# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_lv721
_audit_block_doi                 10.5517/ccdc.csd.cc23rlm3

_database_code_depnum_ccdc_archive 'CCDC 1959095'
loop_
_audit_author_name
_audit_author_address
'Brian Skelton'
;University of Western Australia
Australia
;
_audit_update_record             
;
2019-12-16 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;


_audit_creation_date             2015-01-13T10:03:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C16 H18 Cl4 N4 Zn'
_chemical_formula_moiety         '2(C8 H9 N2), Cl4 Zn'
_chemical_formula_weight         473.51

#----------------------------------------------------------------------------#
#                   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                   9.3908(3)
_cell_length_b                   10.6494(4)
_cell_length_c                   10.7328(3)
_cell_angle_alpha                99.224(3)
_cell_angle_beta                 111.029(3)
_cell_angle_gamma                91.986(3)
_cell_volume                     983.95(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13737
_cell_measurement_theta_min      2.088
_cell_measurement_theta_max      37.101

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

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_F_000             480
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.1154
-1 -15 2 0.1551
1 0 0 0.0459
-1 0 0 0.0943
-1 0 1 0.1355
1 0 2 0.1296
1 1 -1 0.1603
0 -1 -2 0.2503
-1 -2 0 0.1355
-2 -1 0 0.102


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

_exptl_absorpt_coefficient_mu    1.798
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
   CrysAlisPro, Agilent Technologies

;
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_T_max  0.811

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

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      100(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_detector_area_resol_mean 10.4738
_diffrn_orient_matrix_ub_11      -0.0769263
_diffrn_orient_matrix_ub_12      0.0150976
_diffrn_orient_matrix_ub_13      -0.0177416
_diffrn_orient_matrix_ub_21      -0.0236653
_diffrn_orient_matrix_ub_22      -0.0637737
_diffrn_orient_matrix_ub_23      0.0007104
_diffrn_orient_matrix_ub_31      0.0116937
_diffrn_orient_matrix_ub_32      0.0174422
_diffrn_orient_matrix_ub_33      0.0698264
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_number            33095
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.947
_diffrn_reflns_theta_max         37.59
_diffrn_reflns_theta_full        37
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.99
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.99
_diffrn_reflns_point_group_measured_fraction_max 0.962
_reflns_number_total             10024
_reflns_number_gt                8331
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 
;
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'

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

_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
Largest peak is 0.85 Angstroms from Cl4; deepest hole is 0.38 Angstroms 
from N13A.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0496P)²+0.6512P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10024
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.049
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.1062
_refine_ls_wR_factor_gt          0.0984
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.297
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.098

