# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(2)-nov509

_audit_creation_date             2009-11-10T12:17:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C35 H55 N3 Pb'
_chemical_formula_sum            'C35 H55 N3 Pb'
_chemical_formula_weight         725.01
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.4524(1)
_cell_length_b                   20.3151(2)
_cell_length_c                   17.9079(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.358(1)
_cell_angle_gamma                90
_cell_volume                     3464.11(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    39067
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.103
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Plate
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.2761
_exptl_absorpt_correction_T_max  0.5351

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.663227E-1
_diffrn_orient_matrix_ub_12      0.86211E-2
_diffrn_orient_matrix_ub_13      0.351019E-1
_diffrn_orient_matrix_ub_21      -0.460947E-1
_diffrn_orient_matrix_ub_22      0.312583E-1
_diffrn_orient_matrix_ub_23      -0.42132E-1
_diffrn_orient_matrix_ub_31      -0.543424E-1
_diffrn_orient_matrix_ub_32      -0.370357E-1
_diffrn_orient_matrix_ub_33      -0.273886E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_number            53818
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_full        27.17
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             7664
_reflns_number_gt                6565
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 One of the iso-propyl substituents on the amide ligand is disordered and
 was refined with SADI restraints; the lower occupancy positions were left
 isotropic

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0217P)²+3.8769P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7664
_refine_ls_number_parameters     367
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0564
_refine_ls_wR_factor_gt          0.053
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.807
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.089

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.663105(11) 0.757701(5) 0.448612(6) 0.02197(4) Uani 1 1 d . A .
N1 N 0.8426(2) 0.67790(11) 0.51521(14) 0.0212(5) Uani 1 1 d . . .
N2 N 0.8559(2) 0.82571(11) 0.51787(14) 0.0205(5) Uani 1 1 d . . .
N3 N 0.5588(3) 0.76693(13) 0.53013(18) 0.0350(6) Uani 1 1 d D . .
C1 C 0.9558(3) 0.68610(14) 0.50171(18) 0.0239(6) Uani 1 1 d . . .
C2 C 1.0020(3) 0.74803(13) 0.48590(19) 0.0261(6) Uani 1 1 d . . .
H2 H 1.0669 0.7462 0.4613 0.031 Uiso 1 1 calc R . .
C3 C 0.9662(3) 0.81132(14) 0.50113(17) 0.0229(6) Uani 1 1 d . . .
C4 C 1.0488(3) 0.62813(15) 0.5044(2) 0.0350(8) Uani 1 1 d . . .
H4A H 1.023 0.5902 0.5291 0.053 Uiso 1 1 calc R . .
H4B H 1.1472 0.6397 0.5374 0.053 Uiso 1 1 calc R . .
H4C H 1.0364 0.617 0.4486 0.053 Uiso 1 1 calc R . .
C5 C 1.0604(3) 0.86653(15) 0.4973(2) 0.0315(7) Uani 1 1 d . . .
H5A H 1.0183 0.8876 0.4433 0.047 Uiso 1 1 calc R . .
H5B H 1.1527 0.8487 0.5062 0.047 Uiso 1 1 calc R . .
H5C H 1.0711 0.8991 0.5398 0.047 Uiso 1 1 calc R . .
C6 C 0.8053(3) 0.61484(13) 0.53606(18) 0.0231(6) Uani 1 1 d . . .
C7 C 0.8347(3) 0.60251(14) 0.61927(19) 0.0272(7) Uani 1 1 d . . .
C8 C 0.7938(4) 0.54229(15) 0.6388(2) 0.0364(8) Uani 1 1 d . . .
H8 H 0.8143 0.5326 0.6944 0.044 Uiso 1 1 calc R . .
C9 C 0.7240(4) 0.49609(16) 0.5793(2) 0.0440(9) Uani 1 1 d . . .
H9 H 0.6959 0.4555 0.5941 0.053 Uiso 1 1 calc R . .
C10 C 0.6955(4) 0.50894(16) 0.4988(2) 0.0388(8) Uani 1 1 d . . .
H10 H 0.6472 0.4769 0.4584 0.047 Uiso 1 1 calc R . .
C11 C 0.7356(3) 0.56808(14) 0.47507(19) 0.0286(7) Uani 1 1 d . . .
C12 C 0.9115(4) 0.65321(15) 0.68475(19) 0.0349(8) Uani 1 1 d . . .
H12 H 0.8721 0.6974 0.6624 0.042 Uiso 1 1 calc R . .
C13 C 1.0688(4) 0.6549(2) 0.7052(2) 0.0533(11) Uani 1 1 d . . .
H13A H 1.1145 0.6882 0.7474 0.08 Uiso 1 1 calc R . .
H13B H 1.0826 0.6659 0.6557 0.08 Uiso 1 1 calc R . .
H13C H 1.1099 0.6116 0.7254 0.08 Uiso 1 1 calc R . .
C14 C 0.8923(4) 0.64315(18) 0.7642(2) 0.0463(9) Uani 1 1 d . . .
H14A H 0.9435 0.6775 0.8036 0.069 Uiso 1 1 calc R . .
H14B H 0.9289 0.5998 0.7872 0.069 Uiso 1 1 calc R . .
H14C H 0.7923 0.6457 0.7526 0.069 Uiso 1 1 calc R . .
C15 C 0.7026(4) 0.57919(15) 0.38460(19) 0.0319(7) Uani 1 1 d . . .
H15 H 0.7453 0.6221 0.3795 0.038 Uiso 1 1 calc R . .
C16 C 0.5449(4) 0.5833(2) 0.3334(2) 0.0480(9) Uani 1 1 d . . .
H16A H 0.5268 0.5906 0.2758 0.072 Uiso 1 1 calc R . .
H16B H 0.5059 0.6199 0.353 0.072 Uiso 1 1 calc R . .
H16C H 0.5006 0.542 0.3385 0.072 Uiso 1 1 calc R . .
C17 C 0.7661(5) 0.52471(17) 0.3508(2) 0.0485(10) Uani 1 1 d . . .
H17A H 0.8676 0.5224 0.3838 0.073 Uiso 1 1 calc R . .
H17B H 0.7481 0.5346 0.2938 0.073 Uiso 1 1 calc R . .
H17C H 0.7231 0.4824 0.3533 0.073 Uiso 1 1 calc R . .
C18 C 0.8444(3) 0.88940(13) 0.54857(18) 0.0220(6) Uani 1 1 d . . .
C19 C 0.9087(3) 0.90044(14) 0.63392(18) 0.0256(6) Uani 1 1 d . . .
C20 C 0.8903(4) 0.96160(15) 0.6633(2) 0.0328(7) Uani 1 1 d . . .
H20 H 0.9357 0.9704 0.7204 0.039 Uiso 1 1 calc R . .
C21 C 0.8079(4) 1.00963(15) 0.6115(2) 0.0342(8) Uani 1 1 d . . .
H21 H 0.7945 1.0505 0.6331 0.041 Uiso 1 1 calc R . .
C22 C 0.7451(3) 0.99831(14) 0.5286(2) 0.0312(7) Uani 1 1 d . . .
H22 H 0.6887 1.0318 0.4932 0.037 Uiso 1 1 calc R . .
C23 C 0.7623(3) 0.93865(13) 0.49539(18) 0.0245(6) Uani 1 1 d . . .
C24 C 0.9982(3) 0.84829(15) 0.69324(18) 0.0305(7) Uani 1 1 d . . .
H24 H 0.9718 0.8048 0.6649 0.037 Uiso 1 1 calc R . .
C25 C 1.1551(4) 0.8584(2) 0.7173(2) 0.0500(10) Uani 1 1 d . . .
H25A H 1.2082 0.8235 0.7552 0.075 Uiso 1 1 calc R . .
H25B H 1.1838 0.9013 0.744 0.075 Uiso 1 1 calc R . .
H25C H 1.174 0.8568 0.6681 0.075 Uiso 1 1 calc R . .
C26 C 0.9718(4) 0.8444(2) 0.7712(2) 0.0478(9) Uani 1 1 d . . .
H26A H 1.0313 0.81 0.8073 0.072 Uiso 1 1 calc R . .
H26B H 0.8728 0.8338 0.7565 0.072 Uiso 1 1 calc R . .
H26C H 0.9942 0.8869 0.7996 0.072 Uiso 1 1 calc R . .
C27 C 0.6936(3) 0.92981(15) 0.40246(19) 0.0301(7) Uani 1 1 d . . .
H27 H 0.7246 0.8864 0.3894 0.036 Uiso 1 1 calc R . .
C28 C 0.7400(4) 0.98353(16) 0.3589(2) 0.0407(8) Uani 1 1 d . . .
H28A H 0.8427 0.9834 0.3796 0.061 Uiso 1 1 calc R . .
H28B H 0.7084 1.0265 0.3695 0.061 Uiso 1 1 calc R . .
H28C H 0.6988 0.975 0.2998 0.061 Uiso 1 1 calc R . .
C29 C 0.5344(4) 0.92873(19) 0.3699(2) 0.0471(9) Uani 1 1 d . . .
H29A H 0.4938 0.9229 0.3103 0.071 Uiso 1 1 calc R . .
H29B H 0.5015 0.9704 0.3834 0.071 Uiso 1 1 calc R . .
H29C H 0.5053 0.8922 0.3952 0.071 Uiso 1 1 calc R . .
C33 C 0.6132(3) 0.79830(17) 0.61037(19) 0.0342(7) Uani 1 1 d . A .
H33 H 0.7162 0.8048 0.6273 0.041 Uiso 1 1 calc R . .
C34 C 0.5499(4) 0.86642(18) 0.6080(3) 0.0521(10) Uani 1 1 d . . .
H34A H 0.5627 0.8933 0.5661 0.078 Uiso 1 1 calc R A .
H34B H 0.597 0.8876 0.6616 0.078 Uiso 1 1 calc R . .
H34C H 0.4494 0.8621 0.5946 0.078 Uiso 1 1 calc R . .
C35 C 0.5969(6) 0.7563(2) 0.6766(3) 0.0763(16) Uani 1 1 d . . .
H35A H 0.6383 0.7128 0.678 0.114 Uiso 1 1 calc R A .
H35B H 0.497 0.7515 0.6644 0.114 Uiso 1 1 calc R . .
H35C H 0.645 0.7778 0.73 0.114 Uiso 1 1 calc R . .
C30 C 0.4090(4) 0.7481(2) 0.4945(3) 0.0348(12) Uani 0.866(11) 1 d PD A 1
H30 H 0.3704 0.7605 0.5352 0.042 Uiso 0.866(11) 1 calc PR A 1
C31 C 0.3194(5) 0.7827(3) 0.4144(3) 0.0597(18) Uani 0.866(11) 1 d PD A 1
H31A H 0.3298 0.8304 0.4223 0.09 Uiso 0.866(11) 1 calc PR A 1
H31B H 0.2207 0.7705 0.3977 0.09 Uiso 0.866(11) 1 calc PR A 1
H31C H 0.3501 0.7693 0.3718 0.09 Uiso 0.866(11) 1 calc PR A 1
C32 C 0.3933(6) 0.6740(3) 0.4834(5) 0.075(3) Uani 0.866(11) 1 d PD A 1
H32A H 0.4515 0.6522 0.5352 0.112 Uiso 0.866(11) 1 calc PR A 1
H32B H 0.4237 0.6602 0.4408 0.112 Uiso 0.866(11) 1 calc PR A 1
H32C H 0.2948 0.6618 0.467 0.112 Uiso 0.866(11) 1 calc PR A 1
C30A C 0.436(2) 0.7291(12) 0.5240(19) 0.040(9) Uiso 0.134(11) 1 d PD A 2
H30A H 0.3937 0.7514 0.5583 0.047 Uiso 0.134(11) 1 calc PR A 2
C31A C 0.341(3) 0.7413(18) 0.4349(18) 0.047(9) Uiso 0.134(11) 1 d PD A 2
H31D H 0.331 0.7888 0.4246 0.07 Uiso 0.134(11) 1 calc PR A 2
H31E H 0.249 0.7217 0.422 0.07 Uiso 0.134(11) 1 calc PR A 2
H31F H 0.3829 0.7212 0.4003 0.07 Uiso 0.134(11) 1 calc PR A 2
C32A C 0.454(4) 0.6574(12) 0.547(2) 0.051(9) Uiso 0.134(11) 1 d PD A 2
H32D H 0.5118 0.653 0.6055 0.077 Uiso 0.134(11) 1 calc PR A 2
H32E H 0.501 0.6352 0.5161 0.077 Uiso 0.134(11) 1 calc PR A 2
H32F H 0.3622 0.6373 0.5329 0.077 Uiso 0.134(11) 1 calc PR A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N3 2.161(3) . ?
Pb N2 2.333(2) . ?
Pb N1 2.392(2) . ?
N1 C1 1.312(4) . ?
N1 C6 1.433(3) . ?
N2 C3 1.338(4) . ?
N2 C18 1.430(4) . ?
N3 C33 1.456(4) . ?
N3 C30A 1.461(17) . ?
N3 C30 1.477(4) . ?
C1 C2 1.417(4) . ?
C1 C4 1.515(4) . ?
C2 C3 1.397(4) . ?
C2 H2 0.95 . ?
C3 C5 1.513(4) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C11 1.403(4) . ?
C6 C7 1.414(4) . ?
C7 C8 1.387(4) . ?
C7 C12 1.518(4) . ?
C8 C9 1.381(5) . ?
C8 H8 0.95 . ?
C9 C10 1.370(5) . ?
C9 H9 0.95 . ?
C10 C11 1.396(4) . ?
C10 H10 0.95 . ?
C11 C15 1.528(4) . ?
C12 C13 1.530(5) . ?
C12 C14 1.530(5) . ?
C12 H12 1 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 C16 1.522(5) . ?
C15 C17 1.537(5) . ?
C15 H15 1 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 C23 1.404(4) . ?
C18 C19 1.411(4) . ?
C19 C20 1.393(4) . ?
C19 C24 1.519(4) . ?
C20 C21 1.377(5) . ?
C20 H20 0.95 . ?
C21 C22 1.372(5) . ?
C21 H21 0.95 . ?
C22 C23 1.394(4) . ?
C22 H22 0.95 . ?
C23 C27 1.527(4) . ?
C24 C25 1.528(5) . ?
C24 C26 1.533(5) . ?
C24 H24 1 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 C29 1.519(5) . ?
C27 C28 1.532(4) . ?
C27 H27 1 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C33 C34 1.527(5) . ?
C33 C35 1.527(5) . ?
C33 H33 1 . ?
C34 H34A 0.98 . ?
C34 H34B 0.98 . ?
C34 H34C 0.98 . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?
C30 C32 1.517(6) . ?
C30 C31 1.523(7) . ?
C30 H30 1 . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C31 H31C 0.98 . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C30A C32A 1.503(16) . ?
C30A C31A 1.511(16) . ?
C30A H30A 1 . ?
C31A H31D 0.98 . ?
C31A H31E 0.98 . ?
C31A H31F 0.98 . ?
C32A H32D 0.98 . ?
C32A H32E 0.98 . ?
C32A H32F 0.98 . ?

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
N3 Pb N2 98.93(9) . . ?
N3 Pb N1 103.44(10) . . ?
N2 Pb N1 78.97(8) . . ?
C1 N1 C6 121.6(2) . . ?
C1 N1 Pb 113.79(18) . . ?
C6 N1 Pb 119.62(18) . . ?
C3 N2 C18 120.0(2) . . ?
C3 N2 Pb 112.75(18) . . ?
C18 N2 Pb 123.32(18) . . ?
C33 N3 C30 116.9(3) . . ?
C33 N3 Pb 127.2(2) . . ?
C30A N3 Pb 125.2(13) . . ?
C30 N3 Pb 115.2(2) . . ?
N1 C1 C2 123.8(3) . . ?
N1 C1 C4 120.7(3) . . ?
C2 C1 C4 115.4(3) . . ?
C3 C2 C1 129.6(3) . . ?
C3 C2 H2 115.2 . . ?
C1 C2 H2 115.2 . . ?
N2 C3 C2 124.7(3) . . ?
N2 C3 C5 119.1(3) . . ?
C2 C3 C5 116.2(3) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 121.2(3) . . ?
C11 C6 N1 120.8(3) . . ?
C7 C6 N1 118.0(3) . . ?
C8 C7 C6 117.8(3) . . ?
C8 C7 C12 121.6(3) . . ?
C6 C7 C12 120.6(3) . . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C10 C9 C8 119.9(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 121.5(3) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C6 118.0(3) . . ?
C10 C11 C15 119.1(3) . . ?
C6 C11 C15 122.9(3) . . ?
C7 C12 C13 111.9(3) . . ?
C7 C12 C14 113.4(3) . . ?
C13 C12 C14 108.7(3) . . ?
C7 C12 H12 107.5 . . ?
C13 C12 H12 107.5 . . ?
C14 C12 H12 107.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C11 111.2(3) . . ?
C16 C15 C17 109.8(3) . . ?
C11 C15 C17 111.4(3) . . ?
C16 C15 H15 108.1 . . ?
C11 C15 H15 108.1 . . ?
C17 C15 H15 108.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 120.4(3) . . ?
C23 C18 N2 120.6(3) . . ?
C19 C18 N2 118.8(3) . . ?
C20 C19 C18 118.2(3) . . ?
C20 C19 C24 119.9(3) . . ?
C18 C19 C24 121.8(3) . . ?
C21 C20 C19 121.5(3) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C22 C21 C20 119.8(3) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 121.3(3) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
C22 C23 C18 118.7(3) . . ?
C22 C23 C27 118.8(3) . . ?
C18 C23 C27 122.5(3) . . ?
C19 C24 C25 112.6(3) . . ?
C19 C24 C26 112.5(3) . . ?
C25 C24 C26 109.0(3) . . ?
C19 C24 H24 107.5 . . ?
C25 C24 H24 107.5 . . ?
C26 C24 H24 107.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C27 C23 111.6(3) . . ?
C29 C27 C28 110.0(3) . . ?
C23 C27 C28 111.4(3) . . ?
C29 C27 H27 107.9 . . ?
C23 C27 H27 107.9 . . ?
C28 C27 H27 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C33 C34 112.4(3) . . ?
N3 C33 C35 113.5(3) . . ?
C34 C33 C35 110.0(3) . . ?
N3 C33 H33 106.8 . . ?
C34 C33 H33 106.8 . . ?
C35 C33 H33 106.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N3 C30 C32 110.6(4) . . ?
N3 C30 C31 114.7(4) . . ?
C32 C30 C31 110.1(4) . . ?
N3 C30 H30 107 . . ?
C32 C30 H30 107 . . ?
C31 C30 H30 107 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C30A C32A 119(2) . . ?
N3 C30A C31A 99.5(19) . . ?
C32A C30A C31A 113(2) . . ?
N3 C30A H30A 108.2 . . ?
C32A C30A H30A 108.2 . . ?
C31A C30A H30A 108.2 . . ?
C30A C31A H31D 109.5 . . ?
C30A C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
C30A C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C30A C32A H32D 109.5 . . ?
C30A C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
C30A C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 991973'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(3)-may511

_audit_creation_date             2011-05-20T08:08:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C35 H47 N3 Pb'
_chemical_formula_sum            'C35 H47 N3 Pb'
_chemical_formula_weight         716.95
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.3216(2)
_cell_length_b                   29.2568(6)
_cell_length_c                   9.2746(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.849(1)
_cell_angle_gamma                90
_cell_volume                     3246.21(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7536
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    5.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_absorpt_correction_T_min  0.5451
_exptl_absorpt_correction_T_max  0.7456

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0753425
_diffrn_orient_matrix_UB_21      -0.0806267
_diffrn_orient_matrix_UB_31      -0.0124910
_diffrn_orient_matrix_UB_12      -0.0240332
_diffrn_orient_matrix_UB_22      -0.0204154
_diffrn_orient_matrix_UB_32      -0.0131852
_diffrn_orient_matrix_UB_13      0.0308516
_diffrn_orient_matrix_UB_23      0.0131312
_diffrn_orient_matrix_UB_33      -0.0765660
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method       "φ & ω scans'"
_diffrn_detector_area_resol_mean 9.091
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_number            34216
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             7427
_reflns_number_gt                6527
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 The NH hydrogen atom was located and refined, all others are riding

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+3.8820P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7427
_refine_ls_number_parameters     358
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.025
_refine_ls_wR_factor_ref         0.053
_refine_ls_wR_factor_gt          0.0509
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.101

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.184318(8) 0.836645(4) 0.359620(11) 0.01344(4) Uani 1 1 d . . .
N1 N 0.29042(18) 0.89490(8) 0.4989(3) 0.0152(5) Uani 1 1 d . . .
N2 N 0.04507(18) 0.87157(8) 0.4570(2) 0.0131(5) Uani 1 1 d . . .
N3 N 0.2211(2) 0.78947(9) 0.5525(3) 0.0184(5) Uani 1 1 d . . .
H3N H 0.246(3) 0.8001(13) 0.627(4) 0.025(10) Uiso 1 1 d . . .
C1 C 0.2636(2) 0.92115(10) 0.6029(3) 0.0167(6) Uani 1 1 d . . .
C2 C 0.1581(2) 0.92298(10) 0.6347(3) 0.0173(6) Uani 1 1 d . . .
H2 H 0.1552 0.9404 0.7201 0.021 Uiso 1 1 calc R . .
C3 C 0.0552(2) 0.90311(10) 0.5604(3) 0.0159(6) Uani 1 1 d . . .
C4 C 0.3503(3) 0.95373(12) 0.6898(4) 0.0272(7) Uani 1 1 d . . .
H4C H 0.3675 0.9771 0.6228 0.041 Uiso 1 1 calc R . .
H4B H 0.4184 0.9367 0.7354 0.041 Uiso 1 1 calc R . .
H4A H 0.3211 0.9685 0.7676 0.041 Uiso 1 1 calc R . .
C5 C -0.0460(2) 0.92179(12) 0.6068(3) 0.0240(7) Uani 1 1 d . . .
H5C H -0.0443 0.9117 0.708 0.036 Uiso 1 1 calc R . .
H5B H -0.1142 0.9105 0.5387 0.036 Uiso 1 1 calc R . .
H5A H -0.0448 0.9553 0.6037 0.036 Uiso 1 1 calc R . .
C6 C 0.3912(2) 0.90475(10) 0.4503(3) 0.0159(6) Uani 1 1 d . . .
C7 C 0.4900(2) 0.88018(11) 0.5088(3) 0.0196(6) Uani 1 1 d . . .
C8 C 0.5825(2) 0.88852(11) 0.4480(4) 0.0249(7) Uani 1 1 d . . .
H8 H 0.6503 0.8725 0.4863 0.03 Uiso 1 1 calc R . .
C9 C 0.5767(3) 0.91927(12) 0.3346(4) 0.0263(7) Uani 1 1 d . . .
H9 H 0.6396 0.9239 0.2939 0.032 Uiso 1 1 calc R . .
C10 C 0.4792(3) 0.94341(11) 0.2797(3) 0.0232(7) Uani 1 1 d . . .
H10 H 0.4758 0.9648 0.2015 0.028 Uiso 1 1 calc R . .
C11 C 0.3854(2) 0.93687(11) 0.3375(3) 0.0183(6) Uani 1 1 d . . .
C12 C 0.5007(2) 0.84473(12) 0.6314(4) 0.0246(7) Uani 1 1 d . . .
H12 H 0.4259 0.8415 0.6546 0.03 Uiso 1 1 calc R . .
C13 C 0.5849(3) 0.85960(15) 0.7747(4) 0.0391(9) Uani 1 1 d . . .
H13C H 0.6588 0.8636 0.7544 0.059 Uiso 1 1 calc R . .
H13B H 0.589 0.8361 0.8511 0.059 Uiso 1 1 calc R . .
H13A H 0.5605 0.8886 0.8097 0.059 Uiso 1 1 calc R . .
C14 C 0.5337(3) 0.79807(13) 0.5815(4) 0.0337(8) Uani 1 1 d . . .
H14C H 0.4768 0.7878 0.4947 0.051 Uiso 1 1 calc R . .
H14B H 0.5395 0.776 0.6624 0.051 Uiso 1 1 calc R . .
H14A H 0.606 0.8005 0.5554 0.051 Uiso 1 1 calc R . .
C15 C 0.2804(3) 0.96548(12) 0.2762(4) 0.0256(7) Uani 1 1 d . . .
H15 H 0.2261 0.9589 0.3384 0.031 Uiso 1 1 calc R . .
C16 C 0.2243(3) 0.95296(14) 0.1172(4) 0.0413(9) Uani 1 1 d . . .
H16C H 0.2764 0.9582 0.0539 0.062 Uiso 1 1 calc R . .
H16B H 0.1576 0.9719 0.0825 0.062 Uiso 1 1 calc R . .
H16A H 0.2028 0.9206 0.1123 0.062 Uiso 1 1 calc R . .
C17 C 0.3057(3) 1.01686(14) 0.2875(5) 0.0454(10) Uani 1 1 d . . .
H17C H 0.3557 1.0246 0.2233 0.068 Uiso 1 1 calc R . .
H17B H 0.3419 1.0247 0.3906 0.068 Uiso 1 1 calc R . .
H17A H 0.2359 1.0341 0.2559 0.068 Uiso 1 1 calc R . .
C18 C -0.0629(2) 0.85415(10) 0.3822(3) 0.0134(6) Uani 1 1 d . . .
C19 C -0.1116(2) 0.81799(11) 0.4450(3) 0.0168(6) Uani 1 1 d . . .
C20 C -0.2134(2) 0.80027(11) 0.3635(3) 0.0213(7) Uani 1 1 d . . .
H20 H -0.2472 0.7757 0.4035 0.026 Uiso 1 1 calc R . .
C21 C -0.2660(2) 0.81789(12) 0.2258(3) 0.0213(7) Uani 1 1 d . . .
H21 H -0.3358 0.8057 0.173 0.026 Uiso 1 1 calc R . .
C22 C -0.2170(2) 0.85302(12) 0.1656(3) 0.0216(7) Uani 1 1 d . . .
H22 H -0.2536 0.8648 0.071 0.026 Uiso 1 1 calc R . .
C23 C -0.1148(2) 0.87179(10) 0.2403(3) 0.0166(6) Uani 1 1 d . . .
C24 C -0.0590(2) 0.79881(11) 0.5988(3) 0.0186(6) Uani 1 1 d . . .
H24 H 0.0143 0.8145 0.6373 0.022 Uiso 1 1 calc R . .
C25 C -0.0371(3) 0.74762(11) 0.5956(3) 0.0241(7) Uani 1 1 d . . .
H25C H -0.1078 0.7315 0.557 0.036 Uiso 1 1 calc R . .
H25B H -0.0032 0.7369 0.6965 0.036 Uiso 1 1 calc R . .
H25A H 0.0139 0.7415 0.5315 0.036 Uiso 1 1 calc R . .
C26 C -0.1340(3) 0.80907(12) 0.7059(4) 0.0275(7) Uani 1 1 d . . .
H26C H -0.1433 0.8422 0.7129 0.041 Uiso 1 1 calc R . .
H26B H -0.0991 0.7968 0.8044 0.041 Uiso 1 1 calc R . .
H26A H -0.2073 0.7948 0.6687 0.041 Uiso 1 1 calc R . .
C27 C -0.0633(3) 0.91140(11) 0.1733(3) 0.0220(7) Uani 1 1 d . . .
H27 H 0.0161 0.9145 0.2307 0.026 Uiso 1 1 calc R . .
C28 C -0.1229(4) 0.95636(13) 0.1888(5) 0.0474(11) Uani 1 1 d . . .
H28C H -0.202 0.9539 0.137 0.071 Uiso 1 1 calc R . .
H28B H -0.0883 0.9812 0.145 0.071 Uiso 1 1 calc R . .
H28A H -0.1168 0.9628 0.2941 0.071 Uiso 1 1 calc R . .
C29 C -0.0625(3) 0.90286(14) 0.0112(4) 0.0359(9) Uani 1 1 d . . .
H29C H -0.0189 0.8753 0.0041 0.054 Uiso 1 1 calc R . .
H29B H -0.0288 0.9291 -0.0273 0.054 Uiso 1 1 calc R . .
H29A H -0.1394 0.8987 -0.0474 0.054 Uiso 1 1 calc R . .
C30 C 0.2615(2) 0.74568(11) 0.5503(3) 0.0179(6) Uani 1 1 d . . .
C31 C 0.3480(2) 0.72788(12) 0.6656(4) 0.0256(7) Uani 1 1 d . . .
H31 H 0.3778 0.7461 0.7506 0.031 Uiso 1 1 calc R . .
C32 C 0.3898(3) 0.68433(13) 0.6569(4) 0.0333(9) Uani 1 1 d . . .
H32 H 0.4493 0.6736 0.7345 0.04 Uiso 1 1 calc R . .
C33 C 0.3467(3) 0.65631(13) 0.5375(5) 0.0414(10) Uani 1 1 d . . .
H33 H 0.3766 0.6266 0.5316 0.05 Uiso 1 1 calc R . .
C34 C 0.2588(4) 0.67227(13) 0.4262(4) 0.0379(9) Uani 1 1 d . . .
H34 H 0.2268 0.6529 0.3448 0.045 Uiso 1 1 calc R . .
C35 C 0.2169(3) 0.71599(12) 0.4321(3) 0.0261(7) Uani 1 1 d . . .
H35 H 0.1567 0.7261 0.3543 0.031 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N3 2.219(3) . ?
Pb N1 2.340(2) . ?
Pb N2 2.355(2) . ?
N1 C1 1.335(4) . ?
N1 C6 1.447(3) . ?
N2 C3 1.315(4) . ?
N2 C18 1.439(3) . ?
N3 C30 1.376(4) . ?
N3 H3N 0.75(3) . ?
C1 C2 1.401(4) . ?
C1 C4 1.513(4) . ?
C2 C3 1.414(4) . ?
C2 H2 0.95 . ?
C3 C5 1.515(4) . ?
C4 H4C 0.98 . ?
C4 H4B 0.98 . ?
C4 H4A 0.98 . ?
C5 H5C 0.98 . ?
C5 H5B 0.98 . ?
C5 H5A 0.98 . ?
C6 C11 1.396(4) . ?
C6 C7 1.406(4) . ?
C7 C8 1.408(4) . ?
C7 C12 1.521(4) . ?
C8 C9 1.373(5) . ?
C8 H8 0.95 . ?
C9 C10 1.381(5) . ?
C9 H9 0.95 . ?
C10 C11 1.398(4) . ?
C10 H10 0.95 . ?
C11 C15 1.532(4) . ?
C12 C14 1.528(5) . ?
C12 C13 1.540(5) . ?
C12 H12 1 . ?
C13 H13C 0.98 . ?
C13 H13B 0.98 . ?
C13 H13A 0.98 . ?
C14 H14C 0.98 . ?
C14 H14B 0.98 . ?
C14 H14A 0.98 . ?
C15 C16 1.516(5) . ?
C15 C17 1.534(5) . ?
C15 H15 1 . ?
C16 H16C 0.98 . ?
C16 H16B 0.98 . ?
C16 H16A 0.98 . ?
C17 H17C 0.98 . ?
C17 H17B 0.98 . ?
C17 H17A 0.98 . ?
C18 C19 1.409(4) . ?
C18 C23 1.415(4) . ?
C19 C20 1.400(4) . ?
C19 C24 1.525(4) . ?
C20 C21 1.386(4) . ?
C20 H20 0.95 . ?
C21 C22 1.376(5) . ?
C21 H21 0.95 . ?
C22 C23 1.396(4) . ?
C22 H22 0.95 . ?
C23 C27 1.524(4) . ?
C24 C25 1.523(4) . ?
C24 C26 1.540(4) . ?
C24 H24 1 . ?
C25 H25C 0.98 . ?
C25 H25B 0.98 . ?
C25 H25A 0.98 . ?
C26 H26C 0.98 . ?
C26 H26B 0.98 . ?
C26 H26A 0.98 . ?
C27 C29 1.527(4) . ?
C27 C28 1.530(5) . ?
C27 H27 1 . ?
C28 H28C 0.98 . ?
C28 H28B 0.98 . ?
C28 H28A 0.98 . ?
C29 H29C 0.98 . ?
C29 H29B 0.98 . ?
C29 H29A 0.98 . ?
C30 C35 1.404(4) . ?
C30 C31 1.416(4) . ?
C31 C32 1.384(5) . ?
C31 H31 0.95 . ?
C32 C33 1.378(6) . ?
C32 H32 0.95 . ?
C33 C34 1.386(6) . ?
C33 H33 0.95 . ?
C34 C35 1.385(5) . ?
C34 H34 0.95 . ?
C35 H35 0.95 . ?

