# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_Mhy2PbI4_temp_300
_database_code_depnum_ccdc_archive 'CCDC 2298904'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2022-10-17
# start Validation Reply Form
_vrf_PLAT196_Mhy2PbI4_temp_300   
;
PROBLEM: No TEMP record and _measurement_temperature .NE.        293 Degree
RESPONSE: The data was collected at 300 K.
The measurement was done at 300 K.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_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           62
_space_group_name_H-M_alt        'P m c n'
_space_group_name_Hall           '-P 2n 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.684(4)
_cell_length_b                   6.3720(13)
_cell_length_c                   12.769(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1520.2(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3382
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      28.5650
_cell_measurement_theta_min      3.1870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13638
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.084
_diffrn_reflns_theta_min         3.191
_diffrn_ambient_temperature      300(2)
_diffrn_ambient_environment      air
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.924
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0219960000
_diffrn_orient_matrix_UB_12      0.0155943000
_diffrn_orient_matrix_UB_13      -0.0368316000
_diffrn_orient_matrix_UB_21      -0.1078806000
_diffrn_orient_matrix_UB_22      0.0196091000
_diffrn_orient_matrix_UB_23      -0.0065436000
_diffrn_orient_matrix_UB_31      0.0164005000
_diffrn_orient_matrix_UB_32      0.1082181000
_diffrn_orient_matrix_UB_33      0.0064908000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  92.50   0.90   11.50    --   17.79-161.00 -93.00   75
  2  ω     31.00  94.00   0.90   11.50    --   17.79-171.00-176.00   70
  3  ω     -4.00  86.00   0.90   11.50    --   17.79  57.00 -60.00  100
  4  ω    -49.00  38.30   0.90   11.50    --  -18.65  77.00-150.00   97
  5  ω    -39.00  10.50   0.90   11.50    --  -18.65 -77.00  60.00   55
  6  ω    -51.00  39.00   0.90   11.50    --   17.79 -57.00 -30.00  100
  7  ω    -39.00 -12.00   0.90   11.50    --  -18.65 -77.00   0.00   30
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1042
_reflns_number_total             1943
_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 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.933
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1943
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0356P)²+0.7909P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0976
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C1, N3, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim N3 \\sim N2: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
4. Rigid body (RIGU) restrains
 N2, N3, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Rotating group:
 N2(H2A,H2B)
5.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.750000 1.25280(7) 0.04320(3) 0.03037(15) Uani 1 2 d S T P . .
I2 I 0.92014(4) 1.25956(10) 0.04612(6) 0.0640(3) Uani 1 1 d . . . . .
I1 I 0.750000 0.74979(12) 0.06437(7) 0.0532(3) Uani 1 2 d S T P . .
I3 I 0.750000 1.25013(17) 0.29418(7) 0.0793(4) Uani 1 2 d S T P . .
C1 C 0.8837(8) 0.7357(18) 0.3271(10) 0.083(4) Uani 1 1 d . U . . .
H1A H 0.848001 0.829845 0.300260 0.124 Uiso 1 1 calc R U . . .
H1B H 0.915617 0.811103 0.372352 0.124 Uiso 1 1 calc R U . . .
H1C H 0.860852 0.625180 0.365746 0.124 Uiso 1 1 calc R U . . .
N2 N 0.9604(9) 0.7841(17) 0.1900(8) 0.111(5) Uani 1 1 d . U . . .
H2A H 0.990946 0.717312 0.152015 0.134 Uiso 1 1 d R U . . .
H2B H 0.932426 0.856109 0.149993 0.134 Uiso 1 1 d R U . . .
N3 N 0.9218(9) 0.651(2) 0.2451(12) 0.141(6) Uani 1 1 d . U . . .
H3A H 0.950824 0.552629 0.270495 0.169 Uiso 1 1 calc R U . . .
H3B H 0.891111 0.587705 0.202058 0.169 Uiso 1 1 calc R U . . .


_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 3.1793(10) . ?
Pb1 I2 3.1794(10) 7_755 ?
Pb1 I1 3.2166(12) . ?
Pb1 I1 3.1783(12) 1_565 ?
Pb1 I3 3.2048(11) . ?
Pb1 I3 3.1797(11) 2_674 ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 N3 1.376(16) . ?
N2 H2A 0.8621 . ?
N2 H2B 0.8624 . ?
N2 N3 1.317(16) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?

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 177.95(3) . 7_755 ?
I2 Pb1 I1 90.716(17) 7_755 . ?
I2 Pb1 I1 90.716(17) . . ?
I2 Pb1 I3 89.333(16) 7_755 . ?
I2 Pb1 I3 90.676(16) . 2_674 ?
I2 Pb1 I3 90.676(16) 7_755 2_674 ?
I2 Pb1 I3 89.332(16) . . ?
I1 Pb1 I2 89.170(17) 1_565 7_755 ?
I1 Pb1 I2 89.170(17) 1_565 . ?
I1 Pb1 I1 170.30(4) 1_565 . ?
I1 Pb1 I3 85.43(3) 1_565 . ?
I1 Pb1 I3 95.21(3) 1_565 2_674 ?
I3 Pb1 I1 84.88(3) . . ?
I3 Pb1 I1 94.48(3) 2_674 . ?
I3 Pb1 I3 179.359(16) 2_674 . ?
Pb1 I1 Pb1 170.30(4) 1_545 . ?
Pb1 I3 Pb1 179.97(4) 2_675 . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N3 C1 H1A 109.5 . . ?
N3 C1 H1B 109.5 . . ?
N3 C1 H1C 109.5 . . ?
H2A N2 H2B 109.3 . . ?
N3 N2 H2A 110.2 . . ?
N3 N2 H2B 109.1 . . ?
C1 N3 H3A 108.3 . . ?
C1 N3 H3B 108.3 . . ?
N2 N3 C1 115.9(13) . . ?
N2 N3 H3A 108.3 . . ?
N2 N3 H3B 108.3 . . ?
H3A N3 H3B 107.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mhy2pbi4_temp_310
_database_code_depnum_ccdc_archive 'CCDC 2298905'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-11 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_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           62
_space_group_name_H-M_alt        'P m c n'
_space_group_name_Hall           '-P 2n 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.7116(5)
_cell_length_b                   6.3719(2)
_cell_length_c                   12.7687(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1522.39(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3333
_cell_measurement_temperature    310(2)
_cell_measurement_theta_max      28.2280
_cell_measurement_theta_min      3.1840
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.530
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13671
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.084
_diffrn_reflns_theta_min         3.191
_diffrn_ambient_temperature      310(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  92.50   0.90   11.50    --   17.79-161.00 -93.00   75
  2  ω     31.00  94.00   0.90   11.50    --   17.79-171.00-176.00   70
  3  ω     -4.00  86.00   0.90   11.50    --   17.79  57.00 -60.00  100
  4  ω    -49.00  38.30   0.90   11.50    --  -18.65  77.00-150.00   97
  5  ω    -39.00  10.50   0.90   11.50    --  -18.65 -77.00  60.00   55
  6  ω    -51.00  39.00   0.90   11.50    --   17.79 -57.00 -30.00  100
  7  ω    -39.00 -12.00   0.90   11.50    --  -18.65 -77.00   0.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1030
_reflns_number_total             1945
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.872
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1945
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      0.998
_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)+(0.0379P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.1005
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C1, N2, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1, N2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Rotating group:
 N1(H1D,H1E)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.750000 1.25256(7) 0.04308(3) 0.03159(16) Uani 1 2 d S T P . .
I2 I 0.91995(4) 1.25806(11) 0.04594(6) 0.0662(3) Uani 1 1 d . . . . .
I1 I 0.750000 0.74966(13) 0.06388(7) 0.0556(3) Uani 1 2 d S T P . .
I3 I 0.750000 1.25008(17) 0.29400(7) 0.0811(5) Uani 1 2 d S T P . .
C1 C 0.8828(7) 0.7436(17) 0.3260(11) 0.083(4) Uani 1 1 d . U . . .
H1A H 0.863530 0.877721 0.306585 0.125 Uiso 1 1 calc R U . . .
H1B H 0.913238 0.759706 0.385952 0.125 Uiso 1 1 calc R U . . .
H1C H 0.844366 0.649479 0.342807 0.125 Uiso 1 1 calc R U . . .
N1 N 0.9611(9) 0.7857(17) 0.1900(8) 0.115(5) Uani 1 1 d . U . . .
H1D H 0.989760 0.719564 0.147680 0.137 Uiso 1 1 d R U . . .
H1E H 0.933249 0.865989 0.153042 0.137 Uiso 1 1 d R U . . .
N2 N 0.9220(9) 0.662(2) 0.2431(12) 0.136(5) Uani 1 1 d . U . . .
H2A H 0.950027 0.561452 0.268461 0.163 Uiso 1 1 calc R U . . .
H2B H 0.891473 0.601451 0.199141 0.163 Uiso 1 1 calc R U . . .


_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 3.1805(8) . ?
Pb1 I2 3.1806(8) 7_755 ?
Pb1 I1 3.2154(10) . ?
Pb1 I1 3.1786(10) 1_565 ?
Pb1 I3 3.2040(8) . ?
Pb1 I3 3.1805(8) 2_674 ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 N2 1.389(17) . ?
N1 H1D 0.8700 . ?
N1 H1E 0.8693 . ?
N1 N2 1.269(17) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?

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 178.18(3) . 7_755 ?
I2 Pb1 I1 90.575(17) 7_755 . ?
I2 Pb1 I1 90.575(17) . . ?
I2 Pb1 I3 89.345(16) 7_755 . ?
I2 Pb1 I3 90.662(16) . 2_674 ?
I2 Pb1 I3 90.661(16) 7_755 2_674 ?
I2 Pb1 I3 89.345(16) . . ?
I1 Pb1 I2 89.316(17) 1_565 7_755 ?
I1 Pb1 I2 89.315(17) 1_565 . ?
I1 Pb1 I1 170.47(4) 1_565 . ?
I1 Pb1 I3 85.49(3) 1_565 . ?
I1 Pb1 I3 95.10(3) 1_565 2_674 ?
I3 Pb1 I1 84.98(3) . . ?
I3 Pb1 I1 94.44(3) 2_674 . ?
I3 Pb1 I3 179.415(16) 2_674 . ?
Pb1 I1 Pb1 170.47(4) 1_545 . ?
Pb1 I3 Pb1 179.98(4) 2_675 . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1D N1 H1E 108.5 . . ?
N2 N1 H1D 112.8 . . ?
N2 N1 H1E 108.0 . . ?
C1 N2 H2A 107.6 . . ?
C1 N2 H2B 107.6 . . ?
N1 N2 C1 118.7(15) . . ?
N1 N2 H2A 107.6 . . ?
N1 N2 H2B 107.6 . . ?
H2A N2 H2B 107.1 . . ?


_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
;
####################################################################### 
# 
# 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_mhy2pbi4_temp_340
_database_code_depnum_ccdc_archive 'CCDC 2298908'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C N2)'
_chemical_formula_sum            'C2 I4 N4 Pb'
_chemical_formula_weight         794.85
_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'
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           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'

_cell_length_a                   18.8229(6)
_cell_length_b                   6.3753(2)
_cell_length_c                   6.3839(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     766.08(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3034
_cell_measurement_temperature    340(2)
_cell_measurement_theta_max      28.0010
_cell_measurement_theta_min      3.1860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.446
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7032
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.937
_diffrn_reflns_theta_min         3.191
_diffrn_ambient_temperature      340(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  92.50   0.90   11.50    --   17.79-161.00 -93.00   75
  2  ω     31.00  94.00   0.90   11.50    --   17.79-171.00-176.00   70
  3  ω     -4.00  86.00   0.90   11.50    --   17.79  57.00 -60.00  100
  4  ω    -49.00  38.30   0.90   11.50    --  -18.65  77.00-150.00   97
  5  ω    -39.00  10.50   0.90   11.50    --  -18.65 -77.00  60.00   55
  6  ω    -51.00  39.00   0.90   11.50    --   17.79 -57.00 -30.00  100
  7  ω    -39.00 -12.00   0.90   11.50    --  -18.65 -77.00   0.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                890
_reflns_number_total             1057
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.747
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1057
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0458
_refine_ls_restrained_S_all      1.188
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0431P)²+3.5203P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1106
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N1-C1
 1.4 with sigma of 0.1
 N2A-C1 \\sim N1-C1
 with sigma of 0.02
 N2B-N1 \\sim N2B-N2A
 with sigma of 0.02
2. Others
 Fixed Sof: N2A(0.16665) N2B(0.3333) N1(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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
Pb Pb 0.250000 0.750000 0.41574(10) 0.0368(2) Uani 1 4 d S T P . .
I1 I 0.250000 0.250000 0.3765(2) 0.0639(5) Uani 1 4 d S T P . .
I2 I 0.41906(6) 0.750000 0.4091(2) 0.0776(4) Uani 1 2 d S T P . .
I3 I 0.250000 0.750000 0.9148(2) 0.0917(8) Uani 1 4 d S T P . .
C1 C 0.3817(12) 0.250000 -0.150(4) 0.096(7) Uani 1 2 d DS T P . .
N2A N 0.415(3) 0.250000 0.076(5) 0.11(4) Uani 0.3333 2 d DS T P . .
N2B N 0.474(2) 0.220(15) 0.119(5) 0.10(3) Uani 0.3333 1 d D . P . .
N1 N 0.426(2) 0.146(6) 0.030(7) 0.143(15) Uani 0.5 1 d D . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb I1 3.19750(16) 1_565 ?
Pb I1 3.19749(17) . ?
Pb I2 3.1825(12) 2_565 ?
Pb I2 3.1825(12) . ?
Pb I3 3.1981(14) 1_554 ?
Pb I3 3.1858(14) . ?
C1 N2A 1.57(4) . ?
C1 N1 1.56(3) 7_565 ?
C1 N1 1.56(3) . ?
N2A N2B 1.16(5) . ?
N2A N2B 1.16(5) 7_565 ?
N2A N1 0.76(5) 7_565 ?
N2A N1 0.76(5) . ?
N2B N2B 0.4(2) 7_565 ?
N2B N1 1.17(5) . ?
N2B N1 1.37(8) 7_565 ?
N1 N1 1.33(8) 7_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
I1 Pb I1 171.01(6) . 1_565 ?
I1 Pb I3 85.50(3) 1_565 1_554 ?
I1 Pb I3 85.50(3) . 1_554 ?
I2 Pb I1 89.940(2) . . ?
I2 Pb I1 89.940(2) . 1_565 ?
I2 Pb I1 89.940(2) 2_565 . ?
I2 Pb I1 89.940(2) 2_565 1_565 ?
I2 Pb I2 178.47(6) . 2_565 ?
I2 Pb I3 90.76(3) 2_565 . ?
I2 Pb I3 89.24(3) 2_565 1_554 ?
I2 Pb I3 90.76(3) . . ?
I2 Pb I3 89.24(3) . 1_554 ?
I3 Pb I1 94.50(3) . . ?
I3 Pb I1 94.50(3) . 1_565 ?
I3 Pb I3 180.0 . 1_554 ?
Pb I1 Pb 171.01(6) . 1_545 ?
Pb I3 Pb 180.0 . 1_556 ?
N1 C1 N2A 28(2) 7_565 . ?
N1 C1 N2A 28(2) . . ?
N1 C1 N1 50(3) . 7_565 ?
N2B N2A C1 127(3) 7_565 . ?
N2B N2A C1 127(3) . . ?
N2B N2A N2B 19(10) 7_565 . ?
N1 N2A C1 75.8(17) . . ?
N1 N2A C1 75.9(17) 7_565 . ?
N1 N2A N2B 71(2) . . ?
N1 N2A N2B 71(2) 7_565 7_565 ?
N1 N2A N2B 88(9) 7_565 . ?
N1 N2A N2B 88(9) . 7_565 ?
N1 N2A N1 123(9) 7_565 . ?
N2A N2B N1 34(3) . 7_565 ?
N2A N2B N1 38(3) . . ?
N2B N2B N2A 80(5) 7_565 . ?
N2B N2B N1 114(4) 7_565 . ?
N2B N2B N1 51(4) 7_565 7_565 ?
N1 N2B N1 63(3) . 7_565 ?
N2A N1 C1 76.2(18) . . ?
N2A N1 N2B 58(7) . 7_565 ?
N2A N1 N2B 70.9(19) . . ?
N2A N1 N1 29(5) . 7_565 ?
N2B N1 C1 127(4) . . ?
N2B N1 C1 113(5) 7_565 . ?
N2B N1 N2B 15(7) . 7_565 ?
N2B N1 N1 66(4) . 7_565 ?
N1 N1 C1 64.9(16) 7_565 . ?
N1 N1 N2B 51(4) 7_565 7_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
C1 N2A N2B N2B 97(5) . . . 7_565 ?
C1 N2A N2B N1 -55(4) . . . . ?
C1 N2A N2B N1 71(7) . . . 7_565 ?
C1 N2A N1 N2B 137(4) . . . . ?
C1 N2A N1 N2B 129(3) . . . 7_565 ?
C1 N2A N1 N1 62(5) . . . 7_565 ?
N2A C1 N1 N2B -53(4) . . . . ?
N2A C1 N1 N2B -46(6) . . . 7_565 ?
N2A C1 N1 N1 -28(6) . . . 7_565 ?
N2A N2B N1 C1 55(4) . . . . ?
N2A N2B N1 N2B 30(5) . . . 7_565 ?
N2A N2B N1 N1 30(5) . . . 7_565 ?
N2B N2A N2B N1 -26(3) 7_565 . . 7_565 ?
N2B N2A N2B N1 -152(4) 7_565 . . . ?
N2B N2A N1 C1 -137(4) . . . . ?
N2B N2A N1 C1 -129(3) 7_565 . . . ?
N2B N2A N1 N2B 9(4) 7_565 . . . ?
N2B N2A N1 N2B -9(4) . . . 7_565 ?
N2B N2A N1 N1 -66(4) 7_565 . . 7_565 ?
N2B N2A N1 N1 -75(8) . . . 7_565 ?
N2B N2B N1 C1 25(6) 7_565 . . . ?
N2B N2B N1 N2A -30(5) 7_565 . . . ?
N2B N2B N1 N1 0.00(3) 7_565 . . 7_565 ?
N1 C1 N2A N2B -77(11) 7_565 . . . ?
N1 C1 N2A N2B 77(11) . . . 7_565 ?
N1 C1 N2A N2B 53(4) . . . . ?
N1 C1 N2A N2B -53(4) 7_565 . . 7_565 ?
N1 C1 N2A N1 -130(10) 7_565 . . . ?
N1 C1 N2A N1 130(10) . . . 7_565 ?
N1 C1 N1 N2A 28(6) 7_565 . . . ?
N1 C1 N1 N2B -18(5) 7_565 . . 7_565 ?
N1 C1 N1 N2B -25(7) 7_565 . . . ?
N1 N2A N2B N2B 152(4) . . . 7_565 ?
N1 N2A N2B N2B 26(3) 7_565 . . 7_565 ?
N1 N2A N2B N1 126(7) . . . 7_565 ?
N1 N2A N2B N1 -126(7) 7_565 . . . ?
N1 N2A N1 C1 -62(5) 7_565 . . . ?
N1 N2A N1 N2B 75(8) 7_565 . . . ?
N1 N2A N1 N2B 66(4) 7_565 . . 7_565 ?
N1 N2B N1 C1 25(6) 7_565 . . . ?
N1 N2B N1 N2A -30(5) 7_565 . . . ?
N1 N2B N1 N2B 0.00(2) 7_565 . . 7_565 ?

