# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_MHy2PbBr3_7I0_3_380K
_database_code_depnum_ccdc_archive 'CCDC 2189681'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2024-01-08 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_audit_creation_date             2024-01-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3.7 I0.3 Pb, C2 N4'
_chemical_formula_sum            'C2 Br3.70 I0.30 N4 Pb'
_chemical_formula_weight         620.99
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 n m m'
_space_group_name_Hall           '-P 2c 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z'
'-x, y-1/2, z-1/2'

_cell_length_a                   6.097(3)
_cell_length_b                   18.194(3)
_cell_length_c                   6.063(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     672.5(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    587
_cell_measurement_temperature    380.00(10)
_cell_measurement_theta_max      23.9020
_cell_measurement_theta_min      3.3580
_shelx_estimated_absorpt_T_max   0.583
_shelx_estimated_absorpt_T_min   0.113
_exptl_absorpt_coefficient_mu    24.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             535
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            14587
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.665
_diffrn_reflns_theta_min         3.341
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      380.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     32.00  62.00   1.00   15.00    --   13.31  57.00-180.00   30
  2  ω    -24.00  47.00   1.00   15.00    --   13.31 -99.00  60.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0100519262
_diffrn_orient_matrix_UB_12      -0.0345121174
_diffrn_orient_matrix_UB_13      0.0538949151
_diffrn_orient_matrix_UB_21      0.0281491860
_diffrn_orient_matrix_UB_22      0.0181982541
_diffrn_orient_matrix_UB_23      0.0996249682
_diffrn_orient_matrix_UB_31      -0.1136450041
_diffrn_orient_matrix_UB_32      0.0014867990
_diffrn_orient_matrix_UB_33      0.0292264617
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                702
_reflns_number_total             735
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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    ?
_refine_diff_density_max         1.620
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         735
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0343
_refine_ls_restrained_S_all      1.242
_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)+(0.0509P)²+2.3869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0966
_refine_special_details          'disordered organic cations'
_olex2_refinement_description    
;
1. Shared sites
{Br1, I1}
{Br3, I3}
{Br2, I2}
2. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(I1)
Uanis(Br2) = Uanis(I2)
Uanis(Br3) = Uanis(I3)
3. Others
 Fixed Sof: Br1(0.23125) Br3(0.4625) Br2(0.23125) I1(0.01875) I3(0.0375)
 I2(0.01875) N1(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.57881(9) 0.250000 0.250000 0.0412(2) Uani 1 4 d S T P . .
Br1 Br 0.6231(4) 0.250000 0.750000 0.0676(6) Uani 0.925 4 d S T P . .
Br3 Br 0.5917(3) 0.41473(8) 0.250000 0.0816(5) Uani 0.925 2 d S T P . .
Br2 Br 0.0691(3) 0.250000 0.250000 0.0930(9) Uani 0.925 4 d S T P . .
I1 I 0.6231(4) 0.250000 0.750000 0.0676(6) Uani 0.075 4 d S T P . .
I3 I 0.5917(3) 0.41473(8) 0.250000 0.0816(5) Uani 0.075 2 d S T P . .
I2 I 0.0691(3) 0.250000 0.250000 0.0930(9) Uani 0.075 4 d S T P . .
N2 N 0.127(4) 0.5259(18) 0.250000 0.154(10) Uani 1 2 d S T P . .
C1 C -0.160(4) 0.6146(12) 0.250000 0.103(7) Uani 1 2 d S T P . .
N1 N 0.012(5) 0.5854(14) 0.326(4) 0.115(9) Uani 0.5 1 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
Pb1 Br1 3.043(2) 1_554 ?
Pb1 Br1 3.043(2) . ?
Pb1 Br3 2.9982(16) . ?
Pb1 Br3 2.9983(16) 7_565 ?
Pb1 Br2 2.989(2) 1_655 ?
Pb1 Br2 3.107(2) . ?
N2 N1 1.37(3) 6_556 ?
N2 N1 1.37(3) . ?
C1 N1 1.26(3) . ?
C1 N1 1.26(3) 6_556 ?

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
Br1 Pb1 Br1 169.82(8) . 1_554 ?
Br1 Pb1 Br2 95.09(4) . . ?
Br1 Pb1 Br2 95.09(4) 1_554 . ?
Br3 Pb1 Br1 89.867(3) . 1_554 ?
Br3 Pb1 Br1 89.867(3) 7_565 . ?
Br3 Pb1 Br1 89.867(4) 7_565 1_554 ?
Br3 Pb1 Br1 89.867(3) . . ?
Br3 Pb1 Br3 177.01(7) . 7_565 ?
Br3 Pb1 Br2 91.50(3) . . ?
Br3 Pb1 Br2 91.50(3) 7_565 . ?
Br2 Pb1 Br1 84.91(4) 1_655 1_554 ?
Br2 Pb1 Br1 84.91(4) 1_655 . ?
Br2 Pb1 Br3 88.50(3) 1_655 7_565 ?
Br2 Pb1 Br3 88.50(3) 1_655 . ?
Br2 Pb1 Br2 180.0 1_655 . ?
Pb1 Br1 Pb1 169.82(8) 1_556 . ?
Pb1 Br2 Pb1 180.0 1_455 . ?
N1 N2 N1 39(2) . 6_556 ?
N1 C1 N1 43(3) . 6_556 ?
C1 N1 N2 129(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N2 N1 C1 37(4) 6_556 . . . ?
N1 C1 N1 N2 -37(4) 6_556 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.005
_oxdiff_exptl_absorpt_empirical_full_min 0.486
####################################################################### 
# 
# 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_MHy2PbBr1_5I2_5_350K
_database_code_depnum_ccdc_archive 'CCDC 2307123'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_audit_creation_date             2023-11-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I3 Pb1, 0.036(C28.038 N56.076)'
_chemical_formula_sum            'C I3 N2 Pb'
_chemical_formula_weight         627.92
_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      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   6.270(3)
_cell_length_b                   6.270(3)
_cell_length_c                   6.270(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     246.4(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    148
_cell_measurement_temperature    350.00(10)
_cell_measurement_theta_max      19.7790
_cell_measurement_theta_min      4.5500
_shelx_estimated_absorpt_T_max   0.504
_shelx_estimated_absorpt_T_min   0.058
_exptl_absorpt_coefficient_mu    26.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41835
_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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    4.231
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             261
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            551
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.276
_diffrn_reflns_theta_min         3.249
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      350.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00   7.00   1.00   20.00    --  -14.72 -37.00  60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1088934000
_diffrn_orient_matrix_UB_12      -0.0217690000
_diffrn_orient_matrix_UB_13      -0.0228262000
_diffrn_orient_matrix_UB_21      -0.0286941000
_diffrn_orient_matrix_UB_22      -0.0354507000
_diffrn_orient_matrix_UB_23      -0.1033344000
_diffrn_orient_matrix_UB_31      0.0126193000
_diffrn_orient_matrix_UB_32      0.1052434000
_diffrn_orient_matrix_UB_33      -0.0393865000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                63
_reflns_number_total             76
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         0.826
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.245
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8
_refine_ls_number_reflns         76
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.079
_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)+(0.0764P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1230
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{N2, C2}
{C1, N1}
2. Uiso/Uaniso restraints and constraints
Uiso(C1) = Uiso(N1)
Uiso(C2) = Uiso(N2)
3. Others
 Fixed Sof: N2(0.01783) N1(0.02383) C2(0.00892) C1(0.01191)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.000000 1.000000 1.000000 0.0732(12) Uani 1 48 d S T P . .
I1 I 1.000000 1.000000 0.500000 0.169(2) Uani 1 16 d S T P . .
N2 N 0.500000 0.35(3) 0.500000 0.08(4) Uiso 0.1426 8 d S . P . .
N1 N 0.407(12) 0.407(12) 0.407(12) 0.09(4) Uiso 0.143 6 d S . P . .
C2 C 0.500000 0.35(3) 0.500000 0.08(4) Uiso 0.0714 8 d S . P . .
C1 C 0.407(12) 0.407(12) 0.407(12) 0.09(4) Uiso 0.0715 6 d S . 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 3.1348(15) 9_565 ?
Pb1 I1 3.1348(15) 1_556 ?
Pb1 I1 3.1348(15) . ?
Pb1 I1 3.1348(15) 5_655 ?
Pb1 I1 3.1348(15) 5 ?
Pb1 I1 3.1348(15) 9 ?
N2 C2 0.0(3) 46_656 ?
N2 C2 0.0(3) 48 ?
N2 C2 1.3(2) 34_565 ?
N2 C2 0.0(3) 28_655 ?
N2 C2 1.3(2) 13_556 ?
N2 C2 0.0(3) 3_656 ?
N2 C2 1.3(2) 36_556 ?
N2 C2 1.3(2) 15_565 ?
N2 C2 0.0(3) 26_556 ?
N2 C2 0.0(3) 21_556 ?
N2 C2 0.0(3) 23_655 ?
N2 C2 1.3(2) 40_566 ?
C1 C1 0.00(15) 48 ?
C1 C1 0.00(15) 5 ?
C1 C1 0.00(15) 9 ?
C1 C1 0.00(15) 38 ?
C1 C1 0.00(15) 43 ?

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 90.0 9_565 . ?
I1 Pb1 I1 180.0 5 5_655 ?
I1 Pb1 I1 90.0 5 9 ?
I1 Pb1 I1 90.0 1_556 5_655 ?
I1 Pb1 I1 90.0 . 9 ?
I1 Pb1 I1 90.0 1_556 9 ?
I1 Pb1 I1 90.0 . 5_655 ?
I1 Pb1 I1 90.0 9_565 1_556 ?
I1 Pb1 I1 90.0 . 5 ?
I1 Pb1 I1 180.0 9_565 9 ?
I1 Pb1 I1 90.0 1_556 5 ?
I1 Pb1 I1 180.0 . 1_556 ?
I1 Pb1 I1 90.0 9_565 5_655 ?
I1 Pb1 I1 90.0 5_655 9 ?
I1 Pb1 I1 90.0 9_565 5 ?
Pb1 I1 Pb1 180.0 1_554 . ?
C2 N2 C2 0(10) 21_556 36_556 ?
C2 N2 C2 0(10) 3_656 13_556 ?
C2 N2 C2 0(10) 3_656 34_565 ?
C2 N2 C2 0(10) 13_556 36_556 ?
C2 N2 C2 0(10) 28_655 34_565 ?
C2 N2 C2 0(10) 23_655 40_566 ?
C2 N2 C2 0(10) 46_656 36_556 ?
C2 N2 C2 0(10) 28_655 15_565 ?
C2 N2 C2 0(10) 15_565 13_556 ?
C2 N2 C2 0(10) 26_556 40_566 ?
C2 N2 C2 0(10) 23_655 34_565 ?
C2 N2 C2 0(10) 48 15_565 ?
C2 N2 C2 0(10) 15_565 34_565 ?
C2 N2 C2 0(10) 28_655 13_556 ?
C2 N2 C2 0(10) 26_556 36_556 ?
C2 N2 C2 0(10) 23_655 13_556 ?
C2 N2 C2 0(10) 48 36_556 ?
C2 N2 C2 0(10) 23_655 36_556 ?
C2 N2 C2 0(10) 46_656 40_566 ?
C2 N2 C2 0(10) 21_556 13_556 ?
C2 N2 C2 0(10) 46_656 15_565 ?
C2 N2 C2 0(10) 21_556 34_565 ?
C2 N2 C2 0(10) 26_556 15_565 ?
C2 N2 C2 0(10) 15_565 36_556 ?
C2 N2 C2 0(10) 28_655 23_655 ?
C2 N2 C2 0(10) 46_656 34_565 ?
C2 N2 C2 0(10) 26_556 23_655 ?
C2 N2 C2 0(10) 28_655 40_566 ?
C2 N2 C2 0(10) 46_656 21_556 ?
C2 N2 C2 0(10) 13_556 34_565 ?
C2 N2 C2 0(10) 28_655 21_556 ?
C2 N2 C2 0(10) 48 40_566 ?
C2 N2 C2 0(10) 26_556 21_556 ?
C2 N2 C2 0(10) 48 13_556 ?
C2 N2 C2 0(10) 23_655 21_556 ?
C2 N2 C2 0(10) 36_556 40_566 ?
C2 N2 C2 0(10) 46_656 3_656 ?
C2 N2 C2 0(10) 26_556 34_565 ?
C2 N2 C2 0(10) 28_655 3_656 ?
C2 N2 C2 0(10) 3_656 15_565 ?
C2 N2 C2 0(10) 26_556 3_656 ?
C2 N2 C2 0(10) 48 34_565 ?
C2 N2 C2 0(10) 23_655 3_656 ?
C2 N2 C2 0(10) 46_656 13_556 ?
C2 N2 C2 0(10) 21_556 3_656 ?
C2 N2 C2 0(10) 28_655 36_556 ?
C2 N2 C2 0(10) 46_656 48 ?
C2 N2 C2 0(10) 26_556 13_556 ?
C2 N2 C2 0(10) 28_655 48 ?
C2 N2 C2 0(10) 3_656 36_556 ?
C2 N2 C2 0(10) 26_556 48 ?
C2 N2 C2 0(10) 46_656 28_655 ?
C2 N2 C2 0(10) 23_655 48 ?
C2 N2 C2 0(10) 34_565 36_556 ?
C2 N2 C2 0(10) 21_556 48 ?
C2 N2 C2 0(10) 46_656 26_556 ?
C2 N2 C2 0(10) 3_656 40_566 ?
C2 N2 C2 0(10) 21_556 40_566 ?
C2 N2 C2 0(10) 15_565 40_566 ?
C2 N2 C2 0(10) 28_655 26_556 ?
C2 N2 C2 0(10) 34_565 40_566 ?
C2 N2 C2 0(10) 13_556 40_566 ?
C2 N2 C2 0(10) 23_655 15_565 ?
C2 N2 C2 0(10) 46_656 23_655 ?
C2 N2 C2 0(10) 21_556 15_565 ?
C2 N2 C2 0(10) 3_656 48 ?
N1 C1 N1 0(10) 48 9 ?
N1 C1 N1 0(10) 9 43 ?
N1 C1 N1 0(10) 9 38 ?
N1 C1 N1 0(10) 5 38 ?
N1 C1 N1 0(10) 9 5 ?
N1 C1 N1 0(10) 48 38 ?
N1 C1 N1 0(10) 48 43 ?
N1 C1 N1 0(10) 48 5 ?
N1 C1 N1 0(10) 5 43 ?
N1 C1 N1 0(10) 43 38 ?
N1 C1 C2 0(10) 9 3_656 ?
N1 C1 C2 0(10) 38 3_656 ?
N1 C1 C2 0(10) 5 48 ?
N1 C1 C2 0(10) 43 48 ?
N1 C1 C2 0(10) 38 48 ?
N1 C1 C2 0(10) 9 48 ?
N1 C1 C2 0(10) 5 3_656 ?
N1 C1 C2 0(10) 43 3_656 ?
N1 C1 C2 0(10) 48 48 ?
N1 C1 C2 0(10) 48 3_656 ?
N1 C1 C1 0(10) 48 5 ?
N1 C1 C1 0(10) 43 43 ?
N1 C1 C1 0(10) 9 43 ?
N1 C1 C1 0(10) 9 5 ?
N1 C1 C1 0(10) 5 38 ?
N1 C1 C1 0(10) 43 38 ?
N1 C1 C1 0(10) 5 43 ?
N1 C1 C1 0(10) 38 48 ?
N1 C1 C1 0(10) 38 9 ?
N1 C1 C1 0(10) 9 38 ?
N1 C1 C1 0(10) 48 43 ?
N1 C1 C1 0(10) 5 5 ?
N1 C1 C1 0(10) 9 9 ?
N1 C1 C1 0(10) 48 9 ?
N1 C1 C1 0(10) 43 9 ?
N1 C1 C1 0(10) 43 5 ?
N1 C1 C1 0(10) 48 38 ?
N1 C1 C1 0(10) 5 48 ?
N1 C1 C1 0(10) 48 48 ?
N1 C1 C1 0(10) 38 5 ?
N1 C1 C1 0(10) 9 48 ?
N1 C1 C1 0(10) 43 48 ?
N1 C1 C1 0(10) 38 43 ?
N1 C1 C1 0(10) 5 9 ?
N1 C1 C1 0(10) 38 38 ?
C2 C1 C2 0(10) 48 3_656 ?
C1 C1 C2 0(10) 43 48 ?
C1 C1 C2 0(10) 5 48 ?
C1 C1 C2 0(10) 48 48 ?
C1 C1 C2 0(10) 38 3_656 ?
C1 C1 C2 0(10) 5 3_656 ?
C1 C1 C2 0(10) 9 3_656 ?
C1 C1 C2 0(10) 48 3_656 ?
C1 C1 C2 0(10) 43 3_656 ?
C1 C1 C2 0(10) 9 48 ?
C1 C1 C2 0(10) 38 48 ?
C1 C1 C1 0(10) 48 43 ?
C1 C1 C1 0(10) 9 43 ?
C1 C1 C1 0(10) 48 5 ?
C1 C1 C1 0(10) 9 5 ?
C1 C1 C1 0(10) 9 38 ?
C1 C1 C1 0(10) 5 43 ?
C1 C1 C1 0(10) 5 38 ?
C1 C1 C1 0(10) 48 38 ?
C1 C1 C1 0(10) 43 38 ?
C1 C1 C1 0(10) 48 9 ?