#----------------------------------------------------------------------------#
#                   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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.76237(16) 0.54765(13) 0.26683(15) 0.0187(2) Uani 1 d . .
H11 H 0.8364 0.5078 0.3305 0.022 Uiso 1 calc . .
N12 N 0.78854(13) 0.61749(11) 0.18290(12) 0.01682(19) Uani 1 d . .
C12 C 0.93783(17) 0.64341(16) 0.17342(18) 0.0231(3) Uani 1 d . .
H12A H 0.9977 0.5706 0.1931 0.035 Uiso 1 calc . .
H12B H 0.9927 0.7204 0.2393 0.035 Uiso 1 calc . .
H12C H 0.9231 0.6566 0.0815 0.035 Uiso 1 calc . .
C13 C 0.65592(16) 0.65998(13) 0.10480(15) 0.0179(2) Uani 1 d . .
H13 H 0.645 0.7112 0.0377 0.021 Uiso 1 calc . .
N13A N 0.54194(15) 0.61440(12) 0.14206(14) 0.0210(2) Uani 1 d . .
C14 C 0.38157(16) 0.62398(15) 0.09859(16) 0.0215(3) Uani 1 d . .
H14 H 0.3318 0.6683 0.0272 0.026 Uiso 1 calc . .
C15 C 0.30150(19) 0.56832(17) 0.1615(2) 0.0278(3) Uani 1 d . .
H15 H 0.1943 0.5746 0.1343 0.033 Uiso 1 calc . .
C16 C 0.3751(2) 0.50038(17) 0.2682(2) 0.0310(4) Uani 1 d . .
H16 H 0.3165 0.4637 0.3117 0.037 Uiso 1 calc . .
C17 C 0.5268(2) 0.48753(16) 0.30802(19) 0.0265(3) Uani 1 d . .
H17 H 0.5749 0.441 0.3778 0.032 Uiso 1 calc . .
C17A C 0.61109(15) 0.54426(12) 0.24418(13) 0.01406(19) Uani 1 d . .
C21 C 0.29077(17) 0.89766(14) 0.31680(16) 0.0214(3) Uani 1 d . .
H21 H 0.1938 0.897 0.326 0.026 Uiso 1 calc . .
N22 N 0.32633(17) 0.93710(13) 0.21516(13) 0.0226(2) Uani 1 d . .
C22 C 0.2200(3) 0.98895(19) 0.10208(18) 0.0345(4) Uani 1 d . .
H22A H 0.2765 1.0211 0.0507 0.052 Uiso 1 calc . .
H22B H 0.1723 1.059 0.138 0.052 Uiso 1 calc . .
H22C H 0.1404 0.9213 0.0422 0.052 Uiso 1 calc . .
C23 C 0.4731(2) 0.92418(14) 0.23386(15) 0.0220(3) Uani 1 d . .
H23 H 0.5243 0.9445 0.1766 0.026 Uiso 1 calc . .
N23A N 0.53514(15) 0.87718(11) 0.34851(13) 0.0178(2) Uani 1 d . .
C24 C 0.68540(18) 0.84795(15) 0.41248(18) 0.0240(3) Uani 1 d . .
H24 H 0.7613 0.8603 0.375 0.029 Uiso 1 calc . .
C25 C 0.7195(2) 0.80185(16) 0.52862(19) 0.0290(3) Uani 1 d . .
H25 H 0.8203 0.78 0.5723 0.035 Uiso 1 calc . .
C26 C 0.6073(2) 0.78527(16) 0.58727(17) 0.0286(3) Uani 1 d . .
H26 H 0.6354 0.7549 0.6705 0.034 Uiso 1 calc . .
C27 C 0.4620(2) 0.81210(15) 0.52624(16) 0.0236(3) Uani 1 d . .
H27 H 0.3875 0.7997 0.5652 0.028 Uiso 1 calc . .
C27A C 0.42217(16) 0.85923(13) 0.40275(14) 0.0168(2) Uani 1 d . .
Zn1 Zn 0.84597(2) 0.19368(2) 0.25133(2) 0.01713(4) Uani 1 d . .
Cl1 Cl 0.58795(4) 0.19015(4) 0.13678(4) 0.02242(7) Uani 1 d . .
Cl2 Cl 0.98326(4) 0.30043(4) 0.15506(4) 0.02244(7) Uani 1 d . .
Cl3 Cl 0.90087(5) -0.01249(4) 0.24417(4) 0.02630(8) Uani 1 d . .
Cl4 Cl 0.89826(5) 0.30497(4) 0.46509(4) 0.02654(8) Uani 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