_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
;
####################################################################### 
# 
# 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_mhy2pbi4_temp_320
_database_code_depnum_ccdc_archive 'CCDC 2298906'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-28
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_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           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'

_cell_length_a                   18.7487(6)
_cell_length_b                   6.3729(2)
_cell_length_c                   6.3843(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     762.82(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3231
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      28.0600
_cell_measurement_theta_min      3.1860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.522
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7002
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.847
_diffrn_reflns_theta_min         3.191
_diffrn_ambient_temperature      320(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  92.50   0.90   11.50    --   17.79-161.00 -93.00   75
  2  ω     31.00  94.00   0.90   11.50    --   17.79-171.00-176.00   70
  3  ω     -4.00  86.00   0.90   11.50    --   17.79  57.00 -60.00  100
  4  ω    -49.00  38.30   0.90   11.50    --  -18.65  77.00-150.00   97
  5  ω    -39.00  10.50   0.90   11.50    --  -18.65 -77.00  60.00   55
  6  ω    -51.00  39.00   0.90   11.50    --   17.79 -57.00 -30.00  100
  7  ω    -39.00 -12.00   0.90   11.50    --  -18.65 -77.00   0.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                895
_reflns_number_total             1058
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.074
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1058
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0384
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²+2.2177P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0883
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C1 \\sim N2-C1
 with sigma of 0.02
 N3-N1 \\sim N2-N1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N1) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 N2, N1, C1, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H1BC(0.25) H1BD(0.25) H1BE(0.5) H1A(0.25) H1B(0.25) N2(0.25)
 H2A(0.25) H2B(0.25) N3(0.25) H3A(0.25) H3B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), N2(H2A,H2B), N3(H3A,H3B)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.c Idealised Me refined as rotating group:
 C1(H1BC,H1BD,H1BE)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Pb Pb 0.250000 0.750000 0.41402(8) 0.03318(19) Uani 1 4 d S T P . .
I1 I 0.250000 0.250000 0.37300(19) 0.0583(4) Uani 1 4 d S T P . .
I2 I 0.41963(5) 0.750000 0.40835(17) 0.0705(3) Uani 1 2 d S T P . .
I3 I 0.250000 0.750000 0.91245(17) 0.0838(6) Uani 1 4 d S T P . .
C1 C 0.3847(9) 0.250000 -0.148(3) 0.080(5) Uani 1 2 d DS TU P . .
H1AA H 0.397829 0.250000 -0.294771 0.097 Uiso 1 2 calc R U P A 1
H1AB H 0.333891 0.250000 -0.119340 0.097 Uiso 1 2 calc R U P A 1
H1BC H 0.424499 0.293875 -0.231706 0.121 Uiso 0.25 1 calc R U P B 2
H1BD H 0.345608 0.345041 -0.168369 0.121 Uiso 0.25 1 calc R U P B 2
H1BE H 0.370525 0.111083 -0.188373 0.121 Uiso 0.5 1 calc R U P B 2
N1 N 0.4655(12) 0.250000 0.123(2) 0.120(7) Uani 1 2 d DS TU P . .
H1A H 0.498989 0.250000 0.030869 0.144 Uiso 0.5 2 calc R U P C 2
H1B H 0.475794 0.250000 0.254022 0.144 Uiso 0.5 2 calc R U P C 2
N2 N 0.4312(18) 0.146(5) -0.002(5) 0.083(9) Uani 0.25 1 d D U P D 1
H2A H 0.404774 0.055884 0.071800 0.100 Uiso 0.25 1 calc R U P D 1
H2B H 0.462062 0.069582 -0.075631 0.100 Uiso 0.25 1 calc R U P D 1
N3 N 0.4048(16) 0.250000 0.068(4) 0.147(18) Uani 0.5 2 d DS TU P D 2
H3A H 0.384498 0.361994 0.126465 0.176 Uiso 0.25 1 calc R U P D 2
H3B H 0.384498 0.138006 0.126465 0.176 Uiso 0.25 1 calc R U P D 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
Pb I1 3.19719(14) . ?
Pb I1 3.19719(15) 1_565 ?
Pb I2 3.1805(9) 2_565 ?
Pb I2 3.1805(9) . ?
Pb I3 3.2021(11) 1_554 ?
Pb I3 3.1821(11) . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 H1BC 0.96(12) 8_565 ?
C1 H1BC 0.9600 . ?
C1 H1BD 0.9600 . ?
C1 H1BD 0.9600 . ?
C1 H1BE 0.96(8) 8_565 ?
C1 H1BE 0.9600 . ?
C1 N2 1.44(3) 8_565 ?
C1 N2 1.44(3) . ?
C1 N3 1.43(3) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 N2 1.22(3) . ?
N1 N2 1.22(3) 8_565 ?
N1 N3 1.19(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H3A 1.20(5) 8_565 ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?

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 Pb I1 170.60(5) 1_565 . ?
I1 Pb I3 85.30(2) . 1_554 ?
I1 Pb I3 85.30(2) 1_565 1_554 ?
I2 Pb I1 89.947(2) 2_565 1_565 ?
I2 Pb I1 89.947(2) . 1_565 ?
I2 Pb I1 89.947(2) . . ?
I2 Pb I1 89.947(2) 2_565 . ?
I2 Pb I2 178.70(4) . 2_565 ?
I2 Pb I3 90.65(2) 2_565 . ?
I2 Pb I3 89.35(2) 2_565 1_554 ?
I2 Pb I3 90.65(2) . . ?
I2 Pb I3 89.35(2) . 1_554 ?
I3 Pb I1 94.70(2) . . ?
I3 Pb I1 94.70(2) . 1_565 ?
I3 Pb I3 180.0 . 1_554 ?
Pb I1 Pb 170.60(5) 1_545 . ?
Pb I3 Pb 180.0 . 1_556 ?
H1AA C1 H1AB 115.5 . . ?
H1AA C1 H1BC 42.5 . 8_565 ?
H1AA C1 H1BD 93.5 . 8_565 ?
H1AA C1 H1BE 79.0 . 8_565 ?
H1AB C1 H1BC 150.2 . 8_565 ?
H1AB C1 H1BD 43.6 . 8_565 ?
H1AB C1 H1BE 77.2 . 8_565 ?
H1BC C1 H1BD 109.5 . . ?
H1BC C1 H1BE 109.5 . . ?
H1BD C1 H1BE 109.5 . . ?
N2 C1 H1AA 118.2 8_565 . ?
N2 C1 H1AA 118.2 . . ?
N2 C1 H1AB 118.2 8_565 . ?
N2 C1 H1AB 118.2 . . ?
N2 C1 H1BC 91(4) 8_565 8_565 ?
N2 C1 H1BC 76(6) . 8_565 ?
N2 C1 H1BD 147(4) 8_565 8_565 ?
N2 C1 H1BD 105(4) . 8_565 ?
N2 C1 H1BE 140(4) . 8_565 ?
N2 C1 H1BE 85(5) 8_565 8_565 ?
N2 C1 N2 55(2) 8_565 . ?
N3 C1 H1BC 109.5 . . ?
N3 C1 H1BD 109.5 . . ?
N3 C1 H1BE 109.5 . . ?
H1A N1 H1B 120.0 . . ?
N2 N1 N2 66(3) . 8_565 ?
N3 N1 H1A 120.0 . . ?
N3 N1 H1B 120.0 . . ?
C1 N2 H2A 107.5 . . ?
C1 N2 H2B 107.5 . . ?
C1 N2 H3A 91.0(18) . 8_565 ?
N1 N2 C1 119(2) . . ?
N1 N2 H2A 107.5 . . ?
N1 N2 H2B 107.5 . . ?
N1 N2 H3A 88(2) . 8_565 ?
H2A N2 H2B 107.0 . . ?
H2A N2 H3A 37.7 . 8_565 ?
H2B N2 H3A 144.6 . 8_565 ?
C1 N3 H3A 106.8 . . ?
C1 N3 H3B 106.8 . . ?
N1 N3 C1 122(3) . . ?
N1 N3 H3A 106.8 . . ?
N1 N3 H3B 106.8 . . ?
H3A N3 H3B 106.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 N2 N1 4(4) 8_565 . . . ?
N2 N1 N2 C1 -4(4) 8_565 . . . ?

_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
;
####################################################################### 
# 
# 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_mhy2pbi4_temp_330
_database_code_depnum_ccdc_archive 'CCDC 2298907'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-10-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C N2)'
_chemical_formula_sum            'C2 I4 N4 Pb'
_chemical_formula_weight         794.85
_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'
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           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'

_cell_length_a                   18.7824(6)
_cell_length_b                   6.3740(2)
_cell_length_c                   6.3845(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     764.35(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3158
_cell_measurement_temperature    330(2)
_cell_measurement_theta_max      28.0200
_cell_measurement_theta_min      3.1870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7079
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.974
_diffrn_reflns_theta_min         3.191
_diffrn_ambient_temperature      330(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  92.50   0.90   11.50    --   17.79-161.00 -93.00   75
  2  ω     31.00  94.00   0.90   11.50    --   17.79-171.00-176.00   70
  3  ω     -4.00  86.00   0.90   11.50    --   17.79  57.00 -60.00  100
  4  ω    -49.00  38.30   0.90   11.50    --  -18.65  77.00-150.00   97
  5  ω    -39.00  10.50   0.90   11.50    --  -18.65 -77.00  60.00   55
  6  ω    -51.00  39.00   0.90   11.50    --   17.79 -57.00 -30.00  100
  7  ω    -39.00 -12.00   0.90   11.50    --  -18.65 -77.00   0.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                899
_reflns_number_total             1061
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.799
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         1061
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0444
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0456P)²+4.8199P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1080
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N1-N2A \\sim N2B-N2A
 with sigma of 0.02
 N1-C1 \\sim N2B-C1
 with sigma of 0.02
2. Rigid bond restraints
 N2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N2B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C1) \\sim Ueq, Uanis(N2B) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C1, N2B, N1, N2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N2A(0.16665) N2B(0.3333) N1(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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
Pb Pb 0.250000 0.750000 0.41483(10) 0.0346(2) Uani 1 4 d S T P . .
I1 I 0.250000 0.250000 0.3746(2) 0.0605(5) Uani 1 4 d S T P . .
I2 I 0.41941(6) 0.750000 0.4085(2) 0.0736(4) Uani 1 2 d S T P . .
I3 I 0.250000 0.750000 0.9136(2) 0.0876(7) Uani 1 4 d S T P . .
C1 C 0.3826(14) 0.250000 -0.153(5) 0.107(7) Uani 1 2 d DS TU P . .
N2A N 0.399(7) 0.250000 0.002(18) 0.19(2) Uani 0.3333 2 d DS TU P . .
N2B N 0.4577(19) 0.250000 0.108(3) 0.117(10) Uani 0.6666 2 d DS TU P . .
N1 N 0.450(2) 0.153(5) 0.099(5) 0.173(17) Uani 0.5 1 d D U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb I1 3.19733(17) . ?
Pb I1 3.19733(16) 1_565 ?
Pb I2 3.1821(12) 2_565 ?
Pb I2 3.1821(12) . ?
Pb I3 3.2003(14) 1_554 ?
Pb I3 3.1842(14) . ?
C1 N2A 1.04(11) . ?
N2A N2B 1.29(11) . ?
N2A N1 1.30(11) 7_565 ?
N2A N1 1.30(11) . ?
N2B N1 0.64(3) . ?
N2B N1 0.64(3) 7_565 ?
N1 N1 1.24(6) 7_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
I1 Pb I1 170.79(6) 1_565 . ?
I1 Pb I3 85.39(3) 1_565 1_554 ?
I1 Pb I3 85.39(3) . 1_554 ?
I2 Pb I1 89.942(2) 2_565 . ?
I2 Pb I1 89.942(2) . 1_565 ?
I2 Pb I1 89.942(2) 2_565 1_565 ?
I2 Pb I1 89.942(2) . . ?
I2 Pb I2 178.55(5) . 2_565 ?
I2 Pb I3 90.72(3) 2_565 . ?
I2 Pb I3 90.72(3) . . ?
I2 Pb I3 89.28(3) 2_565 1_554 ?
I2 Pb I3 89.28(3) . 1_554 ?
I3 Pb I1 94.61(3) . . ?
I3 Pb I1 94.61(3) . 1_565 ?
I3 Pb I3 180.0 . 1_554 ?
Pb I1 Pb 170.79(6) . 1_545 ?
Pb I3 Pb 180.0 . 1_556 ?
C1 N2A N2B 139(10) . . ?
C1 N2A N1 133(10) . . ?
C1 N2A N1 133(10) . 7_565 ?
N2B N2A N1 29(3) . 7_565 ?
N2B N2A N1 29(3) . . ?
N1 N2A N1 57(6) 7_565 . ?
N1 N2B N2A 76(2) . . ?
N1 N2B N2A 76(2) 7_565 . ?
N1 N2B N1 152(5) . 7_565 ?
N2B N1 N2A 75(2) . . ?
N2B N1 N1 14(3) . 7_565 ?
N1 N1 N2A 61(3) 7_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
C1 N2A N2B N1 -92(6) . . . . ?
C1 N2A N2B N1 92(6) . . . 7_565 ?
C1 N2A N1 N2B 117(11) . . . . ?
C1 N2A N1 N1 120(13) . . . 7_565 ?
N2A N2B N1 N1 -10(22) . . . 7_565 ?
N2B N2A N1 N1 3(6) . . . 7_565 ?
N1 N2A N2B N1 -175(11) . . . 7_565 ?
N1 N2A N2B N1 175(11) 7_565 . . . ?
N1 N2A N1 N2B -3(6) 7_565 . . . ?
N1 N2B N1 N2A 10(22) 7_565 . . . ?

_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
;
####################################################################### 
# 
# 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_mhy2pbi4_temp_370
_database_code_depnum_ccdc_archive 'CCDC 2298910'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-28
# start Validation Reply Form
_vrf_PLAT971_mhy2pbi4_temp_370   
;
PROBLEM: Check Calcd Resid. Dens.  1.94Ang From N1              4.52 eA-3  
RESPONSE: This is an artifact
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C N2)'
_chemical_formula_sum            'C2 I4 N4 Pb'
_chemical_formula_weight         794.85
_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'
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           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'

_cell_length_a                   18.9775(10)
_cell_length_b                   6.3842(2)
_cell_length_c                   6.3817(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     773.18(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2447
_cell_measurement_temperature    370(2)
_cell_measurement_theta_max      27.4650
_cell_measurement_theta_min      3.1850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6997
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.135
_diffrn_reflns_theta_min         3.192
_diffrn_ambient_temperature      370(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  92.50   0.90   11.50    --   17.79-161.00 -93.00   75
  2  ω     31.00  94.00   0.90   11.50    --   17.79-171.00-176.00   70
  3  ω     -4.00  86.00   0.90   11.50    --   17.79  57.00 -60.00  100
  4  ω    -49.00  38.30   0.90   11.50    --  -18.65  77.00-150.00   97
  5  ω    -39.00  10.50   0.90   11.50    --  -18.65 -77.00  60.00   55
  6  ω    -51.00  39.00   0.90   11.50    --   17.79 -57.00 -30.00  100
  7  ω    -39.00 -12.00   0.90   11.50    --  -18.65 -77.00   0.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                798
_reflns_number_total             1050
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         5.038
_refine_diff_density_min         -1.683
_refine_diff_density_rms         0.415
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1050
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0741
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0951P)²+7.7556P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1946
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N1-N2B
 1.3 with sigma of 0.1
 N2B-C1
 1.4 with sigma of 0.1
 N2B-N1 \\sim N2A-N1
 with sigma of 0.02
 N2A-C1 \\sim N2B-C1
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(N2B) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 N2B, N2A, C1, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N2A(0.16665) C1(0.5) N2B(0.3333)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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
Pb Pb 0.250000 0.750000 0.41986(17) 0.0431(4) Uani 1 4 d S T P . .
I1 I 0.250000 0.250000 0.3827(4) 0.0751(9) Uani 1 4 d S T P . .
I2 I 0.41789(11) 0.750000 0.4092(4) 0.0922(8) Uani 1 2 d S T P . .
I3 I 0.250000 0.750000 0.9209(4) 0.1055(14) Uani 1 4 d S T P . .
N2A N 0.410(3) 0.250000 0.049(9) 0.112(19) Uani 0.3333 2 d DS TU P . .
C1 C 0.474(3) 0.206(11) 0.123(7) 0.11(2) Uani 0.5 1 d D U P . .
N2B N 0.419(3) 0.298(15) 0.028(8) 0.104(16) Uani 0.3333 1 d D U P . .
N1 N 0.3803(19) 0.250000 -0.149(6) 0.145(15) Uani 1 2 d DS TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb I1 3.2009(2) . ?
Pb I1 3.2009(2) 1_565 ?
Pb I2 3.187(2) . ?
Pb I2 3.187(2) 2_565 ?
Pb I3 3.184(2) 1_554 ?
Pb I3 3.198(2) . ?
N2A C1 1.34(6) . ?
N2A C1 1.34(6) 8_565 ?
N2A N2B 0.38(14) 8_565 ?
N2A N1 1.38(5) . ?
C1 C1 0.57(14) 8_565 ?
C1 N2B 1.35(6) . ?
C1 N2B 1.21(5) 8_565 ?
N2B N2B 0.61(19) 8_565 ?
N2B N1 1.38(5) . ?

