# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

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

data_10tjr002_0m
_database_code_depnum_ccdc_archive 'CCDC 1444895'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H26 Cl2 N8 O2 Pb2, 2(C H4 O)'
_chemical_formula_sum            'C38 H34 Cl2 N8 O4 Pb2 '
_chemical_formula_weight         1152.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   10.6380(11)
_cell_length_b                   19.076(2)
_cell_length_c                   9.2825(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.396(2)
_cell_angle_gamma                90.00
_cell_volume                     1832.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6716
_cell_measurement_theta_min      2.239
_cell_measurement_theta_max      30.615

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    9.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4147
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   'Apex2  v2009.7-0 (Bruker, 2009)'

_exptl_special_details           
; 
The solvate methanol molecule is disordered over two mutually exclusive 
sites with an occupancy ratio of 0.529(7) to 0.471(7). The overlapping 
carbon atoms were constrained to have the same ADP and to be approximately 
isotropic. The position of H2B was restrained based on hydrogen bonding 
considerations.  
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13654
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         31.05
_reflns_number_total             5424
_reflns_number_gt                4803
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Apex2 v2009.7-0 (Bruker, 2009)'
_computing_cell_refinement       'Apex2 v2009.7-0'
_computing_data_reduction        'Apex2 v2009.7-0'
_computing_structure_solution    
'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL 6.14'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'