_olex2_date_sample_data_collection 2023-03-14
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.761
_oxdiff_exptl_absorpt_empirical_full_min 0.756
####################################################################### 
# 
# 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_MHy2PbBr3_7I0_3_100K
_database_code_depnum_ccdc_archive 'CCDC 2307127'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_audit_creation_date             2023-11-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3.735 I0.265 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 Br3.73 I0.26 N4 Pb'
_chemical_formula_weight         633.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         C2N4PbBr4
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'
Br Br -0.2901 2.4595 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.120(4)
_cell_length_b                   17.609(5)
_cell_length_c                   12.099(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.52(3)
_cell_angle_gamma                90
_cell_volume                     2579.6(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7155
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      29.2280
_cell_measurement_theta_min      3.3330
_shelx_estimated_absorpt_T_max   0.571
_shelx_estimated_absorpt_T_min   0.107
_exptl_absorpt_coefficient_mu    25.247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24035
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.262
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2246
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 4 0.0418
1 0 0 0.0631
-1 0 0 0.0631
0 -1 0 0.0098
0 1 0 0.0164
0 0 -1 0.0604

_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.025
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0001 -0.0004 4.0088 0.1049 0.1873 0.1179
1.0020 0.0004 -0.0003 -0.0029 -0.0128 0.0572
-1.0020 -0.0004 0.0003 0.0029 0.0128 -0.0572
0.0001 -1.0023 -0.0003 -0.0358 0.0186 0.0023
-0.0001 1.0023 0.0003 0.0358 -0.0186 -0.0023
0.0005 0.0002 -1.0023 -0.0270 -0.0500 -0.0152

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8313
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         2.600
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  45.00   1.00   15.00    --   13.31 -37.00 -30.00  111
  2  ω    -78.00 -32.00   1.00   15.00    --   13.31 178.00-150.00   46
  3  ω    -46.00  65.00   1.00   15.00    --  -14.40  37.00-120.00  111
  4  ω    -18.00  32.00   1.00   15.00    --  -14.40-106.00-167.00   50
  5  ω    -47.00  64.00   1.00   15.00    --  -14.40  57.00 -30.00  111
  6  ω    -25.00  30.00   1.00   15.00    --  -14.40 -99.00  60.00   55
  7  ω   -107.00 -35.00   1.00   15.00    --  -14.40-178.00   0.00   72
  8  ω    -25.00   2.00   1.00   15.00    --  -14.40 -99.00 150.00   27
  9  ω    -94.00  17.00   1.00   15.00    --  -14.40 -37.00-120.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0029015000
_diffrn_orient_matrix_UB_12      0.0356858000
_diffrn_orient_matrix_UB_13      0.0268972000
_diffrn_orient_matrix_UB_21      -0.0127714000
_diffrn_orient_matrix_UB_22      -0.0185358000
_diffrn_orient_matrix_UB_23      0.0499014000
_diffrn_orient_matrix_UB_31      0.0570896000
_diffrn_orient_matrix_UB_32      -0.0023411000
_diffrn_orient_matrix_UB_33      0.0151644000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4120
_reflns_number_total             8313
_reflns_special_details          
;
 _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 1.5 (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    ?
_refine_diff_density_max         2.856
_refine_diff_density_min         -2.670
_refine_diff_density_rms         0.419
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         8313
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0476
_refine_ls_restrained_S_all      0.888
_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)+(0.0610P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1263
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.7118(10)
 0.2882(10)
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. Shared sites
{Br1, I1}
{Br5, I5}
{Br2, I2}
{Br3, I3}
{Br6, I6}
{Br4, I4}
{Br8, I8}
{Br7, I7}
4. Restrained distances
 H4D-H1A
 2.1 with sigma of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(I1)
Uanis(Br5) = Uanis(I5)
Uanis(Br2) = Uanis(I2)
Uanis(Br3) = Uanis(I3)
Uanis(Br6) = Uanis(I6)
Uanis(Br4) = Uanis(I4)
Uanis(Br8) = Uanis(I8)
Uanis(Br7) = Uanis(I7)
Uanis(C4) = Uanis(N7) = Uanis(N8)
Uanis(C2) = Uanis(N3) = Uanis(N4)
Uanis(C1) = Uanis(N1) = Uanis(N2)
Uanis(C3) = Uanis(N5) = Uanis(N6)
6. Others
 Fixed Sof: Br1(0.87) Br5(0.87) Br2(0.925) Br3(0.97) Br6(0.925) Br4(0.97)
 Br8(0.97) Br7(0.97) I1(0.13) I5(0.13) I2(0.075) I3(0.03) I6(0.075) I4(0.03)
 I8(0.03) I7(0.03)
7.a Rotating group:
 N6(H6A,H6B), N8(H8A,H8B), N4(H4D,H4E), N2(H2D,H2E)
7.b Secondary CH2 refined with riding coordinates:
 N3(H3D,H3E), N1(H1A,H1B), N5(H5A,H5B), N7(H7A,H7B)
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C1(H1C,H1D,H1E), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.12944(5) 0.25027(6) 0.04349(6) 0.01016(18) Uani 1 1 d . . . . .
Pb2 Pb 0.62569(5) 0.24855(6) 0.04139(6) 0.01129(19) Uani 1 1 d . . . . .
Br1 Br 0.37257(13) 0.24704(13) 0.06038(14) 0.0173(4) Uani 0.87 1 d . . P . .
Br5 Br 0.87238(13) 0.25383(12) 0.07821(14) 0.0155(4) Uani 0.87 1 d . . P . .
Br2 Br 0.13339(14) 0.26326(12) 0.28679(14) 0.0152(5) Uani 0.925 1 d . . P . .
Br3 Br 0.12983(13) 0.42134(13) 0.04812(14) 0.0134(5) Uani 0.97 1 d . . P . .
Br6 Br 0.62734(14) 0.22293(12) 0.29374(15) 0.0174(5) Uani 0.925 1 d . . P . .
Br4 Br 0.13253(14) 0.08370(13) 0.05124(15) 0.0173(5) Uani 0.97 1 d . . P . .
Br8 Br 0.63951(14) 0.08471(13) 0.01892(16) 0.0157(5) Uani 0.97 1 d . . P . .
Br7 Br 0.60988(15) 0.42111(13) 0.07388(16) 0.0175(5) Uani 0.97 1 d . . P . .
I1 I 0.37257(13) 0.24704(13) 0.06038(14) 0.0173(4) Uani 0.13 1 d . . P . .
I5 I 0.87238(13) 0.25383(12) 0.07821(14) 0.0155(4) Uani 0.13 1 d . . P . .
I2 I 0.13339(14) 0.26326(12) 0.28679(14) 0.0152(5) Uani 0.075 1 d . . P . .
I3 I 0.12983(13) 0.42134(13) 0.04812(14) 0.0134(5) Uani 0.03 1 d . . P . .
I6 I 0.62734(14) 0.22293(12) 0.29374(15) 0.0174(5) Uani 0.075 1 d . . P . .
I4 I 0.13253(14) 0.08370(13) 0.05124(15) 0.0173(5) Uani 0.03 1 d . . P . .
I8 I 0.63951(14) 0.08471(13) 0.01892(16) 0.0157(5) Uani 0.03 1 d . . P . .
I7 I 0.60988(15) 0.42111(13) 0.07388(16) 0.0175(5) Uani 0.03 1 d . . P . .
N6 N 0.5813(12) 0.5541(10) 0.3179(13) 0.020(2) Uani 1 1 d . . . . .
H6A H 0.562917 0.601380 0.343961 0.023 Uiso 1 1 d R U . . .
H6B H 0.594975 0.522169 0.377838 0.023 Uiso 1 1 d R U . . .
N8 N 0.8737(13) 0.4565(9) 0.1803(12) 0.020(2) Uani 1 1 d . . . . .
H8A H 0.896280 0.458950 0.111121 0.024 Uiso 1 1 d R U . . .
H8B H 0.806980 0.435851 0.180803 0.024 Uiso 1 1 d R U . . .
N4 N 0.3587(12) 0.5073(10) 0.1955(13) 0.027(3) Uani 1 1 d . . . . .
H4D H 0.336911 0.524143 0.126719 0.032 Uiso 1 1 d DR U . . .
H4E H 0.425690 0.527763 0.214970 0.032 Uiso 1 1 d R U . . .
N3 N 0.3655(12) 0.4246(11) 0.1941(13) 0.027(3) Uani 1 1 d . . . . .
H3D H 0.425287 0.409887 0.156519 0.032 Uiso 1 1 calc R U . . .
H3E H 0.303990 0.405090 0.158848 0.032 Uiso 1 1 calc R U . . .
C4 C 0.8774(15) 0.3798(12) 0.3394(15) 0.020(2) Uani 1 1 d . . . . .
H4A H 0.822688 0.345179 0.305061 0.030 Uiso 1 1 calc R U . . .
H4B H 0.839418 0.419523 0.380017 0.030 Uiso 1 1 calc R U . . .
H4C H 0.926710 0.351446 0.390727 0.030 Uiso 1 1 calc R U . . .
N1 N 0.1668(11) 0.5873(10) 0.2683(11) 0.019(3) Uani 1 1 d . . . . .
H1A H 0.227366 0.563003 0.243999 0.023 Uiso 1 1 calc DR U . . .
H1B H 0.190843 0.626394 0.312346 0.023 Uiso 1 1 calc R U . . .
N5 N 0.6710(12) 0.5604(10) 0.2516(12) 0.020(2) Uani 1 1 d . . . . .
H5A H 0.684883 0.514649 0.220273 0.023 Uiso 1 1 calc R U . . .
H5B H 0.731734 0.574265 0.293742 0.023 Uiso 1 1 calc R U . . .
C3 C 0.6492(15) 0.6181(12) 0.1630(15) 0.020(2) Uani 1 1 d . . . . .
H3A H 0.706194 0.614492 0.108296 0.029 Uiso 1 1 calc R U . . .
H3B H 0.650440 0.669025 0.195749 0.029 Uiso 1 1 calc R U . . .
H3C H 0.576541 0.608681 0.126820 0.029 Uiso 1 1 calc R U . . .
N7 N 0.9443(12) 0.4161(10) 0.2504(12) 0.020(2) Uani 1 1 d . . . . .
H7A H 0.996264 0.447645 0.281770 0.024 Uiso 1 1 calc R U . . .
H7B H 0.979414 0.379552 0.211934 0.024 Uiso 1 1 calc R U . . .
C1 C 0.1046(14) 0.6182(13) 0.1738(15) 0.019(3) Uani 1 1 d . . . . .
H1C H 0.088214 0.577657 0.120082 0.029 Uiso 1 1 calc R U . . .
H1D H 0.148178 0.657854 0.139187 0.029 Uiso 1 1 calc R U . . .
H1E H 0.035366 0.640054 0.198078 0.029 Uiso 1 1 calc R U . . .
C2 C 0.3751(14) 0.3954(15) 0.3080(15) 0.027(3) Uani 1 1 d . . . . .
H2A H 0.377863 0.339824 0.306545 0.041 Uiso 1 1 calc R U . . .
H2B H 0.311058 0.411913 0.348527 0.041 Uiso 1 1 calc R U . . .
H2C H 0.442805 0.415127 0.344910 0.041 Uiso 1 1 calc R U . . .
N2 N 0.1075(12) 0.5370(10) 0.3313(12) 0.019(3) Uani 1 1 d . . . . .
H2D H 0.149612 0.524421 0.389709 0.023 Uiso 1 1 d R U . . .
H2E H 0.045232 0.556820 0.353457 0.023 Uiso 1 1 d 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 Br1 2.945(2) . ?
Pb1 Br5 3.1626(19) 1_455 ?
Pb1 Br2 3.1173(19) 4_565 ?
Pb1 Br2 2.9508(19) . ?
Pb1 Br3 3.013(3) . ?
Pb1 Br4 2.935(3) . ?
Pb2 Br1 3.0867(19) . ?
Pb2 Br5 3.005(2) . ?
Pb2 Br6 3.085(2) . ?
Pb2 Br6 3.039(2) 4_565 ?
Pb2 Br8 2.903(2) . ?
Pb2 Br7 3.071(3) . ?
N6 H6A 0.9217 . ?
N6 H6B 0.9260 . ?
N6 N5 1.384(18) . ?
N8 H8A 0.8925 . ?
N8 H8B 0.8866 . ?
N8 N7 1.38(2) . ?
N4 H4D 0.9110 . ?
N4 H4E 0.9098 . ?
N4 N3 1.46(2) . ?
N3 H3D 0.9100 . ?
N3 H3E 0.9100 . ?
N3 C2 1.47(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 N7 1.52(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C1 1.45(2) . ?
N1 N2 1.39(2) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 C3 1.49(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C1 H1E 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N2 H2D 0.8819 . ?
N2 H2E 0.8837 . ?

