053(4) Uani 1 1 d . . . . .
H30A H -0.191871 0.662440 0.818477 0.079 Uiso 1 1 calc R U . . .
H30B H -0.085548 0.661048 0.836731 0.079 Uiso 1 1 calc R U . . .
H30C H -0.128386 0.623229 0.781932 0.079 Uiso 1 1 calc R U . . .
C31 C -0.3941(8) 0.7889(5) 0.6503(6) 0.045(3) Uani 1 1 d . . . . .
H31A H -0.366632 0.816959 0.677893 0.054 Uiso 1 1 calc R U . . .
C32 C -0.4088(11) 0.8106(6) 0.5808(7) 0.078(5) Uani 1 1 d . . . . .
H32A H -0.350290 0.814183 0.560679 0.117 Uiso 1 1 calc R U . . .
H32B H -0.437832 0.844177 0.582968 0.117 Uiso 1 1 calc R U . . .
H32C H -0.447517 0.787455 0.554199 0.117 Uiso 1 1 calc R U . . .
C33 C -0.4852(9) 0.7762(6) 0.6795(7) 0.066(5) Uani 1 1 d . . . . .
H33A H -0.474528 0.759693 0.722371 0.099 Uiso 1 1 calc R U . . .
H33B H -0.519524 0.752980 0.649899 0.099 Uiso 1 1 calc R U . . .
H33C H -0.519732 0.807701 0.684892 0.099 Uiso 1 1 calc R U . . .
C34 C 0.1708(7) 0.8749(4) 0.5121(5) 0.025(3) Uani 1 1 d . . . . .
C35 C 0.2294(7) 0.8339(4) 0.5337(5) 0.026(3) Uani 1 1 d . . . . .
C36 C 0.2979(8) 0.8424(5) 0.5831(6) 0.037(3) Uani 1 1 d . . . . .
H36A H 0.336610 0.815358 0.597807 0.044 Uiso 1 1 calc R U . . .
C37 C 0.3077(9) 0.8923(5) 0.6104(6) 0.044(4) Uani 1 1 d . . . . .
H37A H 0.353230 0.897642 0.644185 0.053 Uiso 1 1 calc R U . . .
C38 C 0.2548(9) 0.9331(5) 0.5903(6) 0.045(4) Uani 1 1 d . . . . .
H38A H 0.263114 0.966091 0.609089 0.053 Uiso 1 1 calc R U . . .
C39 C 0.1877(8) 0.9235(4) 0.5406(6) 0.036(3) Uani 1 1 d . . . . .
H39A H 0.151380 0.951383 0.525195 0.043 Uiso 1 1 calc R U . . .
C43 C 0.0652(8) 0.9039(4) 0.4251(5) 0.025(3) Uani 1 1 d . . . . .
C44 C -0.0261(8) 0.9178(4) 0.4339(5) 0.025(3) Uani 1 1 d . . . . .
C45 C -0.0686(8) 0.9522(4) 0.3887(6) 0.038(3) Uani 1 1 d . . . . .
H45A H -0.129719 0.961681 0.393881 0.046 Uiso 1 1 calc R U . . .
C46 C -0.0220(9) 0.9728(4) 0.3359(6) 0.039(3) Uani 1 1 d . . . . .
H46A H -0.051901 0.994707 0.304635 0.047 Uiso 1 1 calc R U . . .
C47 C 0.0670(10) 0.9604(4) 0.3309(6) 0.043(4) Uani 1 1 d . . . . .
H47A H 0.099537 0.975261 0.296686 0.051 Uiso 1 1 calc R U . . .
C48 C 0.1126(8) 0.9261(4) 0.3753(5) 0.034(3) Uani 1 1 d . . . . .
C49 C 0.2111(8) 0.9158(4) 0.3642(5) 0.035(3) Uani 1 1 d . . . . .
H49A H 0.233964 0.893517 0.401226 0.042 Uiso 1 1 calc R U . . .