_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)+(0.0218P)²+1.1812P] 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_extinction_coef       ?
_refine_ls_number_reflns         5424
_refine_ls_number_parameters     261
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0514
_refine_ls_wR_factor_gt          0.0497
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2241(3) 0.67444(15) 0.2348(3) 0.0150(6) Uani 1 1 d . . .
H1 H 0.2496 0.7175 0.2843 0.018 Uiso 1 1 calc R . .
C2 C 0.1480(3) 0.67628(15) 0.0923(4) 0.0185(6) Uani 1 1 d . . .
H2 H 0.1225 0.7197 0.0443 0.022 Uiso 1 1 calc R . .
C3 C 0.1096(3) 0.61312(15) 0.0211(4) 0.0173(6) Uani 1 1 d . . .
H3 H 0.0567 0.6126 -0.0766 0.021 Uiso 1 1 calc R . .
C4 C 0.1495(3) 0.55091(15) 0.0944(3) 0.0146(6) Uani 1 1 d . . .
H4 H 0.1241 0.5073 0.0474 0.018 Uiso 1 1 calc R . .
C5 C 0.2269(3) 0.55272(14) 0.2373(3) 0.0109(5) Uani 1 1 d . . .
C6 C 0.2709(2) 0.48869(14) 0.3240(3) 0.0099(5) Uani 1 1 d . . .
C7 C 0.2382(3) 0.41842(14) 0.2552(3) 0.0098(5) Uani 1 1 d . . .
C8 C 0.1677(3) 0.37059(15) 0.3199(3) 0.0131(5) Uani 1 1 d . . .
H8 H 0.1437 0.3821 0.4094 0.016 Uiso 1 1 calc R . .
C9 C 0.1331(3) 0.30601(15) 0.2521(3) 0.0149(6) Uani 1 1 d . . .
H9 H 0.0854 0.2735 0.2957 0.018 Uiso 1 1 calc R . .
C10 C 0.1678(3) 0.28900(15) 0.1219(3) 0.0149(6) Uani 1 1 d . . .
H10 H 0.1430 0.2451 0.0758 0.018 Uiso 1 1 calc R . .
C11 C 0.2384(3) 0.33583(16) 0.0583(3) 0.0150(5) Uani 1 1 d . . .
H11 H 0.2626 0.3238 -0.0309 0.018 Uiso 1 1 calc R . .
C12 C 0.2741(3) 0.40038(15) 0.1248(3) 0.0131(5) Uani 1 1 d . . .
H12 H 0.3231 0.4323 0.0813 0.016 Uiso 1 1 calc R . .
C13 C 0.4232(3) 0.45553(14) 0.6863(3) 0.0101(5) Uani 1 1 d . . .
C14 C 0.4611(3) 0.39256(14) 0.7812(3) 0.0101(5) Uani 1 1 d . . .
C15 C 0.4248(3) 0.32567(14) 0.7278(3) 0.0128(5) Uani 1 1 d . . .
H15 H 0.3731 0.3193 0.6305 0.015 Uiso 1 1 calc R . .
C16 C 0.4653(3) 0.26871(15) 0.8186(3) 0.0160(6) Uani 1 1 d . . .
H16 H 0.4388 0.2234 0.7810 0.019 Uiso 1 1 calc R . .
C17 C 0.5716(3) 0.33779(16) 1.0069(3) 0.0140(5) Uani 1 1 d . . .
H17 H 0.6242 0.3424 1.1042 0.017 Uiso 1 1 calc R . .
C18 C 0.5332(3) 0.39860(14) 0.9266(3) 0.0123(5) Uani 1 1 d . . .
H18 H 0.5555 0.4434 0.9698 0.015 Uiso 1 1 calc R . .
O2A O 0.1216(9) 0.4855(4) 0.7926(7) 0.076(3) Uani 0.529(7) 1 d PD A 1
H2A H 0.1763 0.5126 0.7702 0.114 Uiso 0.529(7) 1 calc PR A 1
C19A C 0.087(4) 0.437(2) 0.687(4) 0.041(3) Uani 0.529(7) 1 d PDU A 1
H19A H 0.0115 0.4539 0.6135 0.061 Uiso 0.529(7) 1 calc PR A 1
H19B H 0.0651 0.3936 0.7316 0.061 Uiso 0.529(7) 1 calc PR A 1
H19C H 0.1587 0.4288 0.6398 0.061 Uiso 0.529(7) 1 calc PR A 1
O2B O 0.0588(5) 0.3778(3) 0.6633(6) 0.0298(16) Uani 0.471(7) 1 d PD A 2
H2B H -0.0010 0.3750 0.5866 0.045 Uiso 0.471(7) 1 calc PRD A 2
C19B C 0.091(5) 0.446(2) 0.692(4) 0.041(3) Uani 0.471(7) 1 d PD A 2
H19D H 0.0190 0.4705 0.7188 0.061 Uiso 0.471(7) 1 calc PR A 2
H19E H 0.1094 0.4675 0.6030 0.061 Uiso 0.471(7) 1 calc PR A 2
H19F H 0.1678 0.4488 0.7735 0.061 Uiso 0.471(7) 1 calc PR A 2
Cl4 Cl 0.17155(7) 0.63240(4) 0.63302(9) 0.01850(14) Uani 1 1 d . . .
N1 N 0.2636(2) 0.61446(12) 0.3059(3) 0.0123(5) Uani 1 1 d . . .
N2 N 0.3334(2) 0.49821(12) 0.4603(3) 0.0106(4) Uani 1 1 d . . .
N3 N 0.3759(2) 0.43940(12) 0.5438(3) 0.0113(4) Uani 1 1 d . . .
N4 N 0.5393(2) 0.27313(13) 0.9560(3) 0.0155(5) Uani 1 1 d . . .
O1 O 0.4366(2) 0.51601(10) 0.7440(2) 0.0149(4) Uani 1 1 d . . .
Pb1 Pb 0.397255(9) 0.612443(5) 0.565380(11) 0.01078(4) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.339(3) . ?
C1 C2 1.382(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.389(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(4) . ?
C4 H4 0.9500 . ?
C5 N1 1.353(3) . ?
C5 C6 1.478(4) . ?
C6 N2 1.298(3) . ?
C6 C7 1.491(4) . ?
C7 C12 1.394(4) . ?
C7 C8 1.401(4) . ?
C8 C9 1.393(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.390(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 O1 1.266(3) . ?
C13 N3 1.338(3) . ?
C13 C14 1.489(4) . ?
C14 C15 1.391(4) . ?
C14 C18 1.394(4) . ?
C15 C16 1.382(4) . ?
C15 H15 0.9500 . ?
C16 N4 1.338(4) . ?
C16 H16 0.9500 . ?
C17 N4 1.337(4) . ?
C17 C18 1.388(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
O2A C19A 1.33(4) . ?
