# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_s-2-i
_database_code_depnum_ccdc_archive 'CCDC 2151395'
loop_
_audit_author_name
_audit_author_address
'Xiaodi Jia'
;Nankai University
China
;
_audit_update_record             
;
2022-03-27 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_audit_creation_date             2022-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        S-2-I
_chemical_formula_moiety         'I3 Pb0.5, C5 H14 N2'
_chemical_formula_sum            'C6 H14 I3 N Pb0.50'
_chemical_formula_weight         584.48
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
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'

_cell_length_a                   14.6367(3)
_cell_length_b                   10.2416(3)
_cell_length_c                   8.7513(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1311.85(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9600
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.8740
_cell_measurement_theta_min      3.9530
_shelx_estimated_absorpt_T_max   0.688
_shelx_estimated_absorpt_T_min   0.057
_exptl_absorpt_coefficient_mu    13.489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.959
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11961
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.629
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     12.00  40.00   0.50    0.50    --   -0.30  32.00  43.00   56
  2  ω    -33.00  29.00   0.50    0.50    --   -0.30 -82.00 -90.00  124
  3  ω    -44.00  24.00   0.50    0.50    --   -0.30 -77.00  30.00  136
  4  ω    -31.00  39.00   0.50    0.50    --   -0.30  77.00 120.00  140
  5  ω     48.00  75.00   0.50    0.50    --   -0.30  32.00  43.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0158956000
_diffrn_orient_matrix_UB_12      0.0348109000
_diffrn_orient_matrix_UB_13      -0.0648295000
_diffrn_orient_matrix_UB_21      0.0117265000
_diffrn_orient_matrix_UB_22      0.0597834000
_diffrn_orient_matrix_UB_23      0.0359138000
_diffrn_orient_matrix_UB_31      0.0442478000
_diffrn_orient_matrix_UB_32      -0.0032476000
_diffrn_orient_matrix_UB_33      -0.0328294000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.914
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                2794
_reflns_number_total             2850
_reflns_odcompleteness_completeness 99.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.814
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 
;
 Flack x determined using 1111 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2850
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0183
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0103P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0400
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C4(H4A,H4B), C2(H2C,H2D), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.5000 0.68742(4) 0.01547(7) Uani 1 2 d S T P . .
I2 I 0.55622(3) 0.72368(4) 0.93237(5) 0.01841(9) Uani 1 1 d . . . . .
I1 I 0.55393(2) 0.68641(4) 0.40958(5) 0.01740(9) Uani 1 1 d . . . . .
I3 I 0.71160(3) 0.41458(4) 0.73818(5) 0.01951(9) Uani 1 1 d . . . . .
N1 N 0.7089(3) 0.8476(5) 0.6521(6) 0.0157(10) Uani 1 1 d . . . . .
H1A H 0.6681 0.8154 0.7173 0.019 Uiso 1 1 calc R . . . .
H1B H 0.6896 0.8302 0.5579 0.019 Uiso 1 1 calc R . . . .
C1 C 0.7142(4) 0.9945(6) 0.6728(7) 0.0191(11) Uani 1 1 d . . . . .
H1 H 0.7561 1.0308 0.5965 0.023 Uiso 1 1 calc R . . . .
N2 N 0.8401(4) 0.9546(6) 0.8577(7) 0.0244(12) Uani 1 1 d . . . . .
H2A H 0.8593 0.9711 0.9522 0.029 Uiso 1 1 calc R . . . .
H2B H 0.8814 0.9864 0.7931 0.029 Uiso 1 1 calc R . . . .
C4 C 0.7991(4) 0.7807(6) 0.6776(8) 0.0198(12) Uani 1 1 d . . . . .
H4A H 0.8431 0.8107 0.6026 0.024 Uiso 1 1 calc R . . . .
H4B H 0.7919 0.6871 0.6659 0.024 Uiso 1 1 calc R . . . .
C2 C 0.7520(4) 1.0218(7) 0.8323(8) 0.0234(14) Uani 1 1 d . . . . .
H2C H 0.7604 1.1151 0.8449 0.028 Uiso 1 1 calc R . . . .
H2D H 0.7082 0.9927 0.9082 0.028 Uiso 1 1 calc R . . . .
C3 C 0.8331(4) 0.8113(7) 0.8362(9) 0.0241(14) Uani 1 1 d . . . . .