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
N3 Pb N1 91.64(9) . . ?
N3 Pb N2 89.31(9) . . ?
N1 Pb N2 80.46(8) . . ?
C1 N1 C6 119.3(2) . . ?
C1 N1 Pb 127.99(18) . . ?
C6 N1 Pb 112.38(17) . . ?
C3 N2 C18 121.0(2) . . ?
C3 N2 Pb 129.29(18) . . ?
C18 N2 Pb 109.64(16) . . ?
C30 N3 Pb 124.9(2) . . ?
C30 N3 H3N 109(3) . . ?
Pb N3 H3N 116(3) . . ?
N1 C1 C2 125.2(3) . . ?
N1 C1 C4 118.8(3) . . ?
C2 C1 C4 115.9(3) . . ?
C1 C2 C3 130.5(3) . . ?
C1 C2 H2 114.7 . . ?
C3 C2 H2 114.7 . . ?
N2 C3 C2 124.2(3) . . ?
N2 C3 C5 121.3(3) . . ?
C2 C3 C5 114.6(3) . . ?
C1 C4 H4C 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4C C4 H4B 109.5 . . ?
C1 C4 H4A 109.5 . . ?
H4C C4 H4A 109.5 . . ?
H4B C4 H4A 109.5 . . ?
C3 C5 H5C 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5C C5 H5B 109.5 . . ?
C3 C5 H5A 109.5 . . ?
H5C C5 H5A 109.5 . . ?
H5B C5 H5A 109.5 . . ?
C11 C6 C7 121.1(3) . . ?
C11 C6 N1 118.3(2) . . ?
C7 C6 N1 120.4(3) . . ?
C6 C7 C8 117.8(3) . . ?
C6 C7 C12 123.3(3) . . ?
C8 C7 C12 118.9(3) . . ?
C9 C8 C7 121.4(3) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 119.9(3) . . ?
C8 C9 H9 120 . . ?
C10 C9 H9 120 . . ?
C9 C10 C11 120.9(3) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C6 C11 C10 118.8(3) . . ?
C6 C11 C15 122.2(3) . . ?
C10 C11 C15 119.0(3) . . ?
C7 C12 C14 111.4(3) . . ?
C7 C12 C13 111.9(3) . . ?
C14 C12 C13 109.9(3) . . ?
C7 C12 H12 107.8 . . ?
C14 C12 H12 107.8 . . ?
C13 C12 H12 107.8 . . ?
C12 C13 H13C 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13C C13 H13B 109.5 . . ?
C12 C13 H13A 109.5 . . ?
H13C C13 H13A 109.5 . . ?
H13B C13 H13A 109.5 . . ?
C12 C14 H14C 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
C12 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
H14B C14 H14A 109.5 . . ?
C16 C15 C11 112.1(3) . . ?
C16 C15 C17 109.9(3) . . ?
C11 C15 C17 111.7(3) . . ?
C16 C15 H15 107.6 . . ?
C11 C15 H15 107.6 . . ?
C17 C15 H15 107.6 . . ?
C15 C16 H16C 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16C C16 H16B 109.5 . . ?
C15 C16 H16A 109.5 . . ?
H16C C16 H16A 109.5 . . ?
H16B C16 H16A 109.5 . . ?
C15 C17 H17C 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17C C17 H17B 109.5 . . ?
C15 C17 H17A 109.5 . . ?
H17C C17 H17A 109.5 . . ?
H17B C17 H17A 109.5 . . ?
C19 C18 C23 121.1(3) . . ?
C19 C18 N2 120.2(2) . . ?
C23 C18 N2 118.6(3) . . ?
C20 C19 C18 118.0(3) . . ?
C20 C19 C24 119.6(3) . . ?
C18 C19 C24 122.4(2) . . ?
C21 C20 C19 121.4(3) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C22 C21 C20 119.9(3) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 121.6(3) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C22 C23 C18 118.1(3) . . ?
C22 C23 C27 120.7(3) . . ?
C18 C23 C27 121.1(3) . . ?
C25 C24 C19 112.4(3) . . ?
C25 C24 C26 109.9(3) . . ?
C19 C24 C26 110.2(2) . . ?
C25 C24 H24 108 . . ?
C19 C24 H24 108 . . ?
C26 C24 H24 108 . . ?
C24 C25 H25C 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25C C25 H25B 109.5 . . ?
C24 C25 H25A 109.5 . . ?
H25C C25 H25A 109.5 . . ?
H25B C25 H25A 109.5 . . ?
C24 C26 H26C 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26C C26 H26B 109.5 . . ?
C24 C26 H26A 109.5 . . ?
H26C C26 H26A 109.5 . . ?
H26B C26 H26A 109.5 . . ?
C23 C27 C29 112.3(3) . . ?
C23 C27 C28 111.1(3) . . ?
C29 C27 C28 110.4(3) . . ?
C23 C27 H27 107.6 . . ?
C29 C27 H27 107.6 . . ?
C28 C27 H27 107.6 . . ?
C27 C28 H28C 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28C C28 H28B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
H28C C28 H28A 109.5 . . ?
H28B C28 H28A 109.5 . . ?
C27 C29 H29C 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29C C29 H29B 109.5 . . ?
C27 C29 H29A 109.5 . . ?
H29C C29 H29A 109.5 . . ?
H29B C29 H29A 109.5 . . ?
N3 C30 C35 120.8(3) . . ?
N3 C30 C31 122.7(3) . . ?
C35 C30 C31 116.5(3) . . ?
C32 C31 C30 121.2(3) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C33 C32 C31 121.2(3) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C32 C33 C34 118.7(3) . . ?
C32 C33 H33 120.6 . . ?
C34 C33 H33 120.6 . . ?
C35 C34 C33 120.9(4) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C30 121.5(3) . . ?
C34 C35 H35 119.3 . . ?
C30 C35 H35 119.3 . . ?
_database_code_depnum_ccdc_archive 'CCDC 991974'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(4)-aug111

_audit_creation_date             2011-08-08T09:11:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38 H53 N3 Pb1'
_chemical_formula_sum            'C38 H53 N3 Pb'
_chemical_formula_weight         759.02
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   27.135(1)
_cell_length_b                   9.337(1)
_cell_length_c                   34.163(4)
_cell_angle_alpha                90
_cell_angle_beta                 123.535(6)
_cell_angle_gamma                90
_cell_volume                     7214.8(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    14175
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      26.733
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3072
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.5484
_exptl_absorpt_correction_T_max  0.6242

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_number            92098
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_full        26.71
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             15257
_reflns_number_gt                10974
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Two of the iso-propyl groups on molecule Pb 1 are disordered and were refined
 with SADI restraints.
 The hydrogen atoms on N3 and N6 were located and refined; all other were
 placed in calculated positions
 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0203P)²+16.3893P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         15257
_refine_ls_number_parameters     816
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.047
_refine_ls_wR_factor_ref         0.0865
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.715
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.141