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 Pb I1 171.51(10) . 1_565 ?
I2 Pb I1 89.909(4) 2_565 1_565 ?
I2 Pb I1 89.909(4) . . ?
I2 Pb I1 89.909(4) . 1_565 ?
I2 Pb I1 89.909(4) 2_565 . ?
I2 Pb I2 177.55(10) . 2_565 ?
I2 Pb I3 91.22(5) . . ?
I2 Pb I3 91.22(5) 2_565 . ?
I3 Pb I1 85.76(5) 1_554 . ?
I3 Pb I1 94.24(5) . . ?
I3 Pb I1 94.24(5) . 1_565 ?
I3 Pb I1 85.76(5) 1_554 1_565 ?
I3 Pb I2 88.78(5) 1_554 . ?
I3 Pb I2 88.78(5) 1_554 2_565 ?
I3 Pb I3 180.0 1_554 . ?
Pb I1 Pb 171.51(10) . 1_545 ?
Pb I3 Pb 180.0 1_556 . ?
C1 N2A C1 24(6) 8_565 . ?
C1 N2A N1 134(6) . . ?
C1 N2A N1 134(6) 8_565 . ?
N2B N2A C1 82(5) 8_565 8_565 ?
N2B N2A C1 62(6) 8_565 . ?
N2B N2A N1 83(4) 8_565 . ?
N2A C1 N2B 16(6) . . ?
C1 C1 N2A 78(3) 8_565 . ?
C1 C1 N2B 91(6) 8_565 8_565 ?
C1 C1 N2B 64(5) 8_565 . ?
N2B C1 N2A 16(6) 8_565 . ?
N2B C1 N2B 27(9) 8_565 . ?
C1 N2B C1 25(6) 8_565 . ?
C1 N2B N1 133(6) . . ?
C1 N2B N1 150(5) 8_565 . ?
N2B N2B C1 64(5) 8_565 . ?
N2B N2B C1 89(6) 8_565 8_565 ?
N2B N2B N1 77(4) 8_565 . ?
N2A N1 N2B 16(6) . 8_565 ?
N2A N1 N2B 16(6) . . ?
N2B N1 N2B 26(8) . 8_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
N2A C1 N2B C1 147(8) . . . 8_565 ?
N2A C1 N2B N2B -33(8) . . . 8_565 ?
N2A C1 N2B N1 -70(6) . . . . ?
C1 N2A C1 N2B -30(7) 8_565 . . . ?
C1 N2A C1 N2B -146(9) 8_565 . . 8_565 ?
C1 N2A N1 N2B 72(8) 8_565 . . 8_565 ?
C1 N2A N1 N2B 38(9) . . . 8_565 ?
C1 N2A N1 N2B -72(8) . . . . ?
C1 N2A N1 N2B -38(9) 8_565 . . . ?
C1 C1 N2B N2B 180.002(19) 8_565 . . 8_565 ?
C1 C1 N2B N1 143(11) 8_565 . . . ?
C1 N2B N1 N2A 100(16) 8_565 . . . ?
C1 N2B N1 N2A 70(6) . . . . ?
C1 N2B N1 N2B 34(11) . . . 8_565 ?
C1 N2B N1 N2B 65(19) 8_565 . . 8_565 ?
N2B N2A C1 C1 146(9) 8_565 . . 8_565 ?
N2B N2A C1 N2B 116(16) 8_565 . . . ?
N2B N2A N1 N2B -110(15) 8_565 . . . ?
N2B C1 N2B C1 179.998(14) 8_565 . . 8_565 ?
N2B C1 N2B N1 -37(11) 8_565 . . . ?
N2B N2B N1 N2A 36(8) 8_565 . . . ?
N1 N2A C1 C1 102(4) . . . 8_565 ?
N1 N2A C1 N2B 72(8) . . . . ?
N1 N2A C1 N2B -44(10) . . . 8_565 ?

_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
;
# END
####################################################################### 
# 
# 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_mhy2pbi4_temp_360
_database_code_depnum_ccdc_archive 'CCDC 2298909'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-28
# start Validation Reply Form
_vrf_PLAT971_mhy2pbi4_temp_360   
;
PROBLEM: Check Calcd Resid. Dens.  1.80Ang From C1              3.49 eA-3  
RESPONSE: This is an artifact
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C N2)'
_chemical_formula_sum            'C2 I4 N4 Pb'
_chemical_formula_weight         794.85
_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'
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           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'

_cell_length_a                   18.9231(9)
_cell_length_b                   6.3804(2)
_cell_length_c                   6.3828(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     770.64(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2833
_cell_measurement_temperature    360(2)
_cell_measurement_theta_max      27.4650
_cell_measurement_theta_min      3.1840
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.425
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7005
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.867
_diffrn_reflns_theta_min         3.192
_diffrn_ambient_temperature      360(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  92.50   0.90   11.50    --   17.79-161.00 -93.00   75
  2  ω     31.00  94.00   0.90   11.50    --   17.79-171.00-176.00   70
  3  ω     -4.00  86.00   0.90   11.50    --   17.79  57.00 -60.00  100
  4  ω    -49.00  38.30   0.90   11.50    --  -18.65  77.00-150.00   97
  5  ω    -39.00  10.50   0.90   11.50    --  -18.65 -77.00  60.00   55
  6  ω    -51.00  39.00   0.90   11.50    --   17.79 -57.00 -30.00  100
  7  ω    -39.00 -12.00   0.90   11.50    --  -18.65 -77.00   0.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                871
_reflns_number_total             1056
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.170
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.325
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         1056
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0613
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0722P)²+12.1737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1613
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N2A-C1 \\sim N2B-C1
 with sigma of 0.02
 N2A-N1 \\sim N2B-N1
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(N2B)
\\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(I2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
3. Rigid body (RIGU) restrains
 N1, C1, N2A, N2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N2A(0.16665) N2B(0.3333)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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
Pb Pb 0.250000 0.750000 0.41813(14) 0.0411(3) Uani 1 4 d S T P . .
I1 I 0.250000 0.250000 0.3804(4) 0.0700(7) Uani 1 4 d S T P . .
I2 I 0.41830(9) 0.750000 0.4091(4) 0.0866(7) Uani 1 2 d S TU P . .
I3 I 0.250000 0.750000 0.9185(3) 0.1016(12) Uani 1 4 d S T P . .
C1 C 0.380(2) 0.250000 -0.147(6) 0.106(8) Uani 1 2 d DS TU P . .
N2A N 0.408(2) 0.250000 0.058(7) 0.107(8) Uani 0.3333 2 d DS TU P . .
N2B N 0.418(2) 0.172(8) 0.027(8) 0.107(8) Uani 0.3333 1 d D U P . .
N1 N 0.4689(19) 0.250000 0.117(5) 0.115(8) Uani 1 2 d DS TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb I1 3.1993(2) . ?
Pb I1 3.1993(2) 1_565 ?
Pb I2 3.1853(17) 2_565 ?
Pb I2 3.1854(17) . ?
Pb I3 3.194(2) . ?
Pb I3 3.189(2) 1_554 ?
C1 N2A 1.40(5) . ?
C1 N2B 1.41(5) . ?
C1 N2B 1.41(5) 7_565 ?
N2A N2B 0.57(8) . ?
N2A N2B 0.57(8) 7_565 ?
N2A N1 1.22(4) . ?
N2B N2B 0.99(11) 7_565 ?
N2B N1 1.22(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
I1 Pb I1 171.36(9) 1_565 . ?
I2 Pb I1 89.922(4) . . ?
I2 Pb I1 89.922(4) 2_565 1_565 ?
I2 Pb I1 89.922(4) 2_565 . ?
I2 Pb I1 89.922(4) . 1_565 ?
I2 Pb I2 177.93(9) 2_565 . ?
I2 Pb I3 91.04(4) . . ?
I2 Pb I3 91.04(4) 2_565 . ?
I2 Pb I3 88.96(4) 2_565 1_554 ?
I2 Pb I3 88.96(4) . 1_554 ?
I3 Pb I1 85.68(4) 1_554 . ?
I3 Pb I1 94.32(4) . 1_565 ?
I3 Pb I1 94.32(4) . . ?
I3 Pb I1 85.68(4) 1_554 1_565 ?
I3 Pb I3 180.0 1_554 . ?
Pb I1 Pb 171.36(9) 1_545 . ?
Pb I3 Pb 180.0 1_556 . ?
N2A C1 N2B 23(3) . 7_565 ?
N2A C1 N2B 23(3) . . ?
N2B C1 N2B 41(5) . 7_565 ?
N2B N2A C1 79(3) 7_565 . ?
N2B N2A C1 79(3) . . ?
N2B N2A N2B 121(9) . 7_565 ?
N2B N2A N1 77(3) . . ?
N2B N2A N1 77(3) 7_565 . ?
N1 N2A C1 130(4) . . ?
N2A N2B C1 78(2) . . ?
N2A N2B N2B 30(5) . 7_565 ?
N2A N2B N1 76(3) . . ?
N2B N2B C1 69(2) 7_565 . ?
N2B N2B N1 66(3) 7_565 . ?
N1 N2B C1 129(4) . . ?
N2A N1 N2B 27(4) . 7_565 ?
N2A N1 N2B 27(4) . . ?
N2B N1 N2B 48(5) 7_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
C1 N2A N2B N2B 70(3) . . . 7_565 ?
C1 N2A N2B N1 135(4) . . . . ?
C1 N2A N1 N2B -63(4) . . . . ?
C1 N2A N1 N2B 63(4) . . . 7_565 ?
C1 N2B N1 N2A 61(4) . . . . ?
C1 N2B N1 N2B 32(7) . . . 7_565 ?
N2A C1 N2B N2B -30(5) . . . 7_565 ?
N2A C1 N2B N1 -61(4) . . . . ?
N2A N2B N1 N2B -30(5) . . . 7_565 ?
N2B C1 N2A N2B 125(9) . . . 7_565 ?
N2B C1 N2A N2B -125(9) 7_565 . . . ?
N2B C1 N2A N1 -62(4) 7_565 . . . ?
N2B C1 N2A N1 62(4) . . . . ?
N2B C1 N2B N2A 30(5) 7_565 . . . ?
N2B C1 N2B N1 -31(7) 7_565 . . . ?
N2B N2A N2B C1 -70(3) 7_565 . . . ?
N2B N2A N2B N1 66(4) 7_565 . . . ?
N2B N2A N1 N2B 126(9) . . . 7_565 ?
N2B N2A N1 N2B -126(9) 7_565 . . . ?
N2B N2B N1 N2A 30(5) 7_565 . . . ?
N1 N2A N2B C1 -135(4) . . . . ?
N1 N2A N2B N2B -66(4) . . . 7_565 ?

_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
;
####################################################################### 
# 
# 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_mhy2pbi4_3_30
_database_code_depnum_ccdc_archive 'CCDC 2298918'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-06 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-10-06
# start Validation Reply Form
_vrf_ATOM007_mhy2pbi4_3_30       
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: The structure was refined isotropically.
Structure is not refined anisotropically because of low resolution.
;
_vrf_PLAT027_mhy2pbi4_3_30       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_3_30       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.314 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT031_mhy2pbi4_3_30       
;
PROBLEM: Refined Extinction Parameter Within Range of ...      1.400 Sigma 
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT082_mhy2pbi4_3_30       
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample
;
_vrf_PLAT201_mhy2pbi4_3_30       
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         10 Report
RESPONSE: The structure was refined isotropically.
Structure is not refined anisotropically because of low resolution.
;
_vrf_PLAT417_mhy2pbi4_3_30       
;
PROBLEM: Short Inter D-H..H-D       H1BD     ..H2CA     .       2.04 Ang.  
RESPONSE: It is very difficult to locate hydrogen atoms 
accurately using X-ray data because these atoms have low 
scattering power. In addition, we have bad quality measurement 
and low resolution data.
;
_vrf_PLAT911_mhy2pbi4_3_30       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        301 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_mhy2pbi4_3_30       
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         18 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT971_mhy2pbi4_3_30       
;
PROBLEM: Check Calcd Resid. Dens.  0.21Ang From Pb1B            2.79 eA-3  
RESPONSE: The structure is not refined anistropically which results in
large value. Also, low resolution of data.
;
_vrf_PLAT972_mhy2pbi4_3_30       
;
PROBLEM: Check Calcd Resid. Dens.  0.57Ang From I2B            -2.90 eA-3  
RESPONSE: The structure is not refined anistropically which results in
large value. Also, low resolution of data.
;
_vrf_PLAT977_mhy2pbi4_3_30       
;
PROBLEM: Check Negative Difference Density on H1CA      .      -1.55 eA-3  
RESPONSE: The structure is not refined anistropically which results in
large value. Also, low resolution of data.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(I2 Pb0.5), 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_chemical_absolute_configuration ?
_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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.1212(3)
_cell_length_b                   12.3727(7)
_cell_length_c                   17.150(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.095(13)
_cell_angle_gamma                90
_cell_volume                     1298.8(4)
_cell_formula_units_Z            4
_cell_measurement_pressure       3300000
_cell_measurement_reflns_used    3431
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.8840
_cell_measurement_theta_min      3.3490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.137
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8.59 1.42 1.86 0.0658
8.61 -1.72 -2.10 0.0649
2.76 16.37 -2.98 0.0943
4.91 -14.35 2.11 0.0661
0.15 1.46 24.25 0.0118
-2.56 -16.19 5.45 0.0596
0.03 -2.45 -24.16 0.0118
-7.73 7.73 -2.42 0.0739

_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.314
_diffrn_reflns_Laue_measured_fraction_max 0.186
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            5966
_diffrn_reflns_point_group_measured_fraction_full 0.318
_diffrn_reflns_point_group_measured_fraction_max 0.183
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.314
_diffrn_reflns_theta_min         3.293
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.314
_diffrn_measured_fraction_theta_max 0.186
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -40.00  -4.00   0.75   10.50    --    0.23  57.00 -30.00   48
  2  ω    -59.00  -3.50   0.75   10.50    --    0.23  97.00 -35.00   74
  3  ω    -54.00 -24.00   0.75   19.00    --  -29.93  37.00   0.00   40
  4  ω     -3.25  23.00   0.75   19.00    --  -29.93 -81.00  29.00   35
  5  ω    -32.25   3.00   0.75   19.00    --  -29.93   0.00  30.00   47
  6  ω    -76.00 -13.00   0.75   19.00    --  -29.93 114.00 -45.00   84
  7  ω    -44.00 -11.00   0.75   19.00    --  -29.93  19.00   0.00   44
  8  ω    -19.00  44.00   0.75   19.00    --  -29.93 -39.00  12.00   84
  9  ω    -22.00  14.00   0.75   19.00    --   30.40  53.00 162.00   48
 10  ω    -30.00  -3.75   0.75   19.00    --   30.40  97.00 -35.00   35
 11  ω    -33.00  19.50   0.75   19.00    --   30.40  19.00-180.00   70
 12  ω     20.00  57.50   0.75   19.00    --   30.40 -77.00-150.00   50
 13  ω     33.75  78.00   0.75   19.00    --   30.40-125.00-120.00   59
 14  ω    -42.00 -10.50   0.75   10.50    --    0.23  19.00  30.00   42
 15  ω    -46.00   8.00   0.75   10.50    --    0.23  67.00 157.00   72
 16  ω     13.00  40.00   0.75   19.00    --  -29.93-114.00-135.00   36
 17  ω    -55.00   8.00   0.75   19.00    --  -29.93  67.00 157.00   84
 18  ω    -14.00  22.00   0.75   19.00    --  -29.93 -53.00-162.00   48
 19  ω    -27.00  36.00   0.75   19.00    --  -29.93 -13.00-176.00   84
 20  ω    -32.25   3.00   0.75   19.00    --   30.40   0.00  30.00   47
 21  ω     23.00  76.25   0.75   19.00    --   30.40-114.00-135.00   71
 22  ω      0.00  49.50   0.75   19.00    --   30.40 -53.00  17.00   66
 23  ω    -16.00   8.00   0.75   19.00    --   30.40  67.00 -23.00   32
 24  ω      8.00  61.25   0.75   10.50    --    0.23 -99.00-150.00   71
 25  ω    -42.00  -3.75   0.75   10.50    --    0.23  57.00 150.00   51
 26  ω    -44.00  19.00   0.75   19.00    --  -29.93  39.00 167.00   84
 27  ω    -30.00  -4.50   0.75   19.00    --   30.40  97.00 143.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.322
_reflns_Friedel_fraction_max     0.180
_reflns_number_gt                808
_reflns_number_total             974
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.372
_refine_diff_density_min         -2.723
_refine_diff_density_rms         0.628
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(13)
_refine_ls_extinction_coef       0.00014(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         974
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1887
_refine_ls_R_factor_gt           0.1556
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1498.4862P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2915
_refine_ls_wR_factor_ref         0.3139
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.53(13)
 0.47(13)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Pb1B-I1B \\sim Pb1A-I1A
 with sigma of 0.01
 Pb1B-I2B \\sim Pb1B-I4B \\sim Pb1A-I4A \\sim Pb1A-I2A
 with sigma of 0.01
 Pb1A-I3A \\sim Pb1B-I3B
 with sigma of 0.01
4. Others
 Fixed Uiso: I1B(0.025) Pb1B(0.025) I3B(0.025) Pb1A(0.03) I3A(0.03) I2B(0.025)
 I1A(0.03) I4B(0.025) I4A(0.03) I2A(0.03) C1A(0.05) N2A(0.05) N1A(0.05)
 N2B(0.05) C1B(0.05) N1B(0.05) C1C(0.05) N2C(0.05) N1C(0.05) N2D(0.05)
 C1D(0.05) N1D(0.05)
5.a Free rotating group:
 C1A(N2A,N1A,N2B,C1B,N1B,C1C,N2C,N1C,N2D,C1D,N1D)
5.b Secondary CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), N2B(H2BA,H2BB), N2C(H2CA,H2CB), N2D(H2DA,H2DB)
5.c X=CH2 refined with riding coordinates:
 N1A(H1AD,H1AE), N1B(H1BD,H1BE), N1C(H1CD,H1CE), N1D(H1DD,H1DE)
5.d Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,
 H1DC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
I1B I -0.475(3) 0.8328(12) 0.988(4) 0.025 Uiso 1 1 d D U . . .
Pb1B Pb -0.5006(16) 0.5824(7) 0.999(4) 0.025 Uiso 1 1 d D U . . .
I3B I -0.010(2) 0.5385(14) 0.993(4) 0.025 Uiso 1 1 d D U . . .
Pb1A Pb -0.0054(16) 0.6652(7) 0.492(3) 0.030 Uiso 1 1 d D U . . .
I3A I 0.487(2) 0.7021(15) 0.503(4) 0.030 Uiso 1 1 d D U . . .
I2B I -0.465(3) 0.5843(12) 1.173(4) 0.025 Uiso 1 1 d D U . . .
I1A I -0.024(3) 0.9171(12) 0.490(4) 0.030 Uiso 1 1 d D U . . .
I4B I -0.503(2) 0.5642(13) 0.826(4) 0.025 Uiso 1 1 d D U . . .
I4A I 0.035(3) 0.6509(13) 0.319(4) 0.030 Uiso 1 1 d D U . . .
I2A I -0.006(3) 0.6727(14) 0.666(4) 0.030 Uiso 1 1 d D U . . .
C1A C -0.031(12) 0.766(7) 0.880(16) 0.050 Uiso 1 1 d G U . . .
H1AA H 0.018244 0.698935 0.858043 0.075 Uiso 1 1 calc R U . . .
H1AB H -0.186281 0.772346 0.872819 0.075 Uiso 1 1 calc R U . . .
H1AC H 0.001018 0.766473 0.935131 0.075 Uiso 1 1 calc R U . . .
N2A N 0.072(14) 0.850(7) 0.845(16) 0.050 Uiso 1 1 d G U . . .
H2AA H 0.170001 0.819237 0.813582 0.060 Uiso 1 1 calc R U . . .
H2AB H 0.149681 0.881261 0.882704 0.060 Uiso 1 1 calc R U . . .
N1A N -0.010(18) 0.940(8) 0.800(17) 0.050 Uiso 1 1 d G U . . .
H1AD H -0.148570 0.946251 0.791582 0.060 Uiso 1 1 calc R U . . .
H1AE H 0.078225 0.987304 0.781038 0.060 Uiso 1 1 calc R U . . .
N2B N 0.59(2) 0.399(8) 0.669(18) 0.050 Uiso 1 1 d G U . . .
H2BA H 0.683253 0.435043 0.698197 0.060 Uiso 1 1 calc R U . . .
H2BB H 0.664739 0.361869 0.634862 0.060 Uiso 1 1 calc R U . . .
C1B C 0.48(2) 0.477(8) 0.626(17) 0.050 Uiso 1 1 d G U . . .
H1BA H 0.328605 0.474935 0.636648 0.075 Uiso 1 1 calc R U . . .
H1BB H 0.507399 0.464155 0.571769 0.075 Uiso 1 1 calc R U . . .
H1BC H 0.539180 0.546907 0.640075 0.075 Uiso 1 1 calc R U . . .
N1B N 0.50(3) 0.320(7) 0.720(18) 0.050 Uiso 1 1 d G U . . .
H1BD H 0.364591 0.315288 0.727894 0.060 Uiso 1 1 calc R U . . .
H1BE H 0.590433 0.275811 0.743360 0.060 Uiso 1 1 calc R U . . .
C1C C 0.04(2) 0.761(10) 1.123(16) 0.050 Uiso 1 1 d G U . . .
H1CA H 0.031569 0.798993 1.074414 0.075 Uiso 1 1 calc R U . . .
H1CB H -0.029426 0.691646 1.117785 0.075 Uiso 1 1 calc R U . . .
H1CC H 0.191073 0.750490 1.136881 0.075 Uiso 1 1 calc R U . . .
N2C N -0.07(2) 0.825(12) 1.185(16) 0.050 Uiso 1 1 d G U . . .
H2CA H -0.207206 0.834442 1.168290 0.060 Uiso 1 1 calc R U . . .
H2CB H -0.080414 0.780651 1.226085 0.060 Uiso 1 1 calc R U . . .
N1C N -0.01(3) 0.920(13) 1.214(16) 0.050 Uiso 1 1 d G U . . .
H1CD H 0.109692 0.950717 1.195841 0.060 Uiso 1 1 calc R U . . .
H1CE H -0.081274 0.951519 1.249559 0.060 Uiso 1 1 calc R U . . .
N2D N 0.60(2) 0.945(8) 0.649(17) 0.050 Uiso 1 1 d G U . . .
H2DA H 0.669740 0.983543 0.684994 0.060 Uiso 1 1 calc R U . . .
H2DB H 0.705184 0.915467 0.619001 0.060 Uiso 1 1 calc R U . . .
C1D C 0.49(3) 1.016(9) 0.602(17) 0.050 Uiso 1 1 d G U . . .
H1DA H 0.585261 1.043267 0.562556 0.075 Uiso 1 1 calc R U . . .
H1DB H 0.438796 1.075474 0.633766 0.075 Uiso 1 1 calc R U . . .
H1DC H 0.367648 0.980455 0.578844 0.075 Uiso 1 1 calc R U . . .
N1D N 0.499(18) 0.861(7) 0.686(17) 0.050 Uiso 1 1 d G U . . .
H1DD H 0.360416 0.852661 0.681414 0.060 Uiso 1 1 calc R U . . .
H1DE H 0.573605 0.817623 0.714930 0.060 Uiso 1 1 calc R U . . .