O2A H2A 0.8400 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
O2B C19B 1.35(4) . ?
O2B H2B 0.8400 . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
Cl4 Pb1 2.6462(8) . ?
N1 Pb1 2.497(2) . ?
N2 N3 1.379(3) . ?
N2 Pb1 2.419(2) . ?
O1 Pb1 2.447(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.7(3) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C3 118.4(3) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 120.9(3) . . ?
N1 C5 C6 116.3(2) . . ?
C4 C5 C6 122.8(2) . . ?
N2 C6 C5 116.2(2) . . ?
N2 C6 C7 124.0(2) . . ?
C5 C6 C7 119.8(2) . . ?
C12 C7 C8 119.5(3) . . ?
C12 C7 C6 120.7(2) . . ?
C8 C7 C6 119.8(2) . . ?
C9 C8 C7 119.6(3) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
O1 C13 N3 127.4(3) . . ?
O1 C13 C14 119.8(2) . . ?
N3 C13 C14 112.8(2) . . ?
C15 C14 C18 117.8(3) . . ?
C15 C14 C13 121.0(2) . . ?
C18 C14 C13 121.3(2) . . ?
C16 C15 C14 118.8(3) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
N4 C16 C15 124.3(3) . . ?
N4 C16 H16 117.8 . . ?
C15 C16 H16 117.8 . . ?
N4 C17 C18 124.2(3) . . ?
N4 C17 H17 117.9 . . ?
C18 C17 H17 117.9 . . ?
C17 C18 C14 118.6(3) . . ?
C17 C18 H18 120.7 . . ?
C14 C18 H18 120.7 . . ?
C19B O2B H2B 109.5 . . ?
O2B C19B H19D 109.5 . . ?
O2B C19B H19E 109.5 . . ?
H19D C19B H19E 109.5 . . ?
O2B C19B H19F 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C1 N1 C5 119.2(3) . . ?
C1 N1 Pb1 122.14(19) . . ?
C5 N1 Pb1 118.58(18) . . ?
C6 N2 N3 117.5(2) . . ?
C6 N2 Pb1 123.47(18) . . ?
N3 N2 Pb1 118.75(16) . . ?
C13 N3 N2 111.6(2) . . ?
C17 N4 C16 116.2(2) . . ?
C13 O1 Pb1 114.44(17) . . ?
N2 Pb1 O1 65.43(7) . . ?
N2 Pb1 N1 65.24(8) . . ?
O1 Pb1 N1 129.42(7) . . ?
N2 Pb1 Cl4 92.29(6) . . ?
O1 Pb1 Cl4 88.26(5) . . ?
N1 Pb1 Cl4 83.19(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.9(5) . . . . ?
C1 C2 C3 C4 -0.5(5) . . . . ?
C2 C3 C4 C5 0.0(5) . . . . ?
C3 C4 C5 N1 0.2(4) . . . . ?
C3 C4 C5 C6 178.5(3) . . . . ?
N1 C5 C6 N2 4.0(4) . . . . ?
C4 C5 C6 N2 -174.3(3) . . . . ?
N1 C5 C6 C7 -178.1(2) . . . . ?
C4 C5 C6 C7 3.5(4) . . . . ?
N2 C6 C7 C12 -125.4(3) . . . . ?
C5 C6 C7 C12 57.0(3) . . . . ?
N2 C6 C7 C8 56.3(4) . . . . ?
C5 C6 C7 C8 -121.4(3) . . . . ?
C12 C7 C8 C9 -0.8(4) . . . . ?
C6 C7 C8 C9 177.5(2) . . . . ?
C7 C8 C9 C10 0.0(4) . . . . ?
C8 C9 C10 C11 0.7(4) . . . . ?
C9 C10 C11 C12 -0.4(4) . . . . ?
C10 C11 C12 C7 -0.4(4) . . . . ?
C8 C7 C12 C11 1.0(4) . . . . ?
C6 C7 C12 C11 -177.3(2) . . . . ?
O1 C13 C14 C15 167.3(3) . . . . ?
N3 C13 C14 C15 -12.1(4) . . . . ?
O1 C13 C14 C18 -12.2(4) . . . . ?
N3 C13 C14 C18 168.3(3) . . . . ?
C18 C14 C15 C16 -2.2(4) . . . . ?
C13 C14 C15 C16 178.2(3) . . . . ?
C14 C15 C16 N4 -0.8(5) . . . . ?
N4 C17 C18 C14 -3.0(4) . . . . ?
C15 C14 C18 C17 3.9(4) . . . . ?
C13 C14 C18 C17 -176.5(3) . . . . ?
C2 C1 N1 C5 -0.7(4) . . . . ?
C2 C1 N1 Pb1 -178.7(2) . . . . ?
C4 C5 N1 C1 0.2(4) . . . . ?
C6 C5 N1 C1 -178.2(2) . . . . ?
C4 C5 N1 Pb1 178.2(2) . . . . ?
C6 C5 N1 Pb1 -0.2(3) . . . . ?
C5 C6 N2 N3 -179.8(2) . . . . ?
C7 C6 N2 N3 2.5(4) . . . . ?
C5 C6 N2 Pb1 -6.3(3) . . . . ?
C7 C6 N2 Pb1 175.99(18) . . . . ?
O1 C13 N3 N2 -3.6(4) . . . . ?
C14 C13 N3 N2 175.8(2) . . . . ?
C6 N2 N3 C13 -171.6(2) . . . . ?
Pb1 N2 N3 C13 14.5(3) . . . . ?
C18 C17 N4 C16 0.0(4) . . . . ?
C15 C16 N4 C17 1.9(4) . . . . ?
N3 C13 O1 Pb1 -8.7(4) . . . . ?
C14 C13 O1 Pb1 171.93(18) . . . . ?
C6 N2 Pb1 O1 172.9(2) . . . . ?
N3 N2 Pb1 O1 -13.60(17) . . . . ?
C6 N2 Pb1 N1 4.5(2) . . . . ?
N3 N2 Pb1 N1 177.9(2) . . . . ?
C6 N2 Pb1 Cl4 85.9(2) . . . . ?
N3 N2 Pb1 Cl4 -100.63(18) . . . . ?
C13 O1 Pb1 N2 10.95(18) . . . . ?
C13 O1 Pb1 N1 24.6(2) . . . . ?
C13 O1 Pb1 Cl4 104.27(18) . . . . ?
C1 N1 Pb1 N2 176.1(2) . . . . ?
C5 N1 Pb1 N2 -1.91(19) . . . . ?
C1 N1 Pb1 O1 162.4(2) . . . . ?
C5 N1 Pb1 O1 -15.5(2) . . . . ?
C1 N1 Pb1 Cl4 80.4(2) . . . . ?
C5 N1 Pb1 Cl4 -97.6(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.924
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.444
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.134
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ira258g
_database_code_depnum_ccdc_archive 'CCDC 1444896'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-02-01 downloaded from the CCDC.
;