C50 C 0.2687(10) 0.9632(5) 0.3668(8) 0.072(5) Uani 1 1 d . . . . .
H50A H 0.255044 0.983357 0.405600 0.108 Uiso 1 1 calc R U . . .
H50B H 0.255874 0.983598 0.327132 0.108 Uiso 1 1 calc R U . . .
H50C H 0.332702 0.953503 0.369395 0.108 Uiso 1 1 calc R U . . .
C51 C 0.2215(10) 0.8844(5) 0.2998(6) 0.056(4) Uani 1 1 d . . . . .
H51A H 0.284561 0.873638 0.296974 0.084 Uiso 1 1 calc R U . . .
H51B H 0.204038 0.905734 0.261687 0.084 Uiso 1 1 calc R U . . .
H51C H 0.182384 0.854239 0.300200 0.084 Uiso 1 1 calc R U . . .
C52 C -0.0764(7) 0.9003(4) 0.4920(5) 0.027(3) Uani 1 1 d . . . . .
H52A H -0.051697 0.866046 0.505306 0.033 Uiso 1 1 calc R U . . .
C53 C -0.0609(9) 0.9357(5) 0.5501(6) 0.046(3) Uani 1 1 d . . . . .
H53A H 0.003830 0.937089 0.562527 0.069 Uiso 1 1 calc R U . . .
H53B H -0.093992 0.922952 0.587265 0.069 Uiso 1 1 calc R U . . .
H53C H -0.082535 0.970019 0.538271 0.069 Uiso 1 1 calc R U . . .
C54 C -0.1787(8) 0.8941(5) 0.4789(7) 0.049(4) Uani 1 1 d . . . . .
H54A H -0.190211 0.871656 0.440911 0.074 Uiso 1 1 calc R U . . .
H54B H -0.206033 0.927586 0.469889 0.074 Uiso 1 1 calc R U . . .
H54C H -0.205189 0.878993 0.517550 0.074 Uiso 1 1 calc R U . . .
C55 C 0.2885(8) 0.7499(4) 0.5048(5) 0.029(3) Uani 1 1 d . . . . .
C56 C 0.3550(8) 0.7491(5) 0.4586(6) 0.036(3) Uani 1 1 d . . . . .
C57 C 0.4204(8) 0.7119(5) 0.4619(7) 0.049(4) Uani 1 1 d . . . . .
H57A H 0.466219 0.712274 0.430933 0.058 Uiso 1 1 calc R U . . .
C58 C 0.4213(9) 0.6742(5) 0.5090(7) 0.046(4) Uani 1 1 d . . . . .
H58A H 0.465598 0.647925 0.509320 0.055 Uiso 1 1 calc R U . . .
C59 C 0.3572(9) 0.6751(5) 0.5553(6) 0.040(3) Uani 1 1 d . . . . .
H59A H 0.359880 0.650060 0.589123 0.048 Uiso 1 1 calc R U . . .
C60 C 0.2889(8) 0.7110(5) 0.5547(6) 0.036(3) Uani 1 1 d . . . . .
C61 C 0.2198(9) 0.7096(5) 0.6062(7) 0.050(4) Uani 1 1 d . . . . .
H61A H 0.180750 0.740586 0.600435 0.060 Uiso 1 1 calc R U . . .
C62 C 0.2577(11) 0.7090(7) 0.6759(7) 0.079(5) Uani 1 1 d . . . . .
H62A H 0.296319 0.738986 0.683732 0.119 Uiso 1 1 calc R U . . .
H62B H 0.293555 0.677872 0.683539 0.119 Uiso 1 1 calc R U . . .
H62C H 0.208042 0.709659 0.705942 0.119 Uiso 1 1 calc R U . . .
C63 C 0.1606(9) 0.6630(6) 0.5935(8) 0.071(5) Uani 1 1 d . . . . .