H3A H 0.7913 0.7752 0.9111 0.029 Uiso 1 1 calc R . . . .
H3B H 0.8925 0.7716 0.8515 0.029 Uiso 1 1 calc R . . . .
C5 C 0.6212(4) 1.0515(7) 0.6491(9) 0.0265(15) Uani 1 1 d . . . . .
H5A H 0.6006 1.0322 0.5474 0.040 Uiso 1 1 calc GR . . . .
H5B H 0.6238 1.1444 0.6630 0.040 Uiso 1 1 calc GR . . . .
H5C H 0.5794 1.0144 0.7218 0.040 Uiso 1 1 calc GR . . . .


_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 3.2435(4) . ?
Pb1 I2 3.2435(4) 2_665 ?
Pb1 I1 3.1906(5) 2_665 ?
Pb1 I1 3.1905(5) . ?
Pb1 I3 3.2489(4) 2_665 ?
Pb1 I3 3.2488(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.517(8) . ?
N1 C4 1.503(7) . ?
C1 H1 0.9800 . ?
C1 C2 1.527(9) . ?
C1 C5 1.496(9) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.478(9) . ?
N2 C3 1.483(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.507(10) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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 97.260(17) . 2_665 ?
I2 Pb1 I3 87.781(11) . 2_665 ?
I2 Pb1 I3 81.835(11) 2_665 2_665 ?
I2 Pb1 I3 87.782(11) 2_665 . ?
I2 Pb1 I3 81.835(11) . . ?
I1 Pb1 I2 91.049(11) 2_665 2_665 ?
I1 Pb1 I2 91.048(11) . . ?
I1 Pb1 I2 171.509(12) 2_665 . ?
I1 Pb1 I2 171.510(12) . 2_665 ?
I1 Pb1 I1 80.705(16) . 2_665 ?
I1 Pb1 I3 91.689(10) . . ?
I1 Pb1 I3 100.307(11) . 2_665 ?
I1 Pb1 I3 100.307(11) 2_665 . ?
I1 Pb1 I3 91.689(11) 2_665 2_665 ?
I3 Pb1 I3 164.282(18) . 2_665 ?
H1A N1 H1B 107.8 . . ?
C1 N1 H1A 109.0 . . ?
C1 N1 H1B 109.0 . . ?
C4 N1 H1A 109.0 . . ?
C4 N1 H1B 109.0 . . ?
C4 N1 C1 112.9(5) . . ?
N1 C1 H1 109.1 . . ?
N1 C1 C2 108.0(5) . . ?
C2 C1 H1 109.1 . . ?
C5 C1 N1 108.9(5) . . ?
C5 C1 H1 109.1 . . ?
C5 C1 C2 112.6(6) . . ?
H2A N2 H2B 107.9 . . ?
C2 N2 H2A 109.1 . . ?
C2 N2 H2B 109.1 . . ?
C2 N2 C3 112.4(5) . . ?
C3 N2 H2A 109.1 . . ?
C3 N2 H2B 109.1 . . ?
N1 C4 H4A 109.8 . . ?
N1 C4 H4B 109.8 . . ?
N1 C4 C3 109.4(5) . . ?
H4A C4 H4B 108.3 . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
C1 C2 H2C 109.3 . . ?
C1 C2 H2D 109.3 . . ?
N2 C2 C1 111.6(5) . . ?
N2 C2 H2C 109.3 . . ?
N2 C2 H2D 109.3 . . ?
H2C C2 H2D 108.0 . . ?
N2 C3 C4 110.2(6) . . ?