_audit_creation_date             2010-09-28T16:37:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H26 I2 N8 O2 Pb2, 2(C H4 O )'
_chemical_formula_sum            'C38 H34 I2 N8 O4 Pb2'
_chemical_formula_weight         1330.88
_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                   10.9695(9)
_cell_length_b                   19.2524(10)
_cell_length_c                   9.5858(8)
_cell_angle_alpha                90
_cell_angle_beta                 105.181(9)
_cell_angle_gamma                90
_cell_volume                     1953.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6603
_cell_measurement_theta_min      4.388
_cell_measurement_theta_max      29.2067
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .10
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    10.237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.48504
_exptl_absorpt_correction_T_max  1

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

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.4547
_diffrn_orient_matrix_ub_11      -0.0188951496
_diffrn_orient_matrix_ub_12      -0.0048903791
_diffrn_orient_matrix_ub_13      -0.0666347459
_diffrn_orient_matrix_ub_21      -0.0271844142
_diffrn_orient_matrix_ub_22      -0.0335588657
_diffrn_orient_matrix_ub_23      0.0077948235
_diffrn_orient_matrix_ub_31      -0.069286389
_diffrn_orient_matrix_ub_32      0.0145556388
_diffrn_orient_matrix_ub_33      -0.0042737207
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_number            12773
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.39
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.853
_reflns_number_total             4510
_reflns_number_gt                3244
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
        (compiled May  6 2009,17:20:42)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   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)+(0.0984P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4510
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1601
_refine_ls_wR_factor_gt          0.1503
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.31
_refine_diff_density_min         -2.691
_refine_diff_density_rms         0.341

#----------------------------------------------------------------------------#
#                   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'
I I -0.4742 1.8119 '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 0.40091(4) 0.110292(19) 0.55776(4) 0.02115(16) Uani 1 1 d . . .
I2 I 0.15135(8) 0.12929(4) 0.62182(9) 0.0326(2) Uani 1 1 d . . .
O1 O 0.4458(8) 0.0159(4) 0.7370(8) 0.0293(19) Uani 1 1 d . . .
N1 N 0.3798(9) -0.0617(5) 0.5426(9) 0.024(2) Uani 1 1 d . . .
N2 N 0.3373(9) -0.0035(5) 0.4589(9) 0.022(2) Uani 1 1 d . . .
N3 N 0.2708(9) 0.1099(4) 0.3005(10) 0.0212(19) Uani 1 1 d . . .
C1 C 0.4294(10) -0.0454(5) 0.6840(11) 0.020(2) Uani 1 1 d . . .
C2 C 0.2797(10) -0.0143(5) 0.3251(11) 0.018(2) Uani 1 1 d . . .
C10 C 0.2464(11) -0.0841(5) 0.2598(11) 0.020(2) Uani 1 1 d . . .
C11 C 0.2815(12) -0.1033(6) 0.1367(12) 0.030(3) Uani 1 1 d . . .
H11 H 0.331 -0.0722 0.0974 0.036 Uiso 1 1 calc R . .
C12 C 0.2468(12) -0.1662(6) 0.0695(12) 0.030(3) Uani 1 1 d . . .
H12 H 0.2721 -0.1773 -0.0154 0.035 Uiso 1 1 calc R . .
C13 C 0.1764(13) -0.2132(6) 0.1226(13) 0.034(3) Uani 1 1 d . . .
H13 H 0.1518 -0.2562 0.0753 0.041 Uiso 1 1 calc R . .
C14 C 0.1425(11) -0.1960(5) 0.2472(12) 0.027(3) Uani 1 1 d . . .
H14 H 0.0941 -0.2278 0.2864 0.032 Uiso 1 1 calc R . .
C15 C 0.1788(11) -0.1313(6) 0.3177(12) 0.025(2) Uani 1 1 d . . .
H15 H 0.1565 -0.1207 0.4046 0.03 Uiso 1 1 calc R . .
C20 C 0.4647(10) -0.1069(5) 0.7795(12) 0.021(2) Uani 1 1 d . . .
C21 C 0.5367(13) -0.1010(5) 0.9205(12) 0.025(3) Uani 1 1 d . . .
H21 H 0.5645 -0.0567 0.9602 0.031 Uiso 1 1 calc R . .
C22 C 0.5675(12) -0.1601(5) 1.0025(13) 0.026(3) Uani 1 1 d . . .
H22 H 0.6098 -0.1541 1.1018 0.032 Uiso 1 1 calc R . .
N4 N 0.5433(10) -0.2249(5) 0.9554(10) 0.031(2) Uani 1 1 d . . .
C24 C 0.4718(13) -0.2285(6) 0.8168(13) 0.033(3) Uani 1 1 d . . .
H24 H 0.4454 -0.2733 0.7795 0.04 Uiso 1 1 calc R . .
C25 C 0.4342(12) -0.1729(6) 0.7255(12) 0.028(3) Uani 1 1 d . . .
H25 H 0.3883 -0.1798 0.6277 0.034 Uiso 1 1 calc R . .
C30 C 0.2321(11) 0.0481(5) 0.2365(11) 0.021(2) Uani 1 1 d . . .
C31 C 0.1501(12) 0.0446(6) 0.0978(12) 0.029(3) Uani 1 1 d . . .
H31 H 0.1235 0.0012 0.0532 0.035 Uiso 1 1 calc R . .
C32 C 0.1094(12) 0.1057(5) 0.0284(14) 0.029(3) Uani 1 1 d . . .
H32 H 0.0534 0.1042 -0.0657 0.034 Uiso 1 1 calc R . .
C33 C 0.1460(13) 0.1683(6) 0.0890(13) 0.032(3) Uani 1 1 d . . .
H33 H 0.1185 0.2104 0.0387 0.039 Uiso 1 1 calc R . .
C34 C 0.2255(12) 0.1684(6) 0.2283(12) 0.028(3) Uani 1 1 d . . .
H34 H 0.2491 0.2118 0.2748 0.034 Uiso 1 1 calc R . .
O2 O 0.1883(15) -0.0341(6) -0.1822(12) 0.079(4) Uani 1 1 d . . .
C40 C 0.1070(17) -0.0730(11) -0.2872(17) 0.065(5) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   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 2.415(9) . ?
Pb1 O1 2.461(8) . ?
Pb1 N3 2.505(10) . ?
Pb1 I2 2.9809(9) . ?
O1 C1 1.279(12) . ?
N1 C1 1.358(12) . ?
N1 N2 1.386(12) . ?
N2 C2 1.290(13) . ?
N3 C34 1.347(13) . ?
N3 C30 1.353(13) . ?
C1 C20 1.485(14) . ?
C2 C30 1.486(14) . ?
C2 C10 1.487(13) . ?
C10 C15 1.377(15) . ?
C10 C11 1.384(16) . ?
C11 C12 1.379(16) . ?
C11 H11 0.95 . ?
C12 C13 1.370(17) . ?
C12 H12 0.95 . ?
C13 C14 1.381(17) . ?
C13 H13 0.95 . ?
C14 C15 1.423(14) . ?
C14 H14 0.95 . ?
C15 H15 0.95 . ?
C20 C25 1.380(15) . ?
C20 C21 1.380(16) . ?
C21 C22 1.374(14) . ?
C21 H21 0.95 . ?
C22 N4 1.330(14) . ?
C22 H22 0.95 . ?
N4 C24 1.357(14) . ?
C24 C25 1.376(15) . ?
C24 H24 0.95 . ?
C25 H25 0.95 . ?
C30 C31 1.399(15) . ?
C31 C32 1.367(15) . ?
C31 H31 0.95 . ?
C32 C33 1.352(16) . ?
C32 H32 0.95 . ?
C33 C34 1.391(17) . ?
C33 H33 0.95 . ?
C34 H34 0.95 . ?
O2 C40 1.38(2) . ?