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
Br1 Pb1 Br5 168.40(5) . 1_455 ?
Br1 Pb1 Br2 87.70(6) . . ?
Br1 Pb1 Br2 90.49(6) . 4_565 ?
Br1 Pb1 Br3 90.99(6) . . ?
Br2 Pb1 Br5 80.73(6) . 1_455 ?
Br2 Pb1 Br5 101.08(5) 4_565 1_455 ?
Br2 Pb1 Br2 178.19(7) . 4_565 ?
Br2 Pb1 Br3 84.49(6) . . ?
Br3 Pb1 Br5 88.77(5) . 1_455 ?
Br3 Pb1 Br2 95.44(6) . 4_565 ?
Br4 Pb1 Br1 88.12(6) . . ?
Br4 Pb1 Br5 91.54(6) . 1_455 ?
Br4 Pb1 Br2 87.40(6) . 4_565 ?
Br4 Pb1 Br2 92.63(6) . . ?
Br4 Pb1 Br3 177.02(6) . . ?
Br5 Pb2 Br1 167.15(5) . . ?
Br5 Pb2 Br6 83.96(6) . . ?
Br5 Pb2 Br6 95.25(6) . 4_565 ?
Br5 Pb2 Br7 91.01(6) . . ?
Br6 Pb2 Br1 97.15(6) 4_565 . ?
Br6 Pb2 Br1 83.59(6) . . ?
Br6 Pb2 Br6 178.67(5) 4_565 . ?
Br6 Pb2 Br7 88.04(6) 4_565 . ?
Br8 Pb2 Br1 93.44(6) . . ?
Br8 Pb2 Br5 89.06(6) . . ?
Br8 Pb2 Br6 87.10(6) . . ?
Br8 Pb2 Br6 93.96(6) . 4_565 ?
Br8 Pb2 Br7 177.98(6) . . ?
Br7 Pb2 Br1 86.05(6) . . ?
Br7 Pb2 Br6 90.90(6) . . ?
Pb1 Br1 Pb2 171.61(7) . . ?
Pb2 Br5 Pb1 163.59(6) . 1_655 ?
Pb1 Br2 Pb1 170.99(8) . 4_566 ?
Pb2 Br6 Pb2 162.06(8) 4_566 . ?
H6A N6 H6B 108.6 . . ?
N5 N6 H6A 109.4 . . ?
N5 N6 H6B 112.6 . . ?
H8A N8 H8B 110.2 . . ?
N7 N8 H8A 113.3 . . ?
N7 N8 H8B 109.1 . . ?
H4D N4 H4E 109.1 . . ?
N3 N4 H4D 109.2 . . ?
N3 N4 H4E 110.3 . . ?
N4 N3 H3D 109.7 . . ?
N4 N3 H3E 109.7 . . ?
N4 N3 C2 109.9(16) . . ?
H3D N3 H3E 108.2 . . ?
C2 N3 H3D 109.7 . . ?
C2 N3 H3E 109.7 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N7 C4 H4A 109.5 . . ?
N7 C4 H4B 109.5 . . ?
N7 C4 H4C 109.5 . . ?
H1A N1 H1B 107.6 . . ?
C1 N1 H1A 108.7 . . ?
C1 N1 H1B 108.7 . . ?
N2 N1 H1A 108.7 . . ?
N2 N1 H1B 108.7 . . ?
N2 N1 C1 114.1(14) . . ?
N6 N5 H5A 109.5 . . ?
N6 N5 H5B 109.5 . . ?
N6 N5 C3 110.7(14) . . ?
H5A N5 H5B 108.1 . . ?
C3 N5 H5A 109.5 . . ?
C3 N5 H5B 109.5 . . ?
N5 C3 H3A 109.5 . . ?
N5 C3 H3B 109.5 . . ?
N5 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N8 N7 C4 108.5(14) . . ?
N8 N7 H7A 110.0 . . ?
N8 N7 H7B 110.0 . . ?
C4 N7 H7A 110.0 . . ?
C4 N7 H7B 110.0 . . ?
H7A N7 H7B 108.4 . . ?
N1 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N3 C2 H2A 109.5 . . ?
N3 C2 H2B 109.5 . . ?
N3 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 N2 H2D 107.8 . . ?
N1 N2 H2E 112.6 . . ?
H2D N2 H2E 109.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N6 H6A Br1 0.92 2.91 3.736(17) 150.4 2_655 yes
N6 H6B Br8 0.93 2.58 3.497(17) 169.9 4_566 yes
N8 H8A Br3 0.89 2.86 3.501(15) 129.6 3_665 yes
N8 H8B Br7 0.89 2.68 3.451(16) 146.1 . yes
N4 H4D Br7 0.91 2.72 3.530(16) 149.4 3_665 yes
N4 H4E N6 0.91 2.26 3.13(2) 159.5 . yes
N3 H3D Br7 0.91 2.50 3.357(15) 157.6 . yes
N3 H3E Br3 0.91 2.47 3.292(16) 151.0 . yes
N1 H1A N4 0.91 1.98 2.890(19) 177.9 . yes
N1 H1B Br5 0.91 2.73 3.514(17) 144.6 2_655 yes
N1 H1B Br8 0.91 2.93 3.407(14) 114.6 2_655 yes
N5 H5A Br7 0.91 2.56 3.325(17) 142.5 . yes
N5 H5A N8 0.91 2.57 3.21(2) 127.9 . yes
N5 H5B Br4 0.91 2.45 3.321(16) 161.5 2_655 yes
N7 H7A N2 0.91 2.14 3.04(2) 168.9 1_655 yes
N7 H7B Br2 0.91 2.89 3.549(17) 130.6 1_655 yes
N7 H7B Br3 0.91 2.85 3.396(14) 120.0 1_655 yes
N2 H2D Br4 0.88 2.74 3.409(16) 133.4 4_566 yes
N2 H2E Br4 0.88 2.53 3.395(15) 165.2 2 yes

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.564
_oxdiff_exptl_absorpt_empirical_full_min 0.587
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7118(10) 14694 29008 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.2882(10) 14640 29008 nmt 0.9998 -0.0001 0.0026 -0.0006 -0.9997 0.0001
-0.0847 -0.0002 -1.0000

_twin_special_details            
;
Component 2 rotated by -179.9848° 
around [1.00 -0.00 -0.04] (reciprocal) or [1.00 -0.00 0.00] (direct)
;
####################################################################### 
# 
# 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_MHy2PbBr2_9I1_1_100K
_database_code_depnum_ccdc_archive 'CCDC 2307124'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT097_MHy2PbBr2_9I1_1_100K 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density      12.55 eA-3
RESPONSE: Twinning of the single crystal in this phase.
;
# Added during the CSD deposition process: Friday 10 November 2023 01:46 PM
# end Validation Reply Form

