# Electronic Supplementary Material (ESI) for Sustainable Energy & Fuels.
# This journal is © The Royal Society of Chemistry 2019

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1902819'
loop_
_audit_author_name
_audit_author_address
'Eleuterio Alvarez'
; Spanish National Research Council 
Spain
;
_audit_update_record             
;
2019-03-13 deposited with the CCDC.	2019-06-27 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         'I3 Pb, C6 H7 N, 2(C3 H7 N O)'
_chemical_formula_sum            'C12 H21 I3 N3 O2 Pb'
_chemical_formula_weight         827.21

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   8.0816(8)
_cell_length_b                   12.3906(12)
_cell_length_c                   12.9013(11)
_cell_angle_alpha                97.876(4)
_cell_angle_beta                 106.389(4)
_cell_angle_gamma                104.083(4)
_cell_volume                     1172.40(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9172
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      30.00

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_F_000             742
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    11.151
_shelx_estimated_absorpt_T_min   0.095
_shelx_estimated_absorpt_T_max   0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4715
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature      193(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-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            15886
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.676
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4246
_reflns_number_gt                3842
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0892P)²+5.4792P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4246
_refine_ls_number_parameters     307
_refine_ls_number_restraints     352
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.1303
_refine_ls_wR_factor_gt          0.1253
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.000000 0.500000 0.000000 0.03091(16) Uani 1 2 d S . P . .
Pb2 Pb 0.500000 0.500000 0.000000 0.03252(16) Uani 1 2 d S . P . .
I1 I 0.84273(10) 0.50189(7) 0.20468(5) 0.0529(2) Uani 1 1 d . . . . .
I2 I 0.61739(7) 0.31660(5) -0.14128(5) 0.03884(18) Uani 1 1 d . . . . .
I3 I 1.20367(8) 0.31028(5) 0.05251(5) 0.04146(19) Uani 1 1 d . . . . .
N1A N -0.1439(19) 0.8156(15) 0.3172(15) 0.041(4) Uani 0.5 1 d D U P A 1
H1A1 H -0.162695 0.777088 0.247588 0.062 Uiso 0.5 1 calc R U P A 1
H1A2 H -0.174847 0.765079 0.358459 0.062 Uiso 0.5 1 calc R U P A 1
H1A3 H -0.212927 0.864008 0.313684 0.062 Uiso 0.5 1 calc R U P A 1
C1A C 0.0452(19) 0.8805(16) 0.3680(13) 0.0404(18) Uani 0.5 1 d D U P A 1
C2A C 0.108(2) 0.9471(14) 0.4755(12) 0.0408(18) Uani 0.5 1 d D U P A 1
H2A H 0.027241 0.948993 0.516529 0.049 Uiso 0.5 1 d R U P A 1
C3A C 0.2890(19) 1.0115(15) 0.5216(15) 0.040(2) Uani 0.5 1 d D U P A 1
H3A H 0.332517 1.055280 0.595479 0.048 Uiso 0.5 1 d R U P A 1
C5A C 0.341(2) 0.9413(17) 0.3558(15) 0.039(2) Uani 0.5 1 d D U P A 1
H5A H 0.422009 0.940238 0.314701 0.047 Uiso 0.5 1 d R U P A 1
C6A C 0.162(2) 0.8745(16) 0.3067(16) 0.0400(19) Uani 0.5 1 d D U P A 1
H6A H 0.121102 0.826361 0.234958 0.048 Uiso 0.5 1 d R U P A 1
N1B N -0.1663(19) 0.7677(16) 0.3225(15) 0.042(3) Uani 0.5 1 d D U P A 2
H1B1 H -0.224816 0.759898 0.373066 0.063 Uiso 0.5 1 calc R U P A 2
H1B2 H -0.205423 0.815408 0.280321 0.063 Uiso 0.5 1 calc R U P A 2
H1B3 H -0.189612 0.698185 0.278239 0.063 Uiso 0.5 1 calc R U P A 2
C1B C 0.0267(19) 0.8147(17) 0.3796(12) 0.0406(18) Uani 0.5 1 d D U P A 2
C2B C 0.094(2) 0.8483(16) 0.4958(11) 0.0401(19) Uani 0.5 1 d D U P A 2
H2B H 0.015966 0.835555 0.538665 0.048 Uiso 0.5 1 d R U P A 2
C3B C 0.2806(18) 0.9019(16) 0.5459(14) 0.040(2) Uani 0.5 1 d D U P A 2
H3B H 0.330409 0.923737 0.624360 0.048 Uiso 0.5 1 d R U P A 2
C5B C 0.326(2) 0.8868(18) 0.3699(16) 0.041(2) Uani 0.5 1 d D U P A 2
H5B H 0.403299 0.899691 0.326844 0.049 Uiso 0.5 1 d R U P A 2
C6B C 0.140(2) 0.8331(17) 0.3179(16) 0.0405(19) Uani 0.5 1 d D U P A 2
H6B H 0.092510 0.808038 0.239541 0.049 Uiso 0.5 1 d R U P A 2