H63A H 0.108194 0.664656 0.620974 0.106 Uiso 1 1 calc R U . . .
H63B H 0.195524 0.632008 0.604317 0.106 Uiso 1 1 calc R U . . .
H63C H 0.139982 0.662087 0.547141 0.106 Uiso 1 1 calc R U . . .
C64 C 0.3572(9) 0.7888(6) 0.4051(6) 0.052(4) Uani 1 1 d . . . . .
H64A H 0.294658 0.803073 0.399959 0.063 Uiso 1 1 calc R U . . .
C65 C 0.4201(10) 0.8342(6) 0.4242(8) 0.072(5) Uani 1 1 d . . . . .
H65A H 0.407194 0.862847 0.394217 0.108 Uiso 1 1 calc R U . . .
H65B H 0.483322 0.823759 0.421275 0.108 Uiso 1 1 calc R U . . .
H65C H 0.409613 0.844882 0.469318 0.108 Uiso 1 1 calc R U . . .
C66 C 0.3782(11) 0.7670(6) 0.3396(7) 0.076(5) Uani 1 1 d . . . . .
H66A H 0.336141 0.739096 0.328419 0.114 Uiso 1 1 calc R U . . .
H66B H 0.440306 0.753963 0.341461 0.114 Uiso 1 1 calc R U . . .
H66C H 0.371908 0.793784 0.306078 0.114 Uiso 1 1 calc R U . . .
Pb2 Pb 0.10730(3) 0.78606(2) 0.42640(2) 0.03017(14) Uani 1 1 d . . . . .
O2 O -0.0027(14) 0.7620(8) 0.5073(10) 0.032(3) Uiso 0.52(3) 1 d . . P B 1
O2A O 0.0142(15) 0.7502(9) 0.5019(11) 0.032(3) Uiso 0.48(3) 1 d . . P B 2
N6 N -0.0762(7) 0.7335(4) 0.4886(6) 0.054(3) Uani 1 1 d . . . . .
C40 C -0.151(3) 0.7599(16) 0.5242(19) 0.070(7) Uiso 0.52(3) 1 d . . P B 1
H40A H -0.208420 0.742254 0.514194 0.104 Uiso 0.52(3) 1 calc R U P B 1
H40B H -0.136851 0.758841 0.571632 0.104 Uiso 0.52(3) 1 calc R U P B 1
H40C H -0.155922 0.795477 0.509651 0.104 Uiso 0.52(3) 1 calc R U P B 1
C41 C -0.079(2) 0.6831(12) 0.5223(18) 0.057(6) Uiso 0.52(3) 1 d . . P B 1
H41A H -0.133259 0.664437 0.506764 0.086 Uiso 0.52(3) 1 calc R U P B 1
H41B H -0.025102 0.663281 0.512444 0.086 Uiso 0.52(3) 1 calc R U P B 1
H41C H -0.080298 0.688347 0.569833 0.086 Uiso 0.52(3) 1 calc R U P B 1
C42 C -0.103(2) 0.7347(14) 0.4229(15) 0.059(6) Uiso 0.52(3) 1 d . . P B 1
H42A H -0.156098 0.712916 0.415145 0.089 Uiso 0.52(3) 1 calc R U P B 1
H42B H -0.117921 0.769893 0.409993 0.089 Uiso 0.52(3) 1 calc R U P B 1
H42C H -0.053533 0.722255 0.396847 0.089 Uiso 0.52(3) 1 calc R U P B 1
C40A C -0.141(3) 0.7510(18) 0.545(2) 0.070(7) Uiso 0.48(3) 1 d . . P B 2
H40D H -0.202177 0.738895 0.534005 0.104 Uiso 0.48(3) 1 calc R U P B 2
H40E H -0.118622 0.736457 0.586761 0.104 Uiso 0.48(3) 1 calc R U P B 2
H40F H -0.140519 0.788340 0.547619 0.104 Uiso 0.48(3) 1 calc R U P B 2
C41A C -0.065(2) 0.6794(12) 0.491(2) 0.057(6) Uiso 0.48(3) 1 d . . P B 2
H41D H -0.124324 0.662962 0.482752 0.086 Uiso 0.48(3) 1 calc R U P B 2
H41E H -0.023931 0.668594 0.457947 0.086 Uiso 0.48(3) 1 calc R U P B 2
H41F H -0.040754 0.669480 0.534886 0.086 Uiso 0.48(3) 1 calc R U P B 2
C42A C -0.122(2) 0.7605(15) 0.4348(17) 0.059(6) Uiso 0.48(3) 1 d . . P B 2
H42D H -0.183522 0.747338 0.428081 0.089 Uiso 0.48(3) 1 calc R U P B 2
H42E H -0.123838 0.797007 0.445032 0.089 Uiso 0.48(3) 1 calc R U P B 2
H42F H -0.088919 0.755318 0.394749 0.089 Uiso 0.48(3) 1 calc R U P B 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
Pb1 N1 2.207(9) . ?