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.434559(9) -0.08422(2) 0.301679(7) 0.02715(6) Uani 1 1 d . . .
Pb2 Pb 0.086390(9) 0.61496(2) 0.381967(8) 0.02793(7) Uani 1 1 d . . .
N1 N 0.34517(18) 0.0241(4) 0.27725(15) 0.0239(10) Uani 1 1 d . . .
N2 N 0.44961(19) -0.0438(5) 0.37535(15) 0.0275(11) Uani 1 1 d . . .
N3 N 0.4617(2) 0.1369(6) 0.30022(19) 0.0344(13) Uani 1 1 d . . .
H3N H 0.450(3) 0.180(6) 0.310(2) 0.03(2) Uiso 1 1 d . . .
N4 N 0.10640(19) 0.5721(4) 0.45638(15) 0.0263(10) Uani 1 1 d . . .
N5 N -0.00298(18) 0.5159(5) 0.35993(15) 0.0274(11) Uani 1 1 d . . .
N6 N 0.1113(2) 0.3948(6) 0.37731(19) 0.0318(12) Uani 1 1 d . . .
H6N H 0.102(3) 0.346(7) 0.389(2) 0.04(2) Uiso 1 1 d . . .
C1 C 0.3378(2) 0.1213(6) 0.3020(2) 0.0277(13) Uani 1 1 d . . .
C2 C 0.3800(2) 0.1513(6) 0.3496(2) 0.0338(14) Uani 1 1 d . . .
H2 H 0.375 0.241 0.3601 0.041 Uiso 1 1 calc R . .
C3 C 0.4283(2) 0.0701(6) 0.38408(19) 0.0295(13) Uani 1 1 d . . .
C4 C 0.2808(2) 0.2068(7) 0.2786(2) 0.0406(16) Uani 1 1 d . . .
H4C H 0.2471 0.1424 0.2601 0.061 Uiso 1 1 calc R . .
H4B H 0.281 0.2792 0.2579 0.061 Uiso 1 1 calc R . .
H4A H 0.2776 0.2542 0.3027 0.061 Uiso 1 1 calc R . .
C5 C 0.4556(3) 0.1188(7) 0.4346(2) 0.0525(19) Uani 1 1 d . . .
H5C H 0.4956 0.1553 0.4473 0.079 Uiso 1 1 calc R . .
H5B H 0.4576 0.0376 0.4536 0.079 Uiso 1 1 calc R . .
H5A H 0.4313 0.1948 0.4354 0.079 Uiso 1 1 calc R . .
C6 C 0.2987(2) -0.0092(6) 0.22969(19) 0.0261(13) Uani 1 1 d . A .
C7 C 0.2881(2) 0.0757(6) 0.1920(2) 0.0300(13) Uani 1 1 d . . .
C8 C 0.2460(3) 0.0285(7) 0.1465(2) 0.0384(15) Uani 1 1 d . . .
H8 H 0.2383 0.0847 0.1206 0.046 Uiso 1 1 calc R . .
C9 C 0.2154(3) -0.0973(7) 0.1384(2) 0.0401(16) Uani 1 1 d . . .
H9 H 0.187 -0.1274 0.1072 0.048 Uiso 1 1 calc R . .
C10 C 0.2260(2) -0.1791(6) 0.1758(2) 0.0375(15) Uani 1 1 d . A .
H10 H 0.2045 -0.2655 0.17 0.045 Uiso 1 1 calc R . .
C11 C 0.2675(2) -0.1381(6) 0.2220(2) 0.0283(13) Uani 1 1 d . . .
C12 C 0.3210(3) 0.2154(6) 0.1982(2) 0.0388(15) Uani 1 1 d . . .
H12 H 0.344 0.2408 0.2323 0.047 Uiso 1 1 calc R . .
C13 C 0.2779(3) 0.3388(7) 0.1709(2) 0.0523(19) Uani 1 1 d . . .
H13C H 0.2537 0.3152 0.1374 0.078 Uiso 1 1 calc R . .
H13B H 0.3003 0.4267 0.1756 0.078 Uiso 1 1 calc R . .
H13A H 0.2522 0.3533 0.1824 0.078 Uiso 1 1 calc R . .
C14 C 0.3646(3) 0.2008(7) 0.1836(2) 0.0488(18) Uani 1 1 d . . .
H14C H 0.394 0.1275 0.2029 0.073 Uiso 1 1 calc R . .
H14B H 0.3844 0.2927 0.1879 0.073 Uiso 1 1 calc R . .
H14A H 0.3433 0.1727 0.1504 0.073 Uiso 1 1 calc R . .
C18 C 0.4919(3) -0.1350(6) 0.41333(19) 0.0297(13) Uani 1 1 d . . .
C19 C 0.5526(2) -0.1157(6) 0.43451(19) 0.0323(14) Uani 1 1 d . . .
C20 C 0.5915(3) -0.2068(7) 0.4707(2) 0.0440(17) Uani 1 1 d . . .
H20 H 0.6329 -0.1948 0.4854 0.053 Uiso 1 1 calc R . .
C21 C 0.5708(3) -0.3141(7) 0.4854(2) 0.0496(18) Uani 1 1 d . . .
H21 H 0.5978 -0.3742 0.5108 0.059 Uiso 1 1 calc R . .
C22 C 0.5112(3) -0.3347(7) 0.4635(2) 0.0485(18) Uani 1 1 d . . .
H22 H 0.4974 -0.4106 0.4736 0.058 Uiso 1 1 calc R . .
C23 C 0.4707(3) -0.2479(7) 0.4273(2) 0.0379(15) Uani 1 1 d . . .
C24 C 0.5774(2) -0.0010(6) 0.4186(2) 0.0362(15) Uani 1 1 d . . .
H24 H 0.5434 0.0558 0.3932 0.043 Uiso 1 1 calc R . .
C25 C 0.6185(3) 0.1027(8) 0.4586(2) 0.061(2) Uani 1 1 d . . .
H25C H 0.5963 0.15 0.4699 0.092 Uiso 1 1 calc R . .
H25B H 0.6336 0.175 0.4471 0.092 Uiso 1 1 calc R . .
H25A H 0.6516 0.0492 0.4845 0.092 Uiso 1 1 calc R . .
C26 C 0.6100(3) -0.0675(8) 0.3978(2) 0.0516(18) Uani 1 1 d . . .
H26C H 0.6425 -0.1276 0.4216 0.077 Uiso 1 1 calc R . .
H26B H 0.6259 0.0088 0.3882 0.077 Uiso 1 1 calc R . .
H26A H 0.5824 -0.1262 0.3705 0.077 Uiso 1 1 calc R . .
C27 C 0.4052(3) -0.2779(7) 0.4039(2) 0.0502(18) Uani 1 1 d . . .
H27 H 0.3831 -0.2171 0.3751 0.06 Uiso 1 1 calc R . .
C28 C 0.3826(4) -0.2397(10) 0.4351(3) 0.099(3) Uani 1 1 d . . .
H28C H 0.3398 -0.2542 0.4174 0.149 Uiso 1 1 calc R . .
H28B H 0.3918 -0.1393 0.4448 0.149 Uiso 1 1 calc R . .
H28A H 0.402 -0.3013 0.4629 0.149 Uiso 1 1 calc R . .
C29 C 0.3896(4) -0.4317(9) 0.3888(4) 0.095(3) Uani 1 1 d . . .
H29C H 0.4006 -0.4554 0.3666 0.142 Uiso 1 1 calc R . .
H29B H 0.347 -0.4457 0.3737 0.142 Uiso 1 1 calc R . .
H29A H 0.4112 -0.4942 0.4164 0.142 Uiso 1 1 calc R . .
C30 C 0.5141(2) 0.1805(6) 0.3060(2) 0.0318(14) Uani 1 1 d . B .
C31 C 0.5382(3) 0.0976(7) 0.2860(2) 0.0446(17) Uani 1 1 d . . .
H31 H 0.5179 0.0144 0.2683 0.054 Uiso 1 1 calc R . .
C32 C 0.5908(3) 0.1362(8) 0.2917(3) 0.053(2) Uani 1 1 d . . .
H32 H 0.6065 0.0785 0.2782 0.064 Uiso 1 1 calc R . .
C33 C 0.6211(3) 0.2570(8) 0.3167(3) 0.055(2) Uani 1 1 d . . .
H33 H 0.6576 0.2825 0.3209 0.066 Uiso 1 1 calc R . .
C34 C 0.5969(3) 0.3394(7) 0.3352(2) 0.0453(17) Uani 1 1 d . B .
H34 H 0.6172 0.4238 0.3519 0.054 Uiso 1 1 calc R . .
C35 C 0.5446(2) 0.3056(7) 0.3308(2) 0.0355(15) Uani 1 1 d . . .
C39 C 0.0846(2) 0.4589(6) 0.46531(19) 0.0295(13) Uani 1 1 d . . .
C40 C 0.0338(2) 0.3845(6) 0.4320(2) 0.0321(14) Uani 1 1 d . . .
H40 H 0.0276 0.2966 0.4426 0.039 Uiso 1 1 calc R . .
C41 C -0.0101(2) 0.4198(6) 0.3845(2) 0.0295(13) Uani 1 1 d . . .
C42 C 0.1145(3) 0.4057(7) 0.5154(2) 0.0454(17) Uani 1 1 d . . .
H42C H 0.1187 0.4851 0.5358 0.068 Uiso 1 1 calc R . .
H42B H 0.1537 0.3675 0.5262 0.068 Uiso 1 1 calc R . .
H42A H 0.0904 0.3299 0.5167 0.068 Uiso 1 1 calc R . .
C43 C -0.0684(2) 0.3429(7) 0.3632(2) 0.0407(16) Uani 1 1 d . . .
H43C H -0.0742 0.2785 0.3383 0.061 Uiso 1 1 calc R . .
H43B H -0.1006 0.413 0.3499 0.061 Uiso 1 1 calc R . .
H43A H -0.0682 0.287 0.3876 0.061 Uiso 1 1 calc R . .
C44 C 0.1523(2) 0.6579(6) 0.49432(18) 0.0276(13) Uani 1 1 d . . .
C45 C 0.2124(2) 0.6255(6) 0.51462(19) 0.0297(13) Uani 1 1 d . . .
C46 C 0.2534(3) 0.7124(7) 0.5513(2) 0.0376(15) Uani 1 1 d . . .
H46 H 0.2943 0.6912 0.5663 0.045 Uiso 1 1 calc R . .
C47 C 0.2375(3) 0.8280(7) 0.5671(2) 0.0414(16) Uani 1 1 d . . .
H47 H 0.2668 0.8833 0.5929 0.05 Uiso 1 1 calc R . .
C48 C 0.1790(3) 0.8622(6) 0.5451(2) 0.0375(15) Uani 1 1 d . . .
H48 H 0.1681 0.944 0.5551 0.045 Uiso 1 1 calc R . .
C49 C 0.1351(3) 0.7803(6) 0.5083(2) 0.0310(13) Uani 1 1 d . . .
C50 C 0.2320(3) 0.5043(7) 0.4972(2) 0.0409(16) Uani 1 1 d . . .
H50 H 0.1959 0.4552 0.4711 0.049 Uiso 1 1 calc R . .
C51 C 0.2671(3) 0.5636(8) 0.4778(2) 0.0528(19) Uani 1 1 d . . .
H51C H 0.2425 0.6316 0.4524 0.079 Uiso 1 1 calc R . .
H51B H 0.2786 0.4846 0.4655 0.079 Uiso 1 1 calc R . .
H51A H 0.3026 0.6125 0.5029 0.079 Uiso 1 1 calc R . .
C52 C 0.2697(3) 0.3925(7) 0.5358(2) 0.063(2) Uani 1 1 d . . .
H52C H 0.3054 0.4387 0.5618 0.094 Uiso 1 1 calc R . .
H52B H 0.2811 0.3158 0.5227 0.094 Uiso 1 1 calc R . .
H52A H 0.2467 0.3522 0.5473 0.094 Uiso 1 1 calc R . .
C53 C 0.0704(3) 0.8202(7) 0.4841(2) 0.0440(16) Uani 1 1 d . . .
H53 H 0.0491 0.7791 0.4517 0.053 Uiso 1 1 calc R . .
C54 C 0.0603(3) 0.9815(7) 0.4791(3) 0.064(2) Uani 1 1 d . . .
H54C H 0.0178 1.0014 0.4611 0.096 Uiso 1 1 calc R . .
H54B H 0.0774 1.0219 0.4626 0.096 Uiso 1 1 calc R . .
H54A H 0.0793 1.025 0.5103 0.096 Uiso 1 1 calc R . .
C55 C 0.0425(3) 0.7568(9) 0.5082(3) 0.083(3) Uani 1 1 d . . .
H55C H 0.0615 0.7973 0.5398 0.124 Uiso 1 1 calc R . .
H55B H 0.0478 0.6527 0.5104 0.124 Uiso 1 1 calc R . .
H55A H 0.0002 0.7795 0.4901 0.124 Uiso 1 1 calc R . .
C56 C -0.0512(2) 0.5548(6) 0.31332(19) 0.0267(13) Uani 1 1 d . . .
C57 C -0.0646(2) 0.4710(6) 0.2744(2) 0.0334(14) Uani 1 1 d . . .
C58 C -0.1098(3) 0.5201(7) 0.2300(2) 0.0387(15) Uani 1 1 d . . .
H58 H -0.1204 0.4643 0.2032 0.046 Uiso 1 1 calc R . .
C59 C -0.1391(3) 0.6453(7) 0.2239(2) 0.0436(17) Uani 1 1 d . . .
H59 H -0.1691 0.6762 0.1932 0.052 Uiso 1 1 calc R . .
C60 C -0.1253(3) 0.7268(7) 0.2623(2) 0.0429(16) Uani 1 1 d . . .
H60 H -0.146 0.8137 0.2578 0.051 Uiso 1 1 calc R . .
C61 C -0.0812(2) 0.6833(6) 0.3077(2) 0.0338(14) Uani 1 1 d . . .
C62 C -0.0330(3) 0.3321(6) 0.2784(2) 0.0381(15) Uani 1 1 d . . .
H62 H -0.0063 0.3079 0.3125 0.046 Uiso 1 1 calc R . .
C63 C -0.0765(3) 0.2070(7) 0.2539(2) 0.057(2) Uani 1 1 d . . .
H63C H -0.0987 0.1924 0.2685 0.085 Uiso 1 1 calc R . .
H63B H -0.0545 0.1197 0.2572 0.085 Uiso 1 1 calc R . .
H63A H -0.104 0.2293 0.2206 0.085 Uiso 1 1 calc R . .
C64 C 0.0053(3) 0.3476(7) 0.2586(2) 0.0542(19) Uani 1 1 d . . .
H64C H -0.0197 0.3733 0.2253 0.081 Uiso 1 1 calc R . .
H64B H 0.0254 0.2567 0.2621 0.081 Uiso 1 1 calc R . .
H64A H 0.0348 0.4229 0.2758 0.081 Uiso 1 1 calc R . .
C65 C -0.0674(3) 0.7735(7) 0.3495(2) 0.0456(17) Uani 1 1 d . . .
H65 H -0.0286 0.7394 0.3771 0.055 Uiso 1 1 calc R . .
C66 C -0.0608(5) 0.9288(8) 0.3438(3) 0.110(4) Uani 1 1 d . . .
H66C H -0.0986 0.967 0.3179 0.165 Uiso 1 1 calc R . .
H66B H -0.0305 0.9423 0.3371 0.165 Uiso 1 1 calc R . .
H66A H -0.0491 0.9793 0.3729 0.165 Uiso 1 1 calc R . .
C67 C -0.1128(5) 0.7512(12) 0.3614(4) 0.138(5) Uani 1 1 d . . .
H67C H -0.1003 0.8019 0.3906 0.207 Uiso 1 1 calc R . .
H67B H -0.1164 0.6487 0.3655 0.207 Uiso 1 1 calc R . .
H67A H -0.1511 0.7886 0.3359 0.207 Uiso 1 1 calc R . .
C68 C 0.1627(2) 0.3544(6) 0.38134(19) 0.0273(13) Uani 1 1 d . . .
C69 C 0.1853(3) 0.4413(6) 0.3612(2) 0.0349(14) Uani 1 1 d . . .
H69 H 0.1642 0.5247 0.3443 0.042 Uiso 1 1 calc R . .
C70 C 0.2377(3) 0.4082(7) 0.3654(2) 0.0433(16) Uani 1 1 d . . .
H70 H 0.2522 0.4693 0.3517 0.052 Uiso 1 1 calc R . .
C71 C 0.2691(3) 0.2868(7) 0.3893(2) 0.0426(16) Uani 1 1 d . . .
H71 H 0.3054 0.2649 0.3926 0.051 Uiso 1 1 calc R . .
C72 C 0.2469(3) 0.1978(7) 0.4084(2) 0.0388(15) Uani 1 1 d . . .
H72 H 0.2681 0.1136 0.4245 0.047 Uiso 1 1 calc R . .
C73 C 0.1942(2) 0.2281(6) 0.40462(19) 0.0317(14) Uani 1 1 d . . .
C74 C 0.1689(3) 0.1262(6) 0.4245(2) 0.0392(15) Uani 1 1 d . . .
H74 H 0.1555 0.1863 0.4412 0.047 Uiso 1 1 calc R . .
C75 C 0.1144(3) 0.0474(7) 0.3848(2) 0.0498(18) Uani 1 1 d . . .
H75C H 0.084 0.1173 0.3642 0.075 Uiso 1 1 calc R . .
H75B H 0.0988 -0.0166 0.3982 0.075 Uiso 1 1 calc R . .
H75A H 0.1255 -0.0089 0.3666 0.075 Uiso 1 1 calc R . .
C76 C 0.2136(3) 0.0175(8) 0.4601(3) 0.064(2) Uani 1 1 d . . .
H76C H 0.1952 -0.0382 0.4731 0.096 Uiso 1 1 calc R . .
H76B H 0.2482 0.0683 0.4856 0.096 Uiso 1 1 calc R . .
H76A H 0.226 -0.0472 0.4445 0.096 Uiso 1 1 calc R . .
C15 C 0.2774(11) -0.2288(18) 0.2632(12) 0.035(5) Uani 0.62 1 d PDU A 1
H15 H 0.3204 -0.224 0.2887 0.042 Uiso 0.62 1 calc PR A 1
C16 C 0.2432(7) -0.1674(16) 0.2828(6) 0.065(4) Uani 0.62 1 d PDU A 1
H16C H 0.2574 -0.0704 0.2947 0.098 Uiso 0.62 1 calc PR A 1
H16B H 0.2491 -0.2284 0.3084 0.098 Uiso 0.62 1 calc PR A 1
H16A H 0.201 -0.1638 0.2579 0.098 Uiso 0.62 1 calc PR A 1
C17 C 0.2619(8) -0.3856(18) 0.2491(6) 0.077(5) Uani 0.62 1 d PDU A 1
H17C H 0.2205 -0.393 0.2229 0.116 Uiso 0.62 1 calc PR A 1
H17B H 0.268 -0.4405 0.2759 0.116 Uiso 0.62 1 calc PR A 1
H17A H 0.2874 -0.424 0.2396 0.116 Uiso 0.62 1 calc PR A 1
C36 C 0.5193(3) 0.4031(7) 0.3513(2) 0.0511(18) Uani 0.64 1 d PD B 1
H36 H 0.5051 0.3361 0.366 0.061 Uiso 0.64 1 calc PR B 1
C37 C 0.4659(4) 0.4748(11) 0.3142(4) 0.048(3) Uani 0.64 1 d PD B 1
H37C H 0.4762 0.5432 0.2981 0.073 Uiso 0.64 1 calc PR B 1
H37B H 0.4473 0.5259 0.3279 0.073 Uiso 0.64 1 calc PR B 1
H37A H 0.4382 0.4036 0.2917 0.073 Uiso 0.64 1 calc PR B 1
C38 C 0.5659(5) 0.4899(13) 0.3911(4) 0.067(4) Uani 0.64 1 d PD B 1
H38C H 0.5979 0.4268 0.414 0.1 Uiso 0.64 1 calc PR B 1
H38B H 0.549 0.5405 0.4062 0.1 Uiso 0.64 1 calc PR B 1
H38A H 0.5818 0.5597 0.3794 0.1 Uiso 0.64 1 calc PR B 1
C15A C 0.2768(18) -0.230(3) 0.261(2) 0.040(8) Uani 0.38 1 d PDU A 2
H15A H 0.3091 -0.1847 0.291 0.048 Uiso 0.38 1 calc PR A 2
C16A C 0.2231(11) -0.240(3) 0.2647(10) 0.078(8) Uani 0.38 1 d PDU A 2
H16F H 0.1875 -0.2577 0.2335 0.117 Uiso 0.38 1 calc PR A 2
H16E H 0.2187 -0.15 0.2772 0.117 Uiso 0.38 1 calc PR A 2
H16D H 0.2287 -0.319 0.2857 0.117 Uiso 0.38 1 calc PR A 2
C17A C 0.2974(10) -0.382(3) 0.2608(10) 0.060(7) Uani 0.38 1 d PDU A 2
H17F H 0.2918 -0.4431 0.2813 0.09 Uiso 0.38 1 calc PR A 2
H17E H 0.3394 -0.3797 0.2722 0.09 Uiso 0.38 1 calc PR A 2
H17D H 0.2744 -0.4194 0.2287 0.09 Uiso 0.38 1 calc PR A 2
C36A C 0.5193(3) 0.4031(7) 0.3513(2) 0.0511(18) Uani 0.36 1 d PD B 2
H36A H 0.4755 0.3979 0.3282 0.061 Uiso 0.36 1 calc PR B 2
C37A C 0.5342(8) 0.5690(13) 0.3547(7) 0.045(5) Uani 0.36 1 d PD B 2
H37F H 0.508 0.6232 0.3607 0.067 Uiso 0.36 1 calc PR B 2
H37E H 0.5284 0.6011 0.3251 0.067 Uiso 0.36 1 calc PR B 2
H37D H 0.5754 0.5851 0.3805 0.067 Uiso 0.36 1 calc PR B 2
C38A C 0.5280(8) 0.3677(17) 0.3972(5) 0.044(5) Uani 0.36 1 d PD B 2
H38F H 0.5699 0.3778 0.4223 0.067 Uiso 0.36 1 calc PR B 2
H38E H 0.5153 0.2689 0.3965 0.067 Uiso 0.36 1 calc PR B 2
H38D H 0.5044 0.4331 0.403 0.067 Uiso 0.36 1 calc PR B 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N3 2.202(5) . ?
Pb1 N1 2.316(4) . ?
Pb1 N2 2.347(4) . ?
Pb2 N6 2.198(5) . ?
Pb2 N5 2.299(4) . ?
Pb2 N4 2.322(4) . ?
N1 C1 1.328(6) . ?
N1 C6 1.436(6) . ?
N2 C3 1.322(7) . ?
N2 C18 1.442(7) . ?
N3 C30 1.384(7) . ?
N3 H3N 0.71(6) . ?
N4 C39 1.326(7) . ?
N4 C44 1.445(7) . ?
N5 C41 1.313(7) . ?
N5 C56 1.441(6) . ?
N6 C68 1.374(7) . ?
N6 H6N 0.73(6) . ?
C1 C2 1.405(7) . ?
C1 C4 1.518(7) . ?
C2 C3 1.405(8) . ?
C2 H2 0.95 . ?
C3 C5 1.524(8) . ?
C4 H4C 0.98 . ?
C4 H4B 0.98 . ?
C4 H4A 0.98 . ?
C5 H5C 0.98 . ?
C5 H5B 0.98 . ?
C5 H5A 0.98 . ?
C6 C7 1.398(8) . ?
C6 C11 1.410(7) . ?
C7 C8 1.397(8) . ?
C7 C12 1.529(8) . ?
C8 C9 1.376(8) . ?
C8 H8 0.95 . ?
C9 C10 1.374(8) . ?
C9 H9 0.95 . ?
C10 C11 1.393(8) . ?
C10 H10 0.95 . ?
C11 C15A 1.49(5) . ?
C11 C15 1.53(3) . ?
C12 C14 1.523(8) . ?
C12 C13 1.536(8) . ?
C12 H12 1 . ?
C13 H13C 0.98 . ?
C13 H13B 0.98 . ?
C13 H13A 0.98 . ?
C14 H14C 0.98 . ?
C14 H14B 0.98 . ?
C14 H14A 0.98 . ?
C18 C19 1.397(8) . ?
C18 C23 1.405(8) . ?
C19 C20 1.387(8) . ?
C19 C24 1.517(8) . ?
C20 C21 1.374(9) . ?
C20 H20 0.95 . ?
C21 C22 1.369(9) . ?
C21 H21 0.95 . ?
C22 C23 1.376(8) . ?
C22 H22 0.95 . ?
C23 C27 1.519(9) . ?
C24 C26 1.537(8) . ?
C24 C25 1.539(8) . ?
C24 H24 1 . ?
C25 H25C 0.98 . ?
C25 H25B 0.98 . ?
C25 H25A 0.98 . ?
C26 H26C 0.98 . ?
C26 H26B 0.98 . ?
C26 H26A 0.98 . ?
C27 C29 1.506(10) . ?
C27 C28 1.533(10) . ?
C27 H27 1 . ?
C28 H28C 0.98 . ?
C28 H28B 0.98 . ?
C28 H28A 0.98 . ?
C29 H29C 0.98 . ?
C29 H29B 0.98 . ?
C29 H29A 0.98 . ?
C30 C31 1.409(8) . ?
C30 C35 1.411(8) . ?
C31 C32 1.378(9) . ?
C31 H31 0.95 . ?
C32 C33 1.379(10) . ?
C32 H32 0.95 . ?
C33 C34 1.373(10) . ?
C33 H33 0.95 . ?
C34 C35 1.380(8) . ?
C34 H34 0.95 . ?
C35 C36 1.524(9) . ?
C39 C40 1.395(7) . ?
C39 C42 1.518(8) . ?
C40 C41 1.424(7) . ?
C40 H40 0.95 . ?
C41 C43 1.508(7) . ?
C42 H42C 0.98 . ?
C42 H42B 0.98 . ?
C42 H42A 0.98 . ?
C43 H43C 0.98 . ?
C43 H43B 0.98 . ?
C43 H43A 0.98 . ?
C44 C45 1.408(7) . ?
C44 C49 1.415(7) . ?
C45 C46 1.389(8) . ?
C45 C50 1.505(8) . ?
C46 C47 1.378(8) . ?
C46 H46 0.95 . ?
C47 C48 1.368(8) . ?
C47 H47 0.95 . ?
C48 C49 1.388(8) . ?
C48 H48 0.95 . ?
C49 C53 1.517(8) . ?
C50 C51 1.536(9) . ?
C50 C52 1.543(8) . ?
C50 H50 1 . ?
C51 H51C 0.98 . ?
C51 H51B 0.98 . ?
C51 H51A 0.98 . ?
C52 H52C 0.98 . ?
C52 H52B 0.98 . ?
C52 H52A 0.98 . ?
C53 C55 1.512(9) . ?
C53 C54 1.524(9) . ?
C53 H53 1 . ?
C54 H54C 0.98 . ?
C54 H54B 0.98 . ?
C54 H54A 0.98 . ?
C55 H55C 0.98 . ?
C55 H55B 0.98 . ?
C55 H55A 0.98 . ?
C56 C61 1.402(8) . ?
C56 C57 1.406(8) . ?
C57 C58 1.401(8) . ?
C57 C62 1.519(8) . ?
C58 C59 1.363(8) . ?
C58 H58 0.95 . ?
C59 C60 1.377(9) . ?
C59 H59 0.95 . ?
C60 C61 1.397(8) . ?
C60 H60 0.95 . ?
C61 C65 1.517(8) . ?
C62 C64 1.527(8) . ?
C62 C63 1.538(8) . ?
C62 H62 1 . ?
C63 H63C 0.98 . ?
C63 H63B 0.98 . ?
C63 H63A 0.98 . ?
C64 H64C 0.98 . ?
C64 H64B 0.98 . ?
C64 H64A 0.98 . ?
C65 C66 1.486(10) . ?
C65 C67 1.510(11) . ?
C65 H65 1 . ?
C66 H66C 0.98 . ?
C66 H66B 0.98 . ?
C66 H66A 0.98 . ?
C67 H67C 0.98 . ?
C67 H67B 0.98 . ?
C67 H67A 0.98 . ?
C68 C69 1.407(8) . ?
C68 C73 1.415(8) . ?
C69 C70 1.382(8) . ?
C69 H69 0.95 . ?
C70 C71 1.382(9) . ?
C70 H70 0.95 . ?
C71 C72 1.384(8) . ?
C71 H71 0.95 . ?
C72 C73 1.392(8) . ?
C72 H72 0.95 . ?
C73 C74 1.533(8) . ?
C74 C76 1.534(8) . ?
C74 C75 1.535(8) . ?
C74 H74 1 . ?
C75 H75C 0.98 . ?
C75 H75B 0.98 . ?
C75 H75A 0.98 . ?
C76 H76C 0.98 . ?
C76 H76B 0.98 . ?
C76 H76A 0.98 . ?
C15 C17 1.526(13) . ?
C15 C16 1.526(13) . ?
C15 H15 1 . ?
C16 H16C 0.98 . ?
C16 H16B 0.98 . ?
C16 H16A 0.98 . ?
C17 H17C 0.98 . ?
C17 H17B 0.98 . ?
C17 H17A 0.98 . ?
C36 C37 1.458(9) . ?
C36 C38 1.486(10) . ?
C36 H36 1 . ?
C37 H37C 0.98 . ?
C37 H37B 0.98 . ?
C37 H37A 0.98 . ?
C38 H38C 0.98 . ?
C38 H38B 0.98 . ?
C38 H38A 0.98 . ?
C15A C17A 1.522(16) . ?
C15A C16A 1.527(15) . ?
C15A H15A 1 . ?
C16A H16F 0.98 . ?
C16A H16E 0.98 . ?
C16A H16D 0.98 . ?
C17A H17F 0.98 . ?
C17A H17E 0.98 . ?
C17A H17D 0.98 . ?
C37A H37F 0.98 . ?
C37A H37E 0.98 . ?
C37A H37D 0.98 . ?
C38A H38F 0.98 . ?
C38A H38E 0.98 . ?
C38A H38D 0.98 . ?

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
N3 Pb1 N1 83.08(17) . . ?
N3 Pb1 N2 90.66(18) . . ?
N1 Pb1 N2 81.00(15) . . ?
N6 Pb2 N5 84.91(18) . . ?
N6 Pb2 N4 91.32(18) . . ?
N5 Pb2 N4 81.69(15) . . ?
C1 N1 C6 121.4(4) . . ?
C1 N1 Pb1 124.4(4) . . ?
C6 N1 Pb1 113.8(3) . . ?
C3 N2 C18 120.1(5) . . ?
C3 N2 Pb1 122.2(4) . . ?
C18 N2 Pb1 116.8(3) . . ?
C30 N3 Pb1 127.1(4) . . ?
C30 N3 H3N 118(5) . . ?
Pb1 N3 H3N 106(5) . . ?
C39 N4 C44 120.5(5) . . ?
C39 N4 Pb2 121.7(4) . . ?
C44 N4 Pb2 116.8(3) . . ?
C41 N5 C56 120.9(4) . . ?
C41 N5 Pb2 124.5(4) . . ?
C56 N5 Pb2 114.2(3) . . ?
C68 N6 Pb2 125.8(4) . . ?
C68 N6 H6N 114(5) . . ?
Pb2 N6 H6N 109(5) . . ?
N1 C1 C2 124.0(5) . . ?
N1 C1 C4 119.5(5) . . ?
C2 C1 C4 116.5(5) . . ?
C1 C2 C3 130.5(5) . . ?
C1 C2 H2 114.8 . . ?
C3 C2 H2 114.8 . . ?
N2 C3 C2 124.5(5) . . ?
N2 C3 C5 119.7(5) . . ?
C2 C3 C5 115.8(5) . . ?
C1 C4 H4C 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4C C4 H4B 109.5 . . ?
C1 C4 H4A 109.5 . . ?
H4C C4 H4A 109.5 . . ?
H4B C4 H4A 109.5 . . ?
C3 C5 H5C 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5C C5 H5B 109.5 . . ?
C3 C5 H5A 109.5 . . ?
H5C C5 H5A 109.5 . . ?
H5B C5 H5A 109.5 . . ?
C7 C6 C11 120.9(5) . . ?
C7 C6 N1 121.6(5) . . ?
C11 C6 N1 117.2(5) . . ?
C8 C7 C6 118.1(5) . . ?
C8 C7 C12 118.5(5) . . ?
C6 C7 C12 123.3(5) . . ?
C9 C8 C7 121.6(6) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C10 C9 C8 119.6(6) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 121.5(6) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C6 118.2(5) . . ?
C10 C11 C15A 119.2(16) . . ?
C6 C11 C15A 122.6(16) . . ?
C10 C11 C15 120.6(10) . . ?
C6 C11 C15 121.1(10) . . ?
C15A C11 C15 1.8(19) . . ?
C14 C12 C7 112.3(5) . . ?
C14 C12 C13 109.8(5) . . ?
C7 C12 C13 111.4(5) . . ?
C14 C12 H12 107.7 . . ?
C7 C12 H12 107.7 . . ?
C13 C12 H12 107.7 . . ?
C12 C13 H13C 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13C C13 H13B 109.5 . . ?
C12 C13 H13A 109.5 . . ?
H13C C13 H13A 109.5 . . ?
H13B C13 H13A 109.5 . . ?
C12 C14 H14C 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
C12 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
H14B C14 H14A 109.5 . . ?
C19 C18 C23 120.5(5) . . ?
C19 C18 N2 120.9(5) . . ?
C23 C18 N2 118.5(5) . . ?
C20 C19 C18 118.8(6) . . ?
C20 C19 C24 118.8(5) . . ?
C18 C19 C24 122.3(5) . . ?
C21 C20 C19 120.6(6) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 120.1(6) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 121.6(6) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C22 C23 C18 118.3(6) . . ?
C22 C23 C27 119.0(6) . . ?
C18 C23 C27 122.7(5) . . ?
C19 C24 C26 111.2(5) . . ?
C19 C24 C25 111.8(5) . . ?
C26 C24 C25 110.3(5) . . ?
C19 C24 H24 107.8 . . ?
C26 C24 H24 107.8 . . ?
C25 C24 H24 107.8 . . ?
C24 C25 H25C 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25C C25 H25B 109.5 . . ?
C24 C25 H25A 109.5 . . ?
H25C C25 H25A 109.5 . . ?
H25B C25 H25A 109.5 . . ?
C24 C26 H26C 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26C C26 H26B 109.5 . . ?
C24 C26 H26A 109.5 . . ?
H26C C26 H26A 109.5 . . ?
H26B C26 H26A 109.5 . . ?
C29 C27 C23 112.4(6) . . ?
C29 C27 C28 108.4(6) . . ?
C23 C27 C28 113.1(6) . . ?
C29 C27 H27 107.6 . . ?
C23 C27 H27 107.6 . . ?
C28 C27 H27 107.6 . . ?
C27 C28 H28C 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28C C28 H28B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
H28C C28 H28A 109.5 . . ?
H28B C28 H28A 109.5 . . ?
C27 C29 H29C 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29C C29 H29B 109.5 . . ?
C27 C29 H29A 109.5 . . ?
H29C C29 H29A 109.5 . . ?
H29B C29 H29A 109.5 . . ?
N3 C30 C31 118.9(6) . . ?
N3 C30 C35 122.8(6) . . ?
C31 C30 C35 118.2(5) . . ?
C32 C31 C30 120.6(7) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C33 121.2(7) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 H32 119.4 . . ?
C34 C33 C32 118.1(6) . . ?
C34 C33 H33 120.9 . . ?
C32 C33 H33 120.9 . . ?
C33 C34 C35 123.2(7) . . ?
C33 C34 H34 118.4 . . ?
C35 C34 H34 118.4 . . ?
C34 C35 C30 118.7(6) . . ?
C34 C35 C36 120.8(6) . . ?
C30 C35 C36 120.6(5) . . ?
N4 C39 C40 125.0(5) . . ?
N4 C39 C42 119.5(5) . . ?
C40 C39 C42 115.4(5) . . ?
C39 C40 C41 130.0(5) . . ?
C39 C40 H40 115 . . ?
C41 C40 H40 115 . . ?
N5 C41 C40 124.0(5) . . ?
N5 C41 C43 120.2(5) . . ?
C40 C41 C43 115.7(5) . . ?
C39 C42 H42C 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42C C42 H42B 109.5 . . ?
C39 C42 H42A 109.5 . . ?
H42C C42 H42A 109.5 . . ?
H42B C42 H42A 109.5 . . ?
C41 C43 H43C 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43C C43 H43B 109.5 . . ?
C41 C43 H43A 109.5 . . ?
H43C C43 H43A 109.5 . . ?
H43B C43 H43A 109.5 . . ?
C45 C44 C49 121.1(5) . . ?
C45 C44 N4 120.9(5) . . ?
C49 C44 N4 117.9(5) . . ?
C46 C45 C44 116.9(5) . . ?
C46 C45 C50 120.9(5) . . ?
C44 C45 C50 122.2(5) . . ?
C47 C46 C45 122.8(6) . . ?
C47 C46 H46 118.6 . . ?
C45 C46 H46 118.6 . . ?
C48 C47 C46 119.2(6) . . ?
C48 C47 H47 120.4 . . ?
C46 C47 H47 120.4 . . ?
C47 C48 C49 121.6(6) . . ?
C47 C48 H48 119.2 . . ?
C49 C48 H48 119.2 . . ?
C48 C49 C44 118.2(5) . . ?
C48 C49 C53 120.9(5) . . ?
C44 C49 C53 120.9(5) . . ?
C45 C50 C51 109.8(5) . . ?
C45 C50 C52 112.6(5) . . ?
C51 C50 C52 109.6(5) . . ?
C45 C50 H50 108.2 . . ?
C51 C50 H50 108.2 . . ?
C52 C50 H50 108.2 . . ?
C50 C51 H51C 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51C C51 H51B 109.5 . . ?
C50 C51 H51A 109.5 . . ?
H51C C51 H51A 109.5 . . ?
H51B C51 H51A 109.5 . . ?
C50 C52 H52C 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52C C52 H52B 109.5 . . ?
C50 C52 H52A 109.5 . . ?
H52C C52 H52A 109.5 . . ?
H52B C52 H52A 109.5 . . ?
C55 C53 C49 112.6(6) . . ?
C55 C53 C54 109.6(6) . . ?
C49 C53 C54 112.6(5) . . ?
C55 C53 H53 107.2 . . ?
C49 C53 H53 107.2 . . ?
C54 C53 H53 107.2 . . ?
C53 C54 H54C 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54C C54 H54B 109.5 . . ?
C53 C54 H54A 109.5 . . ?
H54C C54 H54A 109.5 . . ?
H54B C54 H54A 109.5 . . ?
C53 C55 H55C 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55C C55 H55B 109.5 . . ?
C53 C55 H55A 109.5 . . ?
H55C C55 H55A 109.5 . . ?
H55B C55 H55A 109.5 . . ?
C61 C56 C57 121.3(5) . . ?
C61 C56 N5 118.1(5) . . ?
C57 C56 N5 120.4(5) . . ?
C58 C57 C56 117.1(5) . . ?
C58 C57 C62 119.3(5) . . ?
C56 C57 C62 123.6(5) . . ?
C59 C58 C57 122.3(6) . . ?
C59 C58 H58 118.9 . . ?
C57 C58 H58 118.9 . . ?
C58 C59 C60 119.9(6) . . ?
C58 C59 H59 120 . . ?
C60 C59 H59 120 . . ?
C59 C60 C61 120.8(6) . . ?
C59 C60 H60 119.6 . . ?
C61 C60 H60 119.6 . . ?
C60 C61 C56 118.5(6) . . ?
C60 C61 C65 119.9(5) . . ?
C56 C61 C65 121.5(5) . . ?
C57 C62 C64 111.6(5) . . ?
C57 C62 C63 111.9(5) . . ?
C64 C62 C63 109.7(5) . . ?
C57 C62 H62 107.8 . . ?
C64 C62 H62 107.8 . . ?
C63 C62 H62 107.8 . . ?
C62 C63 H63C 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63C C63 H63B 109.5 . . ?
C62 C63 H63A 109.5 . . ?
H63C C63 H63A 109.5 . . ?
H63B C63 H63A 109.5 . . ?
C62 C64 H64C 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64C C64 H64B 109.5 . . ?
C62 C64 H64A 109.5 . . ?
H64C C64 H64A 109.5 . . ?
H64B C64 H64A 109.5 . . ?
C66 C65 C67 110.1(7) . . ?
C66 C65 C61 113.8(6) . . ?
C67 C65 C61 111.4(6) . . ?
C66 C65 H65 107.1 . . ?
C67 C65 H65 107.1 . . ?
C61 C65 H65 107.1 . . ?
C65 C66 H66C 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66C C66 H66B 109.5 . . ?
C65 C66 H66A 109.5 . . ?
H66C C66 H66A 109.5 . . ?
H66B C66 H66A 109.5 . . ?
C65 C67 H67C 109.5 . . ?
C65 C67 H67B 109.5 . . ?
H67C C67 H67B 109.5 . . ?
C65 C67 H67A 109.5 . . ?
H67C C67 H67A 109.5 . . ?
H67B C67 H67A 109.5 . . ?
N6 C68 C69 119.1(5) . . ?
N6 C68 C73 123.3(5) . . ?
C69 C68 C73 117.6(5) . . ?
C70 C69 C68 121.5(6) . . ?
C70 C69 H69 119.2 . . ?
C68 C69 H69 119.2 . . ?
C69 C70 C71 120.5(6) . . ?
C69 C70 H70 119.7 . . ?
C71 C70 H70 119.7 . . ?
C70 C71 C72 118.9(6) . . ?
C70 C71 H71 120.5 . . ?
C72 C71 H71 120.5 . . ?
C71 C72 C73 121.8(6) . . ?
C71 C72 H72 119.1 . . ?
C73 C72 H72 119.1 . . ?
C72 C73 C68 119.5(6) . . ?
C72 C73 C74 121.4(5) . . ?
C68 C73 C74 119.1(5) . . ?
C73 C74 C76 114.3(5) . . ?
C73 C74 C75 110.8(5) . . ?
C76 C74 C75 109.8(5) . . ?
C73 C74 H74 107.2 . . ?
C76 C74 H74 107.2 . . ?
C75 C74 H74 107.2 . . ?
C74 C75 H75C 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75C C75 H75B 109.5 . . ?
C74 C75 H75A 109.5 . . ?
H75C C75 H75A 109.5 . . ?
H75B C75 H75A 109.5 . . ?
C74 C76 H76C 109.5 . . ?
C74 C76 H76B 109.5 . . ?
H76C C76 H76B 109.5 . . ?
C74 C76 H76A 109.5 . . ?
H76C C76 H76A 109.5 . . ?
H76B C76 H76A 109.5 . . ?
C17 C15 C16 111.7(14) . . ?
C17 C15 C11 111(2) . . ?
C16 C15 C11 110.8(15) . . ?
C17 C15 H15 107.6 . . ?
C16 C15 H15 107.6 . . ?
C11 C15 H15 107.6 . . ?
C15 C16 H16C 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16C C16 H16B 109.5 . . ?
C15 C16 H16A 109.5 . . ?
H16C C16 H16A 109.5 . . ?
H16B C16 H16A 109.5 . . ?
C15 C17 H17C 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17C C17 H17B 109.5 . . ?
C15 C17 H17A 109.5 . . ?
H17C C17 H17A 109.5 . . ?
H17B C17 H17A 109.5 . . ?
C37 C36 C38 118.7(8) . . ?
C37 C36 C35 111.0(6) . . ?
C38 C36 C35 111.9(7) . . ?
C37 C36 H36 104.6 . . ?
C38 C36 H36 104.6 . . ?
C35 C36 H36 104.6 . . ?
C36 C37 H37C 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37C C37 H37B 109.5 . . ?
C36 C37 H37A 109.5 . . ?
H37C C37 H37A 109.5 . . ?
H37B C37 H37A 109.5 . . ?
C36 C38 H38C 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38C C38 H38B 109.5 . . ?
C36 C38 H38A 109.5 . . ?
H38C C38 H38A 109.5 . . ?
H38B C38 H38A 109.5 . . ?
C11 C15A C17A 114(3) . . ?
C11 C15A C16A 114(3) . . ?
C17A C15A C16A 109(2) . . ?
C11 C15A H15A 106.5 . . ?
C17A C15A H15A 106.5 . . ?
C16A C15A H15A 106.5 . . ?
C15A C16A H16F 109.5 . . ?
C15A C16A H16E 109.5 . . ?
H16F C16A H16E 109.5 . . ?
C15A C16A H16D 109.5 . . ?
H16F C16A H16D 109.5 . . ?
H16E C16A H16D 109.5 . . ?
C15A C17A H17F 109.5 . . ?
C15A C17A H17E 109.5 . . ?
H17F C17A H17E 109.5 . . ?
C15A C17A H17D 109.5 . . ?
H17F C17A H17D 109.5 . . ?
H17E C17A H17D 109.5 . . ?
H37F C37A H37E 109.5 . . ?
H37F C37A H37D 109.5 . . ?
H37E C37A H37D 109.5 . . ?
H38F C38A H38E 109.5 . . ?
H38F C38A H38D 109.5 . . ?
H38E C38A H38D 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 991975'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(5)-jun309