C4A C 0.410(2) 1.0114(17) 0.4630(14) 0.040(4) Uani 0.5 1 d D . P . .
C4B C 0.397(2) 0.9239(13) 0.4833(13) 0.035(4) Uani 0.5 1 d D . P A .
O1 O 0.7591(12) -0.0340(8) 0.2261(7) 0.076(3) Uani 1 1 d D . . . .
N2 N 0.7468(15) 0.0483(8) 0.0770(11) 0.070(3) Uani 1 1 d . . . . .
C7 C 0.7501(14) -0.0353(9) 0.1299(8) 0.057(3) Uani 1 1 d D . . . .
H7 H 0.744729 -0.105899 0.087542 0.068 Uiso 1 1 calc R U . . .
C8 C 0.748(3) 0.1578(14) 0.1292(16) 0.097(5) Uani 1 1 d . U . . .
H8A H 0.796912 0.215549 0.092248 0.146 Uiso 1 1 calc R U . . .
H8B H 0.822361 0.176196 0.207375 0.146 Uiso 1 1 calc R U . . .
H8C H 0.623754 0.156877 0.123847 0.146 Uiso 1 1 calc R U . . .
C9 C 0.7398(19) 0.0354(12) -0.0356(12) 0.071(3) Uani 1 1 d . U . . .
H9A H 0.747392 -0.040606 -0.062433 0.107 Uiso 1 1 calc R U . . .
H9B H 0.841243 0.093616 -0.041391 0.107 Uiso 1 1 calc R U . . .
H9C H 0.625838 0.044115 -0.080532 0.107 Uiso 1 1 calc R U . . .
O2A O 0.3338(18) 0.2936(13) 0.5314(13) 0.067(4) Uani 0.57 1 d D . P B 1
N3A N 0.562(2) 0.3695(16) 0.4769(13) 0.065(3) Uani 0.57 1 d D U P B 1
C10A C 0.4927(19) 0.3438(17) 0.5489(16) 0.059(5) Uani 0.57 1 d D . P B 1
H10A H 0.570413 0.364969 0.623648 0.071 Uiso 0.57 1 calc R U P B 1
C11A C 0.747(2) 0.433(2) 0.509(2) 0.089(8) Uani 0.57 1 d D U P B 1
H11A H 0.810144 0.426177 0.583377 0.133 Uiso 0.57 1 calc R U P B 1
H11B H 0.757032 0.513416 0.508609 0.133 Uiso 0.57 1 calc R U P B 1
H11C H 0.800804 0.403193 0.456430 0.133 Uiso 0.57 1 calc R U P B 1
C12A C 0.464(3) 0.344(2) 0.3617(13) 0.074(5) Uani 0.57 1 d D U P B 1
H12A H 0.543817 0.331655 0.319411 0.111 Uiso 0.57 1 calc R U P B 1
H12B H 0.420031 0.408642 0.343091 0.111 Uiso 0.57 1 calc R U P B 1
H12C H 0.361460 0.275613 0.343065 0.111 Uiso 0.57 1 calc R U P B 1
O2B O 0.280(2) 0.1821(16) 0.5141(15) 0.058(3) Uani 0.43 1 d D U P C 2
N3B N 0.480(3) 0.218(2) 0.4227(17) 0.065(3) Uani 0.43 1 d D U P C 2
C10B C 0.431(3) 0.220(2) 0.509(2) 0.062(3) Uani 0.43 1 d D U P C 2
H10B H 0.523581 0.256042 0.578314 0.074 Uiso 0.43 1 calc R U P C 2
C11B C 0.664(3) 0.258(3) 0.428(3) 0.068(4) Uani 0.43 1 d D U P C 2
H11D H 0.739151 0.293875 0.505068 0.102 Uiso 0.43 1 calc R U P C 2
H11E H 0.675199 0.313632 0.381788 0.102 Uiso 0.43 1 calc R U P C 2
H11F H 0.702592 0.193523 0.401528 0.102 Uiso 0.43 1 calc R U P C 2
C12B C 0.360(4) 0.167(3) 0.3133(18) 0.075(5) Uani 0.43 1 d D U P C 2
H12D H 0.241117 0.127414 0.315954 0.112 Uiso 0.43 1 calc R U P C 2
H12E H 0.407118 0.111587 0.277510 0.112 Uiso 0.43 1 calc R U P C 2
H12F H 0.349716 0.225942 0.270837 0.112 Uiso 0.43 1 calc R U P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.2113(6) 2_765 ?
Pb1 I2 3.2113(6) . ?
Pb1 I3 3.2224(6) 2_765 ?
Pb1 I3 3.2225(6) . ?
Pb1 I1 3.2374(6) . ?
Pb1 I1 3.2374(6) 2_765 ?
Pb2 I2 3.2057(6) . ?
Pb2 I2 3.2057(6) 2_665 ?
Pb2 I3 3.2144(6) 2_765 ?
Pb2 I3 3.2144(6) 1_455 ?
Pb2 I1 3.2356(7) . ?
Pb2 I1 3.2356(7) 2_665 ?
N1A C1A 1.451(5) . ?
N1A H1A1 0.9100 . ?
N1A H1A2 0.9100 . ?
N1A H1A3 0.9100 . ?
C1A C2A 1.395(12) . ?
C1A C6A 1.40(3) . ?
C2A C3A 1.395(12) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.395(12) . ?
C3A H3A 0.9500 . ?
C5A C6A 1.396(12) . ?
C5A C4A 1.41(3) . ?
C5A H5A 0.9500 . ?
C6A H6A 0.9500 . ?
N1B C1B 1.451(5) . ?
N1B H1B1 0.9100 . ?
N1B H1B2 0.9100 . ?
N1B H1B3 0.9100 . ?
C1B C6B 1.37(3) . ?
C1B C2B 1.405(11) . ?
C2B C3B 1.405(12) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.405(12) . ?
C3B H3B 0.9500 . ?
C5B C4B 1.38(2) . ?
C5B C6B 1.405(12) . ?
C5B H5B 0.9500 . ?
C6B H6B 0.9500 . ?
C4A C4B 1.14(3) . ?
C4A C4B 1.48(2) 2_676 ?
O1 C7 1.221(5) . ?
N2 C7 1.318(15) . ?
N2 C9 1.423(18) . ?
N2 C8 1.427(19) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O2A C10A 1.223(5) . ?
N3A C10A 1.25(2) . ?
N3A C11A 1.420(5) . ?
N3A C12A 1.422(5) . ?
C10A H10A 0.9500 . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11C 0.9800 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
O2B C10B 1.220(5) . ?
N3B C10B 1.29(3) . ?
N3B C11B 1.420(5) . ?
N3B C12B 1.421(5) . ?
C10B H10B 0.9500 . ?
C11B H11D 0.9800 . ?
C11B H11E 0.9800 . ?
C11B H11F 0.9800 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?