N2 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.571
_oxdiff_exptl_absorpt_empirical_full_min 0.714
####################################################################### 
# 
# 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_r-2-i
_database_code_depnum_ccdc_archive 'CCDC 2151396'
loop_
_audit_author_name
_audit_author_address
'Xiaodi Jia'
;Nankai University
China
;
_audit_update_record             
;
2022-03-27 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_audit_creation_date             2022-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        C5H14N2Pb0.5I3
_chemical_formula_moiety         'I6 Pb, 2(C5 H14 N2)'
_chemical_formula_sum            'C10 H28 I6 N4 Pb'
_chemical_formula_weight         1172.95
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
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'

_cell_length_a                   14.6421(5)
_cell_length_b                   10.2354(3)
_cell_length_c                   8.7575(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1312.47(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8993
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      31.2590
_cell_measurement_theta_min      3.9400
_shelx_estimated_absorpt_T_max   0.688
_shelx_estimated_absorpt_T_min   0.057
_exptl_absorpt_coefficient_mu    13.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.968
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13270
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.892
_diffrn_reflns_theta_min         3.982
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      4.00  29.00   0.50    0.63    --   -0.30  16.00-110.00   50
  2  ω    -54.00 -29.00   0.50    0.63    --   -0.30 -16.00  80.00   50
  3  ω    -40.00  33.00   0.50    0.63    --   -0.30 -82.00-120.00  146
  4  ω    -25.00  40.00   0.50    0.63    --   -0.30  77.00  60.00  130
  5  ω    -20.00   5.00   0.50    0.63    --   -0.30 -82.00-150.00   50
  6  ω      3.00  33.00   0.50    0.63    --   -0.30 -82.00 120.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0059628000
_diffrn_orient_matrix_UB_12      -0.0672602000
_diffrn_orient_matrix_UB_13      -0.0165519000
_diffrn_orient_matrix_UB_21      -0.0479297000
_diffrn_orient_matrix_UB_22      -0.0095600000
_diffrn_orient_matrix_UB_23      0.0044822000
_diffrn_orient_matrix_UB_31      -0.0039582000
_diffrn_orient_matrix_UB_32      0.0135338000
_diffrn_orient_matrix_UB_33      -0.0791579000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_reflns_Friedel_coverage         0.699
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                3558
_reflns_number_total             3742
_reflns_odcompleteness_completeness 99.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.118
_refine_diff_density_min         -1.754
_refine_diff_density_rms         0.246
_refine_ls_abs_structure_details 
;
 Flack x determined using 1387 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         3742
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0280
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0231P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0648
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C4(H4A,H4B), N2(H2A,H2B), C2(H2C,H2D), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.5000 0.68746(4) 0.01675(9) Uani 1 2 d S T P . .
I1 I 0.55619(4) 0.27637(5) 0.93236(6) 0.01943(12) Uani 1 1 d . . . . .
I3 I 0.55396(4) 0.31353(5) 0.40954(6) 0.01862(11) Uani 1 1 d . . . . .
I2 I 0.71164(4) 0.58546(5) 0.73823(6) 0.02053(12) Uani 1 1 d . . . . .
N1 N 0.7088(5) 0.1531(6) 0.6526(8) 0.0184(13) Uani 1 1 d . . . . .
H1A H 0.6890 0.1713 0.5589 0.022 Uiso 1 1 calc R . . . .
H1B H 0.6682 0.1847 0.7187 0.022 Uiso 1 1 calc R . . . .
C1 C 0.7146(6) 0.0064(8) 0.6715(9) 0.0206(15) Uani 1 1 d . . . . .
H1 H 0.7564 -0.0298 0.5948 0.025 Uiso 1 1 calc R . . . .
C4 C 0.7984(6) 0.2187(8) 0.6778(10) 0.0215(15) Uani 1 1 d . . . . .
H4A H 0.7914 0.3124 0.6658 0.026 Uiso 1 1 calc R . . . .
H4B H 0.8421 0.1885 0.6024 0.026 Uiso 1 1 calc R . . . .
N2 N 0.8399(6) 0.0457(8) 0.8571(9) 0.0265(16) Uani 1 1 d . . . . .
H2A H 0.8592 0.0287 0.9514 0.032 Uiso 1 1 calc R . . . .
H2B H 0.8812 0.0140 0.7923 0.032 Uiso 1 1 calc R . . . .
C2 C 0.7517(6) -0.0218(9) 0.8316(10) 0.0251(18) Uani 1 1 d . . . . .
H2C H 0.7078 0.0071 0.9073 0.030 Uiso 1 1 calc R . . . .
H2D H 0.7601 -0.1153 0.8439 0.030 Uiso 1 1 calc R . . . .
C3 C 0.8336(6) 0.1888(8) 0.8366(9) 0.0224(16) Uani 1 1 d . . . . .
H3A H 0.8934 0.2280 0.8504 0.027 Uiso 1 1 calc R . . . .
H3B H 0.7926 0.2254 0.9123 0.027 Uiso 1 1 calc R . . . .
C5 C 0.6209(7) -0.0506(10) 0.6496(12) 0.031(2) Uani 1 1 d . . . . .
H5A H 0.5794 -0.0117 0.7212 0.047 Uiso 1 1 calc GR . . . .