_audit_creation_date             2014-03-12T07:59:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C41 H59 N3 Pb1'
_chemical_formula_sum            'C41 H59 N3 Pb'
_chemical_formula_weight         801.1
_chemical_compound_source        'synthesis as described'


#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.22380(10)
_cell_length_b                   11.4878(2)
_cell_length_c                   19.2046(3)
_cell_angle_alpha                100.7430(10)
_cell_angle_beta                 102.6090(10)
_cell_angle_gamma                99.0180(10)
_cell_volume                     1909.24(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    22842
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.485
_cell_measurement_wavelength     0.71073



#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Needles
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.4868
_exptl_absorpt_correction_T_max  0.6211


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.276721E-1
_diffrn_orient_matrix_ub_12      0.280618E-1
_diffrn_orient_matrix_ub_13      0.546023E-1
_diffrn_orient_matrix_ub_21      -0.108929
_diffrn_orient_matrix_ub_22      -0.244568E-1
_diffrn_orient_matrix_ub_23      0.61E-5
_diffrn_orient_matrix_ub_31      0.160407E-1
_diffrn_orient_matrix_ub_32      -0.825364E-1
_diffrn_orient_matrix_ub_33      0.47994E-2
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_number            34650
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             8691
_reflns_number_gt                7920
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0112P)²+2.2486P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8691
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0494
_refine_ls_wR_factor_gt          0.0478
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.096

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.198192(11) 0.105741(9) 0.219034(5) 0.01614(3) Uani 1 1 d . . .
N1 N 0.2901(2) -0.0575(2) 0.25321(11) 0.0162(5) Uani 1 1 d . . .
N2 N 0.3358(2) 0.2012(2) 0.33831(12) 0.0180(5) Uani 1 1 d . . .
N3 N 0.3995(2) 0.1327(2) 0.17492(12) 0.0201(5) Uani 1 1 d . . .
H3 H 0.457 0.0789 0.1802 0.024 Uiso 1 1 calc R . .
C1 C 0.4141(3) -0.0493(2) 0.30474(14) 0.0184(6) Uani 1 1 d . . .
C2 C 0.4997(3) 0.0586(3) 0.35387(15) 0.0229(6) Uani 1 1 d . . .
H2 H 0.5998 0.0547 0.3779 0.027 Uiso 1 1 calc R . .
C3 C 0.4602(3) 0.1707(3) 0.37276(15) 0.0220(6) Uani 1 1 d . . .
C4 C 0.4705(3) -0.1630(3) 0.31593(17) 0.0278(7) Uani 1 1 d . . .
H4A H 0.3837 -0.2299 0.3071 0.042 Uiso 1 1 calc R . .
H4B H 0.5325 -0.1492 0.3663 0.042 Uiso 1 1 calc R . .
H4C H 0.5321 -0.1835 0.2816 0.042 Uiso 1 1 calc R . .
C5 C 0.5687(4) 0.2612(3) 0.43810(18) 0.0368(8) Uani 1 1 d . . .
H5A H 0.6358 0.3181 0.4209 0.055 Uiso 1 1 calc R . .
H5B H 0.6297 0.2182 0.4689 0.055 Uiso 1 1 calc R . .
H5C H 0.5108 0.3059 0.4667 0.055 Uiso 1 1 calc R . .
C6 C 0.2031(3) -0.1727(2) 0.20864(15) 0.0191(6) Uani 1 1 d . . .
C7 C 0.2474(3) -0.2315(3) 0.14803(15) 0.0234(6) Uani 1 1 d . . .
C8 C 0.1545(4) -0.3398(3) 0.10496(17) 0.0316(7) Uani 1 1 d . . .
H8 H 0.1826 -0.3808 0.0638 0.038 Uiso 1 1 calc R . .
C9 C 0.0228(4) -0.3889(3) 0.12088(19) 0.0380(8) Uani 1 1 d . . .
H9 H -0.0379 -0.4635 0.0911 0.046 Uiso 1 1 calc R . .
C10 C -0.0217(4) -0.3302(3) 0.17993(18) 0.0359(8) Uani 1 1 d . . .
H10 H -0.1136 -0.3643 0.1899 0.043 Uiso 1 1 calc R . .
C11 C 0.0673(3) -0.2214(3) 0.22503(16) 0.0246(6) Uani 1 1 d . . .
C12 C 0.3919(3) -0.1817(3) 0.12817(16) 0.0256(6) Uani 1 1 d . . .
H12 H 0.4486 -0.1085 0.1673 0.031 Uiso 1 1 calc R . .
C13 C 0.4948(4) -0.2751(3) 0.12476(18) 0.0367(8) Uani 1 1 d . . .
H13C H 0.5225 -0.2953 0.1726 0.055 Uiso 1 1 calc R . .
H13B H 0.587 -0.2408 0.112 0.055 Uiso 1 1 calc R . .
H13A H 0.4404 -0.3485 0.0875 0.055 Uiso 1 1 calc R . .
C14 C 0.3565(4) -0.1434(3) 0.05493(17) 0.0347(7) Uani 1 1 d . . .
H14C H 0.2991 -0.2137 0.0159 0.052 Uiso 1 1 calc R . .
H14B H 0.4517 -0.1116 0.0438 0.052 Uiso 1 1 calc R . .
H14A H 0.2962 -0.0805 0.0583 0.052 Uiso 1 1 calc R . .
C15 C 0.0208(3) -0.1596(3) 0.29103(17) 0.0306(7) Uani 1 1 d . . .
H15 H 0.0703 -0.072 0.3025 0.037 Uiso 1 1 calc R . .
C16 C 0.0789(6) -0.2075(5) 0.3580(2) 0.0779(16) Uani 1 1 d . . .
H16C H 0.0371 -0.2946 0.3479 0.117 Uiso 1 1 calc R . .
H16B H 0.0472 -0.1655 0.3997 0.117 Uiso 1 1 calc R . .
H16A H 0.19 -0.1934 0.3698 0.117 Uiso 1 1 calc R . .
C17 C -0.1495(4) -0.1664(4) 0.2775(2) 0.0535(11) Uani 1 1 d . . .
H17C H -0.1838 -0.1274 0.2374 0.08 Uiso 1 1 calc R . .
H17B H -0.1718 -0.1247 0.3221 0.08 Uiso 1 1 calc R . .
H17A H -0.2024 -0.2514 0.2643 0.08 Uiso 1 1 calc R . .
C18 C 0.2865(3) 0.3064(3) 0.37055(14) 0.0198(6) Uani 1 1 d . . .
C19 C 0.3308(3) 0.4193(3) 0.35545(16) 0.0249(6) Uani 1 1 d . . .
C20 C 0.2747(4) 0.5163(3) 0.38618(17) 0.0314(7) Uani 1 1 d . . .
H20 H 0.3035 0.5932 0.376 0.038 Uiso 1 1 calc R . .
C21 C 0.1782(4) 0.5038(3) 0.43112(17) 0.0343(7) Uani 1 1 d . . .
H21 H 0.1429 0.5717 0.4525 0.041 Uiso 1 1 calc R . .
C22 C 0.1338(4) 0.3924(3) 0.44458(16) 0.0321(7) Uani 1 1 d . . .
H22 H 0.0668 0.384 0.4754 0.038 Uiso 1 1 calc R . .
C23 C 0.1840(3) 0.2911(3) 0.41433(15) 0.0251(6) Uani 1 1 d . . .
C24 C 0.4353(4) 0.4385(3) 0.30526(18) 0.0327(7) Uani 1 1 d . . .
H24 H 0.4658 0.3601 0.2891 0.039 Uiso 1 1 calc R . .
C25 C 0.3514(5) 0.4740(3) 0.23740(19) 0.0473(10) Uani 1 1 d . . .
H25C H 0.2627 0.4098 0.211 0.071 Uiso 1 1 calc R . .
H25B H 0.4193 0.4854 0.2054 0.071 Uiso 1 1 calc R . .
H25A H 0.3181 0.5497 0.2522 0.071 Uiso 1 1 calc R . .
C26 C 0.5794(4) 0.5340(3) 0.3446(2) 0.0498(10) Uani 1 1 d . . .
H26C H 0.5519 0.6115 0.3615 0.075 Uiso 1 1 calc R . .
H26B H 0.6437 0.5434 0.3107 0.075 Uiso 1 1 calc R . .
H26A H 0.635 0.5084 0.3868 0.075 Uiso 1 1 calc R . .
C27 C 0.1303(4) 0.1683(3) 0.42917(18) 0.0383(8) Uani 1 1 d . . .
H27 H 0.1479 0.1055 0.39 0.046 Uiso 1 1 calc R . .
C28 C 0.2231(5) 0.1556(5) 0.5023(3) 0.0669(13) Uani 1 1 d . . .
H28C H 0.3302 0.1642 0.5017 0.1 Uiso 1 1 calc R . .
H28B H 0.1863 0.0757 0.5104 0.1 Uiso 1 1 calc R . .
H28A H 0.2125 0.2186 0.5419 0.1 Uiso 1 1 calc R . .
C29 C -0.0387(4) 0.1418(4) 0.4254(2) 0.0554(11) Uani 1 1 d . . .
H29C H -0.0605 0.2033 0.4622 0.083 Uiso 1 1 calc R . .
H29B H -0.0674 0.0617 0.435 0.083 Uiso 1 1 calc R . .
H29A H -0.0969 0.1435 0.3765 0.083 Uiso 1 1 calc R . .
C30 C 0.4500(3) 0.2211(2) 0.14012(14) 0.0171(5) Uani 1 1 d . . .
C31 C 0.3505(3) 0.2473(3) 0.08034(14) 0.0201(6) Uani 1 1 d . . .
C32 C 0.4020(3) 0.3416(3) 0.04988(16) 0.0253(6) Uani 1 1 d . . .
H32 H 0.3339 0.3607 0.0109 0.03 Uiso 1 1 calc R . .
C33 C 0.5487(3) 0.4082(3) 0.07463(16) 0.0281(7) Uani 1 1 d . . .
H33 H 0.5806 0.4739 0.0541 0.034 Uiso 1 1 calc R . .
C34 C 0.6483(3) 0.3775(3) 0.12985(16) 0.0256(6) Uani 1 1 d . . .
H34 H 0.7507 0.4208 0.1456 0.031 Uiso 1 1 calc R . .
C35 C 0.6036(3) 0.2856(2) 0.16301(15) 0.0204(6) Uani 1 1 d . . .
C36 C 0.1889(3) 0.1736(3) 0.04793(15) 0.0261(6) Uani 1 1 d . . .
H36 H 0.1777 0.104 0.0721 0.031 Uiso 1 1 calc R . .
C37 C 0.1574(4) 0.1211(3) -0.03458(17) 0.0421(9) Uani 1 1 d . . .
H37C H 0.1713 0.1873 -0.0597 0.063 Uiso 1 1 calc R . .
H37B H 0.0528 0.0746 -0.0532 0.063 Uiso 1 1 calc R . .
H37A H 0.2279 0.0679 -0.0436 0.063 Uiso 1 1 calc R . .
C38 C 0.0700(4) 0.2470(4) 0.0632(2) 0.0414(9) Uani 1 1 d . . .
H38C H 0.0851 0.2739 0.1163 0.062 Uiso 1 1 calc R . .
H38B H -0.0318 0.1965 0.0415 0.062 Uiso 1 1 calc R . .
H38A H 0.0805 0.3178 0.0416 0.062 Uiso 1 1 calc R . .
C39 C 0.7176(3) 0.2496(3) 0.22129(16) 0.0272(7) Uani 1 1 d . . .
H39 H 0.6682 0.2372 0.2615 0.033 Uiso 1 1 calc R . .
C40 C 0.7569(4) 0.1292(3) 0.1897(2) 0.0410(8) Uani 1 1 d . . .
H40C H 0.6644 0.0658 0.1726 0.061 Uiso 1 1 calc R . .
H40B H 0.8299 0.1072 0.2279 0.061 Uiso 1 1 calc R . .
H40A H 0.8015 0.1377 0.1486 0.061 Uiso 1 1 calc R . .
C41 C 0.8650(4) 0.3448(4) 0.2554(2) 0.0449(9) Uani 1 1 d . . .
H41C H 0.9156 0.3593 0.2171 0.067 Uiso 1 1 calc R . .
H41B H 0.9321 0.3154 0.2922 0.067 Uiso 1 1 calc R . .
H41A H 0.8414 0.4204 0.2788 0.067 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N3 2.206(2) . ?
Pb N1 2.319(2) . ?
Pb N2 2.328(2) . ?
N1 C1 1.317(3) . ?
N1 C6 1.440(3) . ?
N2 C3 1.325(3) . ?
N2 C18 1.438(3) . ?
N3 C30 1.392(3) . ?
N3 H3 0.88 . ?
C1 C2 1.408(4) . ?
C1 C4 1.514(4) . ?
C2 C3 1.398(4) . ?
C2 H2 0.95 . ?
C3 C5 1.515(4) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.407(4) . ?
C6 C11 1.414(4) . ?
C7 C8 1.393(4) . ?
C7 C12 1.521(4) . ?
C8 C9 1.378(5) . ?
C8 H8 0.95 . ?
C9 C10 1.383(5) . ?
C9 H9 0.95 . ?
C10 C11 1.397(4) . ?
C10 H10 0.95 . ?
C11 C15 1.514(4) . ?
C12 C14 1.534(4) . ?
C12 C13 1.542(4) . ?
C12 H12 1 . ?
C13 H13C 0.98 . ?
C13 H13B 0.98 . ?
C13 H13A 0.98 . ?
C14 H14C 0.98 . ?
C14 H14B 0.98 . ?
C14 H14A 0.98 . ?
C15 C16 1.517(5) . ?
C15 C17 1.522(4) . ?
C15 H15 1 . ?
C16 H16C 0.98 . ?
C16 H16B 0.98 . ?
C16 H16A 0.98 . ?
C17 H17C 0.98 . ?
C17 H17B 0.98 . ?
C17 H17A 0.98 . ?
C18 C19 1.400(4) . ?
C18 C23 1.408(4) . ?
C19 C20 1.388(4) . ?
C19 C24 1.525(4) . ?
C20 C21 1.378(4) . ?
C20 H20 0.95 . ?
C21 C22 1.371(5) . ?
C21 H21 0.95 . ?
C22 C23 1.394(4) . ?
C22 H22 0.95 . ?
C23 C27 1.520(4) . ?
C24 C25 1.524(5) . ?
C24 C26 1.529(5) . ?
C24 H24 1 . ?
C25 H25C 0.98 . ?
C25 H25B 0.98 . ?
C25 H25A 0.98 . ?
C26 H26C 0.98 . ?
C26 H26B 0.98 . ?
C26 H26A 0.98 . ?
C27 C28 1.522(5) . ?
C27 C29 1.524(5) . ?
C27 H27 1 . ?
C28 H28C 0.98 . ?
C28 H28B 0.98 . ?
C28 H28A 0.98 . ?
C29 H29C 0.98 . ?
C29 H29B 0.98 . ?
C29 H29A 0.98 . ?
C30 C31 1.416(4) . ?
C30 C35 1.423(4) . ?
C31 C32 1.392(4) . ?
C31 C36 1.526(4) . ?
C32 C33 1.379(4) . ?
C32 H32 0.95 . ?
C33 C34 1.382(4) . ?
C33 H33 0.95 . ?
C34 C35 1.386(4) . ?
C34 H34 0.95 . ?
C35 C39 1.525(4) . ?
C36 C37 1.532(4) . ?
C36 C38 1.529(4) . ?
C36 H36 1 . ?
C37 H37C 0.98 . ?
C37 H37B 0.98 . ?
C37 H37A 0.98 . ?
C38 H38C 0.98 . ?
C38 H38B 0.98 . ?
C38 H38A 0.98 . ?
C39 C40 1.534(5) . ?
C39 C41 1.533(4) . ?
C39 H39 1 . ?
C40 H40C 0.98 . ?
C40 H40B 0.98 . ?
C40 H40A 0.98 . ?
C41 H41C 0.98 . ?
C41 H41B 0.98 . ?
C41 H41A 0.98 . ?

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
N3 Pb N1 84.39(8) . . ?
N3 Pb N2 93.10(8) . . ?
N1 Pb N2 81.36(8) . . ?
C1 N1 C6 121.6(2) . . ?
C1 N1 Pb 125.07(18) . . ?
C6 N1 Pb 113.20(16) . . ?
C3 N2 C18 120.8(2) . . ?
C3 N2 Pb 123.83(18) . . ?
C18 N2 Pb 115.06(16) . . ?
C30 N3 Pb 130.25(17) . . ?
C30 N3 H3 114.9 . . ?
Pb N3 H3 114.9 . . ?
N1 C1 C2 125.2(2) . . ?
N1 C1 C4 119.6(2) . . ?
C2 C1 C4 115.2(2) . . ?
C3 C2 C1 130.0(3) . . ?
C3 C2 H2 115 . . ?
C1 C2 H2 115 . . ?
N2 C3 C2 124.7(2) . . ?
N2 C3 C5 119.1(3) . . ?
C2 C3 C5 116.2(2) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 121.0(2) . . ?
C7 C6 N1 120.9(2) . . ?
C11 C6 N1 118.0(2) . . ?
C8 C7 C6 118.1(3) . . ?
C8 C7 C12 119.2(3) . . ?
C6 C7 C12 122.7(2) . . ?
C9 C8 C7 121.3(3) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C11 120.5(3) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C10 C11 C6 118.4(3) . . ?
C10 C11 C15 120.4(3) . . ?
C6 C11 C15 121.2(3) . . ?
C7 C12 C14 111.4(2) . . ?
C7 C12 C13 111.1(3) . . ?
C14 C12 C13 109.8(2) . . ?
C7 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C13 C12 H12 108.1 . . ?
C12 C13 H13C 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13C C13 H13B 109.5 . . ?
C12 C13 H13A 109.5 . . ?
H13C C13 H13A 109.5 . . ?
H13B C13 H13A 109.5 . . ?
C12 C14 H14C 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
C12 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
H14B C14 H14A 109.5 . . ?
C11 C15 C16 111.6(3) . . ?
C11 C15 C17 113.6(3) . . ?
C16 C15 C17 110.2(3) . . ?
C11 C15 H15 107 . . ?
C16 C15 H15 107 . . ?
C17 C15 H15 107 . . ?
C15 C16 H16C 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16C C16 H16B 109.5 . . ?
C15 C16 H16A 109.5 . . ?
H16C C16 H16A 109.5 . . ?
H16B C16 H16A 109.5 . . ?
C15 C17 H17C 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17C C17 H17B 109.5 . . ?
C15 C17 H17A 109.5 . . ?
H17C C17 H17A 109.5 . . ?
H17B C17 H17A 109.5 . . ?
C19 C18 C23 120.6(3) . . ?
C19 C18 N2 121.4(2) . . ?
C23 C18 N2 117.9(2) . . ?
C20 C19 C18 118.6(3) . . ?
C20 C19 C24 119.2(3) . . ?
C18 C19 C24 122.3(3) . . ?
C21 C20 C19 121.6(3) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C22 C21 C20 119.3(3) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C22 C23 121.8(3) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C18 118.1(3) . . ?
C22 C23 C27 120.5(3) . . ?
C18 C23 C27 121.4(3) . . ?
C19 C24 C25 110.2(3) . . ?
C19 C24 C26 111.9(3) . . ?
C25 C24 C26 110.1(3) . . ?
C19 C24 H24 108.2 . . ?
C25 C24 H24 108.2 . . ?
C26 C24 H24 108.2 . . ?
C24 C25 H25C 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25C C25 H25B 109.5 . . ?
C24 C25 H25A 109.5 . . ?
H25C C25 H25A 109.5 . . ?
H25B C25 H25A 109.5 . . ?
C24 C26 H26C 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26C C26 H26B 109.5 . . ?
C24 C26 H26A 109.5 . . ?
H26C C26 H26A 109.5 . . ?
H26B C26 H26A 109.5 . . ?
C28 C27 C23 111.2(3) . . ?
C28 C27 C29 110.6(3) . . ?
C23 C27 C29 112.8(3) . . ?
C28 C27 H27 107.3 . . ?
C23 C27 H27 107.3 . . ?
C29 C27 H27 107.3 . . ?
C27 C28 H28C 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28C C28 H28B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
H28C C28 H28A 109.5 . . ?
H28B C28 H28A 109.5 . . ?
C27 C29 H29C 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29C C29 H29B 109.5 . . ?
C27 C29 H29A 109.5 . . ?
H29C C29 H29A 109.5 . . ?
H29B C29 H29A 109.5 . . ?
N3 C30 C31 120.7(2) . . ?
N3 C30 C35 120.7(2) . . ?
C31 C30 C35 118.6(2) . . ?
C32 C31 C30 119.2(3) . . ?
C32 C31 C36 119.2(2) . . ?
C30 C31 C36 121.6(2) . . ?
C33 C32 C31 122.0(3) . . ?
C33 C32 H32 119 . . ?
C31 C32 H32 119 . . ?
C32 C33 C34 118.7(3) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
C33 C34 C35 122.1(3) . . ?
C33 C34 H34 119 . . ?
C35 C34 H34 119 . . ?
C34 C35 C30 119.2(2) . . ?
C34 C35 C39 121.0(2) . . ?
C30 C35 C39 119.8(2) . . ?
C31 C36 C37 112.0(2) . . ?
C31 C36 C38 112.2(3) . . ?
C37 C36 C38 109.9(3) . . ?
C31 C36 H36 107.5 . . ?
C37 C36 H36 107.5 . . ?
C38 C36 H36 107.5 . . ?
C36 C37 H37C 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37C C37 H37B 109.5 . . ?
C36 C37 H37A 109.5 . . ?
H37C C37 H37A 109.5 . . ?
H37B C37 H37A 109.5 . . ?
C36 C38 H38C 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38C C38 H38B 109.5 . . ?
C36 C38 H38A 109.5 . . ?
H38C C38 H38A 109.5 . . ?
H38B C38 H38A 109.5 . . ?
C35 C39 C40 110.5(3) . . ?
C35 C39 C41 114.2(3) . . ?
C40 C39 C41 108.9(3) . . ?
C35 C39 H39 107.6 . . ?
C40 C39 H39 107.6 . . ?
C41 C39 H39 107.6 . . ?
C39 C40 H40C 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40C C40 H40B 109.5 . . ?
C39 C40 H40A 109.5 . . ?
H40C C40 H40A 109.5 . . ?
H40B C40 H40A 109.5 . . ?
C39 C41 H41C 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41C C41 H41B 109.5 . . ?
C39 C41 H41A 109.5 . . ?
H41C C41 H41A 109.5 . . ?
H41B C41 H41A 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 991976'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(8)-jun409