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
I2 Pb1 I2 180.0 2_765 . ?
I2 Pb1 I3 94.321(17) 2_765 2_765 ?
I2 Pb1 I3 85.679(17) . 2_765 ?
I2 Pb1 I3 85.680(17) 2_765 . ?
I2 Pb1 I3 94.320(17) . . ?
I3 Pb1 I3 180.0 2_765 . ?
I2 Pb1 I1 94.728(19) 2_765 . ?
I2 Pb1 I1 85.272(19) . . ?
I3 Pb1 I1 83.231(17) 2_765 . ?
I3 Pb1 I1 96.770(17) . . ?
I2 Pb1 I1 85.273(19) 2_765 2_765 ?
I2 Pb1 I1 94.728(19) . 2_765 ?
I3 Pb1 I1 96.769(17) 2_765 2_765 ?
I3 Pb1 I1 83.230(17) . 2_765 ?
I1 Pb1 I1 180.0 . 2_765 ?
I2 Pb2 I2 180.0 . 2_665 ?
I2 Pb2 I3 85.906(17) . 2_765 ?
I2 Pb2 I3 94.095(17) 2_665 2_765 ?
I2 Pb2 I3 94.094(17) . 1_455 ?
I2 Pb2 I3 85.905(17) 2_665 1_455 ?
I3 Pb2 I3 180.0 2_765 1_455 ?
I2 Pb2 I1 85.392(18) . . ?
I2 Pb2 I1 94.608(18) 2_665 . ?
I3 Pb2 I1 83.385(19) 2_765 . ?
I3 Pb2 I1 96.615(19) 1_455 . ?
I2 Pb2 I1 94.608(18) . 2_665 ?
I2 Pb2 I1 85.392(17) 2_665 2_665 ?
I3 Pb2 I1 96.614(19) 2_765 2_665 ?
I3 Pb2 I1 83.386(19) 1_455 2_665 ?
I1 Pb2 I1 180.0 . 2_665 ?
Pb2 I1 Pb1 77.256(15) . . ?
Pb2 I2 Pb1 78.057(15) . . ?
Pb2 I3 Pb1 77.771(14) 1_655 . ?
C1A N1A H1A1 109.5 . . ?
C1A N1A H1A2 109.5 . . ?
H1A1 N1A H1A2 109.5 . . ?
C1A N1A H1A3 109.5 . . ?
H1A1 N1A H1A3 109.5 . . ?
H1A2 N1A H1A3 109.5 . . ?
C2A C1A C6A 121.3(14) . . ?
C2A C1A N1A 120.3(16) . . ?
C6A C1A N1A 118.4(14) . . ?
C3A C2A C1A 119.4(15) . . ?
C3A C2A H2A 120.4 . . ?
C1A C2A H2A 120.2 . . ?
C2A C3A C4A 121.7(16) . . ?
C2A C3A H3A 119.5 . . ?
C4A C3A H3A 118.8 . . ?
C6A C5A C4A 123.5(17) . . ?
C6A C5A H5A 118.6 . . ?
C4A C5A H5A 117.9 . . ?
C5A C6A C1A 117.2(16) . . ?
C5A C6A H6A 121.1 . . ?
C1A C6A H6A 121.6 . . ?
C1B N1B H1B1 109.5 . . ?
C1B N1B H1B2 109.5 . . ?
H1B1 N1B H1B2 109.5 . . ?
C1B N1B H1B3 109.5 . . ?
H1B1 N1B H1B3 109.5 . . ?
H1B2 N1B H1B3 109.5 . . ?
C6B C1B C2B 120.9(14) . . ?
C6B C1B N1B 118.7(14) . . ?
C2B C1B N1B 120.3(16) . . ?
C1B C2B C3B 117.6(15) . . ?
C1B C2B H2B 121.0 . . ?
C3B C2B H2B 121.4 . . ?
C4B C3B C2B 122.0(16) . . ?
C4B C3B H3B 118.6 . . ?
C2B C3B H3B 119.4 . . ?
C4B C5B C6B 120.8(17) . . ?
C4B C5B H5B 119.1 . . ?
C6B C5B H5B 120.1 . . ?
C1B C6B C5B 120.4(17) . . ?
C1B C6B H6B 120.0 . . ?
C5B C6B H6B 119.6 . . ?
C4B C4A C3A 81.0(15) . . ?
C4B C4A C5A 79.4(16) . . ?
C3A C4A C5A 116.8(15) . . ?
C4B C4A C4B 105.2(16) . 2_676 ?
C3A C4A C4B 120.1(15) . 2_676 ?
C5A C4A C4B 122.9(13) . 2_676 ?
C4A C4B C5B 83.0(16) . . ?
C4A C4B C3B 111.1(16) . . ?
C5B C4B C3B 118.3(16) . . ?
C4A C4B C4A 74.8(16) . 2_676 ?
C7 N2 C9 122.5(10) . . ?
C7 N2 C8 121.8(13) . . ?
C9 N2 C8 115.7(12) . . ?
O1 C7 N2 128.5(11) . . ?
O1 C7 H7 115.7 . . ?
N2 C7 H7 115.7 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10A N3A C11A 120.1(18) . . ?
C10A N3A C12A 124.2(17) . . ?
C11A N3A C12A 115.7(19) . . ?
O2A C10A N3A 125.7(18) . . ?
O2A C10A H10A 117.2 . . ?
N3A C10A H10A 117.2 . . ?
N3A C11A H11A 109.5 . . ?
N3A C11A H11B 109.5 . . ?
H11A C11A H11B 109.5 . . ?
N3A C11A H11C 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
N3A C12A H12A 109.5 . . ?
N3A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
N3A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C10B N3B C11B 123(2) . . ?
C10B N3B C12B 124(2) . . ?
C11B N3B C12B 113(2) . . ?
O2B C10B N3B 128(3) . . ?
O2B C10B H10B 116.0 . . ?
N3B C10B H10B 116.0 . . ?
N3B C11B H11D 109.5 . . ?
N3B C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
N3B C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
N3B C12B H12D 109.5 . . ?
N3B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
N3B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?