C11 N12 1.3364(19) . ?
C11 C17A 1.3507(19) . ?
C11 H11 0.95 . ?
N12 C13 1.3674(18) . ?
N12 C12 1.4618(19) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 N13A 1.369(2) . ?
C13 H13 0.95 . ?
N13A C17A 1.4021(19) . ?
N13A C14 1.4205(19) . ?
C14 C15 1.355(2) . ?
C14 H14 0.95 . ?
C15 C16 1.430(3) . ?
C15 H15 0.95 . ?
C16 C17 1.351(3) . ?
C16 H16 0.95 . ?
C17 C17A 1.396(2) . ?
C17 H17 0.95 . ?
C21 N22 1.370(2) . ?
C21 C27A 1.371(2) . ?
C21 H21 0.95 . ?
N22 C23 1.335(2) . ?
N22 C22 1.469(2) . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 N23A 1.344(2) . ?
C23 H23 0.95 . ?
N23A C24 1.401(2) . ?
N23A C27A 1.4021(18) . ?
C24 C25 1.348(3) . ?
C24 H24 0.95 . ?
C25 C26 1.427(3) . ?
C25 H25 0.95 . ?
C26 C27 1.348(3) . ?
C26 H26 0.95 . ?
C27 C27A 1.421(2) . ?
C27 H27 0.95 . ?
Zn1 Cl3 2.2682(4) . ?
Zn1 Cl4 2.2779(4) . ?
Zn1 Cl1 2.2858(4) . ?
Zn1 Cl2 2.2920(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N12 C11 C17A 107.21(12) . . ?
N12 C11 H11 126.4 . . ?
C17A C11 H11 126.4 . . ?
C11 N12 C13 110.85(12) . . ?
C11 N12 C12 124.88(13) . . ?
C13 N12 C12 124.26(13) . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N12 C13 N13A 106.65(12) . . ?
N12 C13 H13 126.7 . . ?
N13A C13 H13 126.7 . . ?
C13 N13A C17A 106.65(12) . . ?
C13 N13A C14 133.89(14) . . ?
C17A N13A C14 119.46(13) . . ?
C15 C14 N13A 118.30(15) . . ?
C15 C14 H14 120.8 . . ?
N13A C14 H14 120.8 . . ?
C14 C15 C16 121.29(15) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 121.04(16) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C17A 118.41(16) . . ?
C16 C17 H17 120.8 . . ?
C17A C17 H17 120.8 . . ?
C11 C17A C17 129.90(14) . . ?
C11 C17A N13A 108.64(12) . . ?
C17 C17A N13A 121.43(13) . . ?
N22 C21 C27A 106.73(13) . . ?
N22 C21 H21 126.6 . . ?
C27A C21 H21 126.6 . . ?
C23 N22 C21 110.58(13) . . ?
C23 N22 C22 124.08(16) . . ?
C21 N22 C22 125.33(16) . . ?
N22 C22 H22A 109.5 . . ?
N22 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N22 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N22 C23 N23A 107.45(13) . . ?
N22 C23 H23 126.3 . . ?
N23A C23 H23 126.3 . . ?
C23 N23A C24 129.71(14) . . ?
C23 N23A C27A 108.90(13) . . ?
C24 N23A C27A 121.39(13) . . ?
C25 C24 N23A 118.25(15) . . ?
C25 C24 H24 120.9 . . ?
N23A C24 H24 120.9 . . ?
C24 C25 C26 121.36(16) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C27 C26 C25 120.97(16) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C27A 118.90(15) . . ?
C26 C27 H27 120.5 . . ?
C27A C27 H27 120.5 . . ?
C21 C27A N23A 106.34(13) . . ?
C21 C27A C27 134.55(14) . . ?
N23A C27A C27 119.09(13) . . ?
Cl3 Zn1 Cl4 113.959(17) . . ?
Cl3 Zn1 Cl1 107.146(17) . . ?
Cl4 Zn1 Cl1 106.697(16) . . ?
Cl3 Zn1 Cl2 110.222(16) . . ?
Cl4 Zn1 Cl2 107.423(16) . . ?
Cl1 Zn1 Cl2 111.392(15) . . ?