_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
I1B Pb1B 3.10(2) 2_457 ?
I1B Pb1B 3.107(18) . ?
Pb1B I3B 3.166(15) 1_455 ?
Pb1B I3B 3.054(12) . ?
Pb1B I2B 2.99(4) . ?
Pb1B I4B 2.98(4) . ?
Pb1A I3A 3.146(15) 1_455 ?
Pb1A I3A 3.056(13) . ?
Pb1A I1A 3.09(2) 2_546 ?
Pb1A I1A 3.119(19) . ?
Pb1A I4A 2.99(4) . ?
Pb1A I2A 2.99(4) . ?
C1A H1AA 0.96 . ?
C1A H1AB 0.96 . ?
C1A H1AC 0.97 . ?
C1A N2A 1.3702(18) . ?
N2A H2AA 0.8900 . ?
N2A H2AB 0.8900 . ?
N2A N1A 1.4(2) . ?
N1A H1AD 0.8600 . ?
N1A H1AE 0.8600 . ?
N2B H2BA 0.8900 . ?
N2B H2BB 0.8700 . ?
N2B C1B 1.4(3) . ?
N2B N1B 1.4052(11) . ?
C1B H1BA 0.95 . ?
C1B H1BB 0.9683 . ?
C1B H1BC 0.9683 . ?
N1B H1BD 0.8400 . ?
N1B H1BE 0.8600 . ?
C1C H1CA 0.96 . ?
C1C H1CB 0.96 . ?
C1C H1CC 0.96 . ?
C1C N2C 1.4918 . ?
N2C H2CA 0.8900 . ?
N2C H2CB 0.8900 . ?
N2C N1C 1.342(3) . ?
N1C H1CD 0.8800 . ?
N1C H1CE 0.8600 . ?
N2D H2DA 0.8900 . ?
N2D H2DB 0.8900 . ?
N2D C1D 1.4(3) . ?
N2D N1D 1.3711(11) . ?
C1D H1DA 0.9649 . ?
C1D H1DB 0.9649 . ?
C1D H1DC 0.95 . ?
N1D H1DD 0.8600 . ?
N1D H1DE 0.8600 . ?

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
Pb1B I1B Pb1B 170(2) 2_457 . ?
I1B Pb1B I1B 179(2) 2_447 . ?
I1B Pb1B I3B 102.6(5) . 1_455 ?
I1B Pb1B I3B 77.5(5) 2_447 1_455 ?
I3B Pb1B I1B 82.7(5) . 2_447 ?
I3B Pb1B I1B 97.2(5) . . ?
I3B Pb1B I3B 159.5(9) . 1_455 ?
I2B Pb1B I1B 92.9(17) . . ?
I2B Pb1B I1B 86.5(17) . 2_447 ?
I2B Pb1B I3B 88.0(17) . . ?
I2B Pb1B I3B 96.0(17) . 1_455 ?
I4B Pb1B I1B 89.8(17) . 2_447 ?
I4B Pb1B I1B 90.8(17) . . ?
I4B Pb1B I3B 87.5(17) . . ?
I4B Pb1B I3B 87.2(17) . 1_455 ?
I4B Pb1B I2B 174.5(6) . . ?
Pb1B I3B Pb1B 159.5(9) . 1_655 ?
I3A Pb1A I3A 161.6(15) . 1_455 ?
I3A Pb1A I1A 83.6(5) . . ?
I3A Pb1A I1A 94.8(6) . 2_546 ?
I1A Pb1A I3A 101.3(6) 2_546 1_455 ?
I1A Pb1A I3A 79.6(5) . 1_455 ?
I1A Pb1A I1A 175(2) 2_546 . ?
I4A Pb1A I3A 89.3(18) . . ?
I4A Pb1A I3A 98.9(17) . 1_455 ?
I4A Pb1A I1A 93.0(17) . . ?
I4A Pb1A I1A 91.9(17) . 2_546 ?
I2A Pb1A I3A 86.1(17) . 1_455 ?
I2A Pb1A I3A 86.3(17) . . ?
I2A Pb1A I1A 86.2(18) . 2_546 ?
I2A Pb1A I1A 88.8(17) . . ?
I2A Pb1A I4A 175.0(6) . . ?
Pb1A I3A Pb1A 161.6(15) . 1_655 ?
Pb1A I1A Pb1A 172(2) 2_556 . ?
H1AA C1A H1AB 109 . . ?
H1AA C1A H1AC 109 . . ?
H1AB C1A H1AC 109 . . ?
N2A C1A H1AA 110 . . ?
N2A C1A H1AB 110 . . ?
N2A C1A H1AC 110 . . ?
C1A N2A H2AA 104.4 . . ?
C1A N2A H2AB 104.4 . . ?
C1A N2A N1A 131.57(19) . . ?
H2AA N2A H2AB 105.6 . . ?
N1A N2A H2AA 104.4 . . ?
N1A N2A H2AB 104.4 . . ?
N2A N1A H1AD 120.0 . . ?
N2A N1A H1AE 120.0 . . ?
H1AD N1A H1AE 120.0 . . ?
H2BA N2B H2BB 108 . . ?
C1B N2B H2BA 104.5 . . ?
C1B N2B H2BB 104.5 . . ?
C1B N2B N1B 130.9(2) . . ?
N1B N2B H2BA 104.5 . . ?
N1B N2B H2BB 104.5 . . ?
N2B C1B H1BA 110.4 . . ?
N2B C1B H1BB 108 . . ?
N2B C1B H1BC 108 . . ?
H1BA C1B H1BB 111 . . ?
H1BA C1B H1BC 110 . . ?
H1BB C1B H1BC 108.5 . . ?
N2B N1B H1BD 122.0 . . ?
N2B N1B H1BE 118.0 . . ?
H1BD N1B H1BE 120.0 . . ?
H1CA C1C H1CB 108.0 . . ?
H1CA C1C H1CC 109 . . ?
H1CB C1C H1CC 109 . . ?
N2C C1C H1CA 111.0 . . ?
N2C C1C H1CB 110.8 . . ?
N2C C1C H1CC 109 . . ?
C1C N2C H2CA 105.7 . . ?
C1C N2C H2CB 105.7 . . ?
H2CA N2C H2CB 105 . . ?
N1C N2C C1C 126.3(3) . . ?
N1C N2C H2CA 105.7 . . ?
N1C N2C H2CB 105.7 . . ?
N2C N1C H1CD 120.0 . . ?
N2C N1C H1CE 122.0 . . ?
H1CD N1C H1CE 120.0 . . ?
H2DA N2D H2DB 106.7 . . ?
C1D N2D H2DA 106.8 . . ?
C1D N2D H2DB 106.8 . . ?
C1D N2D N1D 122.1(2) . . ?
N1D N2D H2DA 108 . . ?
N1D N2D H2DB 106.8 . . ?
N2D C1D H1DA 110.0 . . ?
N2D C1D H1DB 108 . . ?
N2D C1D H1DC 110.0 . . ?
H1DA C1D H1DB 108.9 . . ?
H1DA C1D H1DC 110 . . ?
H1DB C1D H1DC 108.9 . . ?
N2D N1D H1DD 120.0 . . ?
N2D N1D H1DE 120.0 . . ?
H1DD N1D H1DE 120.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.53(13)
2 0.47(13)

####################################################################### 
# 
# 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_mhy2pbi4_0_22
_database_code_depnum_ccdc_archive 'CCDC 2298911'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-26
# start Validation Reply Form
_vrf_RINTA01_mhy2pbi4_0_22       
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT027_mhy2pbi4_0_22       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_0_22       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.398 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT031_mhy2pbi4_0_22       
;
PROBLEM: Refined Extinction Parameter Within Range of ...      0.125 Sigma 
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT088_mhy2pbi4_0_22       
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.76 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT020_mhy2pbi4_0_22       
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.200 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample
;
_vrf_PLAT911_mhy2pbi4_0_22       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         66 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C N3)'
_chemical_formula_sum            'C2 I4 N6 Pb'
_chemical_formula_weight         822.87
_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'
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           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'

_cell_length_a                   18.4404(15)
_cell_length_b                   6.35(9)
_cell_length_c                   6.3926(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     748(10)
_cell_formula_units_Z            2
_cell_measurement_pressure       220000
_cell_measurement_reflns_used    1210
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1850
_cell_measurement_theta_min      3.1870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.482
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 2 1 0.0658
-9 -2 -1 0.0649
-3 -3 8 0.0943
-5 2 -7 0.0661
0 26 1 0.0118
3 5 -8 0.0596
0 -26 -1 0.0118
8 -3 4 0.0739

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.03
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.398     0.454
         range of gasket transmission (min-max)           1.000     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 100.0 microns, radius = 200.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2002
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.398
_diffrn_reflns_Laue_measured_fraction_max 0.279
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1351
_diffrn_reflns_point_group_measured_fraction_full 0.398
_diffrn_reflns_point_group_measured_fraction_max 0.279
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.245
_diffrn_reflns_theta_min         3.373
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.398
_diffrn_measured_fraction_theta_max 0.279
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   15.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   15.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   15.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   15.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   15.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   15.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   15.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   15.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   15.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   15.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   15.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   15.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   15.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   15.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   15.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   15.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                190
_reflns_number_total             236
_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 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.282
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.294
_refine_ls_extinction_coef       0.0001(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         236
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0844
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1440P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2270
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N2-C1
 1.45 with sigma of 0.02
 N2-N1
 1.39 with sigma of 0.02
 N1-C1
 2.4 with sigma of 0.1
2. Rigid bond restraints
 Pb1, I1, I3, I2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, N2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim N2 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
I3 \\sim Pb1 \\sim I1 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(I3) \\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(I1) \\sim Ueq, Uanis(I2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N1, N2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Pb1, I1, I3, I2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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 0.250000 0.750000 0.4098(4) 0.044(4) Uani 1 4 d S TU P . .
I1 I 0.250000 0.250000 0.3628(7) 0.059(4) Uani 1 4 d S TU P . .
I3 I 0.250000 0.750000 0.9073(6) 0.065(4) Uani 1 4 d S TU P . .
I2 I 0.4188(8) 0.750000 0.4078(6) 0.073(4) Uani 1 2 d S TU P . .
C1 C 0.539(8) 0.750000 -0.122(14) 0.14(2) Uani 1 2 d DS TU P . .
N1 N 0.613(10) 0.750000 0.198(10) 0.143(19) Uani 1 2 d DS TU P . .
N2 N 0.595(8) 0.655(9) 0.007(8) 0.143(18) Uani 1 1 d D U . . .


_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 3.19(4) . ?
Pb1 I1 3.19(4) 1_565 ?
Pb1 I3 3.181(3) . ?
Pb1 I3 3.212(3) 1_554 ?
Pb1 I2 3.113(15) . ?
Pb1 I2 3.113(15) 2_565 ?
C1 N2 1.45(2) 8_575 ?
C1 N2 1.45(2) . ?
N1 N2 1.40(2) . ?
N1 N2 1.40(2) 8_575 ?
N2 N2 1.20(11) 8_575 ?

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 169.2(2) 1_565 . ?
I1 Pb1 I3 84.60(12) 1_565 1_554 ?
I1 Pb1 I3 84.60(12) . 1_554 ?
I3 Pb1 I1 95.40(12) . 1_565 ?
I3 Pb1 I1 95.40(12) . . ?
I3 Pb1 I3 180.0 . 1_554 ?
I2 Pb1 I1 89.978(7) . . ?
I2 Pb1 I1 89.978(7) . 1_565 ?
I2 Pb1 I1 89.978(7) 2_565 1_565 ?
I2 Pb1 I1 89.978(7) 2_565 . ?
I2 Pb1 I3 90.23(7) 2_565 . ?
I2 Pb1 I3 89.77(7) 2_565 1_554 ?
I2 Pb1 I3 90.23(7) . . ?
I2 Pb1 I3 89.77(7) . 1_554 ?
I2 Pb1 I2 179.53(14) . 2_565 ?
Pb1 I1 Pb1 169.2(2) 1_545 . ?
Pb1 I3 Pb1 180.0 . 1_556 ?
N2 C1 N2 49(5) 8_575 . ?
N2 N1 N2 51(5) . 8_575 ?
N1 N2 C1 119(6) . . ?
N2 N2 C1 66(2) 8_575 . ?
N2 N2 N1 65(3) 8_575 . ?

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
N2 C1 N2 N1 38(9) 8_575 . . . ?
N2 N1 N2 C1 -38(9) 8_575 . . . ?