H5B H 0.6231 -0.1433 0.6662 0.047 Uiso 1 1 calc GR . . . .
H5C H 0.6004 -0.0334 0.5475 0.047 Uiso 1 1 calc GR . . . .


_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 I1 3.2429(6) . ?
Pb1 I1 3.2429(6) 2_665 ?
Pb1 I3 3.1923(6) . ?
Pb1 I3 3.1923(6) 2_665 ?
Pb1 I2 3.2506(6) . ?
Pb1 I2 3.2505(6) 2_665 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.513(10) . ?
N1 C4 1.491(10) . ?
C1 H1 0.9800 . ?
C1 C2 1.531(11) . ?
C1 C5 1.504(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.514(11) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.482(12) . ?
N2 C3 1.479(11) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
I1 Pb1 I1 97.19(2) . 2_665 ?
I1 Pb1 I2 81.814(14) 2_665 2_665 ?
I1 Pb1 I2 81.814(14) . . ?
I1 Pb1 I2 87.791(15) . 2_665 ?
I1 Pb1 I2 87.791(15) 2_665 . ?
I3 Pb1 I1 91.114(13) . . ?
I3 Pb1 I1 91.114(13) 2_665 2_665 ?
I3 Pb1 I1 171.512(15) 2_665 . ?
I3 Pb1 I1 171.512(15) . 2_665 ?
I3 Pb1 I3 80.64(2) . 2_665 ?
I3 Pb1 I2 100.332(14) 2_665 . ?
I3 Pb1 I2 100.331(14) . 2_665 ?
I3 Pb1 I2 91.676(14) . . ?
I3 Pb1 I2 91.675(14) 2_665 2_665 ?
I2 Pb1 I2 164.28(2) 2_665 . ?
H1A N1 H1B 107.9 . . ?
C1 N1 H1A 109.1 . . ?
C1 N1 H1B 109.1 . . ?
C4 N1 H1A 109.1 . . ?
C4 N1 H1B 109.1 . . ?
C4 N1 C1 112.4(7) . . ?
N1 C1 H1 109.6 . . ?
N1 C1 C2 107.9(7) . . ?
C2 C1 H1 109.6 . . ?
C5 C1 N1 108.6(7) . . ?
C5 C1 H1 109.6 . . ?
C5 C1 C2 111.5(8) . . ?
N1 C4 H4A 109.6 . . ?
N1 C4 H4B 109.6 . . ?
N1 C4 C3 110.1(7) . . ?
H4A C4 H4B 108.1 . . ?
C3 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H2A N2 H2B 107.8 . . ?
C2 N2 H2A 109.0 . . ?
C2 N2 H2B 109.0 . . ?
C3 N2 H2A 109.0 . . ?
C3 N2 H2B 109.0 . . ?
C3 N2 C2 112.9(7) . . ?
C1 C2 H2C 109.4 . . ?
C1 C2 H2D 109.4 . . ?
N2 C2 C1 111.0(7) . . ?
N2 C2 H2C 109.4 . . ?
N2 C2 H2D 109.4 . . ?
H2C C2 H2D 108.0 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
N2 C3 C4 109.5(7) . . ?