_audit_creation_date             2023-11-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br2.95 I1.09 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 Br2.95 I1.09 N4 Pb'
_chemical_formula_weight         675.42
_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'
Br Br -0.2901 2.4595 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.318(4)
_cell_length_b                   17.655(5)
_cell_length_c                   12.297(4)
_cell_angle_alpha                90.04(3)
_cell_angle_beta                 88.85(3)
_cell_angle_gamma                89.98(3)
_cell_volume                     2673.6(14)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    14740
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      29.1230
_cell_measurement_theta_min      3.2760
_shelx_estimated_absorpt_T_max   0.285
_shelx_estimated_absorpt_T_min   0.057
_exptl_absorpt_coefficient_mu    23.919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15915
_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            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.356
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0919
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11196
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.588
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00 -32.00   1.00   12.00    --   13.31 178.00-120.00   46
  2  ω    -25.00  57.00   1.00   12.00    --   13.31 -99.00   0.00   82
  3  ω    -92.00  18.00   1.00   12.00    --  -14.40 -57.00 -60.00  110
  4  ω    -94.00  17.00   1.00   12.00    --  -14.40 -37.00-180.00  111
  5  ω    -46.00  65.00   1.00   12.00    --  -14.40  37.00-120.00  111
  6  ω    -92.00  18.00   1.00   12.00    --  -14.40 -57.00  90.00  110
  7  ω    -74.00   3.00   1.00   12.00    --  -14.40 125.00  33.16   77
  8  ω    -91.00 -14.00   1.00   12.00    --  -14.40 152.00 143.83   77
  9  ω    -43.00  18.00   1.00   12.00    --    6.00 107.00 -13.86   61
 10  ω    -19.00  91.00   1.00   12.00    --   13.31  57.00 -30.00  110
 11  ω    -78.00 -32.00   1.00   12.00    --   13.31 178.00 -30.00   46
 12  ω    -76.00   1.00   1.00   12.00    --  -14.40 128.00 -60.09   77
 13  ω    -25.00  30.00   1.00   12.00    --  -14.40 -99.00 -30.00   55
 14  ω    -89.00 -11.00   1.00   12.00    --  -14.40 148.00-115.18   78
 15  ω    -82.00  53.00   1.00   12.00    --    2.00 -21.00 -41.32  135
 16  ω    -19.00  91.00   1.00   12.00    --   13.31  57.00  30.00  110
 17  ω    -79.00 105.00   1.00   12.00    --   13.31   0.00-180.00  184
 18  ω    -79.00 -14.00   1.00   12.00    --   13.31   0.00-150.00   65
 19  ω    -66.00  14.00   1.00   12.00    --  -14.40 112.00  66.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0147481516
_diffrn_orient_matrix_UB_12      0.0371299333
_diffrn_orient_matrix_UB_13      0.0161378861
_diffrn_orient_matrix_UB_21      -0.0518916165
_diffrn_orient_matrix_UB_22      0.0134255019
_diffrn_orient_matrix_UB_23      -0.0152283259
_diffrn_orient_matrix_UB_31      -0.0200553439
_diffrn_orient_matrix_UB_32      -0.0074480734
_diffrn_orient_matrix_UB_33      0.0532965111
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5598
_reflns_number_total             11196
_reflns_special_details          
;
 _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 1.5 (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  (Sheldrick, 2015)'
_refine_diff_density_max         12.553
_refine_diff_density_min         -5.901
_refine_diff_density_rms         0.864
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         11196
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.1809
_refine_ls_R_factor_gt           0.1067
_refine_ls_restrained_S_all      1.051
_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)+(0.1885P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2724
_refine_ls_wR_factor_ref         0.3142
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.564(3)
 0.436(3)
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. Shared sites
{Br1, I1}
{Br2, I2}
{Br3, I3}
{Br4, I4}
{Br5, I5}
{Br6, I6}
{Br7, I7}
{Br9, I9}
{Br10, I10}
{Br11, I11}
{Br12, I12}
{Br13, I13}
{Br14, I14}
{Br15, I15}
{Br16, I16}
{Br17, I17}
4. Restrained distances
 H5B_$1-H3A
 2.1 with sigma of 0.005
5. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(N9) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(N15) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Pb1) \\sim Ueq, Uanis(Pb2) \\sim Ueq, Uanis(Pb3) \\sim Ueq, Uanis(Pb4)
\\sim Ueq: with sigma of 0.0012 and sigma for terminal atoms of 0.0024
Uanis(Br16) \\sim Ueq, Uanis(I16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(I13) \\sim Ueq, Uanis(Br13) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Br1) = Uanis(I1)
Uanis(C1) = Uanis(N2) = Uanis(N3)
Uanis(N12) = Uanis(N11) = Uanis(C10)
Uanis(N15) = Uanis(N14) = Uanis(C13)
Uanis(C16) = Uanis(N17) = Uanis(N18)
Uanis(C7) = Uanis(N8) = Uanis(N9)
Uanis(N6) = Uanis(N5) = Uanis(C4)
Uanis(C22) = Uanis(N23) = Uanis(N24)
Uanis(N21) = Uanis(N20) = Uanis(C19)
Uanis(Br2) = Uanis(I2)
Uanis(Br3) = Uanis(I3)
Uanis(Br4) = Uanis(I4)
Uanis(Br5) = Uanis(I5)
Uanis(Br6) = Uanis(I6)
Uanis(Br7) = Uanis(I7)
Uanis(Br9) = Uanis(I9)
Uanis(Br10) = Uanis(I10)
Uanis(Br11) = Uanis(I11)
Uanis(Br12) = Uanis(I12)
Uanis(Br13) = Uanis(I13)
Uanis(Br14) = Uanis(I14)
Uanis(Br15) = Uanis(I15)
Uanis(Br16) = Uanis(I16)
Uanis(Br17) = Uanis(I17)
6. Others
 Fixed Sof: Br3(0.67) Br14(0.5) Br2(0.67) Br17(0.67) Br11(0.5) Br6(0.67)
 Br12(0.89) Br10(0.89) Br16(0.89) Br5(0.5) Br15(0.89) Br1(0.89) Br9(0.89)
 Br7(0.5) Br13(0.89) Br4(0.89) I3(0.37) I14(0.5) I2(0.37) I17(0.37) I11(0.5)
 I6(0.37) I12(0.11) I10(0.11) I16(0.11) I5(0.5) I15(0.11) I1(0.11) I9(0.11)
 I7(0.5) I13(0.11) I4(0.11)
7.a Rotating group:
 N24(H24A,H24B), N6(H6A,H6B), N15(H15A,H15B), N18(H18A,H18B), N9(H9A,H9B),
 N3(H3A,H3B), N12(H12A,H12B), N21(H21A,H21B)
7.b Secondary CH2 refined with riding coordinates:
 N11(H11A,H11B), N8(H8A,H8B), N23(H23A,H23B), N17(H17A,H17B), N2(H2A,H2B),
 N5(H5A,H5B), N20(H20A,H20B), N14(H14A,H14B)
7.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C7(H7A,H7B,H7C), C1(H1A,H1B,H1C), C10(H10A,H10B,H10C),
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C4(H4A,H4B,H4C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb4 Pb 0.54386(15) 0.25375(9) 0.87804(14) 0.0226(5) Uani 1 1 d . U . . .
Pb2 Pb 0.04168(15) 0.25583(10) 0.87118(15) 0.0241(5) Uani 1 1 d . U . . .
Pb1 Pb 0.04187(15) 0.24402(10) 0.37137(15) 0.0237(5) Uani 1 1 d . U . . .
Pb3 Pb 0.54353(15) 0.24605(9) 0.37829(14) 0.0224(5) Uani 1 1 d . U . . .
Br3 Br 0.0664(3) 0.25093(17) 0.1269(3) 0.0266(8) Uani 0.67 1 d . . P . .
Br14 Br 0.7900(3) 0.2426(2) 0.8771(3) 0.0321(11) Uani 0.5 1 d . . P . .
Br2 Br 0.5658(3) 0.25589(18) 0.6315(3) 0.0270(8) Uani 0.67 1 d . . P . .
Br17 Br 0.0669(3) 0.24902(17) 0.6271(3) 0.0266(8) Uani 0.67 1 d . . P . .
Br11 Br 0.2923(3) 0.2200(2) 0.3710(3) 0.0336(9) Uani 0.5 1 d . . P . .
Br6 Br 0.5653(3) 0.24396(18) 0.1314(3) 0.0271(8) Uani 0.67 1 d . . P . .
Br12 Br 0.0547(3) 0.0862(2) 0.8672(4) 0.0315(11) Uani 0.89 1 d . . P . .
Br10 Br 0.5669(4) 0.0770(2) 0.3946(3) 0.0289(11) Uani 0.89 1 d . . P . .
Br16 Br 0.5494(3) 0.0828(2) 0.8743(4) 0.0286(10) Uani 0.89 1 d . U P . .
Br5 Br 0.2917(3) 0.2802(2) 0.8719(3) 0.0351(9) Uani 0.5 1 d . . P . .
Br15 Br 0.5678(4) 0.4225(2) 0.8946(3) 0.0268(11) Uani 0.89 1 d . . P . .
Br1 Br 0.0555(3) 0.4140(2) 0.3679(4) 0.0302(10) Uani 0.89 1 d . . P . .
Br9 Br 0.5490(3) 0.4173(2) 0.3747(4) 0.0287(11) Uani 0.89 1 d . . P . .
Br7 Br 0.7911(2) 0.2568(2) 0.3773(3) 0.0291(11) Uani 0.5 1 d . . P . .
Br13 Br 0.0234(4) 0.0767(2) 0.3585(4) 0.0316(11) Uani 0.89 1 d . U P . .
Br4 Br 0.0221(4) 0.4231(2) 0.8591(4) 0.0301(11) Uani 0.89 1 d . . P . .
I3 I 0.0664(3) 0.25093(17) 0.1269(3) 0.0266(8) Uani 0.37 1 d . . P . .
I14 I 0.7900(3) 0.2426(2) 0.8771(3) 0.0321(11) Uani 0.5 1 d . . P . .
I2 I 0.5658(3) 0.25589(18) 0.6315(3) 0.0270(8) Uani 0.37 1 d . . P . .
I17 I 0.0669(3) 0.24902(17) 0.6271(3) 0.0266(8) Uani 0.37 1 d . . P . .
I11 I 0.2923(3) 0.2200(2) 0.3710(3) 0.0336(9) Uani 0.5 1 d . . P . .
I6 I 0.5653(3) 0.24396(18) 0.1314(3) 0.0271(8) Uani 0.37 1 d . . P . .
I12 I 0.0547(3) 0.0862(2) 0.8672(4) 0.0315(11) Uani 0.11 1 d . . P . .
I10 I 0.5669(4) 0.0770(2) 0.3946(3) 0.0289(11) Uani 0.11 1 d . . P . .
I16 I 0.5494(3) 0.0828(2) 0.8743(4) 0.0286(10) Uani 0.11 1 d . U P . .
I5 I 0.2917(3) 0.2802(2) 0.8719(3) 0.0351(9) Uani 0.5 1 d . . P . .
I15 I 0.5678(4) 0.4225(2) 0.8946(3) 0.0268(11) Uani 0.11 1 d . . P . .
I1 I 0.0555(3) 0.4140(2) 0.3679(4) 0.0302(10) Uani 0.11 1 d . . P . .
I9 I 0.5490(3) 0.4173(2) 0.3747(4) 0.0287(11) Uani 0.11 1 d . . P . .
I7 I 0.7911(2) 0.2568(2) 0.3773(3) 0.0291(11) Uani 0.5 1 d . . P . .
I13 I 0.0234(4) 0.0767(2) 0.3585(4) 0.0316(11) Uani 0.11 1 d . U P . .
I4 I 0.0221(4) 0.4231(2) 0.8591(4) 0.0301(11) Uani 0.11 1 d . . P . .
N24 N 0.674(2) 0.4589(18) 0.639(3) 0.035(6) Uani 1 1 d . . . . .
H24A H 0.615337 0.478414 0.606256 0.042 Uiso 1 1 d R U . . .
H24B H 0.648753 0.428228 0.693107 0.042 Uiso 1 1 d R U . . .
N11 N 0.698(3) 0.071(2) 0.633(4) 0.039(6) Uani 1 1 d . . . . .
H11A H 0.659548 0.092969 0.689540 0.046 Uiso 1 1 calc R U . . .
H11B H 0.662601 0.083055 0.571014 0.046 Uiso 1 1 calc R U . . .
N6 N 0.672(3) 0.0414(19) 0.126(3) 0.033(5) Uani 1 1 d . . . . .
H6A H 0.705016 -0.000103 0.151950 0.040 Uiso 1 1 d R U . . .
H6B H 0.644993 0.067388 0.183219 0.040 Uiso 1 1 d R U . . .
C22 C 0.832(3) 0.387(2) 0.624(4) 0.035(6) Uani 1 1 d . . . . .
H22A H 0.889214 0.367403 0.574849 0.053 Uiso 1 1 calc R U . . .
H22B H 0.804395 0.345593 0.670011 0.053 Uiso 1 1 calc R U . . .
H22C H 0.861668 0.426944 0.669637 0.053 Uiso 1 1 calc R U . . .
C7 C 0.335(3) 0.112(2) 0.656(4) 0.036(6) Uani 1 1 d . U . . .
H7A H 0.380956 0.092661 0.595995 0.054 Uiso 1 1 calc R U . . .
H7B H 0.378491 0.114560 0.722329 0.054 Uiso 1 1 calc R U . . .
H7C H 0.308500 0.162372 0.638246 0.054 Uiso 1 1 calc R U . . .
N15 N 0.189(3) 0.449(2) 0.078(3) 0.038(6) Uani 1 1 d . U . . .
H15A H 0.136763 0.413578 0.071116 0.045 Uiso 1 1 d R U . . .
H15B H 0.156661 0.494110 0.080781 0.045 Uiso 1 1 d R U . . .
N8 N 0.245(3) 0.062(2) 0.674(3) 0.036(6) Uani 1 1 d . U . . .
H8A H 0.270908 0.015748 0.695593 0.043 Uiso 1 1 calc R U . . .
H8B H 0.202806 0.080330 0.729293 0.043 Uiso 1 1 calc R U . . .
N23 N 0.745(3) 0.4170(19) 0.561(3) 0.035(6) Uani 1 1 d . . . . .
H23A H 0.706987 0.379015 0.528589 0.042 Uiso 1 1 calc R U . . .
H23B H 0.770841 0.448697 0.508020 0.042 Uiso 1 1 calc R U . . .
N18 N 0.694(4) 0.504(2) 0.141(3) 0.058(8) Uani 1 1 d . . . . .
H18A H 0.734246 0.529293 0.091909 0.070 Uiso 1 1 d R U . . .
H18B H 0.624873 0.518135 0.133895 0.070 Uiso 1 1 d R U . . .
C1 C 0.318(4) 0.115(3) 0.108(4) 0.048(7) Uani 1 1 d . . . . .
H1A H 0.310225 0.120310 0.029594 0.072 Uiso 1 1 calc R U . . .
H1B H 0.380470 0.082498 0.123250 0.072 Uiso 1 1 calc R U . . .
H1C H 0.328299 0.164688 0.141296 0.072 Uiso 1 1 calc R U . . .
C10 C 0.812(3) 0.107(2) 0.628(4) 0.039(6) Uani 1 1 d . . . . .
H10A H 0.841567 0.102785 0.553702 0.058 Uiso 1 1 calc R U . . .
H10B H 0.859127 0.081205 0.678504 0.058 Uiso 1 1 calc R U . . .
H10C H 0.806444 0.161050 0.647755 0.058 Uiso 1 1 calc R U . . .
N17 N 0.702(3) 0.428(2) 0.126(3) 0.058(8) Uani 1 1 d . . . . .
H17A H 0.673556 0.416684 0.059856 0.070 Uiso 1 1 calc R U . . .
H17B H 0.658742 0.404797 0.176993 0.070 Uiso 1 1 calc R U . . .
N2 N 0.225(3) 0.082(2) 0.152(4) 0.048(7) Uani 1 1 d . . . . .
H2A H 0.244692 0.061387 0.216474 0.058 Uiso 1 1 calc R U . . .
H2B H 0.179239 0.120896 0.168512 0.058 Uiso 1 1 calc R U . . .
C13 C 0.333(3) 0.384(3) 0.156(4) 0.038(6) Uani 1 1 d . U . . .
H13A H 0.389459 0.405702 0.108568 0.056 Uiso 1 1 calc R U . . .
H13B H 0.301948 0.339047 0.119853 0.056 Uiso 1 1 calc R U . . .
H13C H 0.364030 0.368418 0.224898 0.056 Uiso 1 1 calc R U . . .
N9 N 0.184(3) 0.052(2) 0.586(3) 0.036(6) Uani 1 1 d . U . . .
H9A H 0.124722 0.023575 0.600779 0.043 Uiso 1 1 d R U . . .
H9B H 0.160025 0.097116 0.561574 0.043 Uiso 1 1 d R U . . .
N3 N 0.167(3) 0.031(2) 0.104(3) 0.048(7) Uani 1 1 d . . . . .
H3A H 0.169389 -0.014850 0.140030 0.058 Uiso 1 1 d DR U . . .
H3B H 0.094777 0.045749 0.101763 0.058 Uiso 1 1 d R U . . .
N5 N 0.747(3) 0.0854(19) 0.066(3) 0.033(5) Uani 1 1 d . . . . .
H5A H 0.710016 0.124210 0.034290 0.040 Uiso 1 1 calc R U . . .
H5B H 0.775607 0.056405 0.011331 0.040 Uiso 1 1 calc R U . . .
N20 N 0.229(3) 0.416(2) 0.666(4) 0.057(8) Uani 1 1 d . . . . .
H20A H 0.253109 0.437364 0.728061 0.069 Uiso 1 1 calc R U . . .
H20B H 0.185436 0.376238 0.684683 0.069 Uiso 1 1 calc R U . . .
C16 C 0.810(4) 0.392(3) 0.130(4) 0.058(8) Uani 1 1 d . . . . .
H16A H 0.861946 0.421314 0.085898 0.088 Uiso 1 1 calc R U . . .
H16B H 0.805898 0.340133 0.100978 0.088 Uiso 1 1 calc R U . . .
H16C H 0.833876 0.390119 0.205345 0.088 Uiso 1 1 calc R U . . .
C4 C 0.832(3) 0.116(2) 0.126(4) 0.033(5) Uani 1 1 d . . . . .
H4A H 0.894078 0.125821 0.077811 0.050 Uiso 1 1 calc R U . . .
H4B H 0.852340 0.079640 0.182488 0.050 Uiso 1 1 calc R U . . .
H4C H 0.807584 0.163235 0.160516 0.050 Uiso 1 1 calc R U . . .
N12 N 0.696(3) -0.0055(19) 0.647(3) 0.039(6) Uani 1 1 d . . . . .
H12A H 0.731708 -0.027590 0.588868 0.046 Uiso 1 1 d R U . . .
H12B H 0.625602 -0.022779 0.648464 0.046 Uiso 1 1 d R U . . .
N14 N 0.252(3) 0.436(2) 0.174(3) 0.038(6) Uani 1 1 d . U . . .
H14A H 0.282600 0.480739 0.195228 0.045 Uiso 1 1 calc R U . . .
H14B H 0.207851 0.419873 0.229675 0.045 Uiso 1 1 calc R U . . .
N21 N 0.166(3) 0.471(2) 0.607(4) 0.057(8) Uani 1 1 d . . . . .
H21A H 0.143822 0.451411 0.543214 0.069 Uiso 1 1 d R U . . .
H21B H 0.106431 0.484456 0.645504 0.069 Uiso 1 1 d R U . . .
C19 C 0.320(4) 0.388(3) 0.604(5) 0.057(8) Uani 1 1 d . . . . .
H19A H 0.301775 0.385242 0.527240 0.086 Uiso 1 1 calc R U . . .
H19B H 0.339216 0.337207 0.630258 0.086 Uiso 1 1 calc R U . . .
H19C H 0.382103 0.422015 0.613272 0.086 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
Pb4 Br14 3.038(4) . ?
Pb4 Br2 3.039(4) . ?
Pb4 Br6 3.137(4) 1_556 ?
Pb4 Br16 3.018(4) . ?
Pb4 Br5 3.144(4) . ?
Pb4 Br15 3.001(5) . ?
Pb2 Br3 3.167(4) 1_556 ?
Pb2 Br14 3.109(4) 1_455 ?
Pb2 Br17 3.013(4) . ?
Pb2 Br12 2.999(4) . ?
Pb2 Br5 3.109(4) . ?
Pb2 Br4 2.967(4) . ?
Pb1 Br3 3.017(4) . ?
Pb1 Br17 3.168(4) . ?
Pb1 Br11 3.114(4) . ?
Pb1 Br1 3.007(4) . ?
Pb1 Br7 3.096(4) 1_455 ?
Pb1 Br13 2.968(5) . ?
Pb3 Br2 3.136(4) . ?
Pb3 Br11 3.132(4) . ?
Pb3 Br6 3.043(4) . ?
Pb3 Br10 3.006(5) . ?
Pb3 Br9 3.024(4) . ?
Pb3 Br7 3.055(4) . ?
N24 H24A 0.9048 . ?
N24 H24B 0.9057 . ?
N24 N23 1.48(5) . ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 C10 1.54(5) . ?
N11 N12 1.37(5) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9018 . ?
N6 N5 1.40(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 N23 1.44(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 N8 1.43(5) . ?
N15 H15A 0.8949 . ?
N15 H15B 0.8956 . ?
N15 N14 1.45(5) . ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 N9 1.35(4) . ?
N23 H23A 0.9100 . ?
N23 H23B 0.9100 . ?
N18 H18A 0.8919 . ?
N18 H18B 0.8914 . ?
N18 N17 1.37(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 N2 1.38(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N17 H17A 0.9100 . ?
N17 H17B 0.9100 . ?
N17 C16 1.47(6) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 N3 1.30(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 N14 1.38(5) . ?
N9 H9A 0.9031 . ?
N9 H9B 0.9015 . ?
N3 H3A 0.9236 . ?
N3 H3B 0.9241 . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 C4 1.40(5) . ?
N20 H20A 0.9100 . ?
N20 H20B 0.9100 . ?
N20 N21 1.44(5) . ?
N20 C19 1.43(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N12 H12A 0.9157 . ?
N12 H12B 0.9161 . ?
N14 H14A 0.9100 . ?
N14 H14B 0.9100 . ?
N21 H21A 0.9066 . ?
N21 H21B 0.8999 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br14 Pb4 Br2 85.88(11) . . ?
Br14 Pb4 Br6 84.05(11) . 1_556 ?
Br14 Pb4 Br5 174.94(13) . . ?
Br2 Pb4 Br6 169.78(11) . 1_556 ?
Br2 Pb4 Br5 92.42(11) . . ?
Br6 Pb4 Br5 97.76(12) 1_556 . ?
Br16 Pb4 Br14 85.02(12) . . ?
Br16 Pb4 Br2 89.80(12) . . ?
Br16 Pb4 Br6 87.54(12) . 1_556 ?
Br16 Pb4 Br5 99.76(12) . . ?
Br15 Pb4 Br14 87.99(13) . . ?
Br15 Pb4 Br2 92.74(11) . . ?
Br15 Pb4 Br6 88.71(11) . 1_556 ?
Br15 Pb4 Br16 172.37(14) . . ?
Br15 Pb4 Br5 87.32(12) . . ?
Br14 Pb2 Br3 95.18(11) 1_455 1_556 ?
Br14 Pb2 Br5 176.09(13) 1_455 . ?
Br17 Pb2 Br3 167.92(11) . 1_556 ?
Br17 Pb2 Br14 95.94(11) . 1_455 ?
Br17 Pb2 Br5 85.73(12) . . ?
Br12 Pb2 Br3 88.98(13) . 1_556 ?
Br12 Pb2 Br14 88.73(12) . 1_455 ?
Br12 Pb2 Br17 86.57(13) . . ?
Br12 Pb2 Br5 94.91(12) . . ?
Br5 Pb2 Br3 83.47(11) . 1_556 ?
Br4 Pb2 Br3 94.99(12) . 1_556 ?
Br4 Pb2 Br14 89.69(12) . 1_455 ?
Br4 Pb2 Br17 89.78(12) . . ?
Br4 Pb2 Br12 175.85(14) . . ?
Br4 Pb2 Br5 86.77(12) . . ?
Br3 Pb1 Br17 168.00(11) . . ?
Br3 Pb1 Br11 85.69(12) . . ?
Br3 Pb1 Br7 95.77(11) . 1_455 ?
Br11 Pb1 Br17 83.61(11) . . ?
Br1 Pb1 Br3 86.58(13) . . ?
Br1 Pb1 Br17 88.87(12) . . ?
Br1 Pb1 Br11 94.63(12) . . ?
Br1 Pb1 Br7 89.04(12) . 1_455 ?
Br7 Pb1 Br17 95.25(11) 1_455 . ?
Br7 Pb1 Br11 176.13(12) 1_455 . ?
Br13 Pb1 Br3 89.67(12) . . ?
Br13 Pb1 Br17 95.11(12) . . ?
Br13 Pb1 Br11 86.66(12) . . ?
Br13 Pb1 Br1 175.93(14) . . ?
Br13 Pb1 Br7 89.76(12) . 1_455 ?
Br11 Pb3 Br2 98.19(12) . . ?
Br6 Pb3 Br2 169.63(11) . . ?
Br6 Pb3 Br11 92.13(11) . . ?
Br6 Pb3 Br7 85.92(11) . . ?
Br10 Pb3 Br2 88.72(11) . . ?
Br10 Pb3 Br11 87.23(12) . . ?
Br10 Pb3 Br6 92.79(12) . . ?
Br10 Pb3 Br9 172.53(14) . . ?
Br10 Pb3 Br7 88.02(12) . . ?
Br9 Pb3 Br2 87.56(12) . . ?
Br9 Pb3 Br11 99.71(12) . . ?
Br9 Pb3 Br6 89.73(13) . . ?
Br9 Pb3 Br7 85.15(12) . . ?
Br7 Pb3 Br2 83.87(11) . . ?
Br7 Pb3 Br11 174.77(12) . . ?
Pb1 Br3 Pb2 168.70(13) . 1_554 ?
Pb4 Br14 Pb2 171.87(15) . 1_655 ?
Pb4 Br2 Pb3 169.15(12) . . ?
Pb2 Br17 Pb1 168.46(12) . . ?
Pb1 Br11 Pb3 163.62(14) . . ?
Pb3 Br6 Pb4 169.41(12) . 1_554 ?
Pb2 Br5 Pb4 163.48(15) . . ?
Pb3 Br7 Pb1 172.17(14) . 1_655 ?
H24A N24 H24B 106.8 . . ?
N23 N24 H24A 111.1 . . ?
N23 N24 H24B 111.5 . . ?
H11A N11 H11B 107.5 . . ?
C10 N11 H11A 108.4 . . ?
C10 N11 H11B 108.4 . . ?
N12 N11 H11A 108.4 . . ?
N12 N11 H11B 108.4 . . ?
N12 N11 C10 115(3) . . ?
H6A N6 H6B 107.1 . . ?
N5 N6 H6A 110.4 . . ?
N5 N6 H6B 111.1 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N23 C22 H22A 109.5 . . ?
N23 C22 H22B 109.5 . . ?
N23 C22 H22C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N8 C7 H7A 109.5 . . ?
N8 C7 H7B 109.5 . . ?
N8 C7 H7C 109.5 . . ?
H15A N15 H15B 107.9 . . ?
N14 N15 H15A 112.1 . . ?
N14 N15 H15B 110.8 . . ?
C7 N8 H8A 108.9 . . ?
C7 N8 H8B 108.9 . . ?
H8A N8 H8B 107.7 . . ?
N9 N8 C7 113(4) . . ?
N9 N8 H8A 108.9 . . ?
N9 N8 H8B 108.9 . . ?
N24 N23 H23A 110.6 . . ?
N24 N23 H23B 110.6 . . ?
C22 N23 N24 105(3) . . ?
C22 N23 H23A 110.6 . . ?
C22 N23 H23B 110.6 . . ?
H23A N23 H23B 108.8 . . ?
H18A N18 H18B 108.4 . . ?
N17 N18 H18A 111.0 . . ?
N17 N18 H18B 108.8 . . ?
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 . . ?
N11 C10 H10A 109.5 . . ?
N11 C10 H10B 109.5 . . ?
N11 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N18 N17 H17A 107.6 . . ?
N18 N17 H17B 107.6 . . ?
N18 N17 C16 119(4) . . ?
H17A N17 H17B 107.1 . . ?
C16 N17 H17A 107.6 . . ?
C16 N17 H17B 107.6 . . ?
C1 N2 H2A 106.0 . . ?
C1 N2 H2B 106.0 . . ?
H2A N2 H2B 106.3 . . ?
N3 N2 C1 125(5) . . ?
N3 N2 H2A 106.0 . . ?
N3 N2 H2B 106.0 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N14 C13 H13A 109.5 . . ?
N14 C13 H13B 109.5 . . ?
N14 C13 H13C 109.5 . . ?
N8 N9 H9A 111.4 . . ?
N8 N9 H9B 110.2 . . ?
H9A N9 H9B 106.8 . . ?
N2 N3 H3A 111.3 . . ?
N2 N3 H3B 111.0 . . ?
H3A N3 H3B 107.8 . . ?
N6 N5 H5A 108.5 . . ?
N6 N5 H5B 108.5 . . ?
N6 N5 C4 115(3) . . ?
H5A N5 H5B 107.5 . . ?
C4 N5 H5A 108.5 . . ?
C4 N5 H5B 108.5 . . ?
H20A N20 H20B 107.8 . . ?
N21 N20 H20A 109.0 . . ?
N21 N20 H20B 109.0 . . ?
C19 N20 H20A 109.0 . . ?
C19 N20 H20B 109.0 . . ?
C19 N20 N21 113(4) . . ?
N17 C16 H16A 109.5 . . ?
N17 C16 H16B 109.5 . . ?
N17 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N11 N12 H12A 108.9 . . ?
N11 N12 H12B 110.4 . . ?
H12A N12 H12B 108.6 . . ?
N15 N14 H14A 109.3 . . ?
N15 N14 H14B 109.3 . . ?
C13 N14 N15 111(3) . . ?
C13 N14 H14A 109.3 . . ?
C13 N14 H14B 109.3 . . ?
H14A N14 H14B 108.0 . . ?
N20 N21 H21A 110.7 . . ?
N20 N21 H21B 111.1 . . ?
H21A N21 H21B 107.1 . . ?
N20 C19 H19A 109.5 . . ?
N20 C19 H19B 109.5 . . ?
N20 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N24 H24A Br9 0.90 2.74 3.52(3) 144.3 2_666 yes
N24 H24B Br15 0.91 2.65 3.44(4) 145.3 . yes
N11 H11A Br16 0.91 2.63 3.46(4) 151.3 . yes
N11 H11B Br10 0.91 2.49 3.38(4) 164.5 . yes
N6 H6A N8 0.90 2.49 3.24(5) 141.7 2_656 yes
N6 H6B Br10 0.90 2.76 3.58(4) 152.5 . yes
N15 H15B Br4 0.90 2.73 3.52(4) 147.2 2_566 yes
N8 H8A Br10 0.91 2.79 3.46(4) 130.9 2_656 yes
N8 H8A N6 0.91 2.53 3.24(5) 135.2 2_656 yes
N8 H8B Br12 0.91 2.47 3.33(4) 159.0 . yes
N23 H23A Br9 0.91 2.82 3.35(3) 118.5 . yes
N23 H23B N21 0.91 2.14 3.05(6) 176.0 2_666 yes
N18 H18A N15 0.89 2.32 3.15(6) 155.5 2_665 yes
N18 H18B Br15 0.89 2.62 3.51(5) 172.0 2_666 yes
N17 H17A Br15 0.91 2.44 3.32(3) 162.8 1_554 yes
N17 H17B Br9 0.91 2.77 3.57(5) 147.3 . yes
N2 H2A N12 0.91 2.10 3.00(6) 172.6 2_656 yes
N2 H2B Br3 0.91 2.74 3.58(4) 155.0 . yes
N9 H9A Br13 0.90 2.58 3.48(4) 170.5 2_556 yes
N5 H5A Br16 0.91 2.91 3.42(3) 116.6 1_554 yes
N5 H5B N3 0.91 2.20 3.10(5) 169.7 2_655 yes
N20 H20A N18 0.91 2.03 2.93(6) 174.1 2_666 yes
N20 H20B Br17 0.91 2.78 3.60(4) 150.1 . yes
N12 H12A N9 0.92 2.40 3.29(6) 163.9 2_656 yes
N12 H12B Br10 0.92 2.62 3.52(3) 166.6 2_656 yes
N14 H14A Br15 0.91 2.73 3.43(4) 134.9 2_666 yes
N14 H14A N24 0.91 2.37 3.10(5) 137.0 2_666 yes
N14 H14B Br1 0.91 2.51 3.38(4) 161.5 . yes
N21 H21A Br1 0.91 2.52 3.42(5) 170.1 . yes
N21 H21B Br1 0.90 2.69 3.41(4) 138.3 2_566 yes