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 O1 65.7(2) . . ?
N2 Pb1 N3 65.1(3) . . ?
O1 Pb1 N3 130.0(3) . . ?
N2 Pb1 I2 90.3(2) . . ?
O1 Pb1 I2 88.5(2) . . ?
N3 Pb1 I2 83.5(2) . . ?
C1 O1 Pb1 115.0(7) . . ?
C1 N1 N2 112.2(8) . . ?
C2 N2 N1 116.6(8) . . ?
C2 N2 Pb1 123.6(7) . . ?
N1 N2 Pb1 119.1(6) . . ?
C34 N3 C30 118.2(10) . . ?
C34 N3 Pb1 122.8(7) . . ?
C30 N3 Pb1 118.6(7) . . ?
O1 C1 N1 125.9(10) . . ?
O1 C1 C20 120.2(9) . . ?
N1 C1 C20 113.8(9) . . ?
N2 C2 C30 116.4(9) . . ?
N2 C2 C10 124.6(9) . . ?
C30 C2 C10 118.7(9) . . ?
C15 C10 C11 117.9(10) . . ?
C15 C10 C2 121.7(10) . . ?
C11 C10 C2 120.4(10) . . ?
C12 C11 C10 121.8(12) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C13 C12 C11 121.4(11) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 118.0(10) . . ?
C12 C13 H13 121 . . ?
C14 C13 H13 121 . . ?
C13 C14 C15 121.0(11) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C10 C15 C14 119.9(10) . . ?
C10 C15 H15 120 . . ?
C14 C15 H15 120 . . ?
C25 C20 C21 117.7(10) . . ?
C25 C20 C1 120.3(10) . . ?
C21 C20 C1 121.9(9) . . ?
C22 C21 C20 118.9(10) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
N4 C22 C21 125.8(12) . . ?
N4 C22 H22 117.1 . . ?
C21 C22 H22 117.1 . . ?
C22 N4 C24 113.2(10) . . ?
N4 C24 C25 125.7(11) . . ?
N4 C24 H24 117.1 . . ?
C25 C24 H24 117.1 . . ?
C24 C25 C20 118.3(11) . . ?
C24 C25 H25 120.8 . . ?
C20 C25 H25 120.8 . . ?
N3 C30 C31 121.3(10) . . ?
N3 C30 C2 115.5(9) . . ?
C31 C30 C2 123.1(10) . . ?
C32 C31 C30 117.9(11) . . ?
C32 C31 H31 121.1 . . ?
C30 C31 H31 121.1 . . ?
C33 C32 C31 122.4(12) . . ?
C33 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
C32 C33 C34 117.0(10) . . ?
C32 C33 H33 121.5 . . ?
C34 C33 H33 121.5 . . ?
N3 C34 C33 123.1(10) . . ?
N3 C34 H34 118.4 . . ?
C33 C34 H34 118.4 . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

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

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1444897'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-02-01 downloaded from the CCDC.
;

_audit_creation_date             2012-06-07T12:02:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 33G
;
_chemical_name_common            33G
_chemical_formula_moiety         'C38 H26 N10 O2 Pb2 S2'
_chemical_formula_sum            'C38 H26 N10 O2 Pb2 S2'
_chemical_formula_weight         1133.19
_chemical_absolute_configuration ad

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.8580(2)
_cell_length_b                   19.6630(5)
_cell_length_c                   21.1860(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3690.07(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1065
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

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

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    2.04
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2144
_exptl_special_details           
;
 60 seconds exposure, 1 degree steps, DX=31.5mm
;

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

_exptl_absorpt_coefficient_mu    9.277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_absorpt_correction_T_min  0.0902
_exptl_absorpt_correction_T_max  0.4573

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

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_number            24901
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.971
_reflns_number_total             8736
_reflns_number_gt                6134
_reflns_threshold_expression     >2σ(I)

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

_computing_data_collection       KappaCCD
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   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 > 2σ(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)+(0.0458P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8736
_refine_ls_number_parameters     488
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   0.95
_refine_ls_restrained_S_all      0.95
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.40(4)
_refine_diff_density_max         5.721
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.202