N2 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.100
_oxdiff_exptl_absorpt_empirical_full_min 0.360
####################################################################### 
# 
# 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_rac-2-i
_database_code_depnum_ccdc_archive 'CCDC 2151397'
loop_
_audit_author_name
_audit_author_address
'Xiaodi Jia'
;Nankai University
China
;
_audit_update_record             
;
2022-03-27 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_audit_creation_date             2022-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        rac-2-I
_chemical_formula_moiety         'I3 Pb0.5, C5 H14 N2, 1.5(H2 O)'
_chemical_formula_sum            'C5 H14 I3 N3.50 O0.25 Pb0.50'
_chemical_formula_weight         611.49
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   9.5613(2)
_cell_length_b                   10.0810(2)
_cell_length_c                   15.1805(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.420(2)
_cell_angle_gamma                90
_cell_volume                     1403.53(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19520
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      31.1920
_cell_measurement_theta_min      4.2530
_shelx_estimated_absorpt_T_max   0.703
_shelx_estimated_absorpt_T_min   0.187
_exptl_absorpt_coefficient_mu    12.620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.894
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23779
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         3.569
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  32.00   0.50    0.50    --   -0.30  58.00 -30.00   50
  2  ω    -59.00 -32.00   0.50    0.50    --   -0.30 -58.00-171.00   54
  3  ω    -32.00  47.00   0.50    0.50    --   -0.30  77.00-180.00  158
  4  ω    -32.00  48.00   0.50    0.50    --   -0.30  77.00  60.00  160
  5  ω    -49.00  31.00   0.50    0.50    --   -0.30 -77.00 -90.00  160
  6  ω     -2.00  32.00   0.50    0.50    --   -0.30  38.00  90.00   68
  7  ω     39.00  65.00   0.50    0.50    --   -0.30  38.00  90.00   52
  8  ω    -86.00  18.00   0.50    0.50    --   -0.30 -38.00-150.00  208
  9  ω    -24.00  44.00   0.50    0.50    --   -0.30  77.00  30.00  136
 10  ω      5.00  30.00   0.50    0.50    --   -0.30  38.00-180.00   50
 11  ω    -11.00  32.00   0.50    0.50    --   -0.30  77.00-120.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0464195000
_diffrn_orient_matrix_UB_12      0.0092268000
_diffrn_orient_matrix_UB_13      -0.0451329000
_diffrn_orient_matrix_UB_21      -0.0408033000
_diffrn_orient_matrix_UB_22      0.0476738000
_diffrn_orient_matrix_UB_23      0.0167000000
_diffrn_orient_matrix_UB_31      0.0465050000
_diffrn_orient_matrix_UB_32      0.0509135000
_diffrn_orient_matrix_UB_33      -0.0075106000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2403
_reflns_number_total             2467
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.532
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2467
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0170
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+2.3039P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0397
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H3D-H1B
 2.1 with sigma of 0.02
 H3D-H4D
 2.1 with sigma of 0.02
 H1B-H3C
 2.1 with sigma of 0.02
 H1B-H3D
 2.1 with sigma of 0.02
3. Others
 Fixed Sof: H4C(0.5) H4D(0.5)
4.a Free rotating group:
 O4(H4C,H4D), O3(H3C,H3D)
4.b Ternary CH refined with riding coordinates:
 C1(H1)
4.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C2(H2C,H2D)
4.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.25573(2) 0.2500 0.01627(6) Uani 1 2 d S T P . .
I1 I 0.70672(2) 0.50698(2) 0.22300(2) 0.01692(7) Uani 1 1 d . . . . .
I2 I 0.64477(2) 0.27957(2) 0.46782(2) 0.01734(7) Uani 1 1 d . . . . .
I3 I 0.28996(2) 0.03080(2) 0.28469(2) 0.01786(7) Uani 1 1 d . . . . .
N2 N 0.6367(3) 0.6464(3) 0.4259(2) 0.0160(6) Uani 1 1 d . . . . .
H2A H 0.5748 0.6392 0.4598 0.019 Uiso 1 1 calc R . . . .
H2B H 0.6159 0.5825 0.3837 0.019 Uiso 1 1 calc R . . . .
N1 N 0.8123(3) 0.8695(3) 0.5088(2) 0.0167(6) Uani 1 1 d . . . . .
H1A H 0.8346 0.9341 0.5503 0.020 Uiso 1 1 calc R . . . .
H1B H 0.8742 0.8739 0.4747 0.020 Uiso 1 1 calc DR . . . .
O4 O 1.0000 0.7387(5) 0.2500 0.0552(17) Uani 1 2 d S T P . .
H4C H 0.9378 0.6762 0.2381 0.083 Uiso 0.5 1 d G . . . .
H4D H 0.9491 0.8091 0.2392 0.083 Uiso 0.5 1 d DG . . . .
C3 C 0.6164(4) 0.7783(3) 0.3791(3) 0.0171(7) Uani 1 1 d . . . . .
H3A H 0.5150 0.7892 0.3443 0.021 Uiso 1 1 calc R . . . .
H3B H 0.6752 0.7826 0.3365 0.021 Uiso 1 1 calc R . . . .
C1 C 0.8287(4) 0.7374(3) 0.5570(3) 0.0150(7) Uani 1 1 d . . . . .
H1 H 0.7616 0.7340 0.5952 0.018 Uiso 1 1 calc R . . . .
C4 C 0.6604(4) 0.8891(3) 0.4489(2) 0.0180(7) Uani 1 1 d . . . . .
H4A H 0.6539 0.9734 0.4173 0.022 Uiso 1 1 calc R . . . .