_audit_creation_date             2009-07-15T11:37:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C24 H36 I2 N2 Pb2), 3(C7 H8)'
_chemical_formula_sum            'C69 H96 I4 N4 Pb4'
_chemical_formula_weight         2317.90
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.2058(2)
_cell_length_b                   14.6460(2)
_cell_length_c                   19.7011(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.4910(10)
_cell_angle_gamma                90
_cell_volume                     3758.27(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    38444
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.485
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2156
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    10.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.3948
_exptl_absorpt_correction_T_max  0.6155

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.01642
_diffrn_orient_matrix_ub_12      0.664573E-1
_diffrn_orient_matrix_ub_13      0.60252E-2
_diffrn_orient_matrix_ub_21      -0.652019E-1
_diffrn_orient_matrix_ub_22      0.97844E-2
_diffrn_orient_matrix_ub_23      0.185868E-1
_diffrn_orient_matrix_ub_31      0.370614E-1
_diffrn_orient_matrix_ub_32      -0.122303E-1
_diffrn_orient_matrix_ub_33      0.476096E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_number            60206
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             8545
_reflns_number_gt                7278
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 A residual peak of ~3 electrons is present near to iodine and is assumed to 
 be spurious 
 The hydrogen atoms on the amide nitrogens were located and refined, all others
 were riding.
 The carbon atoms of the two toluene solvate molecules were left isotropic; the
 C6-ring of the toluene on the inversion centre was refined as a rigid body with
 each carbon atom at 1/2 occupancy

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0258P)²+16.3978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8545
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   1.1
_refine_ls_restrained_S_all      1.1
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.014
_refine_diff_density_min         -2.808
_refine_diff_density_rms         0.162

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.394058(17) 0.145946(14) 0.311709(10) 0.02655(6) Uani 1 1 d . . .
Pb2 Pb 0.510501(17) 0.373624(14) 0.317195(10) 0.02787(6) Uani 1 1 d . . .
I1 I 0.38007(3) 0.11769(3) 0.163799(18) 0.03649(10) Uani 1 1 d . . .
I2 I 0.51698(4) 0.40902(3) 0.17267(2) 0.05006(13) Uani 1 1 d . . .
N1 N 0.5582(4) 0.2185(3) 0.3076(2) 0.0274(10) Uani 1 1 d . . .
H1N H 0.563(5) 0.213(4) 0.267(3) 0.030(17) Uiso 1 1 d . . .
N2 N 0.3496(4) 0.3030(3) 0.2827(2) 0.0273(10) Uani 1 1 d . . .
H2N H 0.349(4) 0.299(4) 0.239(3) 0.022(14) Uiso 1 1 d . . .
C1 C 0.6575(4) 0.1996(4) 0.3446(3) 0.0284(12) Uani 1 1 d . . .
C2 C 0.6731(5) 0.1998(4) 0.4174(3) 0.0378(14) Uani 1 1 d . . .
C3 C 0.7723(6) 0.1863(6) 0.4533(4) 0.0535(19) Uani 1 1 d . . .
H3 H 0.7833 0.186 0.5022 0.064 Uiso 1 1 calc R . .
C4 C 0.8534(6) 0.1737(6) 0.4200(4) 0.064(2) Uani 1 1 d . . .
H4 H 0.9204 0.1657 0.4456 0.077 Uiso 1 1 calc R . .
C5 C 0.8386(6) 0.1723(5) 0.3487(4) 0.0541(19) Uani 1 1 d . . .
H5 H 0.8958 0.1625 0.3261 0.065 Uiso 1 1 calc R . .
C6 C 0.7423(5) 0.1849(4) 0.3097(3) 0.0384(14) Uani 1 1 d . . .
C7 C 0.5838(5) 0.2075(4) 0.4573(3) 0.0395(15) Uani 1 1 d . . .
H7 H 0.5233 0.2315 0.425 0.047 Uiso 1 1 calc R . .
C8 C 0.6045(6) 0.2728(5) 0.5186(4) 0.057(2) Uani 1 1 d . . .
H8C H 0.664 0.2512 0.5511 0.086 Uiso 1 1 calc R . .
H8B H 0.5442 0.2749 0.5417 0.086 Uiso 1 1 calc R . .
H8A H 0.6186 0.334 0.5024 0.086 Uiso 1 1 calc R . .
C9 C 0.5554(7) 0.1122(5) 0.4811(3) 0.0522(19) Uani 1 1 d . . .
H9C H 0.5358 0.0727 0.4409 0.078 Uiso 1 1 calc R . .
H9B H 0.4977 0.1174 0.5064 0.078 Uiso 1 1 calc R . .
H9A H 0.6146 0.0856 0.5112 0.078 Uiso 1 1 calc R . .
C10 C 0.7268(5) 0.1786(5) 0.2313(3) 0.0449(16) Uani 1 1 d . . .
H10 H 0.6764 0.2268 0.2123 0.054 Uiso 1 1 calc R . .
C11 C 0.6813(7) 0.0858(5) 0.2070(4) 0.058(2) Uani 1 1 d . . .
H11C H 0.7281 0.0371 0.2265 0.087 Uiso 1 1 calc R . .
H11B H 0.6717 0.083 0.1567 0.087 Uiso 1 1 calc R . .
H11A H 0.6149 0.078 0.2223 0.087 Uiso 1 1 calc R . .
C12 C 0.8273(7) 0.1951(7) 0.2018(5) 0.080(3) Uani 1 1 d . . .
H12C H 0.8537 0.2562 0.2149 0.12 Uiso 1 1 calc R . .
H12B H 0.8129 0.1903 0.1515 0.12 Uiso 1 1 calc R . .
H12A H 0.8785 0.1493 0.2203 0.12 Uiso 1 1 calc R . .
C13 C 0.2554(5) 0.3416(4) 0.2958(3) 0.0335(13) Uani 1 1 d . . .
C14 C 0.2437(5) 0.3606(5) 0.3637(3) 0.0410(15) Uani 1 1 d . . .
C15 C 0.1515(6) 0.4006(6) 0.3750(4) 0.059(2) Uani 1 1 d . . .
H15 H 0.1428 0.4139 0.4208 0.071 Uiso 1 1 calc R . .
C16 C 0.0749(6) 0.4209(7) 0.3231(5) 0.073(3) Uani 1 1 d . . .
H16 H 0.0138 0.4485 0.3327 0.087 Uiso 1 1 calc R . .
C17 C 0.0852(6) 0.4016(6) 0.2553(4) 0.061(2) Uani 1 1 d . . .
H17 H 0.0311 0.4162 0.2189 0.073 Uiso 1 1 calc R . .
C18 C 0.1746(5) 0.3608(4) 0.2407(3) 0.0394(15) Uani 1 1 d . . .
C19 C 0.3262(5) 0.3424(4) 0.4255(3) 0.0405(15) Uani 1 1 d . . .
H19 H 0.3851 0.3137 0.4074 0.049 Uiso 1 1 calc R . .
C20 C 0.3672(6) 0.4298(5) 0.4621(3) 0.0507(18) Uani 1 1 d . . .
H20C H 0.3967 0.4688 0.43 0.076 Uiso 1 1 calc R . .
H20B H 0.4202 0.4145 0.5014 0.076 Uiso 1 1 calc R . .
H20A H 0.3109 0.4622 0.4785 0.076 Uiso 1 1 calc R . .
C21 C 0.2924(6) 0.2740(5) 0.4762(4) 0.057(2) Uani 1 1 d . . .
H21C H 0.351 0.2588 0.5117 0.086 Uiso 1 1 calc R . .
H21B H 0.2668 0.2184 0.4515 0.086 Uiso 1 1 calc R . .
H21A H 0.2377 0.3011 0.4978 0.086 Uiso 1 1 calc R . .
C22 C 0.1816(6) 0.3415(5) 0.1661(3) 0.0465(17) Uani 1 1 d . . .
H22 H 0.2389 0.2969 0.1661 0.056 Uiso 1 1 calc R . .
C23 C 0.0849(7) 0.2964(7) 0.1271(5) 0.081(3) Uani 1 1 d . . .
H23C H 0.0731 0.2383 0.1492 0.122 Uiso 1 1 calc R . .
H23B H 0.0938 0.2852 0.0794 0.122 Uiso 1 1 calc R . .
H23A H 0.0259 0.3368 0.1277 0.122 Uiso 1 1 calc R . .
C24 C 0.2094(10) 0.4253(7) 0.1285(4) 0.094(4) Uani 1 1 d . . .
H24C H 0.157 0.4724 0.1295 0.141 Uiso 1 1 calc R . .
H24B H 0.213 0.4094 0.0806 0.141 Uiso 1 1 calc R . .
H24A H 0.2762 0.4484 0.151 0.141 Uiso 1 1 calc R . .
C25 C -0.1788(6) 0.4875(5) 0.2168(4) 0.0552(19) Uiso 1 1 d . . .
C26 C -0.1402(7) 0.5729(6) 0.2363(5) 0.072(2) Uiso 1 1 d . . .
H26 H -0.132 0.5915 0.2831 0.087 Uiso 1 1 calc R . .
C27 C -0.1128(9) 0.6326(8) 0.1853(6) 0.091(3) Uiso 1 1 d . . .
H27 H -0.0889 0.6925 0.1974 0.109 Uiso 1 1 calc R . .
C28 C -0.1209(9) 0.6040(8) 0.1210(6) 0.094(3) Uiso 1 1 d . . .
H28 H -0.0996 0.6439 0.0881 0.113 Uiso 1 1 calc R . .
C29 C -0.1574(9) 0.5222(8) 0.0998(6) 0.097(3) Uiso 1 1 d . . .
H29 H -0.1632 0.5046 0.0529 0.116 Uiso 1 1 calc R . .
C30 C -0.1867(7) 0.4632(7) 0.1487(5) 0.070(2) Uiso 1 1 d . . .
H30 H -0.213 0.4046 0.1345 0.084 Uiso 1 1 calc R . .
C31 C -0.2050(9) 0.4214(8) 0.2706(6) 0.104(4) Uiso 1 1 d . . .
H31A H -0.1945 0.4514 0.3157 0.155 Uiso 0.5 1 calc PR . .
H31B H -0.1606 0.3676 0.2723 0.155 Uiso 0.5 1 calc PR . .
H31C H -0.277 0.4026 0.2585 0.155 Uiso 0.5 1 calc PR . .
H31D H -0.2269 0.363 0.2486 0.155 Uiso 0.5 1 calc PR . .
H31E H -0.2608 0.4468 0.292 0.155 Uiso 0.5 1 calc PR . .
H31F H -0.1444 0.4118 0.3059 0.155 Uiso 0.5 1 calc PR . .
C32 C -0.0729(6) 0.0301(6) -0.0261(5) 0.053(4) Uiso 0.5 1 d PG . .
C33 C -0.0028(7) 0.0761(6) 0.0224(5) 0.060(4) Uiso 0.5 1 d PG . .
H33 H -0.0176 0.1363 0.0361 0.073 Uiso 0.5 1 calc PR . .
C34 C 0.0888(7) 0.0342(8) 0.0509(5) 0.062(4) Uiso 0.5 1 d PG . .
H34 H 0.1367 0.0657 0.0841 0.075 Uiso 0.5 1 calc PR . .
C35 C 0.1104(6) -0.0537(8) 0.0310(6) 0.077(5) Uiso 0.5 1 d PG . .
H35 H 0.173 -0.0823 0.0505 0.092 Uiso 0.5 1 calc PR . .
C36 C 0.0403(8) -0.0997(6) -0.0175(6) 0.059(4) Uiso 0.5 1 d PG . .
H36 H 0.0551 -0.1599 -0.0312 0.071 Uiso 0.5 1 calc PR . .
C37 C -0.0513(7) -0.0578(6) -0.0461(5) 0.036(3) Uiso 0.5 1 d PG . .
H37 H -0.0992 -0.0893 -0.0792 0.044 Uiso 0.5 1 calc PR . .
C38 C -0.1620(7) 0.0723(9) -0.0549(6) 0.119(9) Uiso 0.5 1 d PG . .
H38A H -0.2026 0.0309 -0.0878 0.179 Uiso 0.25 1 calc PR . .
H38B H -0.1459 0.1278 -0.0788 0.179 Uiso 0.25 1 calc PR . .
H38C H -0.2015 0.0885 -0.0187 0.179 Uiso 0.25 1 calc PR . .
H38D H -0.1641 0.1339 -0.0357 0.179 Uiso 0.25 1 calc PR . .
H38E H -0.2208 0.037 -0.0447 0.179 Uiso 0.25 1 calc PR . .
H38F H -0.1651 0.0762 -0.1048 0.179 Uiso 0.25 1 calc PR . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.420(5) . ?
Pb1 N1 2.427(5) . ?
Pb1 I1 2.9187(4) . ?
Pb1 Pb2 3.6662(3) . ?
Pb2 N2 2.360(5) . ?
Pb2 N1 2.374(5) . ?
Pb2 I2 2.9092(4) . ?
N1 C1 1.419(7) . ?
N1 H1N 0.82(6) . ?
N2 C13 1.428(7) . ?
N2 H2N 0.86(6) . ?
C1 C2 1.414(8) . ?
C1 C6 1.425(8) . ?
C2 C3 1.396(9) . ?
C2 C7 1.525(9) . ?
C3 C4 1.359(11) . ?
C3 H3 0.95 . ?
C4 C5 1.385(11) . ?
C4 H4 0.95 . ?
C5 C6 1.385(9) . ?
C5 H5 0.95 . ?
C6 C10 1.526(9) . ?
C7 C8 1.530(9) . ?
C7 C9 1.539(9) . ?
C7 H7 1 . ?
C8 H8C 0.98 . ?
C8 H8B 0.98 . ?
C8 H8A 0.98 . ?
C9 H9C 0.98 . ?
C9 H9B 0.98 . ?
C9 H9A 0.98 . ?
C10 C11 1.530(11) . ?
C10 C12 1.553(10) . ?
C10 H10 1 . ?
C11 H11C 0.98 . ?
C11 H11B 0.98 . ?
C11 H11A 0.98 . ?
C12 H12C 0.98 . ?
C12 H12B 0.98 . ?
C12 H12A 0.98 . ?
C13 C14 1.399(9) . ?
C13 C18 1.419(8) . ?
C14 C15 1.401(9) . ?
C14 C19 1.519(9) . ?
C15 C16 1.347(11) . ?
C15 H15 0.95 . ?
C16 C17 1.393(11) . ?
C16 H16 0.95 . ?
C17 C18 1.394(9) . ?
C17 H17 0.95 . ?
C18 C22 1.515(9) . ?
C19 C20 1.523(9) . ?
C19 C21 1.532(9) . ?
C19 H19 1 . ?
C20 H20C 0.98 . ?
C20 H20B 0.98 . ?
C20 H20A 0.98 . ?
C21 H21C 0.98 . ?
C21 H21B 0.98 . ?
C21 H21A 0.98 . ?
C22 C24 1.509(12) . ?
C22 C23 1.527(10) . ?
C22 H22 1 . ?
C23 H23C 0.98 . ?
C23 H23B 0.98 . ?
C23 H23A 0.98 . ?
C24 H24C 0.98 . ?
C24 H24B 0.98 . ?
C24 H24A 0.98 . ?
C25 C30 1.375(11) . ?
C25 C26 1.381(12) . ?
C25 C31 1.517(13) . ?
C26 C27 1.422(14) . ?
C26 H26 0.95 . ?
C27 C28 1.322(14) . ?
C27 H27 0.95 . ?
C28 C29 1.333(15) . ?
C28 H28 0.95 . ?
C29 C30 1.395(14) . ?
C29 H29 0.95 . ?
C30 H30 0.95 . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C31 H31C 0.98 . ?
C31 H31D 0.98 . ?
C31 H31E 0.98 . ?
C31 H31F 0.98 . ?
C32 C38 1.3674 . ?
C32 C33 1.39 . ?
C32 C37 1.39 . ?
C33 C34 1.39 . ?
C33 H33 0.95 . ?
C34 C35 1.39 . ?
C34 H34 0.95 . ?
C35 C36 1.39 . ?
C35 H35 0.95 . ?
C36 C37 1.39 . ?
C36 H36 0.95 . ?
C37 H37 0.95 . ?
C38 H38A 0.98 . ?
C38 H38B 0.98 . ?
C38 H38C 0.98 . ?
C38 H38D 0.98 . ?
C38 H38E 0.98 . ?
C38 H38F 0.98 . ?

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 76.08(16) . . ?
N2 Pb1 I1 85.75(11) . . ?
N1 Pb1 I1 86.47(12) . . ?
N2 Pb1 Pb2 39.33(11) . . ?
N1 Pb1 Pb2 39.68(11) . . ?
I1 Pb1 Pb2 96.637(10) . . ?
N2 Pb2 N1 78.22(16) . . ?
N2 Pb2 I2 88.08(11) . . ?
N1 Pb2 I2 92.38(12) . . ?
N2 Pb2 Pb1 40.52(11) . . ?
N1 Pb2 Pb1 40.75(12) . . ?
I2 Pb2 Pb1 102.303(11) . . ?
C1 N1 Pb2 112.3(3) . . ?
C1 N1 Pb1 130.7(4) . . ?
Pb2 N1 Pb1 99.57(17) . . ?
C1 N1 H1N 106(4) . . ?
Pb2 N1 H1N 104(4) . . ?
Pb1 N1 H1N 101(4) . . ?
C13 N2 Pb2 123.0(3) . . ?
C13 N2 Pb1 121.2(4) . . ?
Pb2 N2 Pb1 100.15(17) . . ?
C13 N2 H2N 110(4) . . ?
Pb2 N2 H2N 100(4) . . ?
Pb1 N2 H2N 97(4) . . ?
C2 C1 N1 119.3(5) . . ?
C2 C1 C6 119.6(5) . . ?
N1 C1 C6 121.0(5) . . ?
C3 C2 C1 118.8(6) . . ?
C3 C2 C7 119.3(6) . . ?
C1 C2 C7 121.7(5) . . ?
C4 C3 C2 121.5(7) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 120.1(7) . . ?
C3 C4 H4 120 . . ?
C5 C4 H4 120 . . ?
C6 C5 C4 121.6(7) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C1 118.3(6) . . ?
C5 C6 C10 120.8(6) . . ?
C1 C6 C10 120.8(5) . . ?
C2 C7 C8 113.6(6) . . ?
C2 C7 C9 109.8(6) . . ?
C8 C7 C9 110.3(5) . . ?
C2 C7 H7 107.6 . . ?
C8 C7 H7 107.6 . . ?
C9 C7 H7 107.6 . . ?
C7 C8 H8C 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8C C8 H8B 109.5 . . ?
C7 C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
C7 C9 H9C 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9C C9 H9B 109.5 . . ?
C7 C9 H9A 109.5 . . ?
H9C C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
C6 C10 C11 110.6(5) . . ?
C6 C10 C12 112.9(6) . . ?
C11 C10 C12 109.7(7) . . ?
C6 C10 H10 107.8 . . ?
C11 C10 H10 107.8 . . ?
C12 C10 H10 107.8 . . ?
C10 C11 H11C 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11C C11 H11B 109.5 . . ?
C10 C11 H11A 109.5 . . ?
H11C C11 H11A 109.5 . . ?
H11B C11 H11A 109.5 . . ?
C10 C12 H12C 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12C C12 H12B 109.5 . . ?
C10 C12 H12A 109.5 . . ?
H12C C12 H12A 109.5 . . ?
H12B C12 H12A 109.5 . . ?
C14 C13 C18 120.2(6) . . ?
C14 C13 N2 119.2(5) . . ?
C18 C13 N2 120.5(5) . . ?
C13 C14 C15 118.1(6) . . ?
C13 C14 C19 123.7(6) . . ?
C15 C14 C19 118.2(6) . . ?
C16 C15 C14 122.3(7) . . ?
C16 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C15 C16 C17 120.2(7) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C16 C17 C18 120.3(7) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C13 118.8(6) . . ?
C17 C18 C22 118.0(6) . . ?
C13 C18 C22 123.1(6) . . ?
C14 C19 C20 112.6(6) . . ?
C14 C19 C21 112.9(6) . . ?
C20 C19 C21 111.1(5) . . ?
C14 C19 H19 106.6 . . ?
C20 C19 H19 106.6 . . ?
C21 C19 H19 106.6 . . ?
C19 C20 H20C 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20C C20 H20B 109.5 . . ?
C19 C20 H20A 109.5 . . ?
H20C C20 H20A 109.5 . . ?
H20B C20 H20A 109.5 . . ?
C19 C21 H21C 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21C C21 H21B 109.5 . . ?
C19 C21 H21A 109.5 . . ?
H21C C21 H21A 109.5 . . ?
H21B C21 H21A 109.5 . . ?
C24 C22 C18 112.5(6) . . ?
C24 C22 C23 110.8(7) . . ?
C18 C22 C23 112.9(7) . . ?
C24 C22 H22 106.7 . . ?
C18 C22 H22 106.7 . . ?
C23 C22 H22 106.7 . . ?
C22 C23 H23C 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23C C23 H23B 109.5 . . ?
C22 C23 H23A 109.5 . . ?
H23C C23 H23A 109.5 . . ?
H23B C23 H23A 109.5 . . ?
C22 C24 H24C 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24C C24 H24B 109.5 . . ?
C22 C24 H24A 109.5 . . ?
H24C C24 H24A 109.5 . . ?
H24B C24 H24A 109.5 . . ?
C30 C25 C26 118.1(8) . . ?
C30 C25 C31 121.8(8) . . ?
C26 C25 C31 120.0(8) . . ?
C25 C26 C27 119.0(9) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
C28 C27 C26 119.4(11) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C27 C28 C29 123.7(12) . . ?
C27 C28 H28 118.2 . . ?
C29 C28 H28 118.2 . . ?
C28 C29 C30 117.8(11) . . ?
C28 C29 H29 121.1 . . ?
C30 C29 H29 121.1 . . ?
C25 C30 C29 121.9(9) . . ?
C25 C30 H30 119 . . ?
C29 C30 H30 119 . . ?
C25 C31 H31A 109.5 . . ?
C25 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C25 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C25 C31 H31D 109.5 . . ?
H31A C31 H31D 141.1 . . ?
H31B C31 H31D 56.3 . . ?
H31C C31 H31D 56.3 . . ?
C25 C31 H31E 109.5 . . ?
H31A C31 H31E 56.3 . . ?
H31B C31 H31E 141.1 . . ?
H31C C31 H31E 56.3 . . ?
H31D C31 H31E 109.5 . . ?
C25 C31 H31F 109.5 . . ?
H31A C31 H31F 56.3 . . ?
H31B C31 H31F 56.3 . . ?
H31C C31 H31F 141.1 . . ?
H31D C31 H31F 109.5 . . ?
H31E C31 H31F 109.5 . . ?
C38 C32 C33 119.7 . . ?
C38 C32 C37 120.3 . . ?
C33 C32 C37 120 . . ?
C32 C33 C34 120 . . ?
C32 C33 H33 120 . . ?
C34 C33 H33 120 . . ?
C35 C34 C33 120 . . ?
C35 C34 H34 120 . . ?
C33 C34 H34 120 . . ?
C36 C35 C34 120 . . ?
C36 C35 H35 120 . . ?
C34 C35 H35 120 . . ?
C35 C36 C37 120 . . ?
C35 C36 H36 120 . . ?
C37 C36 H36 120 . . ?
C36 C37 C32 120 . . ?
C36 C37 H37 120 . . ?
C32 C37 H37 120 . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C32 C38 H38D 109.5 . . ?
H38A C38 H38D 141.1 . . ?
H38B C38 H38D 56.3 . . ?
H38C C38 H38D 56.3 . . ?
C32 C38 H38E 109.5 . . ?
H38A C38 H38E 56.3 . . ?
H38B C38 H38E 141.1 . . ?
H38C C38 H38E 56.3 . . ?
H38D C38 H38E 109.5 . . ?
C32 C38 H38F 109.5 . . ?
H38A C38 H38F 56.3 . . ?
H38B C38 H38F 56.3 . . ?
H38C C38 H38F 141.1 . . ?
H38D C38 H38F 109.5 . . ?
H38E C38 H38F 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 991977'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(12)-apr410

_audit_creation_date             2010-04-21T16:52:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C65 H87 N5 O Sn), C7 H8'
_chemical_formula_sum            'C137 H182 N10 O2 Sn2'
_chemical_formula_weight         2238.35
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8899(2)
_cell_length_b                   11.7384(2)
_cell_length_c                   25.2778(3)
_cell_angle_alpha                93.961(1)
_cell_angle_beta                 99.556(1)
_cell_angle_gamma                103.239(1)
_cell_volume                     3082.37(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    62128
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.103
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1190
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.8604
_exptl_absorpt_correction_T_max  0.9597

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.184057E-1
_diffrn_orient_matrix_ub_12      0.696852E-1
_diffrn_orient_matrix_ub_13      0.277407E-1
_diffrn_orient_matrix_ub_21      0.942523E-1
_diffrn_orient_matrix_ub_22      0.80576E-2
_diffrn_orient_matrix_ub_23      0.24318E-2
_diffrn_orient_matrix_ub_31      0.4754E-3
_diffrn_orient_matrix_ub_32      0.532418E-1
_diffrn_orient_matrix_ub_33      -0.292268E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_number            51415
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_full        27.09
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_reflns_number_total             13304
_reflns_number_gt                11507
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 The toluene solvate is disordered across an inversion centre and was refined
 as a rigid body (AFIX 66) at half occupancy with common displacement para-
 meters; the hydrogen on nitrogen was located on the difference map, all others
 were riding  

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0455P)²+2.8703P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         13304
_refine_ls_number_parameters     664
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1001
_refine_ls_wR_factor_gt          0.0957
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.445
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.075