####################################################################### 
# 
# 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_um1
_database_code_depnum_ccdc_archive 'CCDC 1972389'
loop_
_audit_author_name
_audit_author_address
'Dmytro Nesterov'
;Instituto Superior Tecnico, Universidade de Lisboa
Portugal
;
_audit_update_record             
;
2019-12-16 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H15 Cl N3 O2 Pd, Cl'
_chemical_formula_sum            'C13 H15 Cl2 N3 O2 Pd'
_chemical_formula_weight         422.58

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   8.3872(5)
_cell_length_b                   14.4806(7)
_cell_length_c                   13.0923(9)
_cell_angle_alpha                90
_cell_angle_beta                 102.917(2)
_cell_angle_gamma                90
_cell_volume                     1549.84(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6260
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      26.35

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    1.548
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5728
_exptl_special_details           
;
 The following wavelength and cell were deduced by SADABS from the
 direction cosines etc. They are given here for emergency use only:
 CELL 0.71072    8.390   14.490   13.887   89.986  113.113   90.007
;
_diffrn_ambient_temperature      296(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_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11353
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.813
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1423
_reflns_number_gt                1235
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+7.0040P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1423
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0626
_refine_ls_wR_factor_gt          0.0577
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.53214(5) 0.500000 0.32157(3) 0.02880(16) Uani 1 2 d S T P . .
Cl1 Cl 0.75857(19) 0.500000 0.45862(11) 0.0515(4) Uani 1 2 d S T P . .
O1 O 0.2000(4) 0.3881(2) 0.0735(2) 0.0469(7) Uani 1 1 d . . . . .
N1 N 0.5062(3) 0.36192(19) 0.3091(2) 0.0305(6) Uani 1 1 d . . . . .
N2 N 0.3302(5) 0.500000 0.2015(3) 0.0247(8) Uani 1 2 d S T P . .
C1 C 0.5650(4) 0.2977(2) 0.3813(3) 0.0355(8) Uani 1 1 d . . . . .
H1A H 0.637976 0.315394 0.442625 0.043 Uiso 1 1 calc R U . . .
C2 C 0.5207(5) 0.2065(2) 0.3676(3) 0.0406(9) Uani 1 1 d . . . . .
H2A H 0.563248 0.163097 0.418867 0.049 Uiso 1 1 calc R U . . .
C3 C 0.4130(5) 0.1802(3) 0.2776(3) 0.0425(9) Uani 1 1 d . . . . .
H3A H 0.380808 0.118843 0.267452 0.051 Uiso 1 1 calc R U . . .
C4 C 0.3526(5) 0.2453(2) 0.2019(3) 0.0384(9) Uani 1 1 d . . . . .
H4A H 0.280392 0.228222 0.140027 0.046 Uiso 1 1 calc R U . . .
C5 C 0.4011(4) 0.3366(2) 0.2195(3) 0.0308(8) Uani 1 1 d . . . . .
C6 C 0.3452(4) 0.4129(2) 0.1415(3) 0.0325(8) Uani 1 1 d . . . . .
H6A H 0.428720 0.422424 0.100790 0.039 Uiso 1 1 calc R U . . .
C7 C 0.1829(6) 0.500000 0.2444(4) 0.0337(11) Uani 1 2 d S T P . .
H7A H 0.170255 0.559478 0.274004 0.051 Uiso 0.5 1 calc R U P . .
H7B H 0.193215 0.453623 0.297893 0.051 Uiso 0.5 1 calc R U P . .
H7C H 0.088981 0.486898 0.189440 0.051 Uiso 0.5 1 calc R U P . .
Cl2 Cl 0.26702(17) 0.500000 -0.11076(10) 0.0436(3) Uani 1 2 d S T P . .
H1 H 0.200(7) 0.411(4) 0.020(4) 0.09(2) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.014(3) . ?
Pd1 N1 2.014(3) 6_565 ?
Pd1 N2 2.037(4) . ?
Pd1 Cl1 2.3028(14) . ?
O1 C6 1.386(4) . ?
O1 H1 0.78(5) . ?
N1 C1 1.340(4) . ?
N1 C5 1.351(4) . ?
N2 C7 1.466(6) . ?
N2 C6 1.506(4) 6_565 ?
N2 C6 1.506(4) . ?
C1 C2 1.373(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.369(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.379(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.506(5) . ?
C6 H6A 0.9800 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C7 H7A 0.96(3) 6_565 ?
C7 H7B 0.96(5) 6_565 ?
C7 H7C 0.96(2) 6_565 ?