Pb1 N2 2.210(9) . ?
Pb1 O1 2.379(8) . ?
O1 N3 1.392(12) . ?
N1 C1 1.380(14) . ?
N1 C10 1.442(14) . ?
N2 C2 1.388(14) . ?
N2 C22 1.440(13) . ?
N3 C7 1.474(16) . ?
N3 C8 1.514(15) . ?
N3 C9 1.520(15) . ?
N4 C34 1.381(13) . ?
N4 C43 1.402(13) . ?
N4 Pb2 2.203(9) . ?
N5 C35 1.385(13) . ?
N5 C55 1.439(14) . ?
N5 Pb2 2.183(9) . ?
C1 C6 1.400(16) . ?
C1 C2 1.437(15) . ?
C2 C3 1.383(16) . ?
C3 C4 1.373(16) . ?
C4 C5 1.388(18) . ?
C5 C6 1.373(17) . ?
C10 C11 1.381(16) . ?
C10 C15 1.439(16) . ?
C12 C13 1.374(18) . ?
C12 C11 1.410(18) . ?
C13 C14 1.361(17) . ?
C14 C15 1.385(17) . ?
C15 C16 1.540(17) . ?
C16 C17 1.536(18) . ?
C16 C18 1.54(2) . ?
C11 C19 1.562(18) . ?
C19 C21A 1.37(5) . ?
C19 C20A 1.46(4) . ?
C19 C20 1.72(4) . ?
C19 C21 1.81(5) . ?
C22 C23 1.381(14) . ?
C22 C27 1.462(15) . ?
C23 C24 1.381(15) . ?
C23 C31 1.489(16) . ?
C24 C25 1.389(17) . ?
C25 C26 1.382(16) . ?
C26 C27 1.369(15) . ?
C27 C28 1.462(16) . ?
C28 C29 1.509(18) . ?
C28 C30 1.514(17) . ?
C31 C32 1.534(17) . ?
C31 C33 1.538(18) . ?
C34 C39 1.417(15) . ?
C34 C35 1.435(15) . ?
C35 C36 1.411(15) . ?
C36 C37 1.425(16) . ?
C37 C38 1.376(16) . ?
C38 C39 1.407(15) . ?
C43 C48 1.388(16) . ?
C43 C44 1.420(15) . ?
C44 C45 1.414(14) . ?
C44 C52 1.502(15) . ?
C45 C46 1.413(17) . ?
C46 C47 1.366(17) . ?
C47 C48 1.423(15) . ?
C48 C49 1.511(16) . ?
C49 C50 1.505(17) . ?
C49 C51 1.563(16) . ?
C52 C53 1.513(15) . ?
C52 C54 1.533(15) . ?
C55 C56 1.396(16) . ?
C55 C60 1.440(15) . ?
C56 C57 1.373(16) . ?