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn Sn 0.386268(16) 0.210686(14) 0.173270(6) 0.01857(6) Uani 1 1 d . . .
O O 0.57494(16) 0.28422(14) 0.21545(6) 0.0222(4) Uani 1 1 d . . .
N1 N 0.4665(2) 0.28868(17) 0.10415(8) 0.0220(4) Uani 1 1 d . . .
N2 N 0.42103(19) 0.04973(17) 0.13445(8) 0.0198(4) Uani 1 1 d . . .
N3 N 0.4800(2) 0.18871(17) 0.27648(8) 0.0222(4) Uani 1 1 d . . .
N4 N 0.79063(19) 0.52917(17) 0.35227(8) 0.0202(4) Uani 1 1 d . . .
N5 N 0.86499(19) 0.33787(19) 0.37638(8) 0.0198(4) Uani 1 1 d . . .
H5N H 0.870(3) 0.408(3) 0.3788(11) 0.026(8) Uiso 1 1 d . . .
C1 C 0.4277(2) 0.2325(2) 0.05500(9) 0.0239(5) Uani 1 1 d . . .
C2 C 0.3751(3) 0.1097(2) 0.04524(9) 0.0257(5) Uani 1 1 d . . .
H2 H 0.3285 0.0809 0.0098 0.031 Uiso 1 1 calc R . .
C3 C 0.3829(2) 0.0253(2) 0.08108(9) 0.0220(5) Uani 1 1 d . . .
C4 C 0.4387(3) 0.2982(2) 0.00609(10) 0.0356(7) Uani 1 1 d . . .
H4A H 0.4165 0.3737 0.0123 0.053 Uiso 1 1 calc R . .
H4B H 0.3798 0.2512 -0.0255 0.053 Uiso 1 1 calc R . .
H4C H 0.527 0.3124 -0.0003 0.053 Uiso 1 1 calc R . .
C5 C 0.3476(3) -0.1016(2) 0.05571(11) 0.0308(6) Uani 1 1 d . . .
H5A H 0.392 -0.1485 0.0792 0.046 Uiso 1 1 calc R . .
H5B H 0.3734 -0.105 0.0204 0.046 Uiso 1 1 calc R . .
H5C H 0.2546 -0.1333 0.0511 0.046 Uiso 1 1 calc R . .
C6 C 0.5340(3) 0.4110(2) 0.11286(9) 0.0242(5) Uani 1 1 d . . .
C7 C 0.6689(3) 0.4407(2) 0.12045(10) 0.0280(6) Uani 1 1 d . . .
C8 C 0.7326(3) 0.5600(2) 0.13134(11) 0.0349(7) Uani 1 1 d . . .
H8 H 0.8235 0.5826 0.1356 0.042 Uiso 1 1 calc R . .
C9 C 0.6651(3) 0.6457(2) 0.13607(11) 0.0397(7) Uani 1 1 d . . .
H9 H 0.71 0.7263 0.1438 0.048 Uiso 1 1 calc R . .
C10 C 0.5337(3) 0.6150(2) 0.12967(11) 0.0364(7) Uani 1 1 d . . .
H10 H 0.4888 0.6747 0.1334 0.044 Uiso 1 1 calc R . .
C11 C 0.4648(3) 0.4972(2) 0.11774(10) 0.0285(6) Uani 1 1 d . . .
C12 C 0.7452(3) 0.3481(2) 0.11712(11) 0.0339(6) Uani 1 1 d . . .
H12 H 0.6843 0.2694 0.1153 0.041 Uiso 1 1 calc R . .
C13 C 0.8027(4) 0.3495(4) 0.06590(14) 0.0580(10) Uani 1 1 d . . .
H13A H 0.8511 0.2888 0.065 0.087 Uiso 1 1 calc R . .
H13B H 0.8603 0.4269 0.0657 0.087 Uiso 1 1 calc R . .
H13C H 0.7335 0.3337 0.0342 0.087 Uiso 1 1 calc R . .
C14 C 0.8500(3) 0.3603(3) 0.16667(13) 0.0457(8) Uani 1 1 d . . .
H14A H 0.8963 0.2986 0.1627 0.069 Uiso 1 1 calc R . .
H14B H 0.8112 0.3523 0.1989 0.069 Uiso 1 1 calc R . .
H14C H 0.9101 0.4378 0.1702 0.069 Uiso 1 1 calc R . .
C15 C 0.3195(3) 0.4665(2) 0.11028(12) 0.0360(7) Uani 1 1 d . . .
H15 H 0.2886 0.3793 0.101 0.043 Uiso 1 1 calc R . .
C16 C 0.2589(4) 0.5242(3) 0.06329(15) 0.0552(9) Uani 1 1 d . . .
H16A H 0.1652 0.5022 0.0596 0.083 Uiso 1 1 calc R . .
H16B H 0.2828 0.4971 0.0298 0.083 Uiso 1 1 calc R . .
H16C H 0.2899 0.61 0.0705 0.083 Uiso 1 1 calc R . .
C17 C 0.2733(3) 0.4986(3) 0.16199(15) 0.0495(8) Uani 1 1 d . . .
H17A H 0.1792 0.4773 0.1554 0.074 Uiso 1 1 calc R . .
H17B H 0.3048 0.5835 0.1729 0.074 Uiso 1 1 calc R . .
H17C H 0.3063 0.4555 0.1908 0.074 Uiso 1 1 calc R . .
C18 C 0.4415(2) -0.0401(2) 0.16857(9) 0.0205(5) Uani 1 1 d . . .
C19 C 0.5686(3) -0.0475(2) 0.18713(10) 0.0250(5) Uani 1 1 d . . .
C20 C 0.5877(3) -0.1263(2) 0.22470(11) 0.0326(6) Uani 1 1 d . . .
H20 H 0.6725 -0.1322 0.2381 0.039 Uiso 1 1 calc R . .
C21 C 0.4864(3) -0.1956(2) 0.24281(11) 0.0364(7) Uani 1 1 d . . .
H21 H 0.5018 -0.2484 0.2685 0.044 Uiso 1 1 calc R . .
C22 C 0.3628(3) -0.1885(2) 0.22359(11) 0.0320(6) Uani 1 1 d . . .
H22 H 0.2936 -0.2371 0.2361 0.038 Uiso 1 1 calc R . .
C23 C 0.3373(3) -0.1111(2) 0.18610(10) 0.0250(5) Uani 1 1 d . . .
C24 C 0.6805(3) 0.0307(2) 0.16736(11) 0.0305(6) Uani 1 1 d . . .
H24 H 0.6712 0.1135 0.1712 0.037 Uiso 1 1 calc R . .
C25 C 0.6816(3) -0.0034(3) 0.10794(12) 0.0376(7) Uani 1 1 d . . .
H25A H 0.7544 0.0494 0.0971 0.056 Uiso 1 1 calc R . .
H25B H 0.6014 0.0032 0.0857 0.056 Uiso 1 1 calc R . .
H25C H 0.6896 -0.0848 0.103 0.056 Uiso 1 1 calc R . .
C26 C 0.8119(3) 0.0287(4) 0.19969(14) 0.0512(9) Uani 1 1 d . . .
H26A H 0.8796 0.0806 0.1853 0.077 Uiso 1 1 calc R . .
H26B H 0.8231 -0.0518 0.1967 0.077 Uiso 1 1 calc R . .
H26C H 0.817 0.0561 0.2377 0.077 Uiso 1 1 calc R . .
C27 C 0.1998(3) -0.1025(2) 0.16749(11) 0.0299(6) Uani 1 1 d . . .
H27 H 0.1994 -0.05 0.138 0.036 Uiso 1 1 calc R . .
C28 C 0.1101(3) -0.2236(3) 0.14482(14) 0.0444(8) Uani 1 1 d . . .
H28A H 0.0227 -0.2147 0.1331 0.067 Uiso 1 1 calc R . .
H28B H 0.1103 -0.277 0.1729 0.067 Uiso 1 1 calc R . .
H28C H 0.1401 -0.2561 0.114 0.067 Uiso 1 1 calc R . .
C29 C 0.1513(3) -0.0463(3) 0.21419(13) 0.0401(7) Uani 1 1 d . . .
H29A H 0.0628 -0.041 0.2017 0.06 Uiso 1 1 calc R . .
H29B H 0.2063 0.0328 0.2264 0.06 Uiso 1 1 calc R . .
H29C H 0.1538 -0.095 0.2441 0.06 Uiso 1 1 calc R . .
C30 C 0.5766(2) 0.2667(2) 0.26640(9) 0.0196(5) Uani 1 1 d . . .
C31 C 0.4660(2) 0.1655(2) 0.32962(10) 0.0232(5) Uani 1 1 d . . .
C32 C 0.4839(2) 0.2529(2) 0.37259(10) 0.0257(5) Uani 1 1 d . . .
H32 H 0.5052 0.3336 0.3667 0.031 Uiso 1 1 calc R . .
C33 C 0.4707(3) 0.2227(3) 0.42385(11) 0.0314(6) Uani 1 1 d . . .
H33 H 0.4849 0.283 0.4528 0.038 Uiso 1 1 calc R . .
C34 C 0.4371(3) 0.1059(3) 0.43323(11) 0.0343(6) Uani 1 1 d . . .
H34 H 0.4293 0.0859 0.4685 0.041 Uiso 1 1 calc R . .
C35 C 0.4151(3) 0.0191(3) 0.39085(12) 0.0365(7) Uani 1 1 d . . .
H35 H 0.3903 -0.0612 0.3969 0.044 Uiso 1 1 calc R . .
C36 C 0.4288(3) 0.0478(2) 0.33923(11) 0.0315(6) Uani 1 1 d . . .
H36 H 0.4127 -0.013 0.3103 0.038 Uiso 1 1 calc R . .
C37 C 0.7057(2) 0.4655(2) 0.31259(9) 0.0187(5) Uani 1 1 d . . .
C38 C 0.6882(2) 0.33835(19) 0.30642(9) 0.0170(4) Uani 1 1 d . . .
C39 C 0.7663(2) 0.2801(2) 0.33722(9) 0.0178(5) Uani 1 1 d . . .
C40 C 0.6211(3) 0.5182(2) 0.27246(10) 0.0295(6) Uani 1 1 d . . .
H40A H 0.6412 0.6037 0.2818 0.044 Uiso 1 1 calc R . .
H40B H 0.5307 0.4843 0.2736 0.044 Uiso 1 1 calc R . .
H40C H 0.6368 0.5007 0.2361 0.044 Uiso 1 1 calc R . .
C41 C 0.7463(3) 0.1487(2) 0.32927(10) 0.0256(5) Uani 1 1 d . . .
H41A H 0.8284 0.1293 0.3273 0.038 Uiso 1 1 calc R . .
H41B H 0.6851 0.1169 0.2956 0.038 Uiso 1 1 calc R . .
H41C H 0.7122 0.1143 0.3597 0.038 Uiso 1 1 calc R . .
C42 C 0.8095(2) 0.6541(2) 0.36147(9) 0.0239(5) Uani 1 1 d . . .
C43 C 0.9236(3) 0.7247(2) 0.35001(10) 0.0301(6) Uani 1 1 d . . .
C44 C 0.9460(3) 0.8469(2) 0.36144(12) 0.0398(7) Uani 1 1 d . . .
H44 H 1.0217 0.8964 0.3538 0.048 Uiso 1 1 calc R . .
C45 C 0.8610(3) 0.8970(2) 0.38335(12) 0.0427(8) Uani 1 1 d . . .
H45 H 0.8775 0.9802 0.3902 0.051 Uiso 1 1 calc R . .
C46 C 0.7518(3) 0.8264(2) 0.39535(12) 0.0385(7) Uani 1 1 d . . .
H46 H 0.694 0.862 0.4107 0.046 Uiso 1 1 calc R . .
C47 C 0.7237(3) 0.7035(2) 0.38547(10) 0.0287(6) Uani 1 1 d . . .
C48 C 1.0143(3) 0.6677(3) 0.32472(11) 0.0368(7) Uani 1 1 d . . .
H48 H 1.01 0.5898 0.339 0.044 Uiso 1 1 calc R . .
C49 C 0.9693(4) 0.6433(4) 0.26360(13) 0.0597(11) Uani 1 1 d . . .
H49A H 1.0287 0.6061 0.2478 0.09 Uiso 1 1 calc R . .
H49B H 0.9674 0.7177 0.2484 0.09 Uiso 1 1 calc R . .
H49C H 0.883 0.5907 0.2554 0.09 Uiso 1 1 calc R . .
C50 C 1.1551(3) 0.7373(3) 0.33828(13) 0.0444(8) Uani 1 1 d . . .
H50A H 1.2075 0.6945 0.3207 0.067 Uiso 1 1 calc R . .
H50B H 1.185 0.7468 0.3775 0.067 Uiso 1 1 calc R . .
H50C H 1.1628 0.815 0.3254 0.067 Uiso 1 1 calc R . .
C51 C 0.6072(3) 0.6253(3) 0.40170(12) 0.0367(7) Uani 1 1 d . . .
H51 H 0.5687 0.5605 0.3717 0.044 Uiso 1 1 calc R . .
C52 C 0.5027(4) 0.6878(4) 0.41016(17) 0.0615(10) Uani 1 1 d . . .
H52A H 0.4311 0.6321 0.4205 0.092 Uiso 1 1 calc R . .
H52B H 0.4721 0.7181 0.3766 0.092 Uiso 1 1 calc R . .
H52C H 0.5377 0.7534 0.4389 0.092 Uiso 1 1 calc R . .
C53 C 0.6488(4) 0.5678(3) 0.45237(14) 0.0497(8) Uani 1 1 d . . .
H53A H 0.573 0.5174 0.4624 0.074 Uiso 1 1 calc R . .
H53B H 0.6917 0.6292 0.4822 0.074 Uiso 1 1 calc R . .
H53C H 0.7081 0.52 0.4448 0.074 Uiso 1 1 calc R . .
C54 C 0.9561(2) 0.2819(2) 0.40483(10) 0.0229(5) Uani 1 1 d . . .
C55 C 1.0602(3) 0.2656(2) 0.38129(10) 0.0290(6) Uani 1 1 d . . .
C56 C 1.1429(3) 0.2057(3) 0.40865(12) 0.0392(7) Uani 1 1 d . . .
H56 H 1.2125 0.1916 0.3932 0.047 Uiso 1 1 calc R . .
C57 C 1.1262(3) 0.1665(3) 0.45763(13) 0.0423(7) Uani 1 1 d . . .
H57 H 1.1844 0.1262 0.4756 0.051 Uiso 1 1 calc R . .
C58 C 1.0257(3) 0.1852(3) 0.48064(12) 0.0384(7) Uani 1 1 d . . .
H58 H 1.0164 0.1593 0.5149 0.046 Uiso 1 1 calc R . .
C59 C 0.9370(3) 0.2416(2) 0.45453(10) 0.0274(5) Uani 1 1 d . . .
C60 C 1.0849(3) 0.3134(3) 0.32890(12) 0.0412(7) Uani 1 1 d . . .
H60 H 1.0064 0.3369 0.3115 0.049 Uiso 1 1 calc R . .
C61 C 1.1133(4) 0.2222(4) 0.28931(14) 0.0595(10) Uani 1 1 d . . .
H61A H 1.1285 0.2572 0.2562 0.089 Uiso 1 1 calc R . .
H61B H 1.0397 0.1536 0.2807 0.089 Uiso 1 1 calc R . .
H61C H 1.1897 0.1977 0.3058 0.089 Uiso 1 1 calc R . .
C62 C 1.1966(4) 0.4224(3) 0.34054(16) 0.0602(10) Uani 1 1 d . . .
H62A H 1.212 0.4532 0.3065 0.09 Uiso 1 1 calc R . .
H62B H 1.2739 0.4016 0.3587 0.09 Uiso 1 1 calc R . .
H62C H 1.1758 0.4827 0.3639 0.09 Uiso 1 1 calc R . .
C63 C 0.8251(3) 0.2598(3) 0.47955(11) 0.0327(6) Uani 1 1 d . . .
H63 H 0.7591 0.2751 0.4501 0.039 Uiso 1 1 calc R . .
C64 C 0.7617(3) 0.1512(3) 0.50421(13) 0.0453(8) Uani 1 1 d . . .
H64A H 0.6898 0.167 0.5197 0.068 Uiso 1 1 calc R . .
H64B H 0.8248 0.1327 0.5326 0.068 Uiso 1 1 calc R . .
H64C H 0.7299 0.0841 0.4761 0.068 Uiso 1 1 calc R . .
C65 C 0.8665(3) 0.3677(3) 0.52145(13) 0.0461(8) Uani 1 1 d . . .
H65A H 0.7926 0.3782 0.537 0.069 Uiso 1 1 calc R . .
H65B H 0.8997 0.4376 0.5042 0.069 Uiso 1 1 calc R . .
H65C H 0.9338 0.3566 0.5501 0.069 Uiso 1 1 calc R . .
C1S C -0.0057(7) -0.0263(5) -0.0111(3) 0.1037(14) Uiso 0.5 1 d PG A -1
C2S C -0.0105(8) -0.0083(6) 0.0434(3) 0.1037(14) Uiso 0.5 1 d PG A -1
H2S H -0.0382 -0.0736 0.0624 0.124 Uiso 0.5 1 calc PR A -1
C3S C 0.0253(8) 0.1052(7) 0.0701(2) 0.1037(14) Uiso 0.5 1 d PG A -1
H3S H 0.022 0.1174 0.1073 0.124 Uiso 0.5 1 calc PR A -1
C4S C 0.0658(7) 0.2007(5) 0.0423(3) 0.1037(14) Uiso 0.5 1 d PG A -1
H4S H 0.0903 0.2783 0.0605 0.124 Uiso 0.5 1 calc PR A -1
C5S C 0.0707(7) 0.1828(5) -0.0122(3) 0.1037(14) Uiso 0.5 1 d PG A -1
H5S H 0.0984 0.2481 -0.0312 0.124 Uiso 0.5 1 calc PR A -1
C6S C 0.0349(7) 0.0693(5) -0.0389(2) 0.1037(14) Uiso 0.5 1 d PG A -1
H6S H 0.0382 0.057 -0.0761 0.124 Uiso 0.5 1 calc PR A -1
C7S C -0.0509(10) -0.1571(5) -0.0499(4) 0.1037(14) Uiso 0.5 1 d PG A -1
H7S1 H -0.0377 -0.1452 -0.0867 0.155 Uiso 0.25 1 calc PR A -1
H7S2 H -0.1419 -0.1924 -0.0505 0.155 Uiso 0.25 1 calc PR A -1
H7S3 H 0.0007 -0.2098 -0.035 0.155 Uiso 0.25 1 calc PR A -1
H7S4 H -0.0815 -0.2197 -0.0281 0.155 Uiso 0.25 1 calc PR A -1
H7S5 H 0.0227 -0.1725 -0.0643 0.155 Uiso 0.25 1 calc PR A -1
H7S6 H -0.12 -0.1551 -0.0798 0.155 Uiso 0.25 1 calc PR A -1



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Sn O 2.1063(16) . ?
Sn N2 2.2070(19) . ?
Sn N1 2.239(2) . ?
O C30 1.316(3) . ?
N1 C1 1.320(3) . ?
N1 C6 1.439(3) . ?
N2 C3 1.334(3) . ?
N2 C18 1.440(3) . ?
N3 C30 1.300(3) . ?
N3 C31 1.415(3) . ?
N4 C37 1.301(3) . ?
N4 C42 1.431(3) . ?
N5 C39 1.348(3) . ?
N5 C54 1.435(3) . ?
N5 H5N 0.81(3) . ?
C1 C2 1.411(3) . ?
C1 C4 1.508(3) . ?
C2 C3 1.395(3) . ?
C2 H2 0.95 . ?
C3 C5 1.517(3) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C11 1.403(4) . ?
C6 C7 1.407(4) . ?
C7 C8 1.399(4) . ?
C7 C12 1.518(4) . ?
C8 C9 1.385(4) . ?
C8 H8 0.95 . ?
C9 C10 1.371(5) . ?
C9 H9 0.95 . ?
C10 C11 1.400(4) . ?
C10 H10 0.95 . ?
C11 C15 1.517(4) . ?
C12 C14 1.522(4) . ?
C12 C13 1.528(4) . ?
C12 H12 1 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 C17 1.530(4) . ?
C15 C16 1.536(4) . ?
C15 H15 1 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 C23 1.401(3) . ?
C18 C19 1.411(4) . ?
C19 C20 1.394(4) . ?
C19 C24 1.526(4) . ?
C20 C21 1.377(4) . ?
C20 H20 0.95 . ?
C21 C22 1.376(4) . ?
C21 H21 0.95 . ?
C22 C23 1.396(4) . ?
C22 H22 0.95 . ?
C23 C27 1.521(4) . ?
C24 C25 1.530(4) . ?
C24 C26 1.532(4) . ?
C24 H24 1 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 C29 1.539(4) . ?
C27 C28 1.539(4) . ?
C27 H27 1 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 C38 1.488(3) . ?
C31 C36 1.397(4) . ?
C31 C32 1.399(3) . ?
C32 C33 1.388(4) . ?
C32 H32 0.95 . ?
C33 C34 1.383(4) . ?
C33 H33 0.95 . ?
C34 C35 1.377(4) . ?
C34 H34 0.95 . ?
C35 C36 1.393(4) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C37 C38 1.455(3) . ?
C37 C40 1.515(3) . ?
C38 C39 1.384(3) . ?
C39 C41 1.502(3) . ?
C40 H40A 0.98 . ?
C40 H40B 0.98 . ?
C40 H40C 0.98 . ?
C41 H41A 0.98 . ?
C41 H41B 0.98 . ?
C41 H41C 0.98 . ?
C42 C47 1.401(4) . ?
C42 C43 1.412(4) . ?
C43 C44 1.400(4) . ?
C43 C48 1.512(4) . ?
C44 C45 1.372(5) . ?
C44 H44 0.95 . ?
C45 C46 1.377(5) . ?
C45 H45 0.95 . ?
C46 C47 1.400(4) . ?
C46 H46 0.95 . ?
C47 C51 1.520(4) . ?
C48 C49 1.527(4) . ?
C48 C50 1.532(4) . ?
C48 H48 1 . ?
C49 H49A 0.98 . ?
C49 H49B 0.98 . ?
C49 H49C 0.98 . ?
C50 H50A 0.98 . ?
C50 H50B 0.98 . ?
C50 H50C 0.98 . ?
C51 C52 1.523(4) . ?
C51 C53 1.539(5) . ?
C51 H51 1 . ?
C52 H52A 0.98 . ?
C52 H52B 0.98 . ?
C52 H52C 0.98 . ?
C53 H53A 0.98 . ?
C53 H53B 0.98 . ?
C53 H53C 0.98 . ?
C54 C59 1.403(4) . ?
C54 C55 1.409(4) . ?
C55 C56 1.391(4) . ?
C55 C60 1.514(4) . ?
C56 C57 1.376(4) . ?
C56 H56 0.95 . ?
C57 C58 1.374(4) . ?
C57 H57 0.95 . ?
C58 C59 1.396(4) . ?
C58 H58 0.95 . ?
C59 C63 1.513(4) . ?
C60 C62 1.524(5) . ?
C60 C61 1.532(5) . ?
C60 H60 1 . ?
C61 H61A 0.98 . ?
C61 H61B 0.98 . ?
C61 H61C 0.98 . ?
C62 H62A 0.98 . ?
C62 H62B 0.98 . ?
C62 H62C 0.98 . ?
C63 C65 1.524(4) . ?
C63 C64 1.530(4) . ?
C63 H63 1 . ?
C64 H64A 0.98 . ?
C64 H64B 0.98 . ?
C64 H64C 0.98 . ?
C65 H65A 0.98 . ?
C65 H65B 0.98 . ?
C65 H65C 0.98 . ?
C1S C2S 1.39 . ?
C1S C6S 1.39 . ?
C1S C7S 1.6882 . ?
C2S C3S 1.39 . ?
C2S H2S 0.95 . ?
C3S C4S 1.39 . ?
C3S H3S 0.95 . ?
C4S C5S 1.39 . ?
C4S H4S 0.95 . ?
C5S C6S 1.39 . ?
C5S H5S 0.95 . ?
C6S H6S 0.95 . ?
C7S H7S1 0.98 . ?
C7S H7S2 0.98 . ?
C7S H7S3 0.98 . ?
C7S H7S4 0.98 . ?
C7S H7S5 0.98 . ?
C7S H7S6 0.98 . ?