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 Pd1 N1 166.25(16) . 6_565 ?
N1 Pd1 N2 83.18(8) . . ?
N1 Pd1 N2 83.18(8) 6_565 . ?
N1 Pd1 Cl1 96.81(8) . . ?
N1 Pd1 Cl1 96.81(8) 6_565 . ?
N2 Pd1 Cl1 179.35(11) . . ?
C6 O1 H1 107(4) . . ?
C1 N1 C5 119.4(3) . . ?
C1 N1 Pd1 128.0(2) . . ?
C5 N1 Pd1 112.2(2) . . ?
C7 N2 C6 112.1(2) . 6_565 ?
C7 N2 C6 112.1(2) . . ?
C6 N2 C6 113.7(4) 6_565 . ?
C7 N2 Pd1 109.3(3) . . ?
C6 N2 Pd1 104.5(2) 6_565 . ?
C6 N2 Pd1 104.5(2) . . ?
N1 C1 C2 122.0(3) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 119.0(4) . . ?
C3 C4 H4A 120.5 . . ?
C5 C4 H4A 120.5 . . ?
N1 C5 C4 120.8(3) . . ?
N1 C5 C6 115.7(3) . . ?
C4 C5 C6 123.4(3) . . ?
O1 C6 N2 112.9(3) . . ?
O1 C6 C5 109.9(3) . . ?
N2 C6 C5 108.1(3) . . ?
O1 C6 H6A 108.6 . . ?
N2 C6 H6A 108.6 . . ?
C5 C6 H6A 108.6 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C7 H7A 109.5(6) . 6_565 ?
H7A C7 H7A 127.6 . 6_565 ?
H7B C7 H7A 22.8 . 6_565 ?
H7C C7 H7A 88.8 . 6_565 ?
N2 C7 H7B 109.5(11) . 6_565 ?
H7A C7 H7B 22.8 . 6_565 ?
H7B C7 H7B 88.8 . 6_565 ?
H7C C7 H7B 127.6 . 6_565 ?
H7A C7 H7B 109.5 6_565 6_565 ?
N2 C7 H7C 109.5(5) . 6_565 ?
H7A C7 H7C 88.8 . 6_565 ?
H7B C7 H7C 127.6 . 6_565 ?
H7C C7 H7C 22.8 . 6_565 ?
H7A C7 H7C 109.5 6_565 6_565 ?
H7B C7 H7C 109.5 6_565 6_565 ?

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
C5 N1 C1 C2 -0.5(5) . . . . ?
Pd1 N1 C1 C2 171.4(3) . . . . ?
N1 C1 C2 C3 -0.1(6) . . . . ?
C1 C2 C3 C4 0.7(6) . . . . ?
C2 C3 C4 C5 -0.8(6) . . . . ?
C1 N1 C5 C4 0.5(5) . . . . ?
Pd1 N1 C5 C4 -172.6(3) . . . . ?
C1 N1 C5 C6 -178.3(3) . . . . ?
Pd1 N1 C5 C6 8.6(4) . . . . ?
C3 C4 C5 N1 0.2(5) . . . . ?
C3 C4 C5 C6 178.8(3) . . . . ?
C7 N2 C6 O1 45.9(4) . . . . ?
C6 N2 C6 O1 -82.5(4) 6_565 . . . ?
Pd1 N2 C6 O1 164.1(2) . . . . ?
C7 N2 C6 C5 -75.9(4) . . . . ?
C6 N2 C6 C5 155.7(2) 6_565 . . . ?
Pd1 N2 C6 C5 42.4(3) . . . . ?
N1 C5 C6 O1 -158.8(3) . . . . ?
C4 C5 C6 O1 22.5(5) . . . . ?
N1 C5 C6 N2 -35.2(4) . . . . ?
C4 C5 C6 N2 146.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 Cl2 0.78(5) 2.31(5) 3.061(3) 163(6) .