#----------------------------------------------------------------------------#
#                   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'
S S 0.1246 0.1234 '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
C1 C 0.9193(12) 0.2872(4) 0.1230(5) 0.037(3) Uani 1 1 d . . .
H1 H 0.8738 0.3266 0.1408 0.045 Uiso 1 1 calc R . .
C2 C 1.0374(12) 0.2956(5) 0.0814(6) 0.047(3) Uani 1 1 d . . .
H2 H 1.0726 0.3397 0.0705 0.057 Uiso 1 1 calc R . .
C3 C 1.1026(11) 0.2390(5) 0.0561(5) 0.041(3) Uani 1 1 d . . .
H3 H 1.1844 0.243 0.0273 0.049 Uiso 1 1 calc R . .
C4 C 1.0477(12) 0.1752(5) 0.0730(5) 0.040(3) Uani 1 1 d . . .
H4 H 1.0932 0.1354 0.0562 0.048 Uiso 1 1 calc R . .
C5 C 0.9291(10) 0.1697(4) 0.1135(4) 0.024(2) Uani 1 1 d . . .
C6 C 0.8603(11) 0.1042(4) 0.1323(4) 0.0220(17) Uani 1 1 d . . .
C7 C 0.9244(11) 0.0393(4) 0.1095(5) 0.028(2) Uani 1 1 d . . .
C8 C 1.0687(12) 0.0206(5) 0.1232(5) 0.038(3) Uani 1 1 d . . .
H8 H 1.1329 0.0495 0.1471 0.046 Uiso 1 1 calc R . .
C9 C 1.1202(13) -0.0429(6) 0.1011(5) 0.048(3) Uani 1 1 d . . .
H9 H 1.2205 -0.0569 0.1102 0.058 Uiso 1 1 calc R . .
C10 C 1.0277(14) -0.0846(5) 0.0665(6) 0.052(3) Uani 1 1 d . . .
H10 H 1.064 -0.1275 0.0526 0.063 Uiso 1 1 calc R . .
C11 C 0.8861(13) -0.0655(5) 0.0522(5) 0.047(3) Uani 1 1 d . . .
H11 H 0.8245 -0.0946 0.0274 0.056 Uiso 1 1 calc R . .
C12 C 0.8282(11) -0.0034(5) 0.0732(5) 0.034(2) Uani 1 1 d . . .
H12 H 0.7277 0.0099 0.0635 0.04 Uiso 1 1 calc R . .
C13 C 0.5403(9) 0.0549(4) 0.2107(5) 0.0262(19) Uani 1 1 d . . .
C14 C 0.4566(8) -0.0093(4) 0.2213(5) 0.0230(19) Uani 1 1 d . . .
C15 C 0.5090(10) -0.0718(4) 0.1965(4) 0.031(2) Uani 1 1 d . . .
H15 H 0.5952 -0.0733 0.1698 0.037 Uiso 1 1 calc R . .
C16 C 0.4330(11) -0.1298(5) 0.2116(6) 0.040(2) Uani 1 1 d . . .
H16 H 0.4675 -0.1713 0.1937 0.048 Uiso 1 1 calc R . .
C17 C 0.2645(10) -0.0723(5) 0.2722(5) 0.038(3) Uani 1 1 d . . .
H17 H 0.1774 -0.0726 0.2984 0.046 Uiso 1 1 calc R . .
C18 C 0.3308(8) -0.0115(5) 0.2600(4) 0.022(2) Uani 1 1 d . . .
H18 H 0.2914 0.0291 0.2778 0.026 Uiso 1 1 calc R . .
C19 C 0.4781(11) 0.1721(6) 0.0861(5) 0.042(3) Uani 1 1 d . . .
C20 C 0.5802(11) -0.0954(5) 0.3729(5) 0.036(2) Uani 1 1 d . . .
H20 H 0.6313 -0.1342 0.3567 0.044 Uiso 1 1 calc R . .
C21 C 0.4549(11) -0.1046(5) 0.4125(5) 0.035(2) Uani 1 1 d . . .
H21 H 0.4217 -0.1492 0.4229 0.042 Uiso 1 1 calc R . .
C22 C 0.3813(10) -0.0496(5) 0.4360(5) 0.036(2) Uani 1 1 d . . .
H22 H 0.2954 -0.0545 0.4625 0.043 Uiso 1 1 calc R . .
C23 C 0.4370(10) 0.0151(5) 0.4195(4) 0.029(2) Uani 1 1 d . . .
H23 H 0.3894 0.0545 0.4361 0.035 Uiso 1 1 calc R . .
C24 C 0.5587(10) 0.0222(4) 0.3801(4) 0.026(2) Uani 1 1 d . . .
C25 C 0.6289(10) 0.0879(4) 0.3629(4) 0.0245(19) Uani 1 1 d . . .
C26 C 0.5609(10) 0.1532(4) 0.3869(5) 0.028(2) Uani 1 1 d . . .
C27 C 0.4132(10) 0.1725(5) 0.3722(5) 0.036(2) Uani 1 1 d . . .
H27 H 0.3526 0.1446 0.3459 0.043 Uiso 1 1 calc R . .
C28 C 0.3554(13) 0.2328(5) 0.3963(5) 0.041(2) Uani 1 1 d . . .
H28 H 0.2548 0.2457 0.3863 0.049 Uiso 1 1 calc R . .
C29 C 0.4397(13) 0.2729(5) 0.4334(6) 0.045(3) Uani 1 1 d . . .
H29 H 0.3989 0.3144 0.4488 0.054 Uiso 1 1 calc R . .
C30 C 0.5862(12) 0.2544(5) 0.4498(5) 0.046(3) Uani 1 1 d . . .
H30 H 0.6447 0.2821 0.4772 0.056 Uiso 1 1 calc R . .
C31 C 0.6443(12) 0.1951(4) 0.4252(4) 0.031(2) Uani 1 1 d . . .
H31 H 0.7453 0.1829 0.4351 0.038 Uiso 1 1 calc R . .
C32 C 0.9500(10) 0.1385(4) 0.2902(6) 0.029(2) Uani 1 1 d . . .
C33 C 1.0345(9) 0.2027(4) 0.2762(5) 0.025(2) Uani 1 1 d . . .
C34 C 1.1598(10) 0.2034(4) 0.2380(4) 0.028(2) Uani 1 1 d . . .
H34 H 1.201 0.162 0.2227 0.033 Uiso 1 1 calc R . .
C35 C 1.2258(11) 0.2646(5) 0.2219(6) 0.041(3) Uani 1 1 d . . .
H35 H 1.3055 0.2642 0.1919 0.05 Uiso 1 1 calc R . .
C36 C 1.0627(9) 0.3225(4) 0.2841(6) 0.032(2) Uani 1 1 d . . .
H36 H 1.0269 0.3642 0.301 0.039 Uiso 1 1 calc R . .
C37 C 0.9856(9) 0.2646(4) 0.3004(5) 0.030(2) Uani 1 1 d . . .
H37 H 0.9006 0.2667 0.3277 0.036 Uiso 1 1 calc R . .
C38 C 1.0063(11) 0.0172(5) 0.4202(6) 0.042(3) Uani 1 1 d . . .
N1 N 0.8659(9) 0.2263(3) 0.1395(4) 0.0332(18) Uani 1 1 d . . .
N2 N 0.7440(8) 0.1070(4) 0.1698(3) 0.0241(17) Uani 1 1 d . . .
N3 N 0.6771(8) 0.0469(4) 0.1852(4) 0.0297(19) Uani 1 1 d . . .
N4 N 0.3144(9) -0.1322(4) 0.2495(4) 0.041(2) Uani 1 1 d . . .
N5 N 0.5076(10) 0.2219(5) 0.1116(4) 0.046(2) Uani 1 1 d . . .
N6 N 0.6295(9) -0.0331(3) 0.3573(4) 0.0306(17) Uani 1 1 d . . .
N7 N 0.7465(7) 0.0867(3) 0.3288(4) 0.0234(17) Uani 1 1 d . . .
N8 N 0.8171(7) 0.1473(3) 0.3131(4) 0.0228(18) Uani 1 1 d . . .
N9 N 1.1831(10) 0.3253(4) 0.2467(4) 0.040(2) Uani 1 1 d . . .
N10 N 0.9815(10) -0.0289(5) 0.3854(5) 0.048(2) Uani 1 1 d . . .
O1 O 0.4769(6) 0.1116(3) 0.2245(3) 0.0310(16) Uani 1 1 d . . .
O2 O 1.0165(6) 0.0831(3) 0.2756(4) 0.0347(17) Uani 1 1 d . . .
Pb1 Pb 0.63903(4) 0.210473(15) 0.212257(19) 0.02897(10) Uani 1 1 d . . .
Pb2 Pb 0.85392(4) -0.016657(14) 0.285911(18) 0.02699(9) Uani 1 1 d . . .
S1 S 0.4335(4) 0.10118(17) 0.05167(16) 0.0625(9) Uani 1 1 d . . .
S2 S 1.0394(4) 0.0783(2) 0.4668(2) 0.0866(14) Uani 1 1 d . . .