_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
- B-factor correction
;
####################################################################### 
# 
# 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_mhy2pbi4_1_70
_database_code_depnum_ccdc_archive 'CCDC 2298914'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-27
# start Validation Reply Form
_vrf_PLAT027_mhy2pbi4_1_70       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_1_70       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.444 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_mhy2pbi4_1_70       
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.00 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT987_mhy2pbi4_1_70       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_chemical_absolute_configuration ?
_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           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   17.6111(2)
_cell_length_b                   6.2619(2)
_cell_length_c                   6.201(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     683.8(10)
_cell_formula_units_Z            2
_cell_measurement_pressure       1700000
_cell_measurement_reflns_used    2708
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3960
_cell_measurement_theta_min      3.3300
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.331
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.929
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.444
_diffrn_reflns_Laue_measured_fraction_max 0.320
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3891
_diffrn_reflns_point_group_measured_fraction_full 0.460
_diffrn_reflns_point_group_measured_fraction_max 0.327
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         27.414
_diffrn_reflns_theta_min         3.253
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.444
_diffrn_measured_fraction_theta_max 0.320
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00 -79.00   0.75    9.00    --    0.23 178.00 -90.00   32
  2  ω   -103.00 -79.00   0.75    9.00    --    0.23 178.00  60.00   32
  3  ω      2.00  50.00   0.75    9.00    --    0.23 -57.00-180.00   64
  4  ω     15.00  51.00   0.75    9.00    --    0.23 -77.00-150.00   48
  5  ω    -17.00  22.00   0.75   17.50    --  -31.31 -53.00  17.00   52
  6  ω    -58.00  11.00   0.75   17.50    --  -31.31  67.00 -23.00   92
  7  ω     -6.00  21.00   0.75   17.50    --  -31.31 -81.00  29.00   36
  8  ω    -92.00 -23.00   0.75   17.50    --  -31.31 135.00 123.00   92
  9  ω    -39.00  30.00   0.75   17.50    --  -31.31  13.00 176.00   92
 10  ω    -43.00  26.00   0.75   17.50    --  -31.31  26.00  -7.00   92
 11  ω    -11.00  43.00   0.75   17.50    --   31.78 -26.00   7.00   72
 12  ω    -29.00  22.00   0.75   17.50    --   31.78  39.00 -12.00   68
 13  ω    -35.00   4.00   0.75   17.50    --   31.78   0.00-150.00   52
 14  ω    -53.00   5.50   0.75    9.00    --    0.23  81.00 -29.00   78
 15  ω     23.00  83.00   0.75    9.00    --    0.23-135.00  57.00   80
 16  ω    -22.00  17.00   0.75    9.00    --    0.23 -19.00-150.00   52
 17  ω    -17.00  22.00   0.75   17.50    --  -31.31 -53.00-162.00   52
 18  ω    -58.00  11.00   0.75   17.50    --  -31.31  67.00 157.00   92
 19  ω    -22.00   3.50   0.75   17.50    --  -31.31 -39.00  12.00   34
 20  ω      1.00  29.50   0.75   17.50    --  -31.31 -97.00-143.00   38
 21  ω    -39.00 -10.50   0.75   17.50    --   31.78 114.00 -45.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.482
_reflns_Friedel_fraction_max     0.335
_reflns_number_gt                504
_reflns_number_total             511
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         511
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0273
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0311P)²+9.3150P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0678
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-N1
 1.3 with sigma of 0.08
 N2-C1
 1.45 with sigma of 0.08
 H1A-H2A_$1
 2.2 with sigma of 0.02
3. Rigid bond restraints
 Pb1, I3, I1, I2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Pb1 \\sim I3 \\sim I1 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N1, N2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I1, Pb1, I2, I3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.500000 0.09268(14) 0.26100(13) 0.018(3) Uani 1 2 d S TU P . .
I3 I 0.500000 0.5962(3) 0.2366(4) 0.028(4) Uani 1 2 d S TU P . .
I1 I 0.500000 0.1655(3) 0.7624(5) 0.031(3) Uani 1 2 d S TU P . .
I2 I 0.3245(5) 0.0890(2) 0.2533(5) 0.035(3) Uani 1 1 d . U . . .
N1 N 0.303(3) 0.386(3) 0.730(4) 0.031(11) Uani 1 1 d D U . . .
H1A H 0.304620 0.379400 0.868221 0.037 Uiso 1 1 calc DR U . . .
H1B H 0.278835 0.289274 0.658316 0.037 Uiso 1 1 calc R U . . .
C1 C 0.372(5) 0.684(5) 0.772(13) 0.079(15) Uani 1 1 d D U . . .
H1C H 0.401182 0.782269 0.686295 0.118 Uiso 1 1 calc R U . . .
H1D H 0.405485 0.608537 0.867918 0.118 Uiso 1 1 calc R U . . .
H1E H 0.335098 0.761205 0.854337 0.118 Uiso 1 1 calc R U . . .
N2 N 0.334(3) 0.534(4) 0.633(4) 0.061(19) Uani 1 1 d D . . . .
H2A H 0.299964 0.604103 0.555575 0.073 Uiso 1 1 calc R U . . .
H2B H 0.368388 0.479894 0.542163 0.073 Uiso 1 1 calc R U . . .


_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 I3 3.1567(19) . ?
Pb1 I3 3.1125(19) 1_545 ?
Pb1 I1 3.142(6) . ?
Pb1 I1 3.125(6) 1_554 ?
Pb1 I2 3.092(8) 4_655 ?
Pb1 I2 3.092(8) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 N2 1.24(5) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 N2 1.43(6) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?

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
I3 Pb1 I3 174.47(10) 1_545 . ?
I3 Pb1 I1 101.13(6) 1_545 . ?
I3 Pb1 I1 95.61(7) 1_545 1_554 ?
I1 Pb1 I3 78.87(6) 1_554 . ?
I1 Pb1 I3 84.40(6) . . ?
I1 Pb1 I1 163.27(8) 1_554 . ?
I2 Pb1 I3 89.53(3) . 1_545 ?
I2 Pb1 I3 90.38(3) . . ?
I2 Pb1 I3 89.53(3) 4_655 1_545 ?
I2 Pb1 I3 90.38(3) 4_655 . ?
I2 Pb1 I1 89.19(6) 4_655 1_554 ?
I2 Pb1 I1 90.94(6) 4_655 . ?
I2 Pb1 I1 89.19(6) . 1_554 ?
I2 Pb1 I1 90.94(6) . . ?
I2 Pb1 I2 178.03(11) 4_655 . ?
Pb1 I3 Pb1 174.47(10) 1_565 . ?
Pb1 I1 Pb1 163.27(8) 1_556 . ?
H1A N1 H1B 120.0 . . ?
N2 N1 H1A 120.0 . . ?
N2 N1 H1B 120.0 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N2 C1 H1C 109.5 . . ?
N2 C1 H1D 109.5 . . ?
N2 C1 H1E 109.5 . . ?
N1 N2 C1 114(4) . . ?
N1 N2 H2A 110.00 . . ?
N1 N2 H2B 108.7 . . ?
C1 N2 H2A 108.7 . . ?
C1 N2 H2B 108.7 . . ?
H2A N2 H2B 107.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mhy2pbi4_2_10
_database_code_depnum_ccdc_archive 'CCDC 2298915'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-27
# start Validation Reply Form
_vrf_PLAT027_mhy2pbi4_2_10       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_2_10       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.434 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_mhy2pbi4_2_10       
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.16 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT987_mhy2pbi4_2_10       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_chemical_absolute_configuration ?
_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           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   17.571(18)
_cell_length_b                   6.1827(2)
_cell_length_c                   6.2444(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     678.4(7)
_cell_formula_units_Z            2
_cell_measurement_pressure       2100000
_cell_measurement_reflns_used    2219
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4710
_cell_measurement_theta_min      4.6260
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.501
_exptl_absorpt_correction_T_max  0.282
_exptl_absorpt_correction_T_min  0.235
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.960
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 9 -1 0.0658
-2 -9 1 0.0649
-3 -3 -8 0.0943
2 -5 7 0.0661
25 0 -1 0.0118
6 3 8 0.0596
-24 0 1 0.0118
-3 8 -4 0.0739

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.03
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.402     0.454
         range of gasket transmission (min-max)           1.000     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 100.0 microns, radius = 300.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.434
_diffrn_reflns_Laue_measured_fraction_max 0.264
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3249
_diffrn_reflns_point_group_measured_fraction_full 0.455
_diffrn_reflns_point_group_measured_fraction_max 0.269
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         27.648
_diffrn_reflns_theta_min         3.295
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.434
_diffrn_measured_fraction_theta_max 0.264
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00 -79.00   0.75    9.00    --    0.23 178.00 -90.00   32
  2  ω   -103.00 -79.00   0.75    9.00    --    0.23 178.00  60.00   32
  3  ω      2.00  50.00   0.75    9.00    --    0.23 -57.00-180.00   64
  4  ω     15.00  51.00   0.75    9.00    --    0.23 -77.00-150.00   48
  5  ω    -17.00  22.00   0.75   17.50    --  -31.31 -53.00  17.00   52
  6  ω    -58.00  11.00   0.75   17.50    --  -31.31  67.00 -23.00   92
  7  ω     -6.00  21.00   0.75   17.50    --  -31.31 -81.00  29.00   36
  8  ω    -92.00 -23.00   0.75   17.50    --  -31.31 135.00 123.00   92
  9  ω    -39.00  30.00   0.75   17.50    --  -31.31  13.00 176.00   92
 10  ω    -43.00  26.00   0.75   17.50    --  -31.31  26.00  -7.00   92
 11  ω    -11.00  43.00   0.75   17.50    --   31.78 -26.00   7.00   72
 12  ω    -29.00  22.00   0.75   17.50    --   31.78  39.00 -12.00   68
 13  ω    -35.00   4.00   0.75   17.50    --   31.78   0.00-150.00   52
 14  ω    -53.00   5.50   0.75    9.00    --    0.23  81.00 -29.00   78
 15  ω     23.00  83.00   0.75    9.00    --    0.23-135.00  57.00   80
 16  ω    -22.00  17.00   0.75    9.00    --    0.23 -19.00-150.00   52
 17  ω    -17.00  22.00   0.75   17.50    --  -31.31 -53.00-162.00   52
 18  ω    -58.00  11.00   0.75   17.50    --  -31.31  67.00 157.00   92
 19  ω    -22.00   3.50   0.75   17.50    --  -31.31 -39.00  12.00   34
 20  ω      1.00  29.50   0.75   17.50    --  -31.31 -97.00-143.00   38
 21  ω    -39.00 -10.50   0.75   17.50    --   31.78 114.00 -45.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.484
_reflns_Friedel_fraction_max     0.276
_reflns_number_gt                428
_reflns_number_total             434
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00132(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         434
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0244
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0084P)²+12.9550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0490
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-N1
 1.4 with sigma of 0.08
 H1A_$1-H2A
 2.2 with sigma of 0.02
 N2-C1
 1.4 with sigma of 0.02
3. Rigid bond restraints
 Pb1, I3, I1, I2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Pb1 \\sim I3 \\sim I1 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 N1, N2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I1, Pb1, I2, I3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.500000 0.09245(16) 0.26076(18) 0.021(6) Uani 1 2 d S TU P . .
I3 I 0.500000 0.5962(3) 0.2362(4) 0.036(6) Uani 1 2 d S TU P . .
I1 I 0.500000 0.1670(3) 0.7618(6) 0.036(5) Uani 1 2 d S TU P . .
I2 I 0.3238(5) 0.0888(2) 0.2530(5) 0.037(6) Uani 1 1 d . U . . .
N1 N 0.299(3) 0.385(3) 0.729(5) 0.031(8) Uani 1 1 d D U . . .
H1A H 0.292098 0.389376 0.865581 0.037 Uiso 1 1 calc R U . . .
H1B H 0.277028 0.286390 0.654140 0.037 Uiso 1 1 calc R U . . .
C1 C 0.377(4) 0.689(4) 0.764(11) 0.065(13) Uani 1 1 d D U . . .
H1C H 0.406663 0.786431 0.677808 0.098 Uiso 1 1 calc R U . . .
H1D H 0.409824 0.618709 0.865879 0.098 Uiso 1 1 calc R U . . .
H1E H 0.338284 0.767584 0.837991 0.098 Uiso 1 1 calc R U . . .
N2 N 0.344(3) 0.534(4) 0.633(4) 0.066(17) Uani 1 1 d D . . . .
H2A H 0.316079 0.602163 0.534619 0.079 Uiso 1 1 calc DR U . . .
H2B H 0.380717 0.463902 0.564164 0.079 Uiso 1 1 calc R U . . .


_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 I3 3.072(2) 1_545 ?
Pb1 I3 3.118(2) . ?
Pb1 I1 3.149(4) 1_554 ?
Pb1 I1 3.163(4) . ?
Pb1 I2 3.096(10) . ?
Pb1 I2 3.096(10) 4_655 ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 N2 1.35(6) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 N2 1.39(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?

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
I3 Pb1 I3 174.32(11) 1_545 . ?
I3 Pb1 I1 84.44(7) . . ?
I3 Pb1 I1 78.77(6) . 1_554 ?
I3 Pb1 I1 101.24(7) 1_545 . ?
I3 Pb1 I1 95.55(7) 1_545 1_554 ?
I3 Pb1 I2 89.54(3) 1_545 4_655 ?
I3 Pb1 I2 89.54(3) 1_545 . ?
I1 Pb1 I1 163.21(8) 1_554 . ?
I2 Pb1 I3 90.37(3) . . ?
I2 Pb1 I3 90.37(3) 4_655 . ?
I2 Pb1 I1 89.17(6) 4_655 1_554 ?
I2 Pb1 I1 90.95(6) 4_655 . ?
I2 Pb1 I1 90.95(6) . . ?
I2 Pb1 I1 89.17(6) . 1_554 ?
I2 Pb1 I2 178.02(12) . 4_655 ?
Pb1 I3 Pb1 174.32(11) 1_565 . ?
Pb1 I1 Pb1 163.21(8) 1_556 . ?
H1A N1 H1B 120.0 . . ?
N2 N1 H1A 120.0 . . ?
N2 N1 H1B 120.0 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N2 C1 H1C 109.5 . . ?
N2 C1 H1D 109.5 . . ?
N2 C1 H1E 109.5 . . ?
N1 N2 C1 117(4) . . ?
N1 N2 H2A 108.1 . . ?
N1 N2 H2B 108.1 . . ?
C1 N2 H2A 108.1 . . ?
C1 N2 H2B 108.1 . . ?
H2A N2 H2B 107.3 . . ?

_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
;
####################################################################### 
# 
# 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_mhy2pbi4_2_64
_database_code_depnum_ccdc_archive 'CCDC 2298916'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-27
# start Validation Reply Form
_vrf_PLAT027_mhy2pbi4_2_64       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_2_64       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.394 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_mhy2pbi4_2_64       
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.38 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT911_mhy2pbi4_2_64       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         50 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_mhy2pbi4_2_64       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_chemical_absolute_configuration ?
_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           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   17.24(3)
_cell_length_b                   6.1573(5)
_cell_length_c                   6.2293(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     661.3(12)
_cell_formula_units_Z            2
_cell_measurement_pressure       2640000
_cell_measurement_reflns_used    1209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0630
_cell_measurement_theta_min      4.6230
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.063
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.394
_diffrn_reflns_Laue_measured_fraction_max 0.251
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2880
_diffrn_reflns_point_group_measured_fraction_full 0.424
_diffrn_reflns_point_group_measured_fraction_max 0.259
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.148
_diffrn_reflns_theta_min         4.655
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.394
_diffrn_measured_fraction_theta_max 0.251
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  20.50   0.75   17.50   0.00 -30.00   0.00    --    74
  2  φ    140.00 200.00   0.75   17.50   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   17.50   0.00  30.00   0.00    --    76
  4  φ    -20.00  35.50   0.75   17.50   0.00  30.00   0.00    --    74
  5  ω    -24.00  24.00   0.75   17.50    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   17.50    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   17.50    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   17.50    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -7.75   0.75   17.50    --  -30.00  81.40 -28.90   75
 10  ω    -64.00  -7.75   0.75   17.50    --  -30.00  81.40 151.10   75
 11  ω    -19.00   8.00   0.75   17.50    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   17.50    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -20.50   0.75   17.50    --   30.00 134.60 -56.90   30
 14  ω    -43.00 -20.50   0.75   17.50    --   30.00 134.60 123.10   30
 15  ω    -90.00 -36.00   0.75   17.50    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   17.50    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_full    0.466
_reflns_Friedel_fraction_max     0.270
_reflns_number_gt                335
_reflns_number_total             354
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         354
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0491
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0335P)²+70.5102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1124
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-N1
 1.3 with sigma of 0.08
 H2B-H1A_$1
 2.2 with sigma of 0.02
 N2-C1
 1.4 with sigma of 0.02
 H1E-H1E_$2
 2.2 with sigma of 0.02
3. Rigid bond restraints
 Pb1, I3, I1, I2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Pb1 \\sim I3 \\sim I1 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(I2) \\sim Ueq, Uanis(I1) \\sim Ueq, Uanis(I3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N1, N2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I1, Pb1, I2, I3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.500000 0.0911(4) 0.2602(6) 0.025(9) Uani 1 2 d S TU P . .
I3 I 0.500000 0.5949(7) 0.2338(10) 0.023(6) Uani 1 2 d S TU P . .
I1 I 0.500000 0.1709(8) 0.7640(14) 0.026(6) Uani 1 2 d S TU P . .
I2 I 0.3245(12) 0.0877(6) 0.2497(12) 0.036(8) Uani 1 1 d . U . . .
N1 N 0.300(6) 0.387(7) 0.763(14) 0.035(15) Uani 1 1 d D U . . .
H1A H 0.303662 0.396071 0.900264 0.042 Uiso 1 1 calc R U . . .
H1B H 0.269956 0.293656 0.704748 0.042 Uiso 1 1 calc R U . . .
C1 C 0.397(6) 0.686(10) 0.709(11) 0.04(2) Uani 1 1 d D U . . .
H1C H 0.368762 0.787778 0.796383 0.054 Uiso 1 1 calc R U . . .
H1D H 0.420609 0.760637 0.591402 0.054 Uiso 1 1 calc R U . . .
H1E H 0.436164 0.616919 0.794622 0.054 Uiso 1 1 calc DR U . . .
N2 N 0.346(5) 0.528(11) 0.631(10) 0.052(17) Uani 1 1 d D U . . .
H2A H 0.373549 0.442967 0.545161 0.062 Uiso 1 1 calc R U . . .
H2B H 0.312291 0.598363 0.546546 0.062 Uiso 1 1 calc DR U . . .


_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 I3 3.107(6) . ?
Pb1 I3 3.060(6) 1_545 ?
Pb1 I1 3.176(10) . ?
Pb1 I1 3.130(10) 1_554 ?
Pb1 I2 3.03(2) 4_655 ?
Pb1 I2 3.03(2) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 N2 1.43(10) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 N2 1.40(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?