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
O Sn N2 97.66(7) . . ?
O Sn N1 82.73(7) . . ?
N2 Sn N1 81.85(7) . . ?
C30 O Sn 107.25(14) . . ?
C1 N1 C6 121.1(2) . . ?
C1 N1 Sn 119.94(16) . . ?
C6 N1 Sn 117.19(14) . . ?
C3 N2 C18 121.75(19) . . ?
C3 N2 Sn 117.83(16) . . ?
C18 N2 Sn 116.95(14) . . ?
C30 N3 C31 122.4(2) . . ?
C37 N4 C42 122.1(2) . . ?
C39 N5 C54 123.3(2) . . ?
C39 N5 H5N 111(2) . . ?
C54 N5 H5N 126(2) . . ?
N1 C1 C2 122.5(2) . . ?
N1 C1 C4 120.7(2) . . ?
C2 C1 C4 116.7(2) . . ?
C3 C2 C1 128.2(2) . . ?
C3 C2 H2 115.9 . . ?
C1 C2 H2 115.9 . . ?
N2 C3 C2 124.5(2) . . ?
N2 C3 C5 119.7(2) . . ?
C2 C3 C5 115.8(2) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 121.6(2) . . ?
C11 C6 N1 119.3(2) . . ?
C7 C6 N1 119.0(2) . . ?
C8 C7 C6 117.8(3) . . ?
C8 C7 C12 120.0(3) . . ?
C6 C7 C12 122.1(2) . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 121.1(3) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C6 118.1(3) . . ?
C10 C11 C15 119.6(3) . . ?
C6 C11 C15 122.2(2) . . ?
C7 C12 C14 112.4(2) . . ?
C7 C12 C13 111.6(3) . . ?
C14 C12 C13 110.2(3) . . ?
C7 C12 H12 107.4 . . ?
C14 C12 H12 107.4 . . ?
C13 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 112.1(3) . . ?
C11 C15 C16 111.7(3) . . ?
C17 C15 C16 110.4(3) . . ?
C11 C15 H15 107.5 . . ?
C17 C15 H15 107.5 . . ?
C16 C15 H15 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 121.5(2) . . ?
C23 C18 N2 119.9(2) . . ?
C19 C18 N2 118.4(2) . . ?
C20 C19 C18 117.6(2) . . ?
C20 C19 C24 121.9(2) . . ?
C18 C19 C24 120.5(2) . . ?
C21 C20 C19 121.5(3) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 H21 120 . . ?
C20 C21 H21 120 . . ?
C21 C22 C23 121.3(3) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C18 118.1(2) . . ?
C22 C23 C27 119.6(2) . . ?
C18 C23 C27 122.3(2) . . ?
C19 C24 C25 112.5(2) . . ?
C19 C24 C26 113.2(3) . . ?
C25 C24 C26 107.2(2) . . ?
C19 C24 H24 107.9 . . ?
C25 C24 H24 107.9 . . ?
C26 C24 H24 107.9 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C29 110.2(2) . . ?
C23 C27 C28 111.7(2) . . ?
C29 C27 C28 110.7(2) . . ?
C23 C27 H27 108.1 . . ?
C29 C27 H27 108.1 . . ?
C28 C27 H27 108.1 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 O 116.4(2) . . ?
N3 C30 C38 126.8(2) . . ?
O C30 C38 116.8(2) . . ?
C36 C31 C32 118.2(2) . . ?
C36 C31 N3 117.8(2) . . ?
C32 C31 N3 124.0(2) . . ?
C33 C32 C31 120.4(2) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C34 C33 C32 120.8(3) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C35 C34 C33 119.2(2) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C36 120.7(3) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 120.5(3) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
N4 C37 C38 119.5(2) . . ?
N4 C37 C40 122.6(2) . . ?
C38 C37 C40 117.9(2) . . ?
C39 C38 C37 123.7(2) . . ?
C39 C38 C30 118.3(2) . . ?
C37 C38 C30 117.9(2) . . ?
N5 C39 C38 122.0(2) . . ?
N5 C39 C41 115.7(2) . . ?
C38 C39 C41 122.2(2) . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C43 121.6(2) . . ?
C47 C42 N4 120.9(2) . . ?
C43 C42 N4 117.2(2) . . ?
C44 C43 C42 117.6(3) . . ?
C44 C43 C48 122.4(3) . . ?
C42 C43 C48 119.9(2) . . ?
C45 C44 C43 121.5(3) . . ?
C45 C44 H44 119.3 . . ?
C43 C44 H44 119.3 . . ?
C44 C45 C46 119.9(3) . . ?
C44 C45 H45 120 . . ?
C46 C45 H45 120 . . ?
C45 C46 C47 121.7(3) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C46 C47 C42 117.5(3) . . ?
C46 C47 C51 121.7(3) . . ?
C42 C47 C51 120.7(2) . . ?
C43 C48 C49 110.3(3) . . ?
C43 C48 C50 114.4(2) . . ?
C49 C48 C50 110.2(2) . . ?
C43 C48 H48 107.2 . . ?
C49 C48 H48 107.2 . . ?
C50 C48 H48 107.2 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C51 C52 114.2(3) . . ?
C47 C51 C53 110.2(2) . . ?
C52 C51 C53 110.4(3) . . ?
C47 C51 H51 107.2 . . ?
C52 C51 H51 107.2 . . ?
C53 C51 H51 107.2 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C59 C54 C55 121.7(2) . . ?
C59 C54 N5 119.2(2) . . ?
C55 C54 N5 119.1(2) . . ?
C56 C55 C54 117.5(3) . . ?
C56 C55 C60 120.4(3) . . ?
C54 C55 C60 122.1(2) . . ?
C57 C56 C55 121.5(3) . . ?
C57 C56 H56 119.2 . . ?
C55 C56 H56 119.2 . . ?
C58 C57 C56 120.3(3) . . ?
C58 C57 H57 119.8 . . ?
C56 C57 H57 119.8 . . ?
C57 C58 C59 121.1(3) . . ?
C57 C58 H58 119.5 . . ?
C59 C58 H58 119.5 . . ?
C58 C59 C54 117.9(3) . . ?
C58 C59 C63 120.9(2) . . ?
C54 C59 C63 121.3(2) . . ?
C55 C60 C62 109.8(3) . . ?
C55 C60 C61 112.5(3) . . ?
C62 C60 C61 109.6(3) . . ?
C55 C60 H60 108.3 . . ?
C62 C60 H60 108.3 . . ?
C61 C60 H60 108.3 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 H62A 109.5 . . ?
C60 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C60 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C59 C63 C65 110.8(2) . . ?
C59 C63 C64 112.5(3) . . ?
C65 C63 C64 110.6(2) . . ?
C59 C63 H63 107.6 . . ?
C65 C63 H63 107.6 . . ?
C64 C63 H63 107.6 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C2S C1S C6S 120 . . ?
C2S C1S C7S 126 . . ?
C6S C1S C7S 114 . . ?
C3S C2S C1S 120 . . ?
C3S C2S H2S 120 . . ?
C1S C2S H2S 120 . . ?
C2S C3S C4S 120 . . ?
C2S C3S H3S 120 . . ?
C4S C3S H3S 120 . . ?
C5S C4S C3S 120 . . ?
C5S C4S H4S 120 . . ?
C3S C4S H4S 120 . . ?
C4S C5S C6S 120 . . ?
C4S C5S H5S 120 . . ?
C6S C5S H5S 120 . . ?
C5S C6S C1S 120 . . ?
C5S C6S H6S 120 . . ?
C1S C6S H6S 120 . . ?
C1S C7S H7S1 109.5 . . ?
C1S C7S H7S2 109.5 . . ?
H7S1 C7S H7S2 109.5 . . ?
C1S C7S H7S3 109.5 . . ?
H7S1 C7S H7S3 109.5 . . ?
H7S2 C7S H7S3 109.5 . . ?
C1S C7S H7S4 109.5 . . ?
H7S1 C7S H7S4 141.1 . . ?
H7S2 C7S H7S4 56.3 . . ?
H7S3 C7S H7S4 56.3 . . ?
C1S C7S H7S5 109.5 . . ?
H7S1 C7S H7S5 56.3 . . ?
H7S2 C7S H7S5 141.1 . . ?
H7S3 C7S H7S5 56.3 . . ?
H7S4 C7S H7S5 109.5 . . ?
C1S C7S H7S6 109.5 . . ?
H7S1 C7S H7S6 56.3 . . ?
H7S2 C7S H7S6 56.3 . . ?
H7S3 C7S H7S6 141.1 . . ?
H7S4 C7S H7S6 109.5 . . ?
H7S5 C7S H7S6 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 991978'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_mpc_lh602

_audit_creation_date             2014-03-17T09:52:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C46 H68 N4 O1 Pb1'
_chemical_formula_sum            'C46 H68 N4 O Pb'
_chemical_formula_weight         900.23
_chemical_compound_source        'synthesis as described'


#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c m n'
_symmetry_space_group_name_Hall  '-P 2n 2ac'
_symmetry_Int_Tables_number      62
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   9.30580(10)
_cell_length_b                   19.5694(3)
_cell_length_c                   27.4022(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4990.19(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    88724
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485
_cell_measurement_wavelength     0.71073


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Rod
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.7084
_exptl_absorpt_correction_T_max  0.8032


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.68507E-1
_diffrn_orient_matrix_ub_12      -0.232202E-1
_diffrn_orient_matrix_ub_13      0.227051E-1
_diffrn_orient_matrix_ub_21      -0.753614E-1
_diffrn_orient_matrix_ub_22      0.4036E-3
_diffrn_orient_matrix_ub_23      -0.260134E-1
_diffrn_orient_matrix_ub_31      0.342794E-1
_diffrn_orient_matrix_ub_32      -0.45518E-1
_diffrn_orient_matrix_ub_33      -0.118132E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_number            64880
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        27.5
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             5878
_reflns_number_gt                5009
_reflns_threshold_expression     >2sigma(I)


#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 The molecule lies on a mirror plane.  The diketiminate ligand is disordered
 and was modelled over two positions with each being constrained to be equal
 using the SAME command, and the carbon atoms C1, C2 and C3 isotropic.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0781P)²+54.6317P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5878
_refine_ls_number_parameters     381
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0588
_refine_ls_wR_factor_ref         0.2115
_refine_ls_wR_factor_gt          0.1951
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_restrained_S_all      1.336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.075
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.364

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.09209(5) 0.25 0.879692(16) 0.02682(17) Uani 1 2 d S . .
C1 C 0.029(3) 0.3135(8) 0.9842(7) 0.042(7) Uiso 0.541(12) 1 d PDU . 1
C2 C -0.0398(19) 0.25 0.9935(6) 0.048(4) Uiso 0.541(12) 2 d SPDU . 1
H2 H -0.1346 0.25 1.0064 0.057 Uiso 0.541(12) 2 calc SPR . 1
C3 C -0.017(2) 0.3659(10) 1.0218(7) 0.043(5) Uiso 0.541(12) 1 d PDU . 1
H3A H 0.0245 0.4105 1.0132 0.065 Uiso 0.271(6) 1 calc PR . 1
H3B H 0.0183 0.3521 1.054 0.065 Uiso 0.271(6) 1 calc PR . 1
H3C H -0.1216 0.3693 1.0224 0.065 Uiso 0.271(6) 1 calc PR . 1
H3D H -0.077 0.3441 1.0465 0.065 Uiso 0.271(6) 1 calc PR . 1
H3E H -0.0709 0.4025 1.0057 0.065 Uiso 0.271(6) 1 calc PR . 1
H3F H 0.0691 0.3853 1.0374 0.065 Uiso 0.271(6) 1 calc PR . 1
N1 N 0.0859(18) 0.3341(7) 0.9394(5) 0.033(3) Uani 0.541(12) 1 d PD . 1
C4 C 0.144(2) 0.4004(9) 0.9290(7) 0.037(4) Uani 0.541(12) 1 d PD . 1
C5 C 0.054(2) 0.4489(9) 0.9032(8) 0.042(5) Uani 0.541(12) 1 d PD . 1
C6 C 0.116(2) 0.5130(9) 0.8929(8) 0.042(5) Uani 0.541(12) 1 d PD . 1
H6 H 0.0603 0.5466 0.8765 0.051 Uiso 0.541(12) 1 calc PR . 1
C7 C 0.253(2) 0.5282(9) 0.9058(8) 0.052(6) Uani 0.541(12) 1 d PD . 1
H7 H 0.293 0.5715 0.8978 0.063 Uiso 0.541(12) 1 calc PR . 1
C8 C 0.335(2) 0.4806(11) 0.9305(10) 0.050(6) Uani 0.541(12) 1 d PD . 1
H8 H 0.4299 0.4919 0.9406 0.06 Uiso 0.541(12) 1 calc PR . 1
C9 C 0.2801(19) 0.4168(9) 0.9407(6) 0.039(4) Uani 0.541(12) 1 d PD . 1
C10 C -0.100(2) 0.4346(11) 0.8840(8) 0.053(6) Uani 0.541(12) 1 d PD . 1
H10 H -0.1324 0.3914 0.9 0.064 Uiso 0.541(12) 1 calc PR . 1
C11 C -0.212(2) 0.4902(11) 0.8971(10) 0.062(6) Uani 0.541(12) 1 d PD . 1
H11C H -0.1888 0.5325 0.8797 0.093 Uiso 0.541(12) 1 calc PR . 1
H11B H -0.2097 0.4986 0.9324 0.093 Uiso 0.541(12) 1 calc PR . 1
H11A H -0.3078 0.4745 0.8876 0.093 Uiso 0.541(12) 1 calc PR . 1
C12 C -0.100(3) 0.4213(13) 0.8294(8) 0.057(6) Uani 0.541(12) 1 d PD . 1
H12C H -0.1957 0.4056 0.8194 0.085 Uiso 0.541(12) 1 calc PR . 1
H12B H -0.0288 0.3861 0.8216 0.085 Uiso 0.541(12) 1 calc PR . 1
H12A H -0.0764 0.4635 0.812 0.085 Uiso 0.541(12) 1 calc PR . 1
C13 C 0.373(2) 0.3648(11) 0.9681(7) 0.046(5) Uani 0.541(12) 1 d PD . 1
H13 H 0.345 0.3185 0.9559 0.055 Uiso 0.541(12) 1 calc PR . 1
C14 C 0.348(2) 0.3650(13) 1.0223(7) 0.051(5) Uani 0.541(12) 1 d PD . 1
H14C H 0.371 0.4103 1.0355 0.076 Uiso 0.541(12) 1 calc PR . 1
H14B H 0.4104 0.3308 1.0377 0.076 Uiso 0.541(12) 1 calc PR . 1
H14A H 0.2476 0.3541 1.0291 0.076 Uiso 0.541(12) 1 calc PR . 1
C15 C 0.535(2) 0.3731(11) 0.9578(9) 0.054(6) Uani 0.541(12) 1 d PD . 1
H15C H 0.5686 0.4165 0.9715 0.08 Uiso 0.541(12) 1 calc PR . 1
H15B H 0.5517 0.3727 0.9225 0.08 Uiso 0.541(12) 1 calc PR . 1
H15A H 0.5879 0.3353 0.9729 0.08 Uiso 0.541(12) 1 calc PR . 1
C1A C -0.004(3) 0.3180(8) 0.9781(9) 0.042(8) Uiso 0.459(12) 1 d PDU . 2
C2A C -0.0398(19) 0.25 0.9935(6) 0.048(4) Uiso 0.459(12) 2 d SPDU . 2
H2A H -0.1034 0.25 1.0206 0.057 Uiso 0.459(12) 2 calc SPR . 2
C3A C -0.058(2) 0.3804(9) 1.0045(8) 0.031(4) Uiso 0.459(12) 1 d PDU . 2
H3A1 H -0.0063 0.4209 0.993 0.046 Uiso 0.229(6) 1 calc PR . 2
H3A2 H -0.0432 0.3749 1.0397 0.046 Uiso 0.229(6) 1 calc PR . 2
H3A3 H -0.1612 0.3861 0.998 0.046 Uiso 0.229(6) 1 calc PR . 2
H3A4 H -0.1342 0.367 1.0274 0.046 Uiso 0.229(6) 1 calc PR . 2
H3A5 H -0.0973 0.413 0.9808 0.046 Uiso 0.229(6) 1 calc PR . 2
H3A6 H 0.0208 0.4018 1.0225 0.046 Uiso 0.229(6) 1 calc PR . 2
N1A N 0.1247(16) 0.3189(8) 0.9516(7) 0.023(4) Uiso 0.459(12) 1 d PD . 2
C4A C 0.1988(19) 0.3826(10) 0.9492(8) 0.030(4) Uiso 0.459(12) 1 d PD . 2
C5A C 0.126(2) 0.4355(10) 0.9223(8) 0.030(5) Uiso 0.459(12) 1 d PD . 2
C6A C 0.203(2) 0.4966(10) 0.9165(8) 0.036(5) Uiso 0.459(12) 1 d PD . 2
H6A H 0.1603 0.5332 0.8988 0.043 Uiso 0.459(12) 1 calc PR . 2
C7A C 0.336(3) 0.5048(12) 0.9356(10) 0.035(7) Uiso 0.459(12) 1 d PD . 2
H7A H 0.3862 0.5465 0.9306 0.042 Uiso 0.459(12) 1 calc PR . 2
C8A C 0.400(2) 0.4531(10) 0.9621(8) 0.037(5) Uiso 0.459(12) 1 d PD . 2
H8A H 0.4912 0.4602 0.9766 0.044 Uiso 0.459(12) 1 calc PR . 2
C9A C 0.331(2) 0.3914(11) 0.9676(10) 0.038(6) Uiso 0.459(12) 1 d PD . 2
C10A C -0.022(3) 0.4301(12) 0.8970(8) 0.038(5) Uiso 0.459(12) 1 d PD . 2
H10A H -0.062 0.384 0.9048 0.046 Uiso 0.459(12) 1 calc PR . 2
C11A C -0.133(3) 0.4843(13) 0.9148(10) 0.051(6) Uiso 0.459(12) 1 d PD . 2
H11F H -0.0989 0.5301 0.9061 0.077 Uiso 0.459(12) 1 calc PR . 2
H11E H -0.1429 0.4811 0.9503 0.077 Uiso 0.459(12) 1 calc PR . 2
H11D H -0.2258 0.4757 0.8993 0.077 Uiso 0.459(12) 1 calc PR . 2
C12A C -0.003(3) 0.4336(14) 0.8415(8) 0.052(6) Uiso 0.459(12) 1 d PD . 2
H12F H -0.0951 0.4253 0.8255 0.078 Uiso 0.459(12) 1 calc PR . 2
H12E H 0.0667 0.3988 0.8312 0.078 Uiso 0.459(12) 1 calc PR . 2
H12D H 0.0331 0.479 0.8324 0.078 Uiso 0.459(12) 1 calc PR . 2
C13A C 0.404(2) 0.3342(11) 0.9965(7) 0.038(5) Uiso 0.459(12) 1 d PD . 2
H13A H 0.3739 0.2899 0.9814 0.046 Uiso 0.459(12) 1 calc PR . 2
C14A C 0.356(3) 0.3326(15) 1.0495(9) 0.052(6) Uiso 0.459(12) 1 d PD . 2
H14F H 0.3794 0.3764 1.065 0.078 Uiso 0.459(12) 1 calc PR . 2
H14E H 0.4064 0.2957 1.0666 0.078 Uiso 0.459(12) 1 calc PR . 2
H14D H 0.2523 0.3248 1.0511 0.078 Uiso 0.459(12) 1 calc PR . 2
C15A C 0.570(2) 0.3370(17) 0.9951(11) 0.066(8) Uiso 0.459(12) 1 d PD . 2
H15F H 0.6033 0.3332 0.9613 0.099 Uiso 0.459(12) 1 calc PR . 2
H15E H 0.6097 0.2992 1.0143 0.099 Uiso 0.459(12) 1 calc PR . 2
H15D H 0.6032 0.3805 1.0089 0.099 Uiso 0.459(12) 1 calc PR . 2
O1 O 0.3295(11) 0.256(3) 0.8729(4) 0.047(7) Uani 0.5 1 d P . -1
N2 N 0.4815(15) 0.259(3) 0.8078(6) 0.030(9) Uani 0.5 1 d PD . -1
H2X H 0.469(13) 0.238(7) 0.779(3) 0.00(4) Uiso 0.5 1 d PD A -1
N3 N 0.2516(16) 0.2985(8) 0.8095(6) 0.033(3) Uani 0.5 1 d P . -1
C16 C 0.3524(17) 0.2661(9) 0.8301(6) 0.031(6) Uani 0.5 1 d P . -1
C17 C 0.602(2) 0.2081(13) 0.8273(10) 0.056(5) Uani 0.5 1 d PU . -1
C18 C 0.548(3) 0.1366(13) 0.8365(12) 0.070(7) Uani 0.5 1 d PU . -1
H18A H 0.5071 0.1179 0.8063 0.106 Uiso 0.5 1 calc PR . -1
H18B H 0.4729 0.1378 0.8617 0.106 Uiso 0.5 1 calc PR . -1
H18C H 0.6272 0.1076 0.8474 0.106 Uiso 0.5 1 calc PR . -1
C19 C 0.6621(18) 0.2365(15) 0.8714(8) 0.056(7) Uani 0.5 1 d PU . -1
H19A H 0.5877 0.2388 0.8966 0.083 Uiso 0.5 1 calc PR . -1
H19B H 0.6984 0.2826 0.8647 0.083 Uiso 0.5 1 calc PR . -1
H19C H 0.7412 0.2075 0.8827 0.083 Uiso 0.5 1 calc PR . -1
C20 C 0.706(3) 0.2018(17) 0.7854(12) 0.083(8) Uani 0.5 1 d PU . -1
H20A H 0.6561 0.182 0.7571 0.125 Uiso 0.5 1 calc PR . -1
H20B H 0.7856 0.172 0.7949 0.125 Uiso 0.5 1 calc PR . -1
H20C H 0.7427 0.2471 0.7769 0.125 Uiso 0.5 1 calc PR . -1
C21 C 0.259(3) 0.3153(11) 0.7592(9) 0.038(5) Uani 0.5 1 d P . -1
C22 C 0.276(3) 0.3875(10) 0.7443(9) 0.049(5) Uani 0.5 1 d P . -1
C23 C 0.273(6) 0.4062(15) 0.6978(11) 0.095(16) Uani 0.5 1 d P . -1
H23 H 0.2781 0.4531 0.689 0.114 Uiso 0.5 1 calc PR . -1
C24 C 0.262(5) 0.3561(16) 0.6623(10) 0.101(14) Uani 0.5 1 d P . -1
H24 H 0.2697 0.3692 0.629 0.122 Uiso 0.5 1 calc PR . -1
C25 C 0.241(5) 0.2887(16) 0.6731(9) 0.091(12) Uani 0.5 1 d P . -1
H25 H 0.2264 0.2564 0.6476 0.109 Uiso 0.5 1 calc PR . -1
C26 C 0.240(3) 0.2673(13) 0.7229(8) 0.059(11) Uani 0.5 1 d P . -1
C27 C 0.302(2) 0.4415(11) 0.7862(8) 0.045(5) Uani 0.5 1 d P . -1
H27 H 0.2459 0.4272 0.8157 0.054 Uiso 0.5 1 calc PR . -1
C28 C 0.459(3) 0.4442(14) 0.7992(10) 0.060(7) Uani 0.5 1 d P . -1
H28C H 0.5146 0.4587 0.7707 0.09 Uiso 0.5 1 calc PR . -1
H28B H 0.4912 0.3987 0.8096 0.09 Uiso 0.5 1 calc PR . -1
H28A H 0.4736 0.4768 0.8259 0.09 Uiso 0.5 1 calc PR . -1
C29 C 0.256(3) 0.5096(12) 0.7719(9) 0.064(7) Uani 0.5 1 d P . -1
H29C H 0.2719 0.5414 0.799 0.096 Uiso 0.5 1 calc PR . -1
H29B H 0.1537 0.5088 0.7635 0.096 Uiso 0.5 1 calc PR . -1
H29A H 0.3119 0.5245 0.7434 0.096 Uiso 0.5 1 calc PR . -1
C31 C 0.057(4) 0.152(4) 0.7176(14) 0.16(3) Uani 0.5 1 d P . -1
H31C H -0.0244 0.1759 0.7328 0.234 Uiso 0.5 1 calc PR . -1
H31B H 0.0582 0.1044 0.7288 0.234 Uiso 0.5 1 calc PR . -1
H31A H 0.046 0.1531 0.6821 0.234 Uiso 0.5 1 calc PR . -1
C30 C 0.217(4) 0.1921(14) 0.7341(12) 0.062(9) Uani 0.5 1 d P . -1
H30 H 0.2297 0.186 0.7701 0.074 Uiso 0.5 1 calc PR . -1
C32 C 0.311(5) 0.131(3) 0.7068(15) 0.098(13) Uani 0.5 1 d P . -1
H32C H 0.2994 0.1354 0.6714 0.147 Uiso 0.5 1 calc PR . -1
H32B H 0.2755 0.0865 0.7175 0.147 Uiso 0.5 1 calc PR . -1
H32A H 0.4125 0.1359 0.7154 0.147 Uiso 0.5 1 calc PR . -1