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
C6A C1A C2A C3A 2(3) . . . . ?
N1A C1A C2A C3A -178.0(18) . . . . ?
C1A C2A C3A C4A 0(3) . . . . ?
C4A C5A C6A C1A 1(3) . . . . ?
C2A C1A C6A C5A -2(3) . . . . ?
N1A C1A C6A C5A 177.5(18) . . . . ?
C6B C1B C2B C3B 0(3) . . . . ?
N1B C1B C2B C3B -174.9(18) . . . . ?
C1B C2B C3B C4B 1(3) . . . . ?
C2B C1B C6B C5B 0(3) . . . . ?
N1B C1B C6B C5B 175.0(19) . . . . ?
C4B C5B C6B C1B -1(3) . . . . ?
C2A C3A C4A C4B -74(2) . . . . ?
C2A C3A C4A C5A -1(3) . . . . ?
C2A C3A C4A C4B -176.8(18) . . . 2_676 ?
C6A C5A C4A C4B 75(2) . . . . ?
C6A C5A C4A C3A 1(3) . . . . ?
C6A C5A C4A C4B 176.1(19) . . . 2_676 ?
C4B C4A C4B C5B -124.4(14) 2_676 . . . ?
C4B C4A C4B C3B 118.0(17) 2_676 . . . ?
C3A C4A C4B C4A -118.9(16) . . . 2_676 ?
C5A C4A C4B C4A 121.5(14) . . . 2_676 ?
C4B C4A C4B C4A 0.000(3) 2_676 . . 2_676 ?
C6B C5B C4B C4A -107(2) . . . . ?
C6B C5B C4B C3B 3(3) . . . . ?
C6B C5B C4B C4A -175.0(19) . . . 2_676 ?
C2B C3B C4B C4A 90(2) . . . . ?
C2B C3B C4B C5B -3(3) . . . . ?
C2B C3B C4B C4A 174.9(18) . . . 2_676 ?
C9 N2 C7 O1 178.7(13) . . . . ?
C8 N2 C7 O1 -2(2) . . . . ?
C11A N3A C10A O2A 177(2) . . . . ?
C12A N3A C10A O2A 0(4) . . . . ?
C11B N3B C10B O2B -175(3) . . . . ?
C12B N3B C10B O2B 0(5) . . . . ?