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

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 N1 1.334(11) . ?
C1 C2 1.379(15) . ?
C1 H1 0.95 . ?
C2 C3 1.364(14) . ?
C2 H2 0.95 . ?
C3 C4 1.392(13) . ?
C3 H3 0.95 . ?
C4 C5 1.361(13) . ?
C4 H4 0.95 . ?
C5 N1 1.362(11) . ?
C5 C6 1.479(11) . ?
C6 N2 1.303(11) . ?
C6 C7 1.478(11) . ?
C7 C8 1.361(14) . ?
C7 C12 1.423(13) . ?
C8 C9 1.409(13) . ?
C8 H8 0.95 . ?
C9 C10 1.371(15) . ?
C9 H9 0.95 . ?
C10 C11 1.344(15) . ?
C10 H10 0.95 . ?
C11 C12 1.397(13) . ?
C11 H11 0.95 . ?
C12 H12 0.95 . ?
C13 O1 1.283(10) . ?
C13 N3 1.336(11) . ?
C13 C14 1.481(11) . ?
C14 C18 1.385(11) . ?
C14 C15 1.414(12) . ?
C15 C16 1.363(12) . ?
C15 H15 0.95 . ?
C16 N4 1.324(12) . ?
C16 H16 0.95 . ?
C17 N4 1.346(12) . ?
C17 C18 1.357(12) . ?
C17 H17 0.95 . ?
C18 H18 0.95 . ?
C19 N5 1.148(13) . ?
C19 S1 1.623(13) . ?
C20 N6 1.342(11) . ?
C20 C21 1.404(14) . ?
C20 H20 0.95 . ?
C21 C22 1.358(12) . ?
C21 H21 0.95 . ?
C22 C23 1.407(12) . ?
C22 H22 0.95 . ?
C23 C24 1.371(13) . ?
C23 H23 0.95 . ?
C24 N6 1.345(11) . ?
C24 C25 1.479(12) . ?
C25 N7 1.267(10) . ?
C25 C26 1.506(11) . ?
C26 C31 1.374(13) . ?
C26 C27 1.397(13) . ?
C27 C28 1.387(12) . ?
C27 H27 0.95 . ?
C28 C29 1.342(14) . ?
C28 H28 0.95 . ?
C29 C30 1.391(15) . ?
C29 H29 0.95 . ?
C30 C31 1.377(13) . ?
C30 H30 0.95 . ?
C31 H31 0.95 . ?
C32 O2 1.276(9) . ?
C32 N8 1.285(11) . ?
C32 C33 1.498(11) . ?
C33 C34 1.374(12) . ?
C33 C37 1.389(12) . ?
C34 C35 1.380(12) . ?
C34 H34 0.95 . ?
C35 N9 1.358(12) . ?
C35 H35 0.95 . ?
C36 N9 1.330(12) . ?
C36 C37 1.372(12) . ?
C36 H36 0.95 . ?
C37 H37 0.95 . ?
C38 N10 1.190(13) . ?
C38 S2 1.581(12) . ?
N1 Pb1 2.553(8) . ?
N2 N3 1.361(9) . ?
N2 Pb1 2.412(7) . ?
N5 Pb1 2.441(9) . ?
N6 Pb2 2.518(8) . ?
N7 N8 1.387(9) . ?
N7 Pb2 2.422(6) . ?
N10 Pb2 2.403(9) . ?
O1 Pb1 2.430(6) . ?
O2 Pb2 2.444(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.9(9) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 118.4(10) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.1(10) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 120.3(9) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 N1 120.4(8) . . ?
C4 C5 C6 123.8(8) . . ?
N1 C5 C6 115.7(8) . . ?
N2 C6 C7 122.6(7) . . ?
N2 C6 C5 117.0(7) . . ?
C7 C6 C5 120.4(8) . . ?
C8 C7 C12 121.2(9) . . ?
C8 C7 C6 121.6(9) . . ?
C12 C7 C6 117.1(8) . . ?
C7 C8 C9 118.2(10) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
C10 C9 C8 121.0(10) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C9 120.7(10) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 121.0(10) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C7 117.9(9) . . ?
C11 C12 H12 121.1 . . ?
C7 C12 H12 121.1 . . ?
O1 C13 N3 126.2(8) . . ?
O1 C13 C14 119.2(7) . . ?
N3 C13 C14 114.6(7) . . ?
C18 C14 C15 117.2(8) . . ?
C18 C14 C13 121.2(8) . . ?
C15 C14 C13 121.3(8) . . ?
C16 C15 C14 118.5(8) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
N4 C16 C15 124.3(9) . . ?
N4 C16 H16 117.9 . . ?
C15 C16 H16 117.9 . . ?
N4 C17 C18 124.1(8) . . ?
N4 C17 H17 118 . . ?
C18 C17 H17 118 . . ?
C17 C18 C14 119.2(8) . . ?
C17 C18 H18 120.4 . . ?
C14 C18 H18 120.4 . . ?
N5 C19 S1 178.4(11) . . ?
N6 C20 C21 121.5(9) . . ?
N6 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 119.7(9) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 117.5(9) . . ?
C21 C22 H22 121.3 . . ?
C23 C22 H22 121.3 . . ?
C24 C23 C22 121.3(9) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
N6 C24 C23 120.2(8) . . ?
N6 C24 C25 114.9(8) . . ?
C23 C24 C25 124.8(8) . . ?
N7 C25 C24 118.1(8) . . ?
N7 C25 C26 122.4(8) . . ?
C24 C25 C26 119.5(8) . . ?
C31 C26 C27 118.1(8) . . ?
C31 C26 C25 119.8(8) . . ?
C27 C26 C25 122.1(8) . . ?
C28 C27 C26 119.8(9) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C29 C28 C27 120.8(11) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 120.8(10) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C31 C30 C29 118.4(10) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
C26 C31 C30 122.0(10) . . ?
C26 C31 H31 119 . . ?
C30 C31 H31 119 . . ?
O2 C32 N8 129.1(8) . . ?
O2 C32 C33 116.1(8) . . ?
N8 C32 C33 114.8(7) . . ?
C34 C33 C37 117.4(8) . . ?
C34 C33 C32 122.0(8) . . ?
C37 C33 C32 120.6(8) . . ?
C33 C34 C35 119.8(8) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
N9 C35 C34 123.6(9) . . ?
N9 C35 H35 118.2 . . ?
C34 C35 H35 118.2 . . ?
N9 C36 C37 125.7(9) . . ?
N9 C36 H36 117.1 . . ?
C37 C36 H36 117.1 . . ?
C36 C37 C33 118.6(8) . . ?
C36 C37 H37 120.7 . . ?
C33 C37 H37 120.7 . . ?
N10 C38 S2 179.7(11) . . ?
C1 N1 C5 118.9(8) . . ?
C1 N1 Pb1 123.1(6) . . ?
C5 N1 Pb1 117.9(5) . . ?
C6 N2 N3 117.0(7) . . ?
C6 N2 Pb1 124.6(5) . . ?
N3 N2 Pb1 118.4(5) . . ?
C13 N3 N2 113.0(7) . . ?
C16 N4 C17 116.6(8) . . ?
C19 N5 Pb1 116.2(8) . . ?
C20 N6 C24 119.8(8) . . ?
C20 N6 Pb2 121.5(6) . . ?
C24 N6 Pb2 118.7(6) . . ?
C25 N7 N8 119.5(7) . . ?
C25 N7 Pb2 123.5(6) . . ?
N8 N7 Pb2 117.0(5) . . ?
C32 N8 N7 112.8(7) . . ?
C36 N9 C35 114.6(8) . . ?
C38 N10 Pb2 123.7(8) . . ?
C13 O1 Pb1 114.4(5) . . ?
C32 O2 Pb2 113.0(5) . . ?
N2 Pb1 O1 66.0(2) . . ?
N2 Pb1 N5 86.3(3) . . ?
O1 Pb1 N5 83.4(3) . . ?
N2 Pb1 N1 64.8(2) . . ?
O1 Pb1 N1 128.8(2) . . ?
N5 Pb1 N1 80.6(3) . . ?
N10 Pb2 N7 86.5(3) . . ?
N10 Pb2 O2 83.2(3) . . ?
N7 Pb2 O2 65.9(2) . . ?
N10 Pb2 N6 80.3(3) . . ?
N7 Pb2 N6 64.7(2) . . ?
O2 Pb2 N6 128.5(2) . . ?