C56 C64 1.507(17) . ?
C57 C58 1.377(17) . ?
C58 C59 1.373(17) . ?
C59 C60 1.380(16) . ?
C60 C61 1.501(17) . ?
C61 C62 1.502(19) . ?
C61 C63 1.517(18) . ?
C64 C66 1.498(18) . ?
C64 C65 1.550(19) . ?
Pb2 O2A 2.31(2) . ?
Pb2 O2 2.46(2) . ?
O2 N6 1.36(2) . ?
O2A N6 1.42(2) . ?
N6 C42 1.38(3) . ?
N6 C41A 1.43(3) . ?
N6 C42A 1.44(3) . ?
N6 C41 1.49(3) . ?
N6 C40 1.52(4) . ?
N6 C40A 1.59(5) . ?

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
N1 Pb1 N2 75.6(3) . . ?
N1 Pb1 O1 94.6(3) . . ?
N2 Pb1 O1 90.6(3) . . ?
N3 O1 Pb1 124.1(6) . . ?
C1 N1 C10 119.6(10) . . ?
C1 N1 Pb1 114.7(7) . . ?
C10 N1 Pb1 120.6(8) . . ?
C2 N2 C22 119.9(9) . . ?
C2 N2 Pb1 115.0(7) . . ?
C22 N2 Pb1 123.5(7) . . ?
O1 N3 C7 107.8(10) . . ?
O1 N3 C8 111.5(10) . . ?
C7 N3 C8 108.5(11) . . ?
O1 N3 C9 111.5(9) . . ?
C7 N3 C9 110.5(11) . . ?
C8 N3 C9 107.1(10) . . ?
C34 N4 C43 121.5(9) . . ?
C34 N4 Pb2 113.4(7) . . ?
C43 N4 Pb2 120.0(6) . . ?
C35 N5 C55 120.2(9) . . ?
C35 N5 Pb2 115.0(7) . . ?
C55 N5 Pb2 122.7(7) . . ?
N1 C1 C6 124.1(10) . . ?
N1 C1 C2 118.1(11) . . ?
C6 C1 C2 117.8(11) . . ?
C3 C2 N2 124.5(11) . . ?
C3 C2 C1 119.0(11) . . ?
N2 C2 C1 116.6(11) . . ?
C4 C3 C2 120.5(13) . . ?
C3 C4 C5 122.3(13) . . ?
C6 C5 C4 117.7(13) . . ?
C5 C6 C1 122.7(12) . . ?
C11 C10 C15 119.7(11) . . ?
C11 C10 N1 121.7(11) . . ?
C15 C10 N1 118.6(10) . . ?
C13 C12 C11 122.3(14) . . ?
C14 C13 C12 118.5(12) . . ?
C13 C14 C15 122.7(12) . . ?
C14 C15 C10 118.2(12) . . ?
C14 C15 C16 120.4(11) . . ?
C10 C15 C16 121.4(11) . . ?
C17 C16 C15 110.3(11) . . ?
C17 C16 C18 111.9(12) . . ?
C15 C16 C18 110.3(12) . . ?
C10 C11 C12 118.4(13) . . ?
C10 C11 C19 120.9(11) . . ?
C12 C11 C19 120.6(13) . . ?
C21A C19 C20A 109(3) . . ?
C21A C19 C11 117(3) . . ?
C20A C19 C11 115.3(19) . . ?
C11 C19 C20 105.5(15) . . ?
C11 C19 C21 103.0(17) . . ?
C20 C19 C21 104.1(19) . . ?
C23 C22 N2 118.4(10) . . ?
C23 C22 C27 122.2(10) . . ?
N2 C22 C27 119.4(9) . . ?
C24 C23 C22 116.8(11) . . ?
C24 C23 C31 118.5(11) . . ?
C22 C23 C31 124.6(11) . . ?
C23 C24 C25 124.9(12) . . ?
C26 C25 C24 115.4(12) . . ?