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
N1A H1A2 O2A 0.91 2.25 3.07(2) 149.4 2_566
N1A H1A3 O1 0.91 1.82 2.50(2) 129.8 1_465
N1B H1B1 O2B 0.91 1.75 2.58(3) 151.0 2_566
N1B H1B2 O1 0.91 2.13 3.01(2) 162.1 1_465
N1B H1B3 I1 0.91 2.59 3.46(2) 160.4 1_455

_refine_diff_density_max         2.484
_refine_diff_density_min         -1.683
_refine_diff_density_rms         0.237


# start Validation Reply Form ================================================80

_vrf_PLAT971_3                   
;
PROBLEM:
Alert level B
PLAT971_ALERT_2_B Check Calcd Resid. Dens.  1.64A   From C11A      2.51 eA-3

RESPONSE: The residual electronic density is close to a carbon atom 
belonging to one of the two parts (57:43) in which a DFM molecule of 
crystallization that had positional disorder was modeled. The analysis 
of these residual densities could indicate the presence of another part 
of the positional disorder with a lower contribution. However, a three-part 
disorder was not stable even with the most severe restrictions 
(DFIX, SADI, SIMU, DELU, ISOR...). It could even be due to a very residual 
contribution of a positional disorder of another solvent other than DMF, 
such as disordered toluene. An attempt at resolution in this way also did 
not lead to satisfactory results.
;

# end Validation Reply Form ==================================================80


###END