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

data_p21c
_database_code_depnum_ccdc_archive 'CCDC 1444898'
_audit_update_record             
;
2015-12-31 deposited with the CCDC.
2016-02-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H34 N10 O8 Pb2'
_chemical_formula_weight         1173.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   10.7519(11)
_cell_length_b                   19.718(2)
_cell_length_c                   9.2550(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.250(4)
_cell_angle_gamma                90.00
_cell_volume                     1893.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      40.11

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    8.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4106
_exptl_absorpt_correction_T_max  0.4651
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            85363
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         39.39
_reflns_number_total             11292
_reflns_number_gt                9807
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0127P)²+1.6955P] 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_extinction_coef       ?
_refine_ls_number_reflns         11292
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0197
_refine_ls_wR_factor_ref         0.0400
_refine_ls_wR_factor_gt          0.0383
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.101988(4) 0.397519(2) -0.076118(5) 0.01092(1) Uani 1 1 d . . .
N2 N 0.15723(11) 0.50850(6) 0.03256(13) 0.01056(17) Uani 1 1 d . . .
C2 C 0.22287(12) 0.51735(6) 0.17083(14) 0.01019(19) Uani 1 1 d . . .
O1 O 0.04643(10) 0.49268(5) -0.25472(11) 0.01464(18) Uani 1 1 d . . .
N4 N -0.05109(13) 0.72904(7) -0.46745(15) 0.0167(2) Uani 1 1 d . . .
N3 N 0.23759(11) 0.39563(6) 0.18610(14) 0.01269(18) Uani 1 1 d . . .
N1 N 0.11289(11) 0.56574(6) -0.05073(12) 0.01119(18) Uani 1 1 d . . .
C17 C 0.34847(13) 0.45791(7) 0.40337(16) 0.0137(2) Uani 1 1 d . . .
H17 H 0.3719 0.5003 0.4519 0.016 Uiso 1 1 calc R . .
C15 C 0.35594(15) 0.33642(7) 0.40410(18) 0.0170(2) Uani 1 1 d . . .
H15 H 0.3838 0.2946 0.4528 0.020 Uiso 1 1 calc R . .
C9 C 0.21656(13) 0.60268(7) 0.36978(15) 0.0135(2) Uani 1 1 d . . .
H9 H 0.1668 0.5718 0.4103 0.016 Uiso 1 1 calc R . .
C14 C 0.27858(14) 0.33776(7) 0.25769(17) 0.0147(2) Uani 1 1 d . . .
H14 H 0.2541 0.2960 0.2069 0.018 Uiso 1 1 calc R . .
C18 C 0.27064(12) 0.45532(7) 0.25711(15) 0.0107(2) Uani 1 1 d . . .
C1 C 0.06314(12) 0.55079(7) -0.19550(14) 0.01045(19) Uani 1 1 d . . .
C16 C 0.39132(14) 0.39758(8) 0.47713(17) 0.0173(2) Uani 1 1 d . . .
H16 H 0.4445 0.3982 0.5769 0.021 Uiso 1 1 calc R . .
C4 C -0.04610(14) 0.60724(7) -0.44034(15) 0.0137(2) Uani 1 1 d . . .
H4 H -0.0690 0.5642 -0.4855 0.016 Uiso 1 1 calc R . .
C5 C 0.02503(12) 0.61241(7) -0.29101(15) 0.0113(2) Uani 1 1 d . . .
C8 C 0.25470(12) 0.58519(7) 0.24140(14) 0.01063(19) Uani 1 1 d . . .
C11 C 0.32475(15) 0.71040(7) 0.38012(17) 0.0170(3) Uani 1 1 d . . .
H11 H 0.3485 0.7530 0.4272 0.020 Uiso 1 1 calc R . .
C12 C 0.36344(15) 0.69314(8) 0.25277(16) 0.0166(2) Uani 1 1 d . . .
H12 H 0.4141 0.7239 0.2133 0.020 Uiso 1 1 calc R . .
C13 C 0.32825(14) 0.63101(7) 0.18314(16) 0.0140(2) Uani 1 1 d . . .
H13 H 0.3542 0.6196 0.0957 0.017 Uiso 1 1 calc R . .
C6 C 0.05953(14) 0.67703(7) -0.23359(16) 0.0141(2) Uani 1 1 d . . .
H6 H 0.1092 0.6828 -0.1330 0.017 Uiso 1 1 calc R . .
C7 C 0.02035(15) 0.73278(7) -0.32525(17) 0.0169(2) Uani 1 1 d . . .
H7 H 0.0457 0.7764 -0.2847 0.020 Uiso 1 1 calc R . .
C10 C 0.25127(15) 0.66521(8) 0.43836(17) 0.0165(2) Uani 1 1 d . . .
H10 H 0.2247 0.6770 0.5252 0.020 Uiso 1 1 calc R . .
C3 C -0.08252(14) 0.66653(8) -0.52127(16) 0.0160(2) Uani 1 1 d . . .
H3 H -0.1332 0.6625 -0.6218 0.019 Uiso 1 1 calc R . .
O2 O 0.29973(12) 0.42439(6) -0.14260(15) 0.0230(2) Uani 1 1 d . . .
O3 O 0.31594(15) 0.32109(7) -0.0880(2) 0.0365(3) Uani 1 1 d . . .
N5 N 0.36567(15) 0.36978(9) -0.13310(19) 0.0258(3) Uani 1 1 d . . .
O4 O 0.3623(3) 0.53461(10) 0.69740(19) 0.0633(7) Uani 1 1 d . . .
H4A H 0.3633 0.4970 0.7404 0.095 Uiso 1 1 calc R . .
C19 C 0.4095(2) 0.58420(12) 0.8030(2) 0.0329(4) Uani 1 1 d . . .
H19A H 0.4711 0.5640 0.8895 0.049 Uiso 1 1 calc R . .
H19B H 0.3381 0.6045 0.8352 0.049 Uiso 1 1 calc R . .
H19C H 0.4529 0.6193 0.7592 0.049 Uiso 1 1 calc R . .


_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 2.4163(11) . ?
Pb1 O2 2.4224(12) . ?
Pb1 O1 2.4679(11) . ?
Pb1 N3 2.4810(12) . ?
N2 C2 1.3004(17) . ?
N2 N1 1.3792(16) . ?
C2 C18 1.4770(18) . ?
C2 C8 1.4885(18) . ?
O1 C1 1.2625(16) . ?
N4 C3 1.339(2) . ?
N4 C7 1.340(2) . ?
N3 C14 1.3348(18) . ?
N3 C18 1.3493(17) . ?
N1 C1 1.3383(17) . ?
C17 C16 1.388(2) . ?
C17 C18 1.3926(19) . ?
C15 C16 1.386(2) . ?
C15 C14 1.391(2) . ?
C9 C10 1.392(2) . ?
C9 C8 1.3983(19) . ?
C1 C5 1.4949(19) . ?
C4 C3 1.388(2) . ?
C4 C5 1.3962(19) . ?
C5 C6 1.3927(19) . ?
C8 C13 1.399(2) . ?
C11 C10 1.390(2) . ?
C11 C12 1.391(2) . ?
C12 C13 1.390(2) . ?
C6 C7 1.385(2) . ?
O2 N5 1.279(2) . ?
O3 N5 1.225(2) . ?
O4 C19 1.381(3) . ?

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 O2 76.80(4) . . ?
N2 Pb1 O1 65.16(4) . . ?
O2 Pb1 O1 74.78(4) . . ?
N2 Pb1 N3 65.77(4) . . ?
O2 Pb1 N3 85.56(4) . . ?
O1 Pb1 N3 130.02(4) . . ?
C2 N2 N1 117.29(11) . . ?
C2 N2 Pb1 122.79(9) . . ?
N1 N2 Pb1 119.83(8) . . ?
N2 C2 C18 116.26(11) . . ?
N2 C2 C8 123.72(12) . . ?
C18 C2 C8 119.99(11) . . ?
C1 O1 Pb1 114.68(8) . . ?
C3 N4 C7 116.06(13) . . ?
C14 N3 C18 119.58(12) . . ?
C14 N3 Pb1 122.06(9) . . ?
C18 N3 Pb1 118.36(9) . . ?
C1 N1 N2 111.58(11) . . ?
C16 C17 C18 118.90(13) . . ?
C16 C15 C14 118.39(13) . . ?
C10 C9 C8 120.16(13) . . ?
N3 C14 C15 122.31(13) . . ?
N3 C18 C17 121.29(12) . . ?
N3 C18 C2 116.71(11) . . ?
C17 C18 C2 121.99(12) . . ?
O1 C1 N1 127.46(12) . . ?
O1 C1 C5 119.69(11) . . ?
N1 C1 C5 112.85(11) . . ?
C15 C16 C17 119.52(13) . . ?
C3 C4 C5 118.43(13) . . ?
C6 C5 C4 117.78(12) . . ?
C6 C5 C1 120.92(12) . . ?
C4 C5 C1 121.31(12) . . ?
C9 C8 C13 119.35(12) . . ?
C9 C8 C2 120.63(12) . . ?
C13 C8 C2 119.96(12) . . ?
C10 C11 C12 119.91(13) . . ?
C13 C12 C11 120.19(14) . . ?
C12 C13 C8 120.21(13) . . ?
C7 C6 C5 119.01(13) . . ?
N4 C7 C6 124.15(14) . . ?
C11 C10 C9 120.16(14) . . ?
N4 C3 C4 124.52(13) . . ?
N5 O2 Pb1 107.82(11) . . ?
O3 N5 O2 113.54(15) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        39.39
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.387
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.123