_refine_diff_density_max         1.239
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_lv744f
_database_code_depnum_ccdc_archive 'CCDC 1972254'
loop_
_audit_author_name
_audit_author_address
'Brian Skelton'
;University of Western Australia
Australia
;
_audit_update_record             
;
2019-12-16 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;

_audit_creation_date             2015-12-21T06:13:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_formula_sum            'C8 H9 Cl3 N2 Pb'
_chemical_formula_moiety         'Cl3 Pb, C8 H9 N2'
_chemical_formula_weight         446.71
_chemical_absolute_configuration ad

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_Int_Tables_number      43
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   43.5467(12)
_cell_length_b                   24.8590(7)
_cell_length_c                   4.32220(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4678.9(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7782
_cell_measurement_theta_min      1.903
_cell_measurement_theta_max      32.178

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

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.085
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_F_000             3264
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0371
-1 1 0 0.0477
-3 -1 0 0.0811
3 1 0 0.0252
1 0 1 0.1353
-1 0 -1 0.2313
1 0 0 0.0277
-1 0 0 0.085
2 1 0 0.0209
-2 -1 0 0.0742
1 3 0 0.0292


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

_exptl_absorpt_coefficient_mu    15.07
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
         CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_exptl_absorpt_correction_T_min  0.073
_exptl_absorpt_correction_T_max  0.332

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

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      100(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_detector_area_resol_mean 10.4738
_diffrn_orient_matrix_ub_11      0.013616
_diffrn_orient_matrix_ub_12      -0.0039519
_diffrn_orient_matrix_ub_13      -0.0871415
_diffrn_orient_matrix_ub_21      -0.0003442
_diffrn_orient_matrix_ub_22      0.0273546
_diffrn_orient_matrix_ub_23      -0.0465275
_diffrn_orient_matrix_ub_31      0.0089327
_diffrn_orient_matrix_ub_32      0.0070874
_diffrn_orient_matrix_ub_33      0.1310434
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_number            13122
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         1.871
_diffrn_reflns_theta_max         32.436
_diffrn_reflns_theta_full        31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_reflns_number_total             3868
_reflns_number_gt                3663
_reflns_threshold_expression     'I > 2σ(I)'

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

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'

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

_atom_sites_solution_hydrogens   geom

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

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3868
_refine_ls_number_parameters     129
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.026
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0318
_refine_ls_wR_factor_gt          0.0304
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_restrained_S_all      0.875
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.360(7)
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.236