C27 C26 C25 125.8(12) . . ?
C26 C27 C22 114.8(10) . . ?
C26 C27 C28 123.9(11) . . ?
C22 C27 C28 121.0(11) . . ?
C27 C28 C29 110.9(12) . . ?
C27 C28 C30 111.8(12) . . ?
C29 C28 C30 108.1(11) . . ?
C23 C31 C32 113.5(12) . . ?
C23 C31 C33 113.2(11) . . ?
C32 C31 C33 110.5(11) . . ?
N4 C34 C39 124.5(10) . . ?
N4 C34 C35 118.5(10) . . ?
C39 C34 C35 117.0(10) . . ?
N5 C35 C36 123.1(11) . . ?
N5 C35 C34 116.6(10) . . ?
C36 C35 C34 120.3(10) . . ?
C35 C36 C37 118.6(11) . . ?
C38 C37 C36 123.4(11) . . ?
C37 C38 C39 116.6(11) . . ?
C38 C39 C34 124.0(11) . . ?
C48 C43 N4 120.9(11) . . ?
C48 C43 C44 120.2(10) . . ?
N4 C43 C44 118.7(10) . . ?
C45 C44 C43 118.4(11) . . ?
C45 C44 C52 119.2(10) . . ?
C43 C44 C52 122.2(9) . . ?
C46 C45 C44 121.5(11) . . ?
C47 C46 C45 118.3(11) . . ?
C46 C47 C48 122.1(13) . . ?
C43 C48 C47 119.2(12) . . ?
C43 C48 C49 124.1(10) . . ?
C47 C48 C49 116.6(12) . . ?
C50 C49 C48 113.4(11) . . ?
C50 C49 C51 112.6(12) . . ?
C48 C49 C51 110.8(10) . . ?
C44 C52 C53 111.6(9) . . ?
C44 C52 C54 114.7(9) . . ?
C53 C52 C54 108.2(10) . . ?
C56 C55 N5 120.8(10) . . ?
C56 C55 C60 119.2(11) . . ?
N5 C55 C60 120.0(11) . . ?
C57 C56 C55 119.8(12) . . ?
C57 C56 C64 118.9(12) . . ?
C55 C56 C64 121.3(11) . . ?
C56 C57 C58 121.7(13) . . ?
C59 C58 C57 118.9(12) . . ?
C58 C59 C60 122.5(12) . . ?
C59 C60 C55 117.8(11) . . ?
C59 C60 C61 120.0(11) . . ?
C55 C60 C61 122.1(11) . . ?
C60 C61 C62 115.2(11) . . ?
C60 C61 C63 108.0(12) . . ?
C62 C61 C63 109.8(13) . . ?
C66 C64 C56 113.4(13) . . ?
C66 C64 C65 111.6(13) . . ?
C56 C64 C65 112.4(11) . . ?
N5 Pb2 N4 76.5(3) . . ?
N5 Pb2 O2A 89.6(6) . . ?
N4 Pb2 O2A 97.0(6) . . ?
N5 Pb2 O2 92.0(5) . . ?
N4 Pb2 O2 88.7(6) . . ?
N6 O2 Pb2 120.0(13) . . ?
N6 O2A Pb2 125.8(14) . . ?
O2 N6 C42 116.6(19) . . ?
O2A N6 C41A 101.3(18) . . ?
O2A N6 C42A 113.3(18) . . ?
C41A N6 C42A 124(2) . . ?
O2 N6 C41 113.4(16) . . ?
C42 N6 C41 117(2) . . ?
O2 N6 C40 102.1(19) . . ?
C42 N6 C40 106(2) . . ?
C41 N6 C40 98(2) . . ?
O2A N6 C40A 111.6(19) . . ?
C41A N6 C40A 109(2) . . ?
C42A N6 C40A 98(2) . . ?

_refine_diff_density_max         1.741
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.178