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.405
_oxdiff_exptl_absorpt_empirical_full_min 0.460
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.564(3)
2 0.436(3)

####################################################################### 
# 
# 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_MHy2PbBr2_9I1_1_295K
_database_code_depnum_ccdc_archive 'CCDC 2307126'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_audit_creation_date             2023-11-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br2.904 I1.096 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 Br2.90 I1.10 N4 Pb'
_chemical_formula_weight         672.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C2 N4 Pb Br4'
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'
Br Br -0.2901 2.4595 '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 n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.391(4)
_cell_length_b                   17.892(5)
_cell_length_c                   6.166(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1366.9(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1879
_cell_measurement_temperature    295
_cell_measurement_theta_max      25.6770
_cell_measurement_theta_min      3.4780
_shelx_estimated_absorpt_T_max   0.293
_shelx_estimated_absorpt_T_min   0.059
_exptl_absorpt_coefficient_mu    23.269
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34606
_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            'dark yellow'
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.268
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1183
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8147
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.288
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  93.00   1.00    7.00    --   13.31  37.00-150.00  111
  2  ω     32.00 104.00   1.00    7.00    --   13.31-178.00 150.00   72
  3  ω    -65.00  25.00   1.00    7.00    --   13.31 -57.00-150.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0443197520
_diffrn_orient_matrix_UB_12      -0.0242217800
_diffrn_orient_matrix_UB_13      -0.0191808855
_diffrn_orient_matrix_UB_21      -0.0306782409
_diffrn_orient_matrix_UB_22      0.0305999337
_diffrn_orient_matrix_UB_23      -0.0393049862
_diffrn_orient_matrix_UB_31      0.0193193349
_diffrn_orient_matrix_UB_32      -0.0069427765
_diffrn_orient_matrix_UB_33      -0.1063790263
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                846
_reflns_number_total             1444
_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    ?
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1444
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0315
_refine_ls_restrained_S_all      1.028
_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)+(0.0257P)²+2.0012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0732
_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,H,H,H) groups
2. Shared sites
{Br1, I1}
{Br3, I3}
{Br2, I2}
3. Restrained distances
 N2-C1
 1.5 with sigma of 0.005
 N2A-C1
 1.5 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(N3A) = Uanis(N3) = Uanis(N2) = Uanis(N2A)
Uanis(Br1) = Uanis(I1)
Uanis(Br3) = Uanis(I3)
Uanis(Br2) = Uanis(I2)
5. Others
 Sof(I2)=0.5*(1-FVAR(2))
 Sof(Br2)=0.5*FVAR(2)
 Sof(I3)=1-FVAR(2)
 Sof(Br3)=FVAR(2)
 Sof(I1)=0.5*(1-FVAR(4))
 Sof(Br1)=0.5*FVAR(4)
 Fixed Sof: N3A(0.65) H3AA(0.65) H3AB(0.65) H1BD(0.65) H1BE(0.65) H1BF(0.65)
 H1AA(0.35) H1AB(0.35) H1AC(0.35) N2A(0.65) H2AA(0.65) H2AB(0.65) N3(0.35)
 H3A(0.35) H3B(0.35) N2(0.35) H2A(0.35) H2B(0.35)
6.a Rotating group:
 N3A(H3AA,H3AB), N3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), N2(H2A,H2B)
6.c Idealised Me refined as rotating group:
 C1(H1BD,H1BE,H1BF), C1(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.54186(3) 0.250000 0.25536(7) 0.03718(16) Uani 1 2 d S T P . .
Br1 Br 0.56289(8) 0.250000 0.75135(15) 0.0522(4) Uani 0.629(9) 2 d S T P . .
Br2 Br 0.28972(7) 0.250000 0.2462(2) 0.0833(6) Uani 0.495(11) 2 d S T P . .
Br3 Br 0.54740(7) 0.41810(5) 0.26608(15) 0.0647(4) Uani 0.889(7) 1 d . . P . .
I1 I 0.56289(8) 0.250000 0.75135(15) 0.0522(4) Uani 0.371(9) 2 d S T P . .
I2 I 0.28972(7) 0.250000 0.2462(2) 0.0833(6) Uani 0.505(11) 2 d S T P . .
I3 I 0.54740(7) 0.41810(5) 0.26608(15) 0.0647(4) Uani 0.111(7) 1 d . . P . .
N3A N 0.3249(13) 0.5456(9) 0.197(2) 0.069(3) Uani 0.65 1 d . . P A 2
H3AA H 0.347062 0.582788 0.109292 0.083 Uiso 0.65 1 d R U P A 2
H3AB H 0.383734 0.523509 0.254114 0.083 Uiso 0.65 1 d R U P A 2
C1 C 0.1729(8) 0.6173(6) 0.2549(16) 0.086(3) Uani 1 1 d D . . . .
H1BD H 0.136960 0.586260 0.150523 0.128 Uiso 0.65 1 calc R U P B 2
H1BE H 0.205977 0.658875 0.182252 0.128 Uiso 0.65 1 calc R U P B 2
H1BF H 0.121363 0.635431 0.358611 0.128 Uiso 0.65 1 calc R U P B 2
H1AA H 0.140306 0.599101 0.123953 0.128 Uiso 0.35 1 calc R U P C 1
H1AB H 0.173204 0.670969 0.253493 0.128 Uiso 0.35 1 calc R U P C 1
H1AC H 0.132404 0.599929 0.377692 0.128 Uiso 0.35 1 calc R U P C 1
N2A N 0.2573(9) 0.5730(8) 0.3687(18) 0.069(3) Uani 0.65 1 d D . P A 2
H2AA H 0.294663 0.601523 0.459944 0.083 Uiso 0.65 1 calc R U P A 2
H2AB H 0.227928 0.535318 0.442422 0.083 Uiso 0.65 1 calc R U P A 2
N3 N 0.308(2) 0.5094(17) 0.234(5) 0.069(3) Uani 0.35 1 d . . P A 1
H3A H 0.323576 0.501863 0.094081 0.083 Uiso 0.35 1 d R U P A 1
H3B H 0.249613 0.483653 0.269300 0.083 Uiso 0.35 1 d R U P A 1
N2 N 0.2870(10) 0.5890(17) 0.270(4) 0.069(3) Uani 0.35 1 d D . P A 1
H2A H 0.326385 0.614711 0.175114 0.083 Uiso 0.35 1 calc R U P A 1
H2B H 0.311592 0.600471 0.401529 0.083 Uiso 0.35 1 calc R U P A 1