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
I3 Pb1 I3 173.9(3) 1_545 . ?
I3 Pb1 I1 101.98(18) 1_545 . ?
I3 Pb1 I1 77.93(15) . 1_554 ?
I3 Pb1 I1 84.14(17) . . ?
I3 Pb1 I1 95.9(2) 1_545 1_554 ?
I1 Pb1 I1 162.07(19) 1_554 . ?
I2 Pb1 I3 89.54(9) 4_655 1_545 ?
I2 Pb1 I3 89.54(9) . 1_545 ?
I2 Pb1 I3 90.32(9) . . ?
I2 Pb1 I3 90.32(9) 4_655 . ?
I2 Pb1 I1 91.29(14) 4_655 . ?
I2 Pb1 I1 88.83(14) . 1_554 ?
I2 Pb1 I1 91.29(14) . . ?
I2 Pb1 I1 88.83(14) 4_655 1_554 ?
I2 Pb1 I2 177.4(3) . 4_655 ?
Pb1 I3 Pb1 173.9(3) 1_565 . ?
Pb1 I1 Pb1 162.07(19) 1_556 . ?
H1A N1 H1B 120.0 . . ?
N2 N1 H1A 120.0 . . ?
N2 N1 H1B 120.0 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N2 C1 H1C 109.5 . . ?
N2 C1 H1D 109.5 . . ?
N2 C1 H1E 109.5 . . ?
N1 N2 H2A 106.2 . . ?
N1 N2 H2B 106.2 . . ?
C1 N2 N1 124(7) . . ?
C1 N2 H2A 106.2 . . ?
C1 N2 H2B 106.2 . . ?
H2A N2 H2B 106.4 . . ?

_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
;
####################################################################### 
# 
# 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_mhy2pbi4_3_00
_database_code_depnum_ccdc_archive 'CCDC 2298917'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-27
# start Validation Reply Form
_vrf_PLAT027_mhy2pbi4_3_00       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_3_00       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.366 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_mhy2pbi4_3_00       
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.95 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT987_mhy2pbi4_3_00       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_chemical_absolute_configuration ?
_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           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   17.19(2)
_cell_length_b                   6.2150(3)
_cell_length_c                   6.1341(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     655.3(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2029
_cell_measurement_pressure       3000000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9360
_cell_measurement_theta_min      4.6430
_shelx_estimated_absorpt_T_max   0.402
_shelx_estimated_absorpt_T_min   0.101
_exptl_absorpt_coefficient_mu    22.259
_exptl_absorpt_correction_T_max  0.140
_exptl_absorpt_correction_T_min  0.114
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -9 0 0.0623
0 -1 9 0.0738
0 1 -9 0.1098
1 -9 -1 0.0656
-24 0 0 0.0246
2 9 1 0.0904
24 0 0 0.0266

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.408     0.454
         range of gasket transmission (min-max)           1.000     1.000
         range of P media transmission (min-max)          0.997     0.998

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 250.0 microns, radius = 250.0 microns
    Gasket absorption coeff =         0.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Absorption coeff of pressure medium =   0.01 mm-1
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.366
_diffrn_reflns_Laue_measured_fraction_max 0.221
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2388
_diffrn_reflns_point_group_measured_fraction_full 0.388
_diffrn_reflns_point_group_measured_fraction_max 0.227
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.155
_diffrn_reflns_theta_min         4.669
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.366
_diffrn_measured_fraction_theta_max 0.221
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  20.50   0.75   17.50   0.00 -30.00   0.00    --    74
  2  φ    140.00 200.00   0.75   17.50   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   17.50   0.00  30.00   0.00    --    76
  4  φ    -20.00  35.50   0.75   17.50   0.00  30.00   0.00    --    74
  5  ω    -24.00  24.00   0.75   17.50    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   17.50    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   17.50    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   17.50    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -7.75   0.75   17.50    --  -30.00  81.40 -28.90   75
 10  ω    -64.00  -7.75   0.75   17.50    --  -30.00  81.40 151.10   75
 11  ω    -19.00   8.00   0.75   17.50    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   17.50    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -20.50   0.75   17.50    --   30.00 134.60 -56.90   30
 14  ω    -43.00 -20.50   0.75   17.50    --   30.00 134.60 123.10   30
 15  ω    -90.00 -36.00   0.75   17.50    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   17.50    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.419
_reflns_Friedel_fraction_max     0.235
_reflns_number_gt                294
_reflns_number_total             309
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         309
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+67.1246P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0862
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-N1
 1.3 with sigma of 0.08
 N2-C1
 1.45 with sigma of 0.08
 H1A_$1-H2B
 2.2 with sigma of 0.02
3. Rigid bond restraints
 Pb1, I3, I1, I2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, N2, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 I1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Pb1 \\sim I3 \\sim I1 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim N2 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
I1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C1) \\sim Ueq, Uanis(I3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I1) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(I3) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.08
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(I2) \\sim Ueq, Uanis(I1) \\sim Ueq, Uanis(I3) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
5. Rigid body (RIGU) restrains
 N1, N2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I1, Pb1, I2, I3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.500000 0.0898(5) 0.2619(6) 0.022(7) Uani 1 2 d S TU P . .
I3 I 0.500000 0.5941(8) 0.2340(9) 0.014(3) Uani 1 2 d S TU P . .
I1 I 0.500000 0.1717(8) 0.7646(13) 0.019(3) Uani 1 2 d S TU P . .
I2 I 0.3244(17) 0.0875(6) 0.2510(12) 0.034(5) Uani 1 1 d . U . . .
N1 N 0.298(6) 0.387(7) 0.762(16) 0.034(12) Uani 1 1 d D U . . .
H1A H 0.297120 0.388314 0.901707 0.041 Uiso 1 1 calc R U . . .
H1B H 0.267640 0.300436 0.691436 0.041 Uiso 1 1 calc R U . . .
C1 C 0.407(10) 0.694(9) 0.710(12) 0.028(15) Uani 1 1 d D U . . .
H1C H 0.379812 0.819139 0.761959 0.041 Uiso 1 1 calc R U . . .
H1D H 0.439207 0.733463 0.588547 0.041 Uiso 1 1 calc R U . . .
H1E H 0.438370 0.635778 0.824159 0.041 Uiso 1 1 calc R U . . .
N2 N 0.351(5) 0.534(10) 0.640(9) 0.041(13) Uani 1 1 d D U . . .
H2A H 0.378050 0.446668 0.554345 0.049 Uiso 1 1 calc R U . . .
H2B H 0.319157 0.606040 0.550822 0.049 Uiso 1 1 calc DR U . . .


_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 I3 3.138(6) . ?
Pb1 I3 3.086(6) 1_545 ?
Pb1 I1 3.126(9) . ?
Pb1 I1 3.092(9) 1_554 ?
Pb1 I2 3.02(3) . ?
Pb1 I2 3.02(3) 3_655 ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 N2 1.49(11) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 N2 1.45(11) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?

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
I3 Pb1 I3 173.7(3) 1_545 . ?
I3 Pb1 I1 102.54(18) 1_545 . ?
I3 Pb1 I1 96.29(19) 1_545 1_554 ?
I1 Pb1 I3 77.41(16) 1_554 . ?
I1 Pb1 I3 83.75(17) . . ?
I1 Pb1 I1 161.2(2) 1_554 . ?
I2 Pb1 I3 89.65(10) 3_655 1_545 ?
I2 Pb1 I3 90.21(10) 3_655 . ?
I2 Pb1 I3 89.65(10) . 1_545 ?
I2 Pb1 I3 90.21(10) . . ?
I2 Pb1 I1 88.80(15) . 1_554 ?
I2 Pb1 I1 91.29(16) . . ?
I2 Pb1 I1 88.80(15) 3_655 1_554 ?
I2 Pb1 I1 91.29(16) 3_655 . ?
I2 Pb1 I2 177.4(3) . 3_655 ?
Pb1 I3 Pb1 173.7(3) 1_565 . ?
Pb1 I1 Pb1 161.2(2) 1_556 . ?
H1A N1 H1B 120.0 . . ?
N2 N1 H1A 120.0 . . ?
N2 N1 H1B 120.0 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N2 C1 H1C 109.5 . . ?
N2 C1 H1D 109.5 . . ?
N2 C1 H1E 109.5 . . ?
N1 N2 H2A 104.0 . . ?
N1 N2 H2B 104.0 . . ?
C1 N2 N1 133(7) . . ?
C1 N2 H2A 104.0 . . ?
C1 N2 H2B 104.0 . . ?
H2A N2 H2B 105.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
####################################################################### 
# 
# 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_mhy2pbi4_1_00
_database_code_depnum_ccdc_archive 'CCDC 2298912'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-27
# start Validation Reply Form
_vrf_PLAT027_mhy2pbi4_1_00       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_1_00       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.407 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_mhy2pbi4_1_00       
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.15 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT911_mhy2pbi4_1_00       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         51 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, C2 N4'
_chemical_formula_sum            'C2 I4 N4 Pb'
_chemical_formula_weight         794.85
_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'
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           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'

_cell_length_a                   17.9087(11)
_cell_length_b                   6.30(5)
_cell_length_c                   6.3600(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     718(6)
_cell_formula_units_Z            2
_cell_measurement_pressure       1000000
_cell_measurement_reflns_used    1416
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2950
_cell_measurement_theta_min      3.2290
_shelx_estimated_absorpt_T_max   0.581
_shelx_estimated_absorpt_T_min   0.125
_exptl_absorpt_coefficient_mu    20.312
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.678
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 2 1 0.0634
-9 -2 -1 0.0675
-3 -3 8 0.0828
-5 2 -7 0.0774
0 25 1 0.0122
3 5 -8 0.0711
0 -25 -1 0.0122
8 -3 4 0.0669

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.03
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.389     0.454
         range of gasket transmission (min-max)           1.000     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 100.0 microns, radius = 190.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1517
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.407
_diffrn_reflns_Laue_measured_fraction_max 0.307
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2141
_diffrn_reflns_point_group_measured_fraction_full 0.407
_diffrn_reflns_point_group_measured_fraction_max 0.307
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.285
_diffrn_reflns_theta_min         3.399
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.407
_diffrn_measured_fraction_theta_max 0.307
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   15.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   15.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   15.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   15.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   15.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   15.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   15.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   15.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   15.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   15.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   15.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   15.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   15.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   15.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   15.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   15.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                224
_reflns_number_total             252
_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 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.0012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         252
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0425
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0014P)²+10.3537P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0964
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N2-C1
 1.45 with sigma of 0.02
 N2-N1
 1.39 with sigma of 0.02
 N1-C1
 2.4 with sigma of 0.1
2. Rigid bond restraints
 N1, C1, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim N2: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 N2, C1, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N2(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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 0.250000 0.750000 0.40715(19) 0.046(6) Uani 1 4 d S T P . .
I1 I 0.250000 0.250000 0.3481(4) 0.059(7) Uani 1 4 d S T P . .
I3 I 0.250000 0.750000 0.9040(3) 0.083(8) Uani 1 4 d S T P . .
I2 I 0.4226(7) 0.750000 0.4092(3) 0.071(7) Uani 1 2 d S T P . .
C1 C 0.530(5) 0.750000 -0.116(4) 0.062(9) Uani 1 2 d DS TU P . .
N1 N 0.618(5) 0.750000 0.175(5) 0.085(9) Uani 1 2 d DS TU P . .
N2 N 0.582(5) 0.638(6) 0.018(6) 0.080(9) Uani 0.5 1 d D U P . .


_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 3.17(3) 1_565 ?
Pb1 I1 3.17(3) . ?
Pb1 I3 3.160(2) . ?
Pb1 I3 3.200(2) 1_554 ?
Pb1 I2 3.092(12) . ?
Pb1 I2 3.092(12) 2_565 ?
C1 N2 1.45(2) . ?
C1 N2 1.45(2) 7_575 ?
N1 N2 1.38(2) 7_575 ?
N1 N2 1.38(2) . ?
N2 N2 1.41(8) 7_575 ?

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 166.41(15) . 1_565 ?
I1 Pb1 I3 83.21(8) . 1_554 ?
I1 Pb1 I3 83.21(8) 1_565 1_554 ?
I3 Pb1 I1 96.79(8) . . ?
I3 Pb1 I1 96.79(8) . 1_565 ?
I3 Pb1 I3 180.0 . 1_554 ?
I2 Pb1 I1 90.028(5) . 1_565 ?
I2 Pb1 I1 90.028(5) . . ?
I2 Pb1 I1 90.028(5) 2_565 . ?
I2 Pb1 I1 90.028(5) 2_565 1_565 ?
I2 Pb1 I3 89.76(4) 2_565 . ?
I2 Pb1 I3 90.24(4) 2_565 1_554 ?
I2 Pb1 I3 89.76(4) . . ?
I2 Pb1 I3 90.24(4) . 1_554 ?
I2 Pb1 I2 179.52(8) . 2_565 ?
Pb1 I1 Pb1 166.41(15) . 1_545 ?
Pb1 I3 Pb1 180.0 . 1_556 ?
N2 C1 N2 58(4) . 7_575 ?
N2 N1 N2 61(4) 7_575 . ?
N1 N2 C1 119(4) . . ?
N1 N2 N2 59.4(19) . 7_575 ?
N2 N2 C1 60.9(18) 7_575 . ?

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
N2 C1 N2 N1 14(6) 7_575 . . . ?
N2 N1 N2 C1 -14(6) 7_575 . . . ?

_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
- B-factor correction
;
####################################################################### 
# 
# 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_mhy2pbi4_3_74
_database_code_depnum_ccdc_archive 'CCDC 2298919'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-06 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2022-10-14
# start Validation Reply Form
_vrf_ATOM007_mhy2pbi4_3_74       
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: The structure was refined isotropically.
Structure is not refined anisotropically because of low resolution.
;
_vrf_PLAT027_mhy2pbi4_3_74       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_3_74       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.312 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT417_mhy2pbi4_3_74       
;
PROBLEM: Short Inter D-H..H-D       H1AA      ..H2DA     .       1.70 Ang.  
RESPONSE: It is very difficult to locate hydrogen 
atoms accurately using X-ray data because these atoms 
have low scattering power. In addition, we have bad 
quality measurement and low resolution data.
;
_vrf_PLAT082_mhy2pbi4_3_74       
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample
;
_vrf_PLAT084_mhy2pbi4_3_74       
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample
;
_vrf_PLAT201_mhy2pbi4_3_74       
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          8 Report
RESPONSE: The structure was refined isotropically.
Structure is not refined anisotropically because of low resolution.
;
_vrf_PLAT351_mhy2pbi4_3_74       
;
PROBLEM: Long   C-H (X0.96,N1C.08A)  C1A      - H1AD     .       1.20 Ang.  
RESPONSE: We have bad quality measurement 
and low resolution data.
;
_vrf_PLAT780_mhy2pbi4_3_74       
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do !  
RESPONSE: We have bad quality measurement 
and low resolution data but all atoms are connect
;
_vrf_PLAT987_mhy2pbi4_3_74       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I2 Pb0.5, C0.5 H3.5 I2 N Pb0.5, 1.5(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.995
_chemical_absolute_configuration unk
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           ' P 2yb'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_symmetry_Int_Tables_number      4
_cell_length_a                   6.0985(2)
_cell_length_b                   12.3284(4)
_cell_length_c                   17.049(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.097(12)
_cell_angle_gamma                90
_cell_volume                     1281.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3582
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       3740000
_cell_measurement_theta_max      24.7030
_cell_measurement_theta_min      3.3370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.192
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3.80 15.59 0.97 0.0634
-0.64 17.22 -3.02 0.0669
-0.79 -1.83 -23.88 0.0122
-8.23 -3.68 4.76 0.0711
3.69 -15.78 -1.21 0.0675
-3.61 -15.71 2.28 0.0774
8.39 3.48 -2.29 0.0828
0.46 1.03 23.96 0.0121
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.03
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.3119
_diffrn_reflns_Laue_measured_fraction_max 0.1735
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            6025
_diffrn_reflns_point_group_measured_fraction_full 0.3169
_diffrn_reflns_point_group_measured_fraction_max 0.1717
_diffrn_reflns_theta_full        15.0000
_diffrn_reflns_theta_max         26.60
_diffrn_reflns_theta_min         3.30
_diffrn_measured_fraction_theta_full 0.3119
_diffrn_measured_fraction_theta_max 0.1735
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.170
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              3
_reflns_limit_l_min              -3
_reflns_number_gt                842
_reflns_number_total             926
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.8787
_refine_diff_density_min         -3.9500
_refine_diff_density_rms         0.7587
_refine_ls_abs_structure_details 
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.231(8)
_refine_ls_d_res_high            0.7936
_refine_ls_d_res_low             6.1642
_refine_ls_extinction_coef       0.00073(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0413
_refine_ls_matrix_type           full
_refine_ls_number_constraints    44
_refine_ls_number_parameters     61
_refine_ls_number_reflns         926
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.1645
_refine_ls_restrained_S_all      1.0413
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.00000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0899P)²+1850.0757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3629
_refine_ls_wR_factor_ref         0.3752
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.51(2)
 0.49(2)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Uiso: I1B(0.03) Pb1B(0.03) I3B(0.03) Pb1A(0.03) I3A(0.03) I2B(0.03) I1A(0.03)
 I4B(0.03) I4A(0.03) I2A(0.03) C1B(0.05) N1B(0.05) N2B(0.05) C1D(0.05) N1D(0.05)
 N2D(0.05) C1A(0.05) N1A(0.05) N2A(0.05) C1C(0.05) N1C(0.05) N2C(0.05)
4.a Free rotating group:
 C1B(N1B,N2B), C1D(N1D,N2D), C1A(N1A,N2A), C1C(N1C,N2C)
4.b Secondary CH2 refined with riding coordinates:
 N2D(H2DA,H2DB), N2C(H2CB,H2CA), N2A(H2AA,H2AB), N2B(H2BA,H2BB)
4.c X=CH2 refined with riding coordinates:
 N1D(H1DB,H1DA), N1C(H1CD,H1CB), N1A(H1AA,H1AB), N1B(H1BA,H1BB)
4.d Idealised Me refined as rotating group:
 C1B(H1BD,H1BE,H1BC), C1A(H1AD,H1AE,H1AC), C1C(H1CD,H1CE,H1CC), C1D(H1DD,H1DC,H1DE)
;
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
I1B I 0.536(3) 0.83655(17) 0.977(6) 0.030000 Uiso 1.000000
Pb1B Pb 0.497(2) 0.58594(7) 0.999(4) 0.030000 Uiso 1.000000
I3B I 0.987(3) 0.53358(16) 0.988(6) 0.030000 Uiso 1.000000
Pb1A Pb 0.9863(18) 0.66083(7) 0.499(5) 0.030000 Uiso 1.000000
I3A I 1.478(3) 0.69902(16) 0.499(6) 0.030000 Uiso 1.000000
I2B I 0.564(3) 0.59342(17) 1.191(5) 0.030000 Uiso 1.000000
I1A I 0.961(3) 0.91576(16) 0.494(6) 0.030000 Uiso 1.000000
I4B I 0.485(3) 0.56364(17) 0.830(6) 0.030000 Uiso 1.000000
I4A I 1.014(3) 0.64868(16) 0.322(6) 0.030000 Uiso 1.000000
I2A I 1.007(4) 0.67811(17) 0.685(6) 0.030000 Uiso 1.000000
C1B C 0.66(5) 0.481(3) 0.66(4) 0.050000 Uiso 1.000000
N1B N 0.46(3) 0.316(12) 0.71(5) 0.050000 Uiso 1.000000
N2B N 0.64(3) 0.385(4) 0.70(4) 0.050000 Uiso 1.000000
C1D C 0.58(5) 0.478(3) 1.41(3) 0.050000 Uiso 1.000000
N1D N 0.50(4) 0.335(10) 1.32(3) 0.050000 Uiso 1.000000
N2D N 0.64(3) 0.387(6) 1.37(3) 0.050000 Uiso 1.000000
C1A C 1.02(5) 0.760(3) 0.86(4) 0.050000 Uiso 1.000000
N1A N 0.98(4) 0.913(14) 0.76(4) 0.050000 Uiso 1.000000
N2A N 0.91(3) 0.839(13) 0.82(4) 0.050000 Uiso 1.000000
C1C C 1.01(5) 0.749(3) 1.12(4) 0.050000 Uiso 1.000000
N1C N 0.90(5) 0.889(6) 1.22(4) 0.050000 Uiso 1.000000
N2C N 0.89(3) 0.789(5) 1.19(4) 0.050000 Uiso 1.000000
H1BD H 0.51(6) 0.51(12) 0.65(16) 0.075000 Uiso 1.000000
H1BE H 0.7(4) 0.53(7) 0.69(8) 0.075000 Uiso 1.000000
H1BC H 0.7(4) 0.47(4) 0.61(8) 0.075000 Uiso 1.000000
H1AD H 1.2(2) 0.74(16) 0.83(10) 0.075000 Uiso 1.000000
H1AE H 1.0(4) 0.79(9) 0.91(7) 0.075000 Uiso 1.000000
H1AC H 0.93(18) 0.70(7) 0.86(14) 0.075000 Uiso 1.000000
H1CD H 1.0(3) 0.671(19) 1.12(9) 0.075000 Uiso 1.000000
H1CE H 1.0(2) 0.78(12) 1.08(4) 0.075000 Uiso 1.000000
H1CC H 1.16(5) 0.77(14) 1.13(6) 0.075000 Uiso 1.000000
H1DD H 0.5(5) 0.456(5) 1.46(8) 0.075000 Uiso 1.000000
H1DC H 0.71(7) 0.52(12) 1.42(15) 0.075000 Uiso 1.000000
H1DE H 0.5(3) 0.52(12) 1.38(8) 0.075000 Uiso 1.000000
H2DA H 0.76(3) 0.404(6) 1.34(3) 0.060000 Uiso 1.000000
H2DB H 0.67(3) 0.336(6) 1.41(3) 0.060000 Uiso 1.000000
H2CB H 0.75(3) 0.783(5) 1.17(4) 0.060000 Uiso 1.000000
H2CA H 0.91(3) 0.741(5) 1.22(4) 0.060000 Uiso 1.000000
H2AA H 0.80(3) 0.803(13) 0.79(4) 0.060000 Uiso 1.000000
H2AB H 0.84(3) 0.880(13) 0.85(4) 0.060000 Uiso 1.000000
H2BA H 0.75(3) 0.343(4) 0.68(4) 0.060000 Uiso 1.000000
H2BB H 0.68(3) 0.401(4) 0.75(4) 0.060000 Uiso 1.000000
H1DB H 0.37(4) 0.361(10) 1.31(3) 0.060000 Uiso 1.000000
H1DA H 0.54(4) 0.279(10) 1.29(3) 0.060000 Uiso 1.000000
H1CD H 0.99(5) 0.936(6) 1.21(4) 0.060000 Uiso 1.000000
H1CB H 0.81(5) 0.902(6) 1.26(4) 0.060000 Uiso 1.000000
H1AA H 1.12(4) 0.914(14) 0.75(4) 0.060000 Uiso 1.000000
H1AB H 0.89(4) 0.958(14) 0.74(4) 0.060000 Uiso 1.000000
H1BA H 0.34(3) 0.332(12) 0.69(5) 0.060000 Uiso 1.000000
H1BB H 0.48(3) 0.258(12) 0.74(5) 0.060000 Uiso 1.000000

