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

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

data_AlaPbBr3_300K
_database_code_depnum_ccdc_archive 'CCDC 2164940'
loop_
_audit_author_name
_audit_author_address
'Alejandro Pedro Ayala'
;Universidade Federal do Ceara
Brazil
;
_audit_update_record             
;
2022-04-06 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_audit_creation_date             2022-04-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H8 N O2, H2 O'
_chemical_formula_sum            'C3 H10 Br3 N O3 Pb'
_chemical_formula_weight         555.04
_chemical_absolute_configuration ad
_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 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   21.8573(12)
_cell_length_b                   6.0851(4)
_cell_length_c                   8.7665(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.367(2)
_cell_angle_gamma                90
_cell_volume                     1163.97(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      72.308
_cell_measurement_theta_min      4.051
_shelx_estimated_absorpt_T_max   0.209
_shelx_estimated_absorpt_T_min   0.083
_exptl_absorpt_coefficient_mu    40.057
_exptl_absorpt_correction_T_max  0.7115
_exptl_absorpt_correction_T_min  0.4228
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1620 before and 0.0905 after correction.
The Ratio of minimum to maximum transmission is 0.5942.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.167
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             984
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 1.00 0.0350
-1.00 -1.00 1.00 0.0170
1.00 1.00 -1.00 0.0710
0.00 0.00 1.00 0.0340
0.00 0.00 -1.00 0.0230
1.00 1.00 1.00 0.0730
-1.00 -1.00 -1.00 0.0120
0.00 1.00 1.00 0.0730
0.00 -1.00 -1.00 0.0080
-1.00 1.00 1.00 0.0760
1.00 -1.00 -1.00 0.0080
-1.00 0.00 0.00 0.0390
1.00 0.00 0.00 0.0260
-1.00 1.00 0.00 0.0790
2.00 -1.00 2.00 0.0110
-2.00 1.00 -2.00 0.0430

_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.057
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13066
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.131
_diffrn_reflns_theta_min         5.054
_diffrn_ambient_temperature      298.00
_diffrn_detector                 HPAD
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'Bruker PHOTON II CPAD Area Detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_type              'Incoatec I\ms HB'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                2062
_reflns_number_total             2075
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2075
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0246
_refine_ls_restrained_S_all      1.109
_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)+(0.0316P)²+2.8200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0635
_refine_special_details          'Refined as a 4-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.88(3)
 0.036(19) 0.067(15) 0.013(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3.a Free rotating group:
 O3(H3D,H3E)
3.b Ternary CH refined with riding coordinates:
 C2(H2A)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.50399(2) 0.25020(12) 0.75599(3) 0.03670(14) Uani 1 1 d . . . . .
Br2 Br 0.40570(4) 0.2637(2) 0.50038(11) 0.0438(3) Uani 1 1 d . . . . .
Br3 Br 0.40329(4) 0.2507(4) 0.97229(11) 0.0530(3) Uani 1 1 d . . . . .
Br1 Br 0.51222(5) 0.7376(5) 0.74809(12) 0.0626(3) Uani 1 1 d . . . . .
N1 N 0.1546(3) 0.2681(14) 0.5626(8) 0.0436(15) Uani 1 1 d . . . . .
H1A H 0.182328 0.213877 0.502507 0.052 Uiso 1 1 calc R U . . .
H1B H 0.139230 0.392046 0.522335 0.052 Uiso 1 1 calc R U . . .
H1C H 0.124557 0.170861 0.570974 0.052 Uiso 1 1 calc R U . . .
O3 O 0.3559(4) 0.7870(16) 0.7945(12) 0.084(3) Uani 1 1 d G . . . .
H3D H 0.382562 0.659520 0.800765 0.126 Uiso 1 1 d G U . . .
H3E H 0.360620 0.886356 0.862374 0.126 Uiso 1 1 d G U . . .
C1 C 0.2357(4) 0.4738(17) 0.6947(11) 0.0422(19) Uani 1 1 d . . . . .
O2 O 0.2592(5) 0.5470(17) 0.8277(9) 0.082(3) Uani 1 1 d . . . . .
H2 H 0.279749 0.657264 0.813993 0.123 Uiso 1 1 calc R U . . .
O1 O 0.2517(3) 0.5279(12) 0.5725(8) 0.0544(18) Uani 1 1 d . . . . .
C2 C 0.1841(4) 0.3143(15) 0.7167(12) 0.045(2) Uani 1 1 d . . . . .
H2A H 0.154123 0.382245 0.780937 0.053 Uiso 1 1 calc R U . . .
C3 C 0.2076(7) 0.104(2) 0.7908(16) 0.075(4) Uani 1 1 d . . . . .
H3A H 0.174169 0.003212 0.799637 0.113 Uiso 1 1 calc R U . . .
H3B H 0.225878 0.135636 0.890668 0.113 Uiso 1 1 calc R U . . .
H3C H 0.237717 0.038962 0.729285 0.113 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 Br2 3.0130(9) . ?
Pb1 Br2 3.0783(10) 2_656 ?
Pb1 Br3 3.0355(9) 2_657 ?
Pb1 Br3 2.9883(9) . ?
Pb1 Br1 3.125(3) 1_545 ?
Pb1 Br1 2.973(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.489(12) . ?
O3 H3D 0.9703 . ?
O3 H3E 0.8501 . ?
C1 O2 1.324(13) . ?
C1 O1 1.192(11) . ?
C1 C2 1.509(12) . ?
O2 H2 0.8200 . ?
C2 H2A 0.9800 . ?
C2 C3 1.513(14) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 85.19(3) . 2_656 ?
Br2 Pb1 Br3 176.05(4) . 2_657 ?
Br2 Pb1 Br1 88.29(4) 2_656 1_545 ?
Br2 Pb1 Br1 92.88(4) . 1_545 ?
Br3 Pb1 Br2 172.33(3) . 2_656 ?
Br3 Pb1 Br2 98.38(3) 2_657 2_656 ?
Br3 Pb1 Br2 87.27(3) . . ?
Br3 Pb1 Br3 89.12(2) . 2_657 ?
Br3 Pb1 Br1 93.47(5) . 1_545 ?
Br3 Pb1 Br1 88.95(6) 2_657 1_545 ?
Br1 Pb1 Br2 89.83(4) . . ?
Br1 Pb1 Br2 85.07(4) . 2_656 ?
Br1 Pb1 Br3 88.79(6) . 2_657 ?
Br1 Pb1 Br3 93.54(5) . . ?
Br1 Pb1 Br1 172.60(4) . 1_545 ?
Pb1 Br2 Pb1 94.73(3) . 2_656 ?
Pb1 Br3 Pb1 90.88(2) . 2_657 ?
Pb1 Br1 Pb1 172.60(4) . 1_565 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H3D O3 H3E 118.7 . . ?
O2 C1 C2 111.0(9) . . ?
O1 C1 O2 125.4(9) . . ?
O1 C1 C2 123.6(9) . . ?
C1 O2 H2 109.5 . . ?
N1 C2 C1 107.0(7) . . ?
N1 C2 H2A 109.4 . . ?
N1 C2 C3 110.4(8) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 C3 111.2(8) . . ?
C3 C2 H2A 109.4 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 N1 171.5(9) . . . . ?
O2 C1 C2 C3 -67.9(12) . . . . ?
O1 C1 C2 N1 -7.2(13) . . . . ?
O1 C1 C2 C3 113.4(12) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.88(3)
2 0.036(19)
3 0.067(15)
4 0.013(19)