_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 Br1 3.0693(18) . ?
Pb1 Br1 3.1186(18) 1_554 ?
Pb1 Br2 3.1247(13) . ?
Pb1 Br2 3.0711(13) 6_656 ?
Pb1 Br3 3.0092(12) 7_565 ?
Pb1 Br3 3.0092(12) . ?
N3A H3AA 0.9007 . ?
N3A H3AB 0.9003 . ?
N3A N2A 1.435(19) . ?
C1 H1BD 0.9600 . ?
C1 H1BE 0.9600 . ?
C1 H1BF 0.9600 . ?
C1 H1AA 0.9600 . ?
C1 H1AB 0.9600 . ?
C1 H1AC 0.9600 . ?
C1 N2A 1.488(5) . ?
C1 N2 1.504(5) . ?
N2A H2AA 0.8900 . ?
N2A H2AB 0.8900 . ?
N3 H3A 0.8907 . ?
N3 H3B 0.8896 . ?
N3 N2 1.47(4) . ?
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
Br1 Pb1 Br1 170.34(4) . 1_554 ?
Br1 Pb1 Br2 85.31(3) . 6_656 ?
Br1 Pb1 Br2 93.75(3) 1_554 . ?
Br1 Pb1 Br2 95.91(3) . . ?
Br2 Pb1 Br1 85.03(3) 6_656 1_554 ?
Br2 Pb1 Br2 178.784(16) 6_656 . ?
Br3 Pb1 Br1 91.14(2) . 1_554 ?
Br3 Pb1 Br1 88.64(2) . . ?
Br3 Pb1 Br1 88.64(2) 7_565 . ?
Br3 Pb1 Br1 91.14(2) 7_565 1_554 ?
Br3 Pb1 Br2 91.329(19) . . ?
Br3 Pb1 Br2 91.330(19) 7_565 . ?
Br3 Pb1 Br2 88.697(19) 7_565 6_656 ?
Br3 Pb1 Br2 88.697(19) . 6_656 ?
Br3 Pb1 Br3 176.37(4) 7_565 . ?
Pb1 Br1 Pb1 170.34(4) . 1_556 ?
Pb1 Br2 Pb1 179.14(5) 6_556 . ?
H3AA N3A H3AB 108.2 . . ?
N2A N3A H3AA 111.7 . . ?
N2A N3A H3AB 109.6 . . ?
H1BD C1 H1BE 109.5 . . ?
H1BD C1 H1BF 109.5 . . ?
H1BE C1 H1BF 109.5 . . ?
H1AA C1 H1AB 109.5 . . ?
H1AA C1 H1AC 109.5 . . ?
H1AB C1 H1AC 109.5 . . ?
N2A C1 H1BD 109.5 . . ?
N2A C1 H1BE 109.5 . . ?
N2A C1 H1BF 109.5 . . ?
N2 C1 H1AA 109.5 . . ?
N2 C1 H1AB 109.5 . . ?
N2 C1 H1AC 109.5 . . ?
N3A N2A C1 104.2(11) . . ?
N3A N2A H2AA 110.9 . . ?
N3A N2A H2AB 110.9 . . ?
C1 N2A H2AA 110.9 . . ?
C1 N2A H2AB 110.9 . . ?
H2AA N2A H2AB 108.9 . . ?
H3A N3 H3B 109.5 . . ?
N2 N3 H3A 109.5 . . ?
N2 N3 H3B 108.5 . . ?
C1 N2 H2A 107.5 . . ?
C1 N2 H2B 107.5 . . ?
N3 N2 C1 119(2) . . ?
N3 N2 H2A 107.5 . . ?
N3 N2 H2B 107.5 . . ?
H2A N2 H2B 107.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3A H3AA Br3 0.90 2.66 3.329(12) 132.0 5_665 yes
N3A H3AB Br3 0.90 2.77 3.604(18) 154.4 . yes
N2A H2AA Br3 0.89 2.61 3.309(11) 136.2 5_666 yes
N2A H2AB N3A 0.89 2.24 3.105(18) 165.7 2_565 yes
N3 H3B Br3 0.89 2.78 3.62(3) 159.8 6_556 yes
N2 H2A Br1 0.89 2.82 3.43(3) 127.2 5_666 yes
N2 H2B Br3 0.89 2.71 3.52(2) 151.7 5_666 yes

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.467
_oxdiff_exptl_absorpt_empirical_full_min 0.680
####################################################################### 
# 
# 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_MHy2PbBr1_65I2_35_295K-aver
_database_code_depnum_ccdc_archive 'CCDC 2324607'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2024-01-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_audit_creation_date             2024-01-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br1.772 I2.228 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 Br1.77 I2.23 N4 Pb'
_chemical_formula_weight         725.67
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C Pb Br4'
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'
Br Br -0.2901 2.4595 '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 n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.600(4)
_cell_length_b                   18.024(5)
_cell_length_c                   6.303(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1431.5(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7620
_cell_measurement_temperature    295
_cell_measurement_theta_max      28.5500
_cell_measurement_theta_min      3.3870
_shelx_estimated_absorpt_T_max   0.615
_shelx_estimated_absorpt_T_min   0.099
_exptl_absorpt_coefficient_mu    21.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29436
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            27011
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.341
_diffrn_reflns_theta_min         3.234
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -78.00 -32.00   1.00   30.00    --   13.31 178.00  30.00   46
  2  ω    -25.00  57.00   1.00   30.00    --   13.31 -99.00  60.00   82
  3  ω    -94.00  17.00   1.00   30.00    --  -14.40 -37.00  30.00  111
  4  ω    -99.00  43.00   1.00   30.00    --  -14.40 -19.00  90.00  142
  5  ω    -25.00  30.00   1.00   30.00    --  -14.40 -99.00-120.00   55
  6  ω    -94.00  17.00   1.00   30.00    --  -14.40 -37.00-120.00  111
  7  ω    -67.00  11.00   1.00   30.00    --  -14.40 115.00-176.00   78
  8  ω    -25.00  30.00   1.00   30.00    --  -14.40 -99.00 -30.00   55
  9  ω    -50.00  23.00   1.00   30.00    --  -14.40  77.00 150.00   73
 10  ω    -46.00  65.00   1.00   30.00    --  -14.40  37.00-180.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0143449690
_diffrn_orient_matrix_UB_12      0.0294600638
_diffrn_orient_matrix_UB_13      -0.0689433869
_diffrn_orient_matrix_UB_21      0.0030921009
_diffrn_orient_matrix_UB_22      -0.0253233352
_diffrn_orient_matrix_UB_23      -0.0858518636
_diffrn_orient_matrix_UB_31      -0.0543487186
_diffrn_orient_matrix_UB_32      0.0063336110
_diffrn_orient_matrix_UB_33      -0.0230810206
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1101
_reflns_number_total             1509
_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    ?
_refine_diff_density_max         2.419
_refine_diff_density_min         -2.863
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1509
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0414
_refine_ls_restrained_S_all      1.101
_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)+(0.0536P)²+16.7406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1244
_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. Shared sites
{Br1, I1}
{Br3, I3}
{Br2, I2}
3. Restrained distances
 N1-C1
 1.45 with sigma of 0.002
 N2-N1
 1.4 with sigma of 0.002
 H2A-H1E_$1
 2.2 with sigma of 0.01
 H2B-H1E_$1
 2.2 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(I1)
Uanis(Br2) = Uanis(I2)
Uanis(C1) = Uanis(N1) = Uanis(N2)
Uanis(Br3) = Uanis(I3)
5. Others
 Sof(I1)=0.5*(1-FVAR(2))
 Sof(Br1)=0.5*FVAR(2)
 Sof(I2)=0.5*(1-FVAR(3))
 Sof(Br2)=0.5*FVAR(3)
 Sof(I3)=1-FVAR(3)
 Sof(Br3)=FVAR(3)
6.a Rotating group:
 N2(H2A,H2B)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1D,H1E)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.54194(4) 0.250000 0.25610(8) 0.0386(2) Uani 1 2 d S T P . .
Br1 Br 0.55892(11) 0.250000 0.75207(16) 0.0573(5) Uani 0.263(17) 2 d S T P . .
Br2 Br 0.29199(9) 0.250000 0.2489(2) 0.1128(12) Uani 0.11(2) 2 d S T P . .
Br3 Br 0.54826(12) 0.41931(6) 0.2674(2) 0.0772(6) Uani 0.700(13) 1 d . . P . .
I1 I 0.55892(11) 0.250000 0.75207(16) 0.0573(5) Uani 0.737(17) 2 d S T P . .
I2 I 0.29199(9) 0.250000 0.2489(2) 0.1128(12) Uani 0.89(2) 2 d S T P . .
I3 I 0.54826(12) 0.41931(6) 0.2674(2) 0.0772(6) Uani 0.300(13) 1 d . . P . .
N2 N 0.3303(12) 0.5413(11) 0.203(3) 0.139(4) Uani 1 1 d D . . . .
H2A H 0.334873 0.490731 0.216881 0.167 Uiso 1 1 d DR U . . .
H2B H 0.310214 0.548922 0.063602 0.167 Uiso 1 1 d DR U . . .
C1 C 0.1712(14) 0.6183(15) 0.258(3) 0.139(4) Uani 1 1 d D . . . .
H1A H 0.120634 0.622237 0.371736 0.209 Uiso 1 1 calc R U . . .
H1B H 0.142411 0.587895 0.147424 0.209 Uiso 1 1 calc R U . . .
H1C H 0.186537 0.666804 0.203633 0.209 Uiso 1 1 calc R U . . .
N1 N 0.2681(11) 0.5849(7) 0.338(3) 0.139(4) Uani 1 1 d D . . . .
H1D H 0.308987 0.621438 0.386062 0.167 Uiso 1 1 calc R U . . .
H1E H 0.250654 0.557021 0.448979 0.167 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 Br1 3.1842(19) 1_554 ?
Pb1 Br1 3.1336(19) . ?
Pb1 Br2 3.1508(16) 6_656 ?
Pb1 Br2 3.1496(16) . ?
Pb1 Br3 3.0536(14) . ?
Pb1 Br3 3.0536(14) 7_565 ?
N2 H2A 0.9169 . ?
N2 H2B 0.9250 . ?
N2 N1 1.398(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 N1 1.449(2) . ?
N1 H1D 0.8900 . ?
N1 H1E 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
Br1 Pb1 Br1 172.23(5) . 1_554 ?
Br1 Pb1 Br2 94.75(4) . . ?
Br1 Pb1 Br2 86.65(4) . 6_656 ?
Br2 Pb1 Br1 93.02(4) . 1_554 ?
Br2 Pb1 Br1 85.58(4) 6_656 1_554 ?
Br2 Pb1 Br2 178.602(18) . 6_656 ?
Br3 Pb1 Br1 88.57(3) . . ?
Br3 Pb1 Br1 91.23(3) . 1_554 ?
Br3 Pb1 Br1 88.57(3) 7_565 . ?
Br3 Pb1 Br1 91.23(3) 7_565 1_554 ?
Br3 Pb1 Br2 91.51(3) . . ?
Br3 Pb1 Br2 88.52(3) 7_565 6_656 ?
Br3 Pb1 Br2 88.52(3) . 6_656 ?
Br3 Pb1 Br2 91.52(3) 7_565 . ?
Br3 Pb1 Br3 175.99(6) . 7_565 ?
Pb1 Br1 Pb1 172.23(5) . 1_556 ?
Pb1 Br2 Pb1 179.74(5) . 6_556 ?
H2A N2 H2B 104.8 . . ?
N1 N2 H2A 122.4 . . ?
N1 N2 H2B 109.9 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
N2 N1 C1 119.7(16) . . ?
N2 N1 H1D 107.4 . . ?
N2 N1 H1E 107.4 . . ?
C1 N1 H1D 107.4 . . ?
C1 N1 H1E 107.4 . . ?
H1D N1 H1E 106.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2B Br3 0.92 2.80 3.412(18) 124.3 5_665 yes
N1 H1D Br3 0.89 2.92 3.399(15) 115.2 5_666 yes
N1 H1E N2 0.89 2.60 3.465(8) 165.4 2_565 yes