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
I1B Pb1B 3.107(16) 2_657 ?
I1B Pb1B 3.121(16) . ?
Pb1B I3B 3.06(2) . ?
Pb1B I3B 3.18(2) 1_455 ?
Pb1B I2B 3.29(8) . ?
Pb1B I4B 2.89(10) . ?
Pb1A I3A 3.132(19) 1_455 ?
Pb1A I3A 3.038(19) . ?
Pb1A I1A 3.041(6) 2_746 ?
Pb1A I1A 3.148(5) . ?
Pb1A I4A 3.04(9) . ?
Pb1A I2A 3.18(10) . ?
C1B N2B 1.4(5) . ?
C1B H1BD 1(2) . ?
C1B H1BE 1(2) . ?
C1B H1BC 1(2) . ?
N1B N2B 1.4(4) . ?
N1B H1BA 0.8(6) . ?
N1B H1BB 0.9(7) . ?
N2B H2BA 0.9(5) . ?
N2B H2BB 0.9(9) . ?
C1D N2D 1.4(4) . ?
C1D H1DD 1(2) . ?
C1D H1DC 1(2) . ?
C1D H1DE 1(2) . ?
N1D N2D 1.4(5) . ?
N1D H1DB 0.9(4) . ?
N1D H1DA 0.9(4) . ?
N2D H2DA 0.9(4) . ?
N2D H2DB 1.0(5) . ?
C1A N2A 1.4(5) . ?
C1A H1AD 1.2(16) . ?
C1A H1AE 1(2) . ?
C1A H1AC 0.9(17) . ?
N1A N2A 1.4(7) . ?
N1A H1AA 0.9(5) . ?
N1A H1AB 0.9(5) . ?
N2A H2AA 1.0(5) . ?
N2A H2AB 0.8(6) . ?
C1C N2C 1.5(8) . ?
C1C H1CD 1.0(14) . ?
C1C H1CE 0.8(15) . ?
C1C H1CC 1.0(14) . ?
N1C N2C 1.3(4) . ?
N1C H1CD 0.8(5) . ?
N1C H1CB 0.9(7) . ?
N2C H2CB 0.9(5) . ?
N2C H2CA 0.8(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3B Pb1B I1B 97.3(6) . . ?
I3B Pb1B I1B 75.2(4) 1_455 2_647 ?
I3B Pb1B I1B 82.1(5) . 2_647 ?
I3B Pb1B I1B 105.5(6) 1_455 . ?
I2B Pb1B I1B 85(2) . 2_647 ?
I2B Pb1B I1B 95(2) . . ?
I2B Pb1B I3B 87(2) . . ?
I2B Pb1B I3B 101(2) . 1_455 ?
I4B Pb1B I1B 89(2) . . ?
I4B Pb1B I1B 92(2) . 2_647 ?
I4B Pb1B I3B 87(2) . . ?
I4B Pb1B I3B 84(2) . 1_455 ?
I4B Pb1B I2B 173.2(7) . . ?
I1A Pb1A I3A 83.9(4) . . ?
I1A Pb1A I3A 104.7(4) 2_746 1_455 ?A
I1A Pb1A I3A 92.9(4) 2_746 . ?
I1A Pb1A I3A 78.6(4) . 1_455 ?
I4A Pb1A I3A 87(2) . . ?
I4A Pb1A I3A 94(2) . 1_455 ?
I4A Pb1A I1A 91(2) . . ?
I4A Pb1A I1A 89(2) . 2_746 ?
I2A Pb1A I3A 87(2) . . ?
I2A Pb1A I3A 92(2) . 1_455 ?
I2A Pb1A I1A 88(2) . . ?
I2A Pb1A I1A 91(2) . 2_746 ?
I2A Pb1A I4A 174.4(6) . . ?
H1BD C1B N2B 108 . . ?
H1BE C1B N2B 109.5 . . ?
H1BE C1B H1BD 97 . . ?
H1BC C1B N2B 112 . . ?
H1BC C1B H1BD 98 . . ?
H1BC C1B H1BE 128 . . ?
H1BA N1B N2B 120.0 . . ?
H1BB N1B N2B 117.0 . . ?
H1BB N1B H1BA 123.0 . . ?
N1B N2B C1B 131 . . ?
H2BA N2B C1B 104 . . ?
H2BA N2B N1B 106 . . ?
H2BB N2B C1B 105 . . ?
H2BB N2B N1B 103 . . ?
H2BB N2B H2BA 105.7 . . ?
H1DD C1D N2D 109.5 . . ?
H1DC C1D N2D 108 . . ?
H1DC C1D H1DD 113 . . ?
H1DE C1D N2D 109.5 . . ?
H1DE C1D H1DD 112 . . ?
H1DE C1D H1DC 104 . . ?
H1DB N1D N2D 120.0 . . ?
H1DA N1D N2D 123.0 . . ?
H1DA N1D H1DB 115.0 . . ?
N1D N2D C1D 122 . . ?
H2DA N2D C1D 108 . . ?
H2DA N2D N1D 105 . . ?
H2DB N2D C1D 104 . . ?
H2DB N2D N1D 105 . . ?
H2DB N2D H2DA 114.0 . . ?
H1AD C1A N2A 112 . . ?
H1AE C1A N2A 96 . . ?
H1AE C1A H1AD 125 . . ?
H1AC C1A N2A 106 . . ?
H1AC C1A H1AD 112 . . ?
H1AC C1A H1AE 104 . . ?
H1AA N1A N2A 116 . . ?
H1AB N1A N2A 120.0 . . ?
H1AB N1A H1AA 123 . . ?
N1A N2A C1A 132 . . ?
H2AA N2A C1A 106 . . ?
H2AA N2A N1A 97 . . ?
H2AB N2A C1A 112 . . ?
H2AB N2A N1A 102 . . ?
H2AB N2A H2AA 105 . . ?
H1CD C1C N2C 108 . . ?
H1CE C1C N2C 120 . . ?
H1CE C1C H1CD 119 . . ?
H1CC C1C N2C 104 . . ?
H1CC C1C H1CD 109 . . ?
H1CC C1C H1CE 96 . . ?
H1CD N1C N2C 127 . . ?
H1CB N1C N2C 116 . . ?
H1CB N1C H1CD 117 . . ?
N1C N2C C1C 126 . . ?
H2CB N2C C1C 98 . . ?
H2CB N2C N1C 105 . . ?
H2CA N2C C1C 101 . . ?
H2CA N2C N1C 116 . . ?
H2CA N2C H2CB 109 . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(2)
2 0.49(2)

####################################################################### 
# 
# 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_mhy2pbi4_4_20
_database_code_depnum_ccdc_archive 'CCDC 2298920'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-10-02
# start Validation Reply Form
_vrf_ATOM007_mhy2pbi4_4_20       
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: The structure was refined isotropically.
Structure is not refined anisotropically because of low resolution.
;
_vrf_PLAT027_mhy2pbi4_4_20       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_4_20       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.389 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT415_mhy2pbi4_4_20       
;
PROBLEM: Short Inter D-H..H-X       H1AA     ..H1BD     .       1.70 Ang.  
RESPONSE: It is very difficult to locate hydrogen 
atoms accurately using X-ray data because these atoms 
have low scattering power. In addition, we have bad 
quality measurement and low resolution data.
;
_vrf_PLAT971_mhy2pbi4_4_20       
;
PROBLEM: Check Calcd Resid. Dens.  1.09Ang From I1B             4.00 eA-3  
RESPONSE: The structure is not refined anistropically which results in
large value. Also, low resolution of data.
;
_vrf_PLAT972_mhy2pbi4_4_20       
;
PROBLEM: Check Calcd Resid. Dens.  0.64Ang From I3B            -4.30 eA-3  
RESPONSE: The structure is not refined anistropically which results in
large value. Also, low resolution of data.
;
_vrf_PLAT082_mhy2pbi4_4_20       
;
PROBLEM: High R1 Value ..................................       0.17 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample
;
_vrf_PLAT084_mhy2pbi4_4_20       
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample
;
_vrf_PLAT201_mhy2pbi4_4_20       
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          8 Report
RESPONSE: The structure was refined isotropically.
Structure is not refined anisotropically because of low resolution.
;
_vrf_PLAT780_mhy2pbi4_4_20       
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do !  
RESPONSE: We have bad quality measurement 
and low resolution data but all atoms are connect
;
_vrf_PLAT911_mhy2pbi4_4_20       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        292 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_mhy2pbi4_4_20       
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         24 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(I2 Pb0.5), 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_chemical_absolute_configuration ?
_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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.1302(5)
_cell_length_b                   12.3747(10)
_cell_length_c                   16.73(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.30(3)
_cell_angle_gamma                90
_cell_volume                     1269(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2645
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9950
_cell_measurement_theta_min      3.7360
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.988
_exptl_absorpt_correction_T_max  0.320
_exptl_absorpt_correction_T_min  0.087
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.234
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 17 0 0.0685
0 0 -24 0.0075
-10 3 0 0.1092
-1 17 0 0.0540
1 -17 1 0.0758
0 0 24 0.0075
9 0 0 0.0761

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.015
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.396     0.454
         range of gasket transmission (min-max)           0.312     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 213.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.389
_diffrn_reflns_Laue_measured_fraction_max 0.266
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6862
_diffrn_reflns_point_group_measured_fraction_full 0.385
_diffrn_reflns_point_group_measured_fraction_max 0.256
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.353
_diffrn_reflns_theta_min         3.293
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.389
_diffrn_measured_fraction_theta_max 0.266
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00   0.00   0.75    6.00    --    0.16   0.00-150.00   40
  2  ω    -50.00 -20.75   0.75    6.00    --    0.16  77.00 150.00   39
  3  ω    -53.00 -26.00   0.75    6.00    --    0.16  38.00   0.00   36
  4  ω    -43.25  19.00   0.75   22.50    --  -30.24  39.00 -12.00   83
  5  ω    -43.25 -11.00   0.75   22.50    --  -30.24  19.00   0.00   43
  6  ω    -88.25 -26.00   0.75   22.50    --  -30.24 135.00 123.00   83
  7  ω    -26.25  36.00   0.75   22.50    --  -30.24 -13.00   3.00   83
  8  ω      0.00  31.50   0.75   22.50    --  -30.24 -97.00-143.00   42
  9  ω     23.00  47.00   0.75   22.50    --  -30.24-125.00-120.00   32
 10  ω    -56.00 -20.75   0.75   22.50    --  -30.24  77.00 150.00   47
 11  ω    -48.25  14.00   0.75   22.50    --  -30.24  53.00 162.00   83
 12  ω      6.00  41.25   0.75   22.50    --   30.56 -57.00  30.00   47
 13  ω    -31.00  -4.75   0.75   22.50    --   30.56  97.00 -35.00   35
 14  ω     36.50  89.00   0.75   22.50    --   30.56-135.00  57.00   70
 15  ω    -23.00  15.25   0.75   22.50    --   30.56  53.00 162.00   51
 16  ω    -34.25  19.00   0.75   22.50    --   30.56  39.00 -12.00   71
 17  ω    -16.00   8.00   0.75   22.50    --   30.56  67.00 157.00   32
 18  ω      4.00  62.50   0.75    6.00    --    0.16 -99.00-150.00   78
 19  ω    -52.00 -25.75   0.75    6.00    --    0.16  38.00-150.00   35
 20  ω     -5.25  21.00   0.75   22.50    --  -30.24 -77.00  30.00   35
 21  ω    -15.00  23.25   0.75   22.50    --  -30.24 -53.00-162.00   51
 22  ω    -26.25  36.00   0.75   22.50    --  -30.24 -13.00-176.00   83
 23  ω    -56.00 -20.75   0.75   22.50    --  -30.24  77.00 -30.00   47
 24  ω      8.00  41.00   0.75   22.50    --  -30.24-114.00  45.00   44
 25  ω    -15.00  23.25   0.75   22.50    --  -30.24 -53.00  17.00   51
 26  ω    -30.00   0.00   0.75   22.50    --   30.56   0.00  30.00   40
 27  ω    -40.00 -13.00   0.75   22.50    --   30.56 114.00 -45.00   36
 28  ω     21.00  56.25   0.75   22.50    --   30.56 -77.00  30.00   47
 29  ω    -30.00   0.00   0.75   22.50    --   30.56   0.00-150.00   40
 30  ω     21.00  50.25   0.75    6.00    --    0.16 -77.00  30.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.381
_reflns_Friedel_fraction_max     0.245
_reflns_number_gt                1238
_reflns_number_total             1327
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         3.916
_refine_diff_density_min         -4.037
_refine_diff_density_rms         0.880
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.54(12)
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1327
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1849
_refine_ls_R_factor_gt           0.1730
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+2045.6992P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3591
_refine_ls_wR_factor_ref         0.3691
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.46(12)
 0.54(12)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Uiso: Pb1A(0.02) I1A(0.02) I3A(0.02) Pb1B(0.02) I1B(0.02) I3B(0.02)
 N2A(0.02) N1A(0.02) N1B(0.02) N2B(0.02) C1A(0.02) C1B(0.02) N1C(0.02)
 N2C(0.02) C1C(0.02) N2D(0.02) N1D(0.02) C1D(0.02)
4.a Free rotating group:
 N2A(N1A,N1B,N2B,C1A,C1B,N1C,N2C,C1C,N2D,N1D,C1D)
4.b Secondary CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), N2B(H2BA,H2BB), N2C(H2CA,H2CB), N2D(H2DA,H2DB)
4.c X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), N1B(H1BA,H1BB), N1C(H1CA,H1CB), N1D(H1DA,H1DB)
4.d Idealised Me refined as rotating group:
 C1A(H1AC,H1AD,H1AE), C1B(H1BC,H1BD,H1BE), C1C(H1CC,H1CD,H1CE), C1D(H1DC,H1DD,
 H1DE)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Pb1A Pb 0.5145(15) 0.0955(7) 0.0049(19) 0.020 Uiso 1 1 d . U . . .
I1A I 0.454(2) 0.3441(13) 0.009(3) 0.020 Uiso 1 1 d . U . . .
I2A I 0.505(3) 0.0680(15) 0.181(4) 0.036(5) Uiso 1 1 d . . . . .
I3A I 1.025(2) 0.0489(13) 0.012(3) 0.020 Uiso 1 1 d . U . . .
I4A I 0.448(2) 0.1056(13) -0.180(3) 0.023(4) Uiso 1 1 d . . . . .
Pb1B Pb 0.0205(15) 0.1685(7) 0.494(2) 0.020 Uiso 1 1 d . U . . .
I1B I 0.045(2) 0.4184(14) 0.513(3) 0.020 Uiso 1 1 d . U . . .
I2B I -0.045(3) 0.1571(15) 0.677(3) 0.034(4) Uiso 1 1 d . . . . .
I3B I 0.533(2) 0.2192(13) 0.490(3) 0.020 Uiso 1 1 d . U . . .
I4B I 0.015(2) 0.1888(12) 0.317(3) 0.022(4) Uiso 1 1 d . . . . .
N2A N 0.884(14) 0.345(7) 0.209(11) 0.020 Uiso 1 1 d G U . . .
H2AA H 0.823366 0.304917 0.246909 0.024 Uiso 1 1 calc R U . . .
H2AB H 0.775536 0.371070 0.179047 0.024 Uiso 1 1 calc R U . . .
N1A N 0.991(13) 0.439(7) 0.249(11) 0.020 Uiso 1 1 d G U . . .
H1AA H 1.127919 0.450320 0.242467 0.024 Uiso 1 1 calc R U . . .
H1AB H 0.915368 0.481181 0.278666 0.024 Uiso 1 1 calc R U . . .
N1B N 0.633(9) 0.417(5) 0.418(11) 0.020 Uiso 1 1 d G U . . .
H1BA H 0.711352 0.374722 0.389600 0.024 Uiso 1 1 calc R U . . .
H1BB H 0.683974 0.443010 0.462166 0.024 Uiso 1 1 calc R U . . .
N2B N 0.423(10) 0.445(6) 0.393(11) 0.020 Uiso 1 1 d G U . . .
H2BA H 0.416148 0.516683 0.388346 0.024 Uiso 1 1 calc R U . . .
H2BB H 0.329619 0.425559 0.430667 0.024 Uiso 1 1 calc R U . . .
C1A C 1.008(18) 0.272(8) 0.159(11) 0.020 Uiso 1 1 d G U . . .
H1AC H 0.972923 0.198944 0.171750 0.030 Uiso 1 1 calc R U . . .
H1AD H 1.161281 0.284370 0.167164 0.030 Uiso 1 1 calc R U . . .
H1AE H 0.972764 0.285733 0.103501 0.030 Uiso 1 1 calc R U . . .
C1B C 0.348(11) 0.395(9) 0.314(11) 0.020 Uiso 1 1 d G U . . .
H1BC H 0.412495 0.325116 0.308082 0.030 Uiso 1 1 calc R U . . .
H1BD H 0.393308 0.440822 0.270550 0.030 Uiso 1 1 calc R U . . .
H1BE H 0.192339 0.389061 0.313653 0.030 Uiso 1 1 calc R U . . .
N1C N 0.581(13) 0.496(6) 0.603(11) 0.020 Uiso 1 1 d G U . . .
H1CA H 0.466826 0.504681 0.573868 0.024 Uiso 1 1 calc R U . . .
H1CB H 0.686599 0.541399 0.600838 0.024 Uiso 1 1 calc R U . . .
N2C N 0.595(10) 0.401(7) 0.659(11) 0.020 Uiso 1 1 d G U . . .
H2CA H 0.714064 0.363555 0.646180 0.024 Uiso 1 1 calc R U . . .
H2CB H 0.615338 0.426430 0.708125 0.024 Uiso 1 1 calc R U . . .
C1C C 0.410(10) 0.326(5) 0.660(11) 0.020 Uiso 1 1 d G U . . .
H1CC H 0.426501 0.273145 0.619004 0.030 Uiso 1 1 calc R U . . .
H1CD H 0.276879 0.365465 0.652053 0.030 Uiso 1 1 calc R U . . .
H1CE H 0.405229 0.290549 0.711435 0.030 Uiso 1 1 calc R U . . .
N2D N 0.105(14) 0.319(7) 0.858(11) 0.020 Uiso 1 1 d G U . . .
H2DA H 0.212858 0.291092 0.829127 0.024 Uiso 1 1 calc R U . . .
H2DB H 0.165850 0.356740 0.897440 0.024 Uiso 1 1 calc R U . . .
N1D N -0.019(17) 0.228(8) 0.894(11) 0.020 Uiso 1 1 d G U . . .
H1DA H -0.156385 0.221622 0.884420 0.024 Uiso 1 1 calc R U . . .
H1DB H 0.046621 0.182320 0.924166 0.024 Uiso 1 1 calc R U . . .
C1D C -0.018(12) 0.396(7) 0.806(11) 0.020 Uiso 1 1 d G U . . .
H1DC H -0.021508 0.465889 0.830811 0.030 Uiso 1 1 calc R U . . .
H1DD H -0.164570 0.370269 0.798441 0.030 Uiso 1 1 calc R U . . .
H1DE H 0.052396 0.401469 0.754961 0.030 Uiso 1 1 calc R U . . .