H4B H 0.5938 0.8915 0.4866 0.022 Uiso 1 1 calc R . . . .
C2 C 0.7890(4) 0.6280(3) 0.4859(2) 0.0155(7) Uani 1 1 d . . . . .
H2C H 0.8562 0.6290 0.4486 0.019 Uiso 1 1 calc R . . . .
H2D H 0.7972 0.5426 0.5165 0.019 Uiso 1 1 calc R . . . .
C5 C 0.9836(4) 0.7223(4) 0.6184(3) 0.0256(9) Uani 1 1 d . . . . .
H5A H 1.0498 0.7191 0.5812 0.038 Uiso 1 1 calc GR . . . .
H5B H 0.9914 0.6418 0.6532 0.038 Uiso 1 1 calc GR . . . .
H5C H 1.0076 0.7965 0.6596 0.038 Uiso 1 1 calc GR . . . .
O3 O 1.0185(4) 0.8926(4) 0.4088(2) 0.0600(11) Uani 1 1 d . . . . .
H3C H 0.9646 0.9501 0.3744 0.090 Uiso 1 1 d DG . . . .
H3D H 0.9907 0.8190 0.3824 0.090 Uiso 1 1 d DG . . . .


_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 I1 3.3087(3) 2_655 ?
Pb1 I1 3.3087(3) . ?
Pb1 I2 3.2124(2) 2_655 ?
Pb1 I2 3.2124(2) . ?
Pb1 I3 3.1702(3) . ?
Pb1 I3 3.1701(3) 2_655 ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C3 1.495(4) . ?
N2 C2 1.495(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.507(4) . ?
N1 C4 1.492(4) . ?
O4 H4C 0.8502 . ?
O4 H4D 0.8498 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.515(5) . ?
C1 H1 0.9800 . ?
C1 C2 1.514(5) . ?
C1 C5 1.518(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
O3 H3C 0.8497 . ?
O3 H3D 0.8497 . ?

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
I1 Pb1 I1 80.098(8) . 2_655 ?
I2 Pb1 I1 85.061(6) 2_655 . ?
I2 Pb1 I1 88.371(6) . . ?
I2 Pb1 I1 88.371(6) 2_655 2_655 ?
I2 Pb1 I1 85.061(6) . 2_655 ?
I2 Pb1 I2 171.419(10) 2_655 . ?
I3 Pb1 I1 95.642(6) 2_655 . ?
I3 Pb1 I1 95.643(6) . 2_655 ?
I3 Pb1 I1 175.389(7) 2_655 2_655 ?
I3 Pb1 I1 175.390(7) . . ?
I3 Pb1 I2 96.640(6) . 2_655 ?
I3 Pb1 I2 89.507(6) 2_655 2_655 ?
I3 Pb1 I2 96.640(6) 2_655 . ?
I3 Pb1 I2 89.507(6) . . ?
I3 Pb1 I3 88.667(9) 2_655 . ?
H2A N2 H2B 107.9 . . ?
C3 N2 H2A 109.2 . . ?
C3 N2 H2B 109.2 . . ?
C2 N2 H2A 109.2 . . ?
C2 N2 H2B 109.2 . . ?
C2 N2 C3 111.9(3) . . ?
H1A N1 H1B 108.0 . . ?
C1 N1 H1A 109.4 . . ?
C1 N1 H1B 109.4 . . ?
C4 N1 H1A 109.4 . . ?
C4 N1 H1B 109.4 . . ?
C4 N1 C1 111.3(3) . . ?
H4C O4 H4D 104.5 . . ?
N2 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
N2 C3 C4 110.5(3) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
N1 C1 H1 108.8 . . ?
N1 C1 C2 109.1(3) . . ?
N1 C1 C5 109.7(3) . . ?
C2 C1 H1 108.8 . . ?
C2 C1 C5 111.7(3) . . ?
C5 C1 H1 108.8 . . ?
N1 C4 C3 111.0(3) . . ?
N1 C4 H4A 109.4 . . ?
N1 C4 H4B 109.4 . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C2 C1 110.4(3) . . ?
N2 C2 H2C 109.6 . . ?
N2 C2 H2D 109.6 . . ?
C1 C2 H2C 109.6 . . ?
C1 C2 H2D 109.6 . . ?
H2C C2 H2D 108.1 . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
H3C O3 H3D 104.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.640
_oxdiff_exptl_absorpt_empirical_full_min 0.760