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.555
_oxdiff_exptl_absorpt_empirical_full_min 0.688
####################################################################### 
# 
# 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_MHy2PbBr3_7I0_3_295K
_database_code_depnum_ccdc_archive 'CCDC 2307125'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_audit_creation_date             2023-11-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3.734 I0.266 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 Br3.73 I0.26 N4 Pb'
_chemical_formula_weight         633.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         C2N4Br3.7I0.3Pb
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'
Br Br -0.2901 2.4595 '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 n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.205(4)
_cell_length_b                   17.858(5)
_cell_length_c                   6.054(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1319.7(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5613
_cell_measurement_temperature    294.9(2)
_cell_measurement_theta_max      28.4690
_cell_measurement_theta_min      3.3430
_shelx_estimated_absorpt_T_max   0.577
_shelx_estimated_absorpt_T_min   0.110
_exptl_absorpt_coefficient_mu    24.676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23998
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1123
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 0 1 0.0411
-1 0 0 0.0553
0 1 5 0.0557
0 -1 -5 0.0656
0 1 0 0.0131
0 -1 0 0.0131

_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.025
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.0000 -0.0000 1.0000 0.1245 0.2187 0.1867
-1.0000 0.0000 0.0000 -0.0265 -0.0496 -0.0147
-0.0001 1.0000 5.0000 -0.0761 -0.1277 0.5680
0.0001 -1.0000 -5.0000 0.0761 0.1277 -0.5680
-0.0000 1.0000 0.0000 -0.0352 0.0182 0.0021
0.0000 -1.0000 -0.0000 0.0352 -0.0182 -0.0021

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            20001
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.338
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  45.00   1.00   15.00    --   13.31 -37.00 -30.00  111
  2  ω    -78.00 -32.00   1.00   15.00    --   13.31 178.00-150.00   46
  3  ω    -46.00  65.00   1.00   15.00    --  -14.40  37.00-120.00  111
  4  ω    -18.00  32.00   1.00   15.00    --  -14.40-106.00-167.00   50
  5  ω    -47.00  64.00   1.00   15.00    --  -14.40  57.00 -30.00  111
  6  ω    -25.00  30.00   1.00   15.00    --  -14.40 -99.00  60.00   55
  7  ω   -107.00 -35.00   1.00   15.00    --  -14.40-178.00   0.00   72
  8  ω    -25.00   2.00   1.00   15.00    --  -14.40 -99.00 150.00   27
  9  ω    -94.00  17.00   1.00   15.00    --  -14.40 -37.00-120.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0265296900
_diffrn_orient_matrix_UB_12      -0.0352294204
_diffrn_orient_matrix_UB_13      -0.0081787303
_diffrn_orient_matrix_UB_21      0.0495754656
_diffrn_orient_matrix_UB_22      0.0182084320
_diffrn_orient_matrix_UB_23      -0.0291747906
_diffrn_orient_matrix_UB_31      0.0146960772
_diffrn_orient_matrix_UB_32      0.0021466604
_diffrn_orient_matrix_UB_33      0.1131732171
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                940
_reflns_number_total             1394
_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    ?
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         1394
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0259
_refine_ls_restrained_S_all      1.053
_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)+(0.0306P)²+2.9268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0691
_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,H,H,H) groups
2. Shared sites
{Br1, I1}
{Br3, I3}
{Br2, I2}
3. Restrained distances
 N2-C1
 1.5 with sigma of 0.005
 C1-N2A
 1.5 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(I1)
Uanis(N2) = Uanis(N2A) = Uanis(N3A) = Uanis(N3)
Uanis(Br2) = Uanis(I2)
Uanis(Br3) = Uanis(I3)
5. Others
 Sof(I1)=0.5*(1-FVAR(2))
 Sof(Br1)=0.5*FVAR(2)
 Sof(I2)=0.5*(1-FVAR(3))
 Sof(Br2)=0.5*FVAR(3)
 Fixed Sof: Br3(0.97) I3(0.03) N3A(0.65) H3AA(0.65) H3AB(0.65) H1AA(0.65)
 H1AB(0.65) H1AC(0.65) H1BD(0.35) H1BE(0.35) H1BF(0.35) N2A(0.65) H2AA(0.65)
 H2AB(0.65) N2(0.35) H2A(0.35) H2B(0.35) N3(0.35) H3A(0.35) H3B(0.35)
6.a Rotating group:
 N3A(H3AA,H3AB), N3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), N2(H2A,H2B)
6.c Idealised Me refined as rotating group:
 C1(H1AA,H1AB,H1AC), C1(H1BD,H1BE,H1BF)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.54200(2) 0.250000 0.25372(5) 0.03042(13) Uani 1 2 d S T P . .
Br1 Br 0.56712(8) 0.250000 0.75031(12) 0.0492(4) Uani 0.928(9) 2 d S T P . .
Br2 Br 0.28692(7) 0.250000 0.24231(16) 0.0680(5) Uani 0.866(11) 2 d S T P . .
Br3 Br 0.54666(7) 0.41707(4) 0.26391(11) 0.0572(2) Uani 0.97 1 d . . P . .
I1 I 0.56712(8) 0.250000 0.75031(12) 0.0492(4) Uani 0.072(9) 2 d S T P . .
I2 I 0.28692(7) 0.250000 0.24231(16) 0.0680(5) Uani 0.134(11) 2 d S T P . .
I3 I 0.54666(7) 0.41707(4) 0.26391(11) 0.0572(2) Uani 0.03 1 d . . P . .
N3A N 0.3259(11) 0.5436(8) 0.2057(19) 0.063(2) Uani 0.65 1 d . . P A 1
H3AA H 0.345129 0.578573 0.107325 0.076 Uiso 0.65 1 d R U P A 1
H3AB H 0.386300 0.525833 0.270486 0.076 Uiso 0.65 1 d R U P A 1
C1 C 0.1658(7) 0.6172(5) 0.2539(12) 0.069(2) Uani 1 1 d D . . . .
H1AA H 0.118056 0.582194 0.181891 0.104 Uiso 0.65 1 calc R U P B 1
H1AB H 0.197216 0.650240 0.145907 0.104 Uiso 0.65 1 calc R U P B 1
H1AC H 0.124752 0.645965 0.359319 0.104 Uiso 0.65 1 calc R U P B 1
H1BD H 0.137572 0.608489 0.108180 0.104 Uiso 0.35 1 calc R U P C 2
H1BE H 0.163908 0.669916 0.285374 0.104 Uiso 0.35 1 calc R U P C 2
H1BF H 0.121752 0.590933 0.359865 0.104 Uiso 0.35 1 calc R U P C 2
N2A N 0.2548(8) 0.5759(6) 0.3694(15) 0.063(2) Uani 0.65 1 d D . P A 1
H2AA H 0.292416 0.607080 0.455484 0.076 Uiso 0.65 1 calc R U P A 1
H2AB H 0.226306 0.540059 0.453829 0.076 Uiso 0.65 1 calc R U P A 1
N2 N 0.2818(9) 0.5897(14) 0.267(3) 0.063(2) Uani 0.35 1 d D . P A 2
H2A H 0.320526 0.615122 0.167300 0.076 Uiso 0.35 1 calc R U P A 2
H2B H 0.307699 0.602385 0.399081 0.076 Uiso 0.35 1 calc R U P A 2
N3 N 0.3056(18) 0.5095(15) 0.234(4) 0.063(2) Uani 0.35 1 d . . P A 2
H3A H 0.286869 0.483126 0.354029 0.076 Uiso 0.35 1 d R U P A 2
H3B H 0.265962 0.493003 0.118964 0.076 Uiso 0.35 1 d R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.0222(17) . ?
Pb1 Br1 3.0633(17) 1_554 ?
Pb1 Br2 3.1140(13) . ?
Pb1 Br2 2.9895(13) 6_656 ?
Pb1 Br3 2.9847(11) 7_565 ?
Pb1 Br3 2.9847(11) . ?
N3A H3AA 0.8941 . ?
N3A H3AB 0.8931 . ?
N3A N2A 1.439(16) . ?
C1 H1AA 0.9600 . ?
C1 H1AB 0.9600 . ?
C1 H1AC 0.9600 . ?
C1 H1BD 0.9600 . ?
C1 H1BE 0.9600 . ?
C1 H1BF 0.9600 . ?
C1 N2A 1.487(5) . ?
C1 N2 1.501(5) . ?
N2A H2AA 0.8900 . ?
N2A H2AB 0.8900 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 N3 1.48(4) . ?
N3 H3A 0.8963 . ?
N3 H3B 0.8966 . ?

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
Br1 Pb1 Br1 168.43(4) . 1_554 ?
Br1 Pb1 Br2 97.09(3) . . ?
Br1 Pb1 Br2 94.48(3) 1_554 . ?
Br2 Pb1 Br1 83.72(3) 6_656 . ?
Br2 Pb1 Br1 84.71(3) 6_656 1_554 ?
Br2 Pb1 Br2 179.190(11) 6_656 . ?
Br3 Pb1 Br1 91.069(16) 7_565 1_554 ?
Br3 Pb1 Br1 88.711(16) . . ?
Br3 Pb1 Br1 88.711(16) 7_565 . ?
Br3 Pb1 Br1 91.069(16) . 1_554 ?
Br3 Pb1 Br2 91.119(16) 7_565 . ?
Br3 Pb1 Br2 91.118(16) . . ?
Br3 Pb1 Br2 88.898(16) 7_565 6_656 ?
Br3 Pb1 Br2 88.898(16) . 6_656 ?
Br3 Pb1 Br3 176.78(3) 7_565 . ?
Pb1 Br1 Pb1 168.43(4) . 1_556 ?
Pb1 Br2 Pb1 178.27(4) 6_556 . ?
H3AA N3A H3AB 108.9 . . ?
N2A N3A H3AA 109.7 . . ?
N2A N3A H3AB 109.7 . . ?
H1AA C1 H1AB 109.5 . . ?
H1AA C1 H1AC 109.5 . . ?
H1AB C1 H1AC 109.5 . . ?
H1BD C1 H1BE 109.5 . . ?
H1BD C1 H1BF 109.5 . . ?
H1BE C1 H1BF 109.5 . . ?
N2A C1 H1AA 109.5 . . ?
N2A C1 H1AB 109.5 . . ?
N2A C1 H1AC 109.5 . . ?
N2 C1 H1BD 109.5 . . ?
N2 C1 H1BE 109.5 . . ?
N2 C1 H1BF 109.5 . . ?
N3A N2A C1 108.4(9) . . ?
N3A N2A H2AA 110.0 . . ?
N3A N2A H2AB 110.0 . . ?
C1 N2A H2AA 110.0 . . ?
C1 N2A H2AB 110.0 . . ?
H2AA N2A H2AB 108.4 . . ?
C1 N2 H2A 107.4 . . ?
C1 N2 H2B 107.4 . . ?
H2A N2 H2B 106.9 . . ?
N3 N2 C1 119.8(18) . . ?
N3 N2 H2A 107.4 . . ?
N3 N2 H2B 107.4 . . ?
N2 N3 H3A 110.5 . . ?
N2 N3 H3B 108.5 . . ?
H3A N3 H3B 108.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3A H3AA Br3 0.89 2.61 3.316(11) 136.7 5_665 yes
N3A H3AB Br3 0.89 2.76 3.534(15) 146.0 . yes
N2A H2AA Br3 0.89 2.63 3.289(9) 131.4 5_666 yes
N2A H2AB N3A 0.89 2.23 3.110(17) 170.9 2_565 yes
N2 H2A Br1 0.89 2.82 3.41(3) 125.1 5_666 yes
N2 H2B Br3 0.89 2.73 3.531(17) 150.7 5_666 yes
N3 H3A N3 0.90 2.56 3.335(19) 144.4 2_565 yes
N3 H3B N3 0.90 2.49 3.335(19) 157.1 2_564 yes

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.718
_oxdiff_exptl_absorpt_empirical_full_min 0.634
####################################################################### 
# 
# 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_MHy2PbBr0_9I3_1_295K-average
_database_code_depnum_ccdc_archive 'CCDC 2307128'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_MHy2PbBr0_9I3_1_295K-average 
;
PROBLEM: Check Calcd Resid. Dens.  1.14Ang From I2             -3.09 eA-3
RESPONSE: High positional displacement due to modulation.
;
# Added during the CSD deposition process: Friday 10 November 2023 01:46 PM
# end Validation Reply Form