_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
Pb1A I1A 3.126(19) 2_645 ?
Pb1A I1A 3.099(19) . ?
Pb1A I2A 2.97(6) . ?
Pb1A I3A 3.059(16) 1_455 ?
Pb1A I3A 3.184(17) . ?
Pb1A I4A 3.12(5) . ?
Pb1B I1B 3.11(2) . ?
Pb1B I1B 3.122(19) 2_546 ?
Pb1B I2B 3.10(6) . ?
Pb1B I3B 3.207(16) . ?
Pb1B I3B 3.053(17) 1_455 ?
Pb1B I4B 2.98(5) . ?
N2A H2AA 0.8900 . ?
N2A H2AB 0.8900 . ?
N2A N1A 1.4909 . ?
N2A C1A 1.4486 . ?
N1A H1AA 0.8600 . ?
N1A H1AB 0.8600 . ?
N1B H1BA 0.8600 . ?
N1B H1BB 0.8600 . ?
N1B N2B 1.3944 . ?
N2B H2BA 0.8900 . ?
N2B H2BB 0.8900 . ?
N2B C1B 1.5(2) . ?
C1A H1AC 0.95 . ?
C1A H1AD 0.96 . ?
C1A H1AE 0.97 . ?
C1B H1BC 0.96 . ?
C1B H1BD 0.96 . ?
C1B H1BE 0.96 . ?
N1C H1CA 0.8600 . ?
N1C H1CB 0.8600 . ?
N1C N2C 1.51(18) . ?
N2C H2CA 0.8900 . ?
N2C H2CB 0.8900 . ?
N2C C1C 1.4686 . ?
C1C H1CC 0.95 . ?
C1C H1CD 0.9620 . ?
C1C H1CE 0.9620 . ?
N2D H2DA 0.8900 . ?
N2D H2DB 0.8900 . ?
N2D N1D 1.4860(12) . ?
N2D C1D 1.4923 . ?
N1D H1DA 0.8600 . ?
N1D H1DB 0.8600 . ?
C1D H1DC 0.96 . ?
C1D H1DD 0.96 . ?
C1D H1DE 0.96 . ?

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
I1A Pb1A I1A 175.5(9) . 2_645 ?
I1A Pb1A I3A 107.2(5) . . ?
I1A Pb1A I3A 76.3(4) 2_645 . ?
I1A Pb1A I4A 88.2(11) . . ?
I2A Pb1A I1A 95.0(11) . . ?
I2A Pb1A I1A 87.9(12) . 2_645 ?
I2A Pb1A I3A 88.0(11) . . ?
I2A Pb1A I3A 85.0(11) . 1_455 ?
I2A Pb1A I4A 170.3(6) . . ?
I3A Pb1A I1A 82.8(5) 1_455 2_645 ?
I3A Pb1A I1A 94.0(5) 1_455 . ?
I3A Pb1A I3A 158.2(8) 1_455 . ?
I3A Pb1A I4A 85.7(11) 1_455 . ?
I4A Pb1A I1A 88.4(11) . 2_645 ?
I4A Pb1A I3A 99.8(11) . . ?
Pb1A I1A Pb1A 168.2(9) . 2_655 ?
Pb1A I3A Pb1A 158.2(8) 1_655 . ?
I1B Pb1B I1B 174.0(8) . 2_546 ?
I1B Pb1B I3B 76.2(5) . . ?
I1B Pb1B I3B 108.6(5) 2_546 . ?
I2B Pb1B I1B 88.5(11) . 2_546 ?
I2B Pb1B I1B 87.1(12) . . ?
I2B Pb1B I3B 99.4(12) . . ?
I3B Pb1B I1B 81.1(5) 1_455 . ?
I3B Pb1B I1B 94.4(5) 1_455 2_546 ?
I3B Pb1B I2B 84.4(12) 1_455 . ?
I3B Pb1B I3B 156.7(7) 1_455 . ?
I4B Pb1B I1B 91.1(11) . . ?
I4B Pb1B I1B 92.6(11) . 2_546 ?
I4B Pb1B I2B 171.7(5) . . ?
I4B Pb1B I3B 87.3(12) . 1_455 ?
I4B Pb1B I3B 88.1(11) . . ?
Pb1B I1B Pb1B 167.1(11) . 2_556 ?
Pb1B I3B Pb1B 156.7(7) 1_655 . ?
H2AA N2A H2AB 106.8 . . ?
N1A N2A H2AA 107.1 . . ?
N1A N2A H2AB 106.9 . . ?
C1A N2A H2AA 107.2 . . ?
C1A N2A H2AB 107.2 . . ?
C1A N2A N1A 120.9 . . ?
N2A N1A H1AA 120.0 . . ?
N2A N1A H1AB 120.0 . . ?
H1AA N1A H1AB 120.0 . . ?
H1BA N1B H1BB 120.0 . . ?
N2B N1B H1BA 120.0 . . ?
N2B N1B H1BB 120.0 . . ?
N1B N2B H2BA 108.3 . . ?
N1B N2B H2BB 108.3 . . ?
N1B N2B C1B 115.9 . . ?
H2BA N2B H2BB 107.4 . . ?
C1B N2B H2BA 108.3 . . ?
C1B N2B H2BB 108.3 . . ?
N2A C1A H1AC 110 . . ?
N2A C1A H1AD 110 . . ?
N2A C1A H1AE 109 . . ?
H1AC C1A H1AD 110 . . ?
H1AC C1A H1AE 109 . . ?
H1AD C1A H1AE 109 . . ?
N2B C1B H1BC 109 . . ?
N2B C1B H1BD 109 . . ?
N2B C1B H1BE 109 . . ?
H1BC C1B H1BD 109.0 . . ?
H1BC C1B H1BE 110.0 . . ?
H1BD C1B H1BE 109.0 . . ?
H1CA N1C H1CB 120.0 . . ?
N2C N1C H1CA 120.0 . . ?
N2C N1C H1CB 120.0 . . ?
N1C N2C H2CA 107.9 . . ?
N1C N2C H2CB 107.9 . . ?
H2CA N2C H2CB 107.2 . . ?
C1C N2C N1C 117.6 . . ?
C1C N2C H2CA 107.9 . . ?
C1C N2C H2CB 109 . . ?
N2C C1C H1CC 109.7 . . ?
N2C C1C H1CD 109.7 . . ?
N2C C1C H1CE 109.7 . . ?
H1CC C1C H1CD 109.3 . . ?
H1CC C1C H1CE 109.3 . . ?
H1CD C1C H1CE 109.3 . . ?
H2DA N2D H2DB 107.2 . . ?
N1D N2D H2DA 107.9 . . ?
N1D N2D H2DB 107.9 . . ?
N1D N2D C1D 117.44(10) . . ?
C1D N2D H2DA 107.9 . . ?
C1D N2D H2DB 107.9 . . ?
N2D N1D H1DA 120.0 . . ?
N2D N1D H1DB 120.0 . . ?
H1DA N1D H1DB 120.0 . . ?
N2D C1D H1DC 110 . . ?
N2D C1D H1DD 110 . . ?
N2D C1D H1DE 110 . . ?
H1DC C1D H1DD 109 . . ?
H1DC C1D H1DE 109 . . ?
H1DD C1D H1DE 109 . . ?

_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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.46(12)
2 0.54(12)
# end
####################################################################### 
# 
# 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_mhy2pbi4_1_30
_database_code_depnum_ccdc_archive 'CCDC 2298913'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University, Poznan, Poland
Poland
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_audit_creation_date             2023-09-27
# start Validation Reply Form
_vrf_RINTA01_mhy2pbi4_1_30       
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT027_mhy2pbi4_1_30       
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_mhy2pbi4_1_30       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.409 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT031_mhy2pbi4_1_30       
;
PROBLEM: Refined Extinction Parameter Within Range of ...      0.714 Sigma 
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT020_mhy2pbi4_1_30       
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.194 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT090_mhy2pbi4_1_30       
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.05 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT911_mhy2pbi4_1_30       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         69 Report
RESPONSE: These reflections were probably affected by 
unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_mhy2pbi4_1_30       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'methylhydrazinium tetraiodoplumbate'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 I4 N4 Pb'
_chemical_formula_weight         808.96
_chemical_absolute_configuration ?
_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           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   17.8170(11)
_cell_length_b                   6.2811(10)
_cell_length_c                   6.22(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     696(7)
_cell_formula_units_Z            2
_cell_measurement_pressure       1300000
_cell_measurement_reflns_used    1060
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2630
_cell_measurement_theta_min      3.2010
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.969
_exptl_absorpt_correction_T_max  0.282
_exptl_absorpt_correction_T_min  0.231
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.862
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 2 1 0.0658
-9 -2 -1 0.0649
-3 -3 8 0.0943
8 -3 4 0.0739
0 -25 -1 0.0118
0 25 1 0.0118
3 5 -8 0.0596
-5 2 -7 0.0661

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.03
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.401     0.454
         range of gasket transmission (min-max)           1.000     1.000
         range of P media transmission (min-max)          0.991     0.992

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 100.0 microns, radius = 200.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Absorption coeff of pressure medium =   0.10 mm-1
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1945
_diffrn_reflns_av_unetI/netI     0.1161
_diffrn_reflns_Laue_measured_fraction_full 0.409
_diffrn_reflns_Laue_measured_fraction_max 0.276
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1298
_diffrn_reflns_point_group_measured_fraction_full 0.434
_diffrn_reflns_point_group_measured_fraction_max 0.284
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.802
_diffrn_reflns_theta_min         3.439
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.409
_diffrn_measured_fraction_theta_max 0.276
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   15.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   15.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   15.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   15.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   15.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   15.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   15.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   15.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   15.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   15.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   15.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   15.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   15.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   15.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   15.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   15.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.469
_reflns_Friedel_fraction_max     0.294
_reflns_number_gt                276
_reflns_number_total             363
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.256
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.0005(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         363
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0720
_refine_ls_restrained_S_all      0.952
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0834P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1736
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-N1
 1.3 with sigma of 0.08
 N2-C1
 1.45 with sigma of 0.08
 H1A_$1-H2A
 2.2 with sigma of 0.02
3. Rigid bond restraints
 Pb1, I3, I1, I2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Pb1 \\sim I3 \\sim I1 \\sim I2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(I3) \\sim Ueq, Uanis(I1) \\sim Ueq, Uanis(I2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N1, N2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I1, Pb1, I2, I3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.500000 0.0902(3) 0.26495(2) 0.055(7) Uani 1 2 d S TU P . .
I3 I 0.500000 0.5923(6) 0.254(3) 0.068(5) Uani 1 2 d S TU P . .
I1 I 0.500000 0.1380(7) 0.768(3) 0.060(5) Uani 1 2 d S TU P . .
I2 I 0.6689(9) 0.0917(6) 0.261(2) 0.084(6) Uani 1 1 d . U . . .
N1 N 0.289(5) 0.379(8) 0.709(12) 0.08(2) Uani 1 1 d D U . . .
H1A H 0.259216 0.404257 0.815437 0.097 Uiso 1 1 calc R U . . .
H1B H 0.281692 0.268838 0.629556 0.097 Uiso 1 1 calc R U . . .
C1 C 0.383(9) 0.707(11) 0.74(3) 0.10(3) Uani 1 1 d D U . . .
H1C H 0.366185 0.742967 0.881795 0.143 Uiso 1 1 calc R U . . .
H1D H 0.370691 0.820338 0.642359 0.143 Uiso 1 1 calc R U . . .
H1E H 0.436085 0.684482 0.740473 0.143 Uiso 1 1 calc R U . . .
N2 N 0.345(4) 0.509(8) 0.668(10) 0.073(17) Uani 1 1 d D U . . .
H2A H 0.336264 0.538127 0.530324 0.087 Uiso 1 1 calc DR U . . .
H2B H 0.383015 0.417821 0.666265 0.087 Uiso 1 1 calc R U . . .


_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 I3 3.154(3) . ?
Pb1 I3 3.129(3) 1_545 ?
Pb1 I1 3.14(4) . ?
Pb1 I1 3.10(4) 1_554 ?
Pb1 I2 3.010(16) 4_655 ?
Pb1 I2 3.010(16) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 N2 1.31(10) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 N2 1.49(9) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?

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
I3 Pb1 I3 177.6(6) 1_545 . ?
I3 Pb1 I1 96.7(3) 1_545 . ?
I1 Pb1 I3 94.3(3) 1_554 1_545 ?
I1 Pb1 I3 83.2(3) 1_554 . ?
I1 Pb1 I3 85.7(3) . . ?
I1 Pb1 I1 169.0(2) 1_554 . ?
I2 Pb1 I3 89.82(7) . . ?
I2 Pb1 I3 90.16(7) . 1_545 ?
I2 Pb1 I3 89.82(7) 4_655 . ?
I2 Pb1 I3 90.16(7) 4_655 1_545 ?
I2 Pb1 I1 90.5(3) 4_655 . ?
I2 Pb1 I1 89.5(3) . 1_554 ?
I2 Pb1 I1 89.5(3) 4_655 1_554 ?
I2 Pb1 I1 90.5(3) . . ?
I2 Pb1 I2 178.9(5) 4_655 . ?
Pb1 I3 Pb1 177.6(6) 1_565 . ?
Pb1 I1 Pb1 169.0(2) 1_556 . ?
H1A N1 H1B 120.0 . . ?
N2 N1 H1A 120.0 . . ?
N2 N1 H1B 120.0 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N2 C1 H1C 109.5 . . ?
N2 C1 H1D 109.5 . . ?
N2 C1 H1E 109.5 . . ?
N1 N2 C1 144(10) . . ?
N1 N2 H2A 100.9 . . ?
N1 N2 H2B 100.9 . . ?
C1 N2 H2A 100.9 . . ?
C1 N2 H2B 100.9 . . ?
H2A N2 H2B 104.4 . . ?

_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
;