#----------------------------------------------------------------------------#
#                   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'
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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.77530(2) 0.56395(2) 0.35137(11) 0.01193(4) Uani 1 d . .
Cl1 Cl 0.75969(3) 0.63403(4) 0.8464(4) 0.0199(2) Uani 1 d . .
Cl2 Cl 0.83226(3) 0.60435(4) 0.3631(4) 0.0167(2) Uani 1 d . .
Cl3 Cl 0.79101(3) 0.48755(5) 0.8390(4) 0.0188(2) Uani 1 d . .
C1 C 0.87600(12) 0.76791(19) 0.6536(11) 0.0154(11) Uani 1 d . .
H1 H 0.8952 0.7855 0.6315 0.018 Uiso 1 calc . .
N2 N 0.87001(10) 0.72313(14) 0.8317(11) 0.0152(8) Uani 1 d . .
C2 C 0.89310(13) 0.6941(2) 1.0156(11) 0.0212(13) Uani 1 d . .
H2A H 0.883 0.666 1.1376 0.032 Uiso 1 calc . .
H2B H 0.9035 0.7193 1.1549 0.032 Uiso 1 calc . .
H2C H 0.9082 0.6776 0.8768 0.032 Uiso 1 calc . .
C3 C 0.84067(13) 0.7100(2) 0.8090(13) 0.0169(11) Uani 1 d . .
H3 H 0.8309 0.681 0.9121 0.02 Uiso 1 calc . .
N3A N 0.82708(9) 0.74512(14) 0.6139(12) 0.0150(8) Uani 1 d . .
C4 C 0.79684(12) 0.7476(2) 0.5152(11) 0.0159(11) Uani 1 d . .
H4 H 0.7823 0.7216 0.5815 0.019 Uiso 1 calc . .
C5 C 0.78855(12) 0.78772(19) 0.3234(15) 0.0195(11) Uani 1 d . .
H5 H 0.7678 0.7902 0.2558 0.023 Uiso 1 calc . .
C6 C 0.81043(14) 0.8266(2) 0.2195(11) 0.0177(11) Uani 1 d . .
H6 H 0.8041 0.8548 0.0854 0.021 Uiso 1 calc . .
C7 C 0.84010(12) 0.82345(19) 0.3118(12) 0.0152(11) Uani 1 d . .
H7 H 0.8547 0.8489 0.2394 0.018 Uiso 1 calc . .
C7A C 0.84928(12) 0.78203(19) 0.5163(10) 0.0116(10) Uani 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 Cl2 2.6767(12) . ?
Pb1 Cl1 2.8418(15) . ?
Pb1 Cl1 2.8740(15) 1_554 ?
Pb1 Cl3 2.9185(15) . ?
Pb1 Cl3 2.9966(16) 1_554 ?
Pb1 Cl3 3.1593(12) 10_664 ?
Cl1 Pb1 2.8740(15) 1_556 ?
Cl3 Pb1 2.9966(16) 1_556 ?
Cl3 Pb1 3.1591(12) 10_665 ?
C1 C7A 1.352(7) . ?
C1 N2 1.378(6) . ?
C1 H1 0.95 . ?
N2 C3 1.322(6) . ?
N2 C2 1.471(6) . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 N3A 1.350(7) . ?
C3 H3 0.95 . ?
N3A C4 1.385(6) . ?
N3A C7A 1.398(6) . ?
C4 C5 1.346(7) . ?
C4 H4 0.95 . ?
C5 C6 1.430(7) . ?
C5 H5 0.95 . ?
C6 C7 1.354(7) . ?
C6 H6 0.95 . ?
C7 C7A 1.415(7) . ?
C7 H7 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
Cl2 Pb1 Cl1 88.70(4) . . ?
Cl2 Pb1 Cl1 90.35(4) . 1_554 ?
Cl1 Pb1 Cl1 98.26(3) . 1_554 ?
Cl2 Pb1 Cl3 90.76(4) . . ?
Cl1 Pb1 Cl3 84.91(4) . . ?
Cl1 Pb1 Cl3 176.67(5) 1_554 . ?
Cl2 Pb1 Cl3 92.30(4) . 1_554 ?
Cl1 Pb1 Cl3 178.44(4) . 1_554 ?
Cl1 Pb1 Cl3 82.93(4) 1_554 1_554 ?
Cl3 Pb1 Cl3 93.88(3) . 1_554 ?
Cl2 Pb1 Cl3 178.13(3) . 10_664 ?
Cl1 Pb1 Cl3 92.44(4) . 10_664 ?
Cl1 Pb1 Cl3 90.95(4) 1_554 10_664 ?
Cl3 Pb1 Cl3 87.87(4) . 10_664 ?
Cl3 Pb1 Cl3 86.53(4) 1_554 10_664 ?
Pb1 Cl1 Pb1 98.26(3) . 1_556 ?
Pb1 Cl3 Pb1 93.88(3) . 1_556 ?
Pb1 Cl3 Pb1 93.53(4) . 10_665 ?
Pb1 Cl3 Pb1 92.04(4) 1_556 10_665 ?
C7A C1 N2 107.0(5) . . ?
C7A C1 H1 126.5 . . ?
N2 C1 H1 126.5 . . ?
C3 N2 C1 109.9(5) . . ?
C3 N2 C2 125.4(5) . . ?
C1 N2 C2 124.7(5) . . ?
N2 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 N3A 108.1(5) . . ?
N2 C3 H3 125.9 . . ?
N3A C3 H3 125.9 . . ?
C3 N3A C4 129.7(4) . . ?
C3 N3A C7A 108.0(4) . . ?
C4 N3A C7A 122.3(4) . . ?
C5 C4 N3A 118.6(5) . . ?
C5 C4 H4 120.7 . . ?
N3A C4 H4 120.7 . . ?
C4 C5 C6 121.0(5) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 120.2(5) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C7A 119.8(5) . . ?
C6 C7 H7 120.1 . . ?
C7A C7 H7 120.1 . . ?
C1 C7A N3A 107.0(4) . . ?
C1 C7A C7 134.9(5) . . ?
N3A C7A C7 118.1(5) . . ?