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O1 2.219(11) 8_565 ?
Pb O1 2.219(11) . ?
Pb N1 2.321(13) . ?
Pb N1 2.321(13) 8_565 ?
Pb N1A 2.406(16) . ?
Pb N1A 2.406(16) 8_565 ?
Pb N3 2.608(15) 8_565 ?
Pb N3 2.608(15) . ?
Pb C16 2.795(17) 8_565 ?
Pb C16 2.795(17) . ?
C1 N1 1.400(18) . ?
C1 C2 1.419(16) . ?
C1 C3 1.513(19) . ?
C2 C1 1.419(16) 8_565 ?
C2 H2 0.95 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C3 H3D 0.98 . ?
C3 H3E 0.98 . ?
C3 H3F 0.98 . ?
N1 C4 1.434(18) . ?
C4 C9 1.34(2) . ?
C4 C5 1.45(2) . ?
C5 C6 1.41(2) . ?
C5 C10 1.55(3) . ?
C6 C7 1.36(2) . ?
C6 H6 0.95 . ?
C7 C8 1.38(3) . ?
C7 H7 0.95 . ?
C8 C9 1.38(2) . ?
C8 H8 0.95 . ?
C9 C13 1.53(2) . ?
C10 C12 1.52(3) . ?
C10 C11 1.55(3) . ?
C10 H10 1 . ?
C11 H11C 0.98 . ?
C11 H11B 0.98 . ?
C11 H11A 0.98 . ?
C12 H12C 0.98 . ?
C12 H12B 0.98 . ?
C12 H12A 0.98 . ?
C13 C14 1.50(2) . ?
C13 C15 1.54(2) . ?
C13 H13 1 . ?
C14 H14C 0.98 . ?
C14 H14B 0.98 . ?
C14 H14A 0.98 . ?
C15 H15C 0.98 . ?
C15 H15B 0.98 . ?
C15 H15A 0.98 . ?
C1A N1A 1.399(19) . ?
C1A C3A 1.509(19) . ?
C3A H3A1 0.98 . ?
C3A H3A2 0.98 . ?
C3A H3A3 0.98 . ?
C3A H3A4 0.98 . ?
C3A H3A5 0.98 . ?
C3A H3A6 0.98 . ?
N1A C4A 1.43(2) . ?
C4A C9A 1.34(3) . ?
C4A C5A 1.44(2) . ?
C5A C6A 1.40(2) . ?
C5A C10A 1.55(3) . ?
C6A C7A 1.36(3) . ?
C6A H6A 0.95 . ?
C7A C8A 1.38(3) . ?
C7A H7A 0.95 . ?
C8A C9A 1.38(3) . ?
C8A H8A 0.95 . ?
C9A C13A 1.53(2) . ?
C10A C12A 1.53(3) . ?
C10A C11A 1.56(3) . ?
C10A H10A 1 . ?
C11A H11F 0.98 . ?
C11A H11E 0.98 . ?
C11A H11D 0.98 . ?
C12A H12F 0.98 . ?
C12A H12E 0.98 . ?
C12A H12D 0.98 . ?
C13A C14A 1.52(2) . ?
C13A C15A 1.55(2) . ?
C13A H13A 1 . ?
C14A H14F 0.98 . ?
C14A H14E 0.98 . ?
C14A H14D 0.98 . ?
C15A H15F 0.98 . ?
C15A H15E 0.98 . ?
C15A H15D 0.98 . ?
O1 C16 1.21(2) . ?
N2 C16 1.36(2) . ?
N2 C17 1.59(4) . ?
N2 H2X 0.91(2) . ?
N3 C16 1.26(2) . ?
N3 C21 1.42(3) . ?
C17 C19 1.44(4) . ?
C17 C20 1.50(3) . ?
C17 C18 1.51(4) . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C21 C26 1.38(3) . ?
C21 C22 1.48(3) . ?
C22 C23 1.33(4) . ?
C22 C27 1.58(3) . ?
C23 C24 1.39(4) . ?
C23 H23 0.95 . ?
C24 C25 1.37(4) . ?
C24 H24 0.95 . ?
C25 C26 1.43(3) . ?
C25 H25 0.95 . ?
C26 C30 1.52(4) . ?
C27 C29 1.45(3) . ?
C27 C28 1.51(3) . ?
C27 H27 1 . ?
C28 H28C 0.98 . ?
C28 H28B 0.98 . ?
C28 H28A 0.98 . ?
C29 H29C 0.98 . ?
C29 H29B 0.98 . ?
C29 H29A 0.98 . ?
C31 C30 1.75(6) . ?
C31 H31C 0.98 . ?
C31 H31B 0.98 . ?
C31 H31A 0.98 . ?
C30 C32 1.65(5) . ?
C30 H30 1 . ?
C32 H32C 0.98 . ?
C32 H32B 0.98 . ?
C32 H32A 0.98 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb O1 6(3) 8_565 . ?
O1 Pb N1 96.8(12) 8_565 . ?
O1 Pb N1 92.8(10) . . ?
O1 Pb N1 92.8(10) 8_565 8_565 ?
O1 Pb N1 96.8(12) . 8_565 ?
N1 Pb N1 90.4(8) . 8_565 ?
O1 Pb N1A 88.3(10) 8_565 . ?
O1 Pb N1A 85.1(8) . . ?
N1 Pb N1A 13.8(4) . . ?
N1 Pb N1A 79.9(7) 8_565 . ?
O1 Pb N1A 85.1(8) 8_565 8_565 ?
O1 Pb N1A 88.3(10) . 8_565 ?
N1 Pb N1A 79.9(7) . 8_565 ?
N1 Pb N1A 13.8(4) 8_565 8_565 ?
N1A Pb N1A 68.1(9) . 8_565 ?
O1 Pb N3 49.7(8) 8_565 8_565 ?
O1 Pb N3 52.4(7) . 8_565 ?
N1 Pb N3 142.3(5) . 8_565 ?
N1 Pb N3 106.0(5) 8_565 8_565 ?
N1A Pb N3 137.3(5) . 8_565 ?
N1A Pb N3 109.2(5) 8_565 8_565 ?
O1 Pb N3 52.4(7) 8_565 . ?
O1 Pb N3 49.7(8) . . ?
N1 Pb N3 106.0(5) . . ?
N1 Pb N3 142.3(5) 8_565 . ?
N1A Pb N3 109.2(5) . . ?
N1A Pb N3 137.3(5) 8_565 . ?
N3 Pb N3 42.6(7) 8_565 . ?
O1 Pb C16 24.7(6) 8_565 8_565 ?
O1 Pb C16 26.2(6) . 8_565 ?
N1 Pb C16 116.4(5) . 8_565 ?
N1 Pb C16 106.5(5) 8_565 8_565 ?
N1A Pb C16 110.6(5) . 8_565 ?
N1A Pb C16 103.0(5) 8_565 8_565 ?
N3 Pb C16 26.8(5) 8_565 8_565 ?
N3 Pb C16 35.8(5) . 8_565 ?
O1 Pb C16 26.2(6) 8_565 . ?
O1 Pb C16 24.7(6) . . ?
N1 Pb C16 106.5(5) . . ?
N1 Pb C16 116.4(5) 8_565 . ?
N1A Pb C16 103.0(5) . . ?
N1A Pb C16 110.6(5) 8_565 . ?
N3 Pb C16 35.8(5) 8_565 . ?
N3 Pb C16 26.8(5) . . ?
C16 Pb C16 12.9(7) 8_565 . ?
N1 C1 C2 125.5(15) . . ?
N1 C1 C3 120.5(14) . . ?
C2 C1 C3 110.4(14) . . ?
C1 C2 C1 122(2) . 8_565 ?
C1 C2 H2 118.9 . . ?
C1 C2 H2 118.9 8_565 . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C3 H3D 109.5 . . ?
H3A C3 H3D 141.1 . . ?
H3B C3 H3D 56.3 . . ?
H3C C3 H3D 56.3 . . ?
C1 C3 H3E 109.5 . . ?
H3A C3 H3E 56.3 . . ?
H3B C3 H3E 141.1 . . ?
H3C C3 H3E 56.3 . . ?
H3D C3 H3E 109.5 . . ?
C1 C3 H3F 109.5 . . ?
H3A C3 H3F 56.3 . . ?
H3B C3 H3F 56.3 . . ?
H3C C3 H3F 141.1 . . ?
H3D C3 H3F 109.5 . . ?
H3E C3 H3F 109.5 . . ?
C1 N1 C4 125.4(13) . . ?
C1 N1 Pb 115.1(10) . . ?
C4 N1 Pb 119.5(10) . . ?
C9 C4 N1 121.6(19) . . ?
C9 C4 C5 120.4(16) . . ?
N1 C4 C5 117.9(16) . . ?
C6 C5 C4 116.1(18) . . ?
C6 C5 C10 118.1(18) . . ?
C4 C5 C10 125.7(16) . . ?
C7 C6 C5 121.9(18) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C8 120.0(17) . . ?
C6 C7 H7 120 . . ?
C8 C7 H7 120 . . ?
C9 C8 C7 120(2) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C4 C9 C8 121.2(19) . . ?
C4 C9 C13 119.3(17) . . ?
C8 C9 C13 119.4(17) . . ?
C12 C10 C5 111.7(16) . . ?
C12 C10 C11 110(2) . . ?
C5 C10 C11 114.6(17) . . ?
C12 C10 H10 106.6 . . ?
C5 C10 H10 106.6 . . ?
C11 C10 H10 106.6 . . ?
C10 C11 H11C 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11C C11 H11B 109.5 . . ?
C10 C11 H11A 109.5 . . ?
H11C C11 H11A 109.5 . . ?
H11B C11 H11A 109.5 . . ?
C10 C12 H12C 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12C C12 H12B 109.5 . . ?
C10 C12 H12A 109.5 . . ?
H12C C12 H12A 109.5 . . ?
H12B C12 H12A 109.5 . . ?
C14 C13 C9 113.3(17) . . ?
C14 C13 C15 109.3(16) . . ?
C9 C13 C15 113.1(16) . . ?
C14 C13 H13 106.9 . . ?
C9 C13 H13 106.9 . . ?
C15 C13 H13 106.9 . . ?
C13 C14 H14C 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
C13 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
H14B C14 H14A 109.5 . . ?
C13 C15 H15C 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15C C15 H15B 109.5 . . ?
C13 C15 H15A 109.5 . . ?
H15C C15 H15A 109.5 . . ?
H15B C15 H15A 109.5 . . ?
N1A C1A C3A 121.9(15) . . ?
C1A C3A H3A1 109.5 . . ?
C1A C3A H3A2 109.5 . . ?
H3A1 C3A H3A2 109.5 . . ?
C1A C3A H3A3 109.5 . . ?
H3A1 C3A H3A3 109.5 . . ?
H3A2 C3A H3A3 109.5 . . ?
C1A C3A H3A4 109.5 . . ?
H3A1 C3A H3A4 141.1 . . ?
H3A2 C3A H3A4 56.3 . . ?
H3A3 C3A H3A4 56.3 . . ?
C1A C3A H3A5 109.5 . . ?
H3A1 C3A H3A5 56.3 . . ?
H3A2 C3A H3A5 141.1 . . ?
H3A3 C3A H3A5 56.3 . . ?
H3A4 C3A H3A5 109.5 . . ?
C1A C3A H3A6 109.5 . . ?
H3A1 C3A H3A6 56.3 . . ?
H3A2 C3A H3A6 56.3 . . ?
H3A3 C3A H3A6 141.1 . . ?
H3A4 C3A H3A6 109.5 . . ?
H3A5 C3A H3A6 109.5 . . ?
C1A N1A C4A 116.6(14) . . ?
C1A N1A Pb 108.1(13) . . ?
C4A N1A Pb 120.9(13) . . ?
C9A C4A N1A 123(2) . . ?
C9A C4A C5A 122.1(17) . . ?
N1A C4A C5A 115.2(16) . . ?
C6A C5A C4A 115.6(19) . . ?
C6A C5A C10A 117.5(19) . . ?
C4A C5A C10A 126.8(16) . . ?
C7A C6A C5A 122(2) . . ?
C7A C6A H6A 119.2 . . ?
C5A C6A H6A 119.2 . . ?
C6A C7A C8A 121(2) . . ?
C6A C7A H7A 119.7 . . ?
C8A C7A H7A 119.7 . . ?
C9A C8A C7A 120(2) . . ?
C9A C8A H8A 119.9 . . ?
C7A C8A H8A 119.9 . . ?
C4A C9A C8A 120(2) . . ?
C4A C9A C13A 120.5(19) . . ?
C8A C9A C13A 119.5(18) . . ?
C12A C10A C5A 109.7(19) . . ?
C12A C10A C11A 111(2) . . ?
C5A C10A C11A 113.7(19) . . ?
C12A C10A H10A 107.3 . . ?
C5A C10A H10A 107.3 . . ?
C11A C10A H10A 107.3 . . ?
C10A C11A H11F 109.5 . . ?
C10A C11A H11E 109.5 . . ?
H11F C11A H11E 109.5 . . ?
C10A C11A H11D 109.5 . . ?
H11F C11A H11D 109.5 . . ?
H11E C11A H11D 109.5 . . ?
C10A C12A H12F 109.5 . . ?
C10A C12A H12E 109.5 . . ?
H12F C12A H12E 109.5 . . ?
C10A C12A H12D 109.5 . . ?
H12F C12A H12D 109.5 . . ?
H12E C12A H12D 109.5 . . ?
C14A C13A C9A 112.4(18) . . ?
C14A C13A C15A 108.4(19) . . ?
C9A C13A C15A 113.8(19) . . ?
C14A C13A H13A 107.3 . . ?
C9A C13A H13A 107.3 . . ?
C15A C13A H13A 107.3 . . ?
C13A C14A H14F 109.5 . . ?
C13A C14A H14E 109.5 . . ?
H14F C14A H14E 109.5 . . ?
C13A C14A H14D 109.5 . . ?
H14F C14A H14D 109.5 . . ?
H14E C14A H14D 109.5 . . ?
C13A C15A H15F 109.5 . . ?
C13A C15A H15E 109.5 . . ?
H15F C15A H15E 109.5 . . ?
C13A C15A H15D 109.5 . . ?
H15F C15A H15D 109.5 . . ?
H15E C15A H15D 109.5 . . ?
C16 O1 Pb 105.4(11) . . ?
C16 N2 C17 122(2) . . ?
C16 N2 H2X 109(8) . . ?
C17 N2 H2X 96(9) . . ?
C16 N3 C21 120.8(17) . . ?
C16 N3 Pb 84.9(11) . . ?
C21 N3 Pb 146.0(14) . . ?
O1 C16 N3 113(2) . . ?
O1 C16 N2 125.2(18) . . ?
N3 C16 N2 121(2) . . ?
O1 C16 Pb 50.0(8) . . ?
N3 C16 Pb 68.3(10) . . ?
N2 C16 Pb 168(2) . . ?
C19 C17 C20 115(2) . . ?
C19 C17 C18 110(2) . . ?
C20 C17 C18 105(2) . . ?
C19 C17 N2 108(2) . . ?
C20 C17 N2 104(2) . . ?
C18 C17 N2 114(2) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 N3 122.3(18) . . ?
C26 C21 C22 118(2) . . ?
N3 C21 C22 120(2) . . ?
C23 C22 C21 122(2) . . ?
C23 C22 C27 121(2) . . ?
C21 C22 C27 117(2) . . ?
C22 C23 C24 119(2) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C25 C24 C23 123(2) . . ?
C25 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
C24 C25 C26 119(3) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C21 C26 C25 119(2) . . ?
C21 C26 C30 122(2) . . ?
C25 C26 C30 119(2) . . ?
C29 C27 C28 108(2) . . ?
C29 C27 C22 112(2) . . ?
C28 C27 C22 110(2) . . ?
C29 C27 H27 108.8 . . ?
C28 C27 H27 108.8 . . ?
C22 C27 H27 108.8 . . ?
C27 C28 H28C 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28C C28 H28B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
H28C C28 H28A 109.5 . . ?
H28B C28 H28A 109.5 . . ?
C27 C29 H29C 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29C C29 H29B 109.5 . . ?
C27 C29 H29A 109.5 . . ?
H29C C29 H29A 109.5 . . ?
H29B C29 H29A 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31C C31 H31B 109.5 . . ?
C30 C31 H31A 109.5 . . ?
H31C C31 H31A 109.5 . . ?
H31B C31 H31A 109.5 . . ?
C26 C30 C32 122(3) . . ?
C26 C30 C31 120(4) . . ?
C32 C30 C31 91(3) . . ?
C26 C30 H30 107.5 . . ?
C32 C30 H30 107.5 . . ?
C31 C30 H30 107.5 . . ?
C30 C32 H32C 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32C C32 H32B 109.5 . . ?
C30 C32 H32A 109.5 . . ?
H32C C32 H32A 109.5 . . ?
H32B C32 H32A 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 991979'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(15)-may207

_audit_creation_date             2007-05-01T13:45:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H46 N2'
_chemical_formula_sum            'C36 H46 N2'
_chemical_formula_weight         506.75
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.2095(3)
_cell_length_b                   8.8710(2)
_cell_length_c                   26.1615(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.691(1)
_cell_angle_gamma                90
_cell_volume                     3064.31(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    17454
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      26.022
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.62763E-1
_diffrn_orient_matrix_ub_12      -0.56432E-1
_diffrn_orient_matrix_ub_13      0.105016E-1
_diffrn_orient_matrix_ub_21      0.94936E-2
_diffrn_orient_matrix_ub_22      0.678416E-1
_diffrn_orient_matrix_ub_23      0.03029
_diffrn_orient_matrix_ub_31      -0.413114E-1
_diffrn_orient_matrix_ub_32      -0.701448E-1
_diffrn_orient_matrix_ub_33      0.208468E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_number            20035
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_reflns_number_total             5950
_reflns_number_gt                4443
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0599P)²+1.0334P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5950
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1195
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.038

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.25297(9) 0.41165(14) 0.34471(4) 0.0265(3) Uani 1 1 d . . .
N2 N 0.28773(9) 0.52901(14) 0.46650(4) 0.0256(3) Uani 1 1 d . . .
C1 C 0.31783(11) 0.31763(17) 0.36329(5) 0.0258(3) Uani 1 1 d . . .
C2 C 0.32869(11) 0.30745(17) 0.41987(5) 0.0250(3) Uani 1 1 d . . .
C3 C 0.25650(11) 0.40170(17) 0.45001(5) 0.0253(3) Uani 1 1 d . . .
C4 C 0.38168(12) 0.21478(19) 0.33163(6) 0.0342(4) Uani 1 1 d . . .
H4A H 0.3674 0.2341 0.2952 0.051 Uiso 1 1 calc R . .
H4B H 0.3656 0.1096 0.3395 0.051 Uiso 1 1 calc R . .
H4C H 0.4535 0.2338 0.3396 0.051 Uiso 1 1 calc R . .
C5 C 0.15381(12) 0.3346(2) 0.45795(7) 0.0386(4) Uani 1 1 d . . .
H5A H 0.1596 0.2528 0.483 0.058 Uiso 1 1 calc R . .
H5B H 0.1265 0.2947 0.4254 0.058 Uiso 1 1 calc R . .
H5C H 0.1083 0.4125 0.4706 0.058 Uiso 1 1 calc R . .
C6 C 0.23418(11) 0.42346(17) 0.29073(5) 0.0268(3) Uani 1 1 d . . .
C7 C 0.16655(11) 0.32276(18) 0.26605(6) 0.0286(3) Uani 1 1 d . . .
C8 C 0.14613(12) 0.3411(2) 0.21411(6) 0.0346(4) Uani 1 1 d . . .
H8 H 0.1011 0.2732 0.1969 0.041 Uiso 1 1 calc R . .
C9 C 0.19015(13) 0.4563(2) 0.18685(6) 0.0396(4) Uani 1 1 d . . .
H9 H 0.1754 0.4671 0.1513 0.048 Uiso 1 1 calc R . .
C10 C 0.25561(13) 0.5555(2) 0.21154(6) 0.0378(4) Uani 1 1 d . . .
H10 H 0.2853 0.6347 0.1927 0.045 Uiso 1 1 calc R . .
C11 C 0.27895(12) 0.54160(18) 0.26366(6) 0.0310(4) Uani 1 1 d . . .
C12 C 0.11535(12) 0.19839(18) 0.29583(6) 0.0326(4) Uani 1 1 d . . .
H12 H 0.1647 0.1634 0.323 0.039 Uiso 1 1 calc R . .
C13 C 0.02233(14) 0.2592(2) 0.32255(7) 0.0487(5) Uani 1 1 d . . .
H13A H 0.0414 0.3485 0.3427 0.073 Uiso 1 1 calc R . .
H13B H -0.0041 0.1815 0.3452 0.073 Uiso 1 1 calc R . .
H13C H -0.03 0.2866 0.2969 0.073 Uiso 1 1 calc R . .
C14 C 0.08590(15) 0.0616(2) 0.26337(7) 0.0472(5) Uani 1 1 d . . .
H14A H 0.0294 0.0882 0.24 0.071 Uiso 1 1 calc R . .
H14B H 0.0654 -0.021 0.2857 0.071 Uiso 1 1 calc R . .
H14C H 0.144 0.0297 0.2436 0.071 Uiso 1 1 calc R . .
C15 C 0.35442(13) 0.64746(19) 0.28957(6) 0.0369(4) Uani 1 1 d . . .
H15 H 0.341 0.6478 0.327 0.044 Uiso 1 1 calc R . .
C16 C 0.46243(14) 0.5908(2) 0.28285(8) 0.0507(5) Uani 1 1 d . . .
H16A H 0.4701 0.4911 0.2987 0.076 Uiso 1 1 calc R . .
H16B H 0.5104 0.6613 0.2993 0.076 Uiso 1 1 calc R . .
H16C H 0.4761 0.5836 0.2463 0.076 Uiso 1 1 calc R . .
C17 C 0.34580(18) 0.8094(2) 0.27030(8) 0.0563(5) Uani 1 1 d . . .
H17A H 0.3675 0.8143 0.2348 0.084 Uiso 1 1 calc R . .
H17B H 0.3891 0.875 0.2917 0.084 Uiso 1 1 calc R . .
H17C H 0.2753 0.843 0.272 0.084 Uiso 1 1 calc R . .
C18 C 0.22182(11) 0.62607(17) 0.49397(5) 0.0255(3) Uani 1 1 d . . .
C19 C 0.22090(11) 0.61968(18) 0.54748(6) 0.0302(4) Uani 1 1 d . . .
C20 C 0.16133(13) 0.7238(2) 0.57303(6) 0.0375(4) Uani 1 1 d . . .
H20 H 0.1598 0.7208 0.6093 0.045 Uiso 1 1 calc R . .
C21 C 0.10467(13) 0.8308(2) 0.54686(6) 0.0400(4) Uani 1 1 d . . .
H21 H 0.064 0.8998 0.5649 0.048 Uiso 1 1 calc R . .
C22 C 0.10749(12) 0.8369(2) 0.49417(6) 0.0370(4) Uani 1 1 d . . .
H22 H 0.0687 0.9112 0.4762 0.044 Uiso 1 1 calc R . .
C23 C 0.16610(11) 0.73634(18) 0.46676(6) 0.0293(3) Uani 1 1 d . . .
C24 C 0.28446(13) 0.5069(2) 0.57789(6) 0.0352(4) Uani 1 1 d . . .
H24 H 0.3156 0.4368 0.5529 0.042 Uiso 1 1 calc R . .
C25 C 0.37028(19) 0.5865(3) 0.60679(10) 0.0721(7) Uani 1 1 d . . .
H25A H 0.3424 0.6511 0.6333 0.108 Uiso 1 1 calc R . .
H25B H 0.4084 0.6483 0.583 0.108 Uiso 1 1 calc R . .
H25C H 0.4155 0.5114 0.6228 0.108 Uiso 1 1 calc R . .
C26 C 0.2230(2) 0.4131(3) 0.61343(12) 0.0888(9) Uani 1 1 d . . .
H26A H 0.1932 0.4784 0.6392 0.133 Uiso 1 1 calc R . .
H26B H 0.2669 0.3381 0.6304 0.133 Uiso 1 1 calc R . .
H26C H 0.1689 0.3617 0.5938 0.133 Uiso 1 1 calc R . .
C27 C 0.16946(13) 0.74790(19) 0.40885(6) 0.0355(4) Uani 1 1 d . . .
H27 H 0.2193 0.6714 0.3971 0.043 Uiso 1 1 calc R . .
C28 C 0.06783(17) 0.7114(3) 0.38317(8) 0.0644(6) Uani 1 1 d . . .
H28A H 0.0183 0.7885 0.3921 0.097 Uiso 1 1 calc R . .
H28B H 0.0447 0.6126 0.3948 0.097 Uiso 1 1 calc R . .
H28C H 0.0749 0.7096 0.346 0.097 Uiso 1 1 calc R . .
C29 C 0.20714(18) 0.9020(2) 0.39258(7) 0.0572(6) Uani 1 1 d . . .
H29A H 0.2112 0.9052 0.3553 0.086 Uiso 1 1 calc R . .
H29B H 0.2744 0.9203 0.4081 0.086 Uiso 1 1 calc R . .
H29C H 0.1601 0.9798 0.4039 0.086 Uiso 1 1 calc R . .
C30 C 0.39579(12) 0.21471(18) 0.44265(6) 0.0310(4) Uani 1 1 d . . .
H30 H 0.4388 0.1603 0.4208 0.037 Uiso 1 1 calc R . .
C31 C 0.41042(12) 0.18739(18) 0.49848(6) 0.0309(4) Uani 1 1 d . . .
C32 C 0.35142(14) 0.0820(2) 0.52319(7) 0.0422(4) Uani 1 1 d . . .
H32 H 0.2988 0.0311 0.5046 0.051 Uiso 1 1 calc R . .
C33 C 0.36818(16) 0.0501(2) 0.57454(7) 0.0501(5) Uani 1 1 d . . .
H33 H 0.3275 -0.0227 0.5909 0.06 Uiso 1 1 calc R . .
C34 C 0.44404(16) 0.1239(2) 0.60195(7) 0.0515(5) Uani 1 1 d . . .
H34 H 0.4549 0.1038 0.6374 0.062 Uiso 1 1 calc R . .
C35 C 0.50388(15) 0.2269(3) 0.57756(7) 0.0519(5) Uani 1 1 d . . .
H35 H 0.5569 0.2766 0.5962 0.062 Uiso 1 1 calc R . .
C36 C 0.48769(14) 0.2587(2) 0.52625(7) 0.0436(4) Uani 1 1 d . . .
H36 H 0.5297 0.3298 0.5099 0.052 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
N1 C1 1.2811(19) . ?
N1 C6 1.4306(18) . ?
N2 C3 1.2733(19) . ?
N2 C18 1.4326(19) . ?
C1 C2 1.486(2) . ?
C1 C4 1.507(2) . ?
C2 C30 1.337(2) . ?
C2 C3 1.508(2) . ?
C3 C5 1.501(2) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C11 1.405(2) . ?
C6 C7 1.407(2) . ?
C7 C8 1.387(2) . ?
C7 C12 1.521(2) . ?
C8 C9 1.384(2) . ?
C8 H8 0.95 . ?
C9 C10 1.381(2) . ?
C9 H9 0.95 . ?
C10 C11 1.395(2) . ?
C10 H10 0.95 . ?
C11 C15 1.515(2) . ?
C12 C14 1.525(2) . ?
C12 C13 1.530(2) . ?
C12 H12 1 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 C17 1.526(3) . ?
C15 C16 1.528(3) . ?
C15 H15 1 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 C19 1.402(2) . ?
C18 C23 1.405(2) . ?
C19 C20 1.396(2) . ?
C19 C24 1.516(2) . ?
C20 C21 1.378(2) . ?
C20 H20 0.95 . ?
C21 C22 1.381(2) . ?
C21 H21 0.95 . ?
C22 C23 1.394(2) . ?
C22 H22 0.95 . ?
C23 C27 1.520(2) . ?
C24 C26 1.504(3) . ?
C24 C25 1.518(3) . ?
C24 H24 1 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 C28 1.518(3) . ?
C27 C29 1.520(3) . ?
C27 H27 1 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 C31 1.487(2) . ?
C30 H30 0.95 . ?
C31 C36 1.388(2) . ?
C31 C32 1.389(2) . ?
C32 C33 1.384(2) . ?
C32 H32 0.95 . ?
C33 C34 1.380(3) . ?
C33 H33 0.95 . ?
C34 C35 1.377(3) . ?
C34 H34 0.95 . ?
C35 C36 1.382(3) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?

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
C1 N1 C6 121.12(12) . . ?
C3 N2 C18 120.49(13) . . ?
N1 C1 C2 117.47(13) . . ?
N1 C1 C4 124.38(13) . . ?
C2 C1 C4 118.13(13) . . ?
C30 C2 C1 121.66(13) . . ?
C30 C2 C3 121.97(13) . . ?
C1 C2 C3 116.31(12) . . ?
N2 C3 C5 126.13(14) . . ?
N2 C3 C2 117.74(13) . . ?
C5 C3 C2 116.13(13) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 120.89(14) . . ?
C11 C6 N1 119.26(13) . . ?
C7 C6 N1 119.74(13) . . ?
C8 C7 C6 118.55(14) . . ?
C8 C7 C12 120.68(14) . . ?
C6 C7 C12 120.76(13) . . ?
C9 C8 C7 121.25(16) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C10 C9 C8 119.77(15) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 121.22(15) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 118.33(15) . . ?
C10 C11 C15 120.41(14) . . ?
C6 C11 C15 121.21(14) . . ?
C7 C12 C14 113.70(13) . . ?
C7 C12 C13 110.70(14) . . ?
C14 C12 C13 109.88(15) . . ?
C7 C12 H12 107.4 . . ?
C14 C12 H12 107.4 . . ?
C13 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 113.21(15) . . ?
C11 C15 C16 110.42(14) . . ?
C17 C15 C16 109.43(16) . . ?
C11 C15 H15 107.9 . . ?
C17 C15 H15 107.9 . . ?
C16 C15 H15 107.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 120.95(13) . . ?
C19 C18 N2 119.99(13) . . ?
C23 C18 N2 118.77(13) . . ?
C20 C19 C18 118.23(14) . . ?
C20 C19 C24 119.75(14) . . ?
C18 C19 C24 122.00(13) . . ?
C21 C20 C19 121.54(15) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C20 C21 C22 119.52(15) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C21 C22 C23 121.33(15) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C18 118.40(14) . . ?
C22 C23 C27 120.16(14) . . ?
C18 C23 C27 121.43(13) . . ?
C26 C24 C19 112.88(15) . . ?
C26 C24 C25 111.0(2) . . ?
C19 C24 C25 110.41(15) . . ?
C26 C24 H24 107.4 . . ?
C19 C24 H24 107.4 . . ?
C25 C24 H24 107.4 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C29 111.13(16) . . ?
C28 C27 C23 112.03(15) . . ?
C29 C27 C23 111.05(14) . . ?
C28 C27 H27 107.5 . . ?
C29 C27 H27 107.5 . . ?
C23 C27 H27 107.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C2 C30 C31 127.10(14) . . ?
C2 C30 H30 116.4 . . ?
C31 C30 H30 116.4 . . ?
C36 C31 C32 118.50(15) . . ?
C36 C31 C30 120.80(15) . . ?
C32 C31 C30 120.55(15) . . ?
C33 C32 C31 120.90(17) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C34 C33 C32 120.00(19) . . ?
C34 C33 H33 120 . . ?
C32 C33 H33 120 . . ?
C35 C34 C33 119.47(17) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 120.73(18) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C31 120.38(18) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?

#===END


_database_code_depnum_ccdc_archive 'CCDC 991980'