_audit_creation_date             2023-11-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br0.984 I3.016 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 Br0.98 I3.02 N4 Pb'
_chemical_formula_weight         762.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C Pb I4'
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'
Br Br -0.2901 2.4595 '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 n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.713(4)
_cell_length_b                   18.269(5)
_cell_length_c                   6.362(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1477.6(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16365
_cell_measurement_temperature    295
_cell_measurement_theta_max      29.1840
_cell_measurement_theta_min      3.2010
_shelx_estimated_absorpt_T_max   0.351
_shelx_estimated_absorpt_T_min   0.064
_exptl_absorpt_coefficient_mu    20.346
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46680
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1321
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.065
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0084
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            55660
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_min         3.205
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     32.00 104.00   1.00   15.00    --   13.31-178.00-120.00   72
  2  ω    -25.00  57.00   1.00   15.00    --   13.31 -99.00-150.00   82
  3  ω    -92.00  18.00   1.00   15.00    --  -14.40 -57.00 -60.00  110
  4  ω    -99.00  43.00   1.00   15.00    --  -14.40 -19.00  30.00  142
  5  ω   -107.00 -35.00   1.00   15.00    --  -14.40-178.00-180.00   72
  6  ω    -92.00  18.00   1.00   15.00    --  -14.40 -57.00-180.00  110
  7  ω    -95.00 -17.00   1.00   15.00    --  -14.40 157.00 -40.84   78
  8  ω    -78.00 -32.00   1.00   15.00    --   13.31 178.00 -60.00   46
  9  ω      9.00  83.00   1.00   15.00    --   13.31-143.00 -48.00   74
 10  ω    -79.00 105.00   1.00   15.00    --   13.31   0.00-180.00  184
 11  ω    -79.00 105.00   1.00   15.00    --   13.31   0.00-150.00  184
 12  ω    -79.00 105.00   1.00   15.00    --   13.31   0.00-120.00  184
 13  ω    -87.00 -10.00   1.00   15.00    --  -14.40 146.00  47.11   77
 14  ω    -79.00  29.00   1.00   15.00    --   13.31   0.00 -60.00  108
 15  ω    -79.00 105.00   1.00   15.00    --   13.31   0.00 -90.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0029647421
_diffrn_orient_matrix_UB_12      0.0412337751
_diffrn_orient_matrix_UB_13      -0.0360042821
_diffrn_orient_matrix_UB_21      0.0021807748
_diffrn_orient_matrix_UB_22      0.1035440256
_diffrn_orient_matrix_UB_23      0.0143059479
_diffrn_orient_matrix_UB_31      0.0556860212
_diffrn_orient_matrix_UB_32      -0.0018734526
_diffrn_orient_matrix_UB_33      -0.0024797116
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1173
_reflns_number_total             1548
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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         2.307
_refine_diff_density_min         -2.653
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1548
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.115
_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)+(0.0474P)²+16.7077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1135
_refine_special_details          'averaged structure of the modulated phase'
_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. Shared sites
{Br1, I1}
{Br3, I3}
{Br2, I2}
3. Restrained distances
 N3-C1
 1.45 with sigma of 0.002
 N1-N3
 1.4 with sigma of 0.002
 H1A-H3B_$1
 2.2 with sigma of 0.01
 H3B_$1-H1B
 2.2 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(I1)
Uanis(Br2) = Uanis(I2)
Uanis(C1) = Uanis(N3) = Uanis(N1)
Uanis(Br3) = Uanis(I3)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I1)=0.5*(1-FVAR(2))
 Sof(Br1)=0.5*FVAR(2)
 Sof(I3)=1-FVAR(2)
 Sof(Br3)=FVAR(2)
 Fixed Sof: Br2(0.005) I2(0.495)
7.a Rotating group:
 N1(H1A,H1B)
7.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B)
7.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.54224(4) 0.250000 0.25516(7) 0.0350(2) Uani 1 2 d S T P . .
Br1 Br 0.55989(9) 0.250000 0.75167(13) 0.0558(5) Uani 0.106(16) 2 d S T P . .
Br2 Br 0.29301(8) 0.250000 0.2503(2) 0.1080(8) Uani 0.01 2 d S T P . .
Br3 Br 0.54761(10) 0.42005(5) 0.26496(16) 0.0747(5) Uani 0.434(13) 1 d . . P .
.
I1 I 0.55989(9) 0.250000 0.75167(13) 0.0558(5) Uani 0.894(16) 2 d S T P . .
I2 I 0.29301(8) 0.250000 0.2503(2) 0.1080(8) Uani 0.99 2 d S T P . .
I3 I 0.54761(10) 0.42005(5) 0.26496(16) 0.0747(5) Uani 0.566(13) 1 d . . P . .
N1 N 0.3277(12) 0.5428(10) 0.211(2) 0.138(4) Uani 1 1 d D . . . .
H1A H 0.333980 0.491879 0.222498 0.166 Uiso 1 1 d DR U . . .
H1B H 0.306412 0.550460 0.072830 0.166 Uiso 1 1 d DR U . . .
C1 C 0.1690(15) 0.6191(15) 0.262(3) 0.138(4) Uani 1 1 d D . . . .
H1C H 0.114023 0.616188 0.364796 0.207 Uiso 1 1 calc R U . . .
H1D H 0.147010 0.594614 0.135596 0.207 Uiso 1 1 calc R U . . .
H1E H 0.183687 0.669501 0.231000 0.207 Uiso 1 1 calc R U . . .
N3 N 0.2630(11) 0.5843(7) 0.343(2) 0.138(4) Uani 1 1 d D . . . .
H3A H 0.302843 0.619291 0.398604 0.166 Uiso 1 1 calc R U . . .
H3B H 0.243203 0.555228 0.447889 0.166 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 Br1 3.2111(18) 1_554 ?
Pb1 Br1 3.1669(18) . ?
Pb1 Br2 3.1881(15) 6_656 ?
Pb1 Br2 3.1686(15) . ?
Pb1 Br3 3.1080(13) . ?
Pb1 Br3 3.1081(13) 7_565 ?
N1 H1A 0.9368 . ?
N1 H1B 0.9281 . ?
N1 N3 1.398(2) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 N3 1.449(2) . ?
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
Br1 Pb1 Br1 171.93(5) . 1_554 ?
Br1 Pb1 Br2 94.63(3) . . ?
Br1 Pb1 Br2 86.56(3) . 6_656 ?
Br2 Pb1 Br1 93.44(3) . 1_554 ?
Br2 Pb1 Br1 85.38(3) 6_656 1_554 ?
Br2 Pb1 Br2 178.817(15) . 6_656 ?
Br3 Pb1 Br1 88.76(2) . . ?
Br3 Pb1 Br1 91.06(2) . 1_554 ?
Br3 Pb1 Br1 88.76(2) 7_565 . ?
Br3 Pb1 Br1 91.06(2) 7_565 1_554 ?
Br3 Pb1 Br2 91.27(3) . . ?
Br3 Pb1 Br2 88.76(3) 7_565 6_656 ?
Br3 Pb1 Br2 88.75(3) . 6_656 ?
Br3 Pb1 Br2 91.27(3) 7_565 . ?
Br3 Pb1 Br3 176.59(4) . 7_565 ?
Pb1 Br1 Pb1 171.93(5) . 1_556 ?
Pb1 Br2 Pb1 179.95(5) . 6_556 ?
H1A N1 H1B 104.5 . . ?
N3 N1 H1A 122.7 . . ?
N3 N1 H1B 108.4 . . ?
H1C C1 H1D 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N3 C1 H1C 109.5 . . ?
N3 C1 H1D 109.5 . . ?
N3 C1 H1E 109.5 . . ?
N1 N3 C1 120.6(16) . . ?
N1 N3 H3A 107.2 . . ?
N1 N3 H3B 107.2 . . ?
C1 N3 H3A 107.2 . . ?
C1 N3 H3B 107.2 . . ?
H3A N3 H3B 106.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1B Br3 0.93 2.89 3.483(17) 122.9 5_665 yes
N3 H3B N1 0.89 2.61 3.492(7) 171.1 2_565 yes

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.881
_oxdiff_exptl_absorpt_empirical_full_min 0.788
####################################################################### 
# 
# 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_MHy2PbBr1_5I2_5_295K-average
_database_code_depnum_ccdc_archive 'CCDC 2307129'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_MHy2PbBr1_5I2_5_295K-average 
;
PROBLEM: Check Calcd Resid. Dens.  1.13Ang From I2             -3.72 eA-3
RESPONSE: High positional displacement due to modulation.
;
_vrf_PLAT971_MHy2PbBr1_5I2_5_295K-average 
;
PROBLEM: Check Calcd Resid. Dens.  0.57Ang From I2              2.91 eA-3
RESPONSE: High positional displacement due to modulation.
;
_vrf_PLAT972_MHy2PbBr1_5I2_5_295K-average_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.13Ang From I2             -2.66 eA-3
RESPONSE: High positional displacement due to modulation.
;
# Added during the CSD deposition process: Friday 10 November 2023 01:46 PM
# end Validation Reply Form

_audit_creation_date             2023-11-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br1.612 I2.388 Pb, 2(C H7 N2)'
_chemical_formula_sum            'C2 H14 Br1.61 I2.39 N4 Pb'
_chemical_formula_weight         733.19
_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'
Br Br -0.2901 2.4595 '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 n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.642(4)
_cell_length_b                   18.070(5)
_cell_length_c                   6.330(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1446.2(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13741
_cell_measurement_temperature    295
_cell_measurement_theta_max      28.1930
_cell_measurement_theta_min      3.2530
_shelx_estimated_absorpt_T_max   0.569
_shelx_estimated_absorpt_T_min   0.076
_exptl_absorpt_coefficient_mu    21.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18679
_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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.368
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            54228
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.360
_diffrn_reflns_theta_min         3.223
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  97.00   1.00   12.00    --   13.31  77.00-150.00  120
  2  ω    -25.00  57.00   1.00   12.00    --   13.31 -99.00  90.00   82
  3  ω    -25.00  57.00   1.00   12.00    --   13.31 -99.00-150.00   82
  4  ω    -19.00  91.00   1.00   12.00    --   13.31  57.00   0.00  110
  5  ω    -94.00  17.00   1.00   12.00    --  -14.40 -37.00  30.00  111
  6  ω    -47.00  64.00   1.00   12.00    --  -14.40  57.00 -30.00  111
  7  ω     35.00 106.00   1.00   12.00    --   13.31 178.00  90.00   71
  8  ω    -78.00 -32.00   1.00   12.00    --   13.31 178.00  60.00   46
  9  ω    -86.00  -9.00   1.00   12.00    --  -14.40 144.00 -35.08   77
 10  ω    -77.00  -1.00   1.00   12.00    --  -14.40 130.00  25.68   76
 11  ω    -74.00   3.00   1.00   12.00    --  -14.40 125.00 176.48   77
 12  ω     10.00  83.00   1.00   12.00    --   13.31-144.00  -1.00   73
 13  ω    -79.00 105.00   1.00   12.00    --   13.31   0.00-180.00  184
 14  ω    -79.00 105.00   1.00   12.00    --   13.31   0.00-150.00  184
 15  ω    -79.00 105.00   1.00   12.00    --   13.31   0.00-120.00  184
 16  ω    -25.00  30.00   1.00   12.00    --  -14.40 -99.00-150.00   55
 17  ω    -79.00  -6.00   1.00   12.00    --   13.31   0.00 -90.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0030677951
_diffrn_orient_matrix_UB_12      -0.0358301830
_diffrn_orient_matrix_UB_13      -0.0453022905
_diffrn_orient_matrix_UB_21      0.0145015253
_diffrn_orient_matrix_UB_22      -0.0158582652
_diffrn_orient_matrix_UB_23      0.0983093284
_diffrn_orient_matrix_UB_31      -0.0541253455
_diffrn_orient_matrix_UB_32      -0.0022141761
_diffrn_orient_matrix_UB_33      0.0289207898
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1111
_reflns_number_total             1523
_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    ?
_refine_diff_density_max         2.894
_refine_diff_density_min         -3.252
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1523
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      1.130
_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)+(0.0631P)²+21.2638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1457
_refine_special_details          'averaged structure of the modulated phase'
_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. Shared sites
{Br1, I1}
{Br3, I3}
{Br2, I2}
3. Restrained distances
 N2-C1
 1.45 with sigma of 0.002
 N3-N2
 1.4 with sigma of 0.002
 H2B_$1-H3B
 2.2 with sigma of 0.01
 H2B_$1-H3A
 2.2 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(I1)
Uanis(Br2) = Uanis(I2)
Uanis(C1) = Uanis(N2) = Uanis(N3)
Uanis(Br3) = Uanis(I3)
5. Others
 Sof(I1)=0.5*(1-FVAR(2))
 Sof(Br1)=0.5*FVAR(2)
 Sof(I2)=0.5*(1-FVAR(3))
 Sof(Br2)=0.5*FVAR(3)
 Sof(I3)=1-FVAR(3)
 Sof(Br3)=FVAR(3)
6.a Rotating group:
 N3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.54192(4) 0.250000 0.25604(8) 0.0380(3) Uani 1 2 d S T P . .
Br1 Br 0.55841(12) 0.250000 0.75223(16) 0.0562(6) Uani 0.23(2) 2 d S T P . .
Br2 Br 0.29216(10) 0.250000 0.2494(2) 0.1155(14) Uani 0.06(3) 2 d S T P . .
Br3 Br 0.54798(14) 0.41958(7) 0.2666(2) 0.0768(7) Uani 0.660(16) 1 d . . P . .
I1 I 0.55841(12) 0.250000 0.75223(16) 0.0562(6) Uani 0.77(2) 2 d S T P . .
I2 I 0.29216(10) 0.250000 0.2494(2) 0.1155(14) Uani 0.94(3) 2 d S T P . .
I3 I 0.54798(14) 0.41958(7) 0.2666(2) 0.0768(7) Uani 0.340(16) 1 d . . P . .
N3 N 0.3299(14) 0.5401(13) 0.204(3) 0.145(5) Uani 1 1 d D . . . .
H3A H 0.331264 0.488915 0.219241 0.173 Uiso 1 1 d DR U . . .
H3B H 0.315763 0.546715 0.055990 0.173 Uiso 1 1 d DR U . . .
C1 C 0.1714(17) 0.6200(19) 0.259(3) 0.145(5) Uani 1 1 d D . . . .
H1A H 0.120558 0.621436 0.371678 0.217 Uiso 1 1 calc R U . . .
H1B H 0.143189 0.592030 0.143118 0.217 Uiso 1 1 calc R U . . .
H1C H 0.186610 0.669492 0.213220 0.217 Uiso 1 1 calc R U . . .
N2 N 0.2678(13) 0.5853(8) 0.334(3) 0.145(5) Uani 1 1 d D . . . .
H2A H 0.309609 0.621438 0.379765 0.173 Uiso 1 1 calc R U . . .
H2B H 0.250344 0.558328 0.445988 0.173 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 Br1 3.1961(19) 1_554 ?
Pb1 Br1 3.1479(19) . ?
Pb1 Br2 3.1639(17) 6_656 ?
Pb1 Br2 3.1577(17) . ?
Pb1 Br3 3.0660(16) 7_565 ?
Pb1 Br3 3.0660(16) . ?
N3 H3A 0.9293 . ?
N3 H3B 0.9611 . ?
N3 N2 1.399(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 N2 1.449(2) . ?
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
Br1 Pb1 Br1 172.46(6) . 1_554 ?
Br1 Pb1 Br2 94.56(4) . . ?
Br1 Pb1 Br2 86.83(4) . 6_656 ?
Br2 Pb1 Br1 92.98(4) . 1_554 ?
Br2 Pb1 Br1 85.64(4) 6_656 1_554 ?
Br2 Pb1 Br2 178.614(19) . 6_656 ?
Br3 Pb1 Br1 88.66(3) 7_565 . ?
Br3 Pb1 Br1 91.15(3) 7_565 1_554 ?
Br3 Pb1 Br1 88.66(3) . . ?
Br3 Pb1 Br1 91.15(3) . 1_554 ?
Br3 Pb1 Br2 91.45(3) 7_565 . ?
Br3 Pb1 Br2 88.58(3) . 6_656 ?
Br3 Pb1 Br2 88.58(3) 7_565 6_656 ?
Br3 Pb1 Br2 91.45(3) . . ?
Br3 Pb1 Br3 176.20(6) 7_565 . ?
Pb1 Br1 Pb1 172.46(6) . 1_556 ?
Pb1 Br2 Pb1 179.86(5) . 6_556 ?
H3A N3 H3B 103.3 . . ?
N2 N3 H3A 122.0 . . ?
N2 N3 H3B 113.2 . . ?
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 . . ?
N3 N2 C1 122.3(19) . . ?
N3 N2 H2A 106.8 . . ?
N3 N2 H2B 106.8 . . ?
C1 N2 H2A 106.8 . . ?
C1 N2 H2B 106.8 . . ?
H2A N2 H2B 106.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.402
_oxdiff_exptl_absorpt_empirical_full_min 0.560
