# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_G2PbI4_1_02
_database_code_depnum_ccdc_archive 'CCDC 2428383'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_systematic        'Guanidinium lead(II) tetraiodide'
_chemical_formula_sum            'C2 H12 I4 N6 Pb'
_chemical_formula_weight         834.97
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   9.1051(7)
_cell_length_b                   12.466(4)
_cell_length_c                   14.0938(16)
_cell_angle_alpha                67.82(2)
_cell_angle_beta                 85.226(7)
_cell_angle_gamma                87.169(14)
_cell_volume                     1475.9(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    938
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       1020000(30000)
_cell_measurement_theta_max      21.1040
_cell_measurement_theta_min      2.2280
_exptl_absorpt_coefficient_mu    19.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 0.15(3) GPa
(150000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.758
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.032
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.1264
_diffrn_reflns_Laue_measured_fraction_full 0.175
_diffrn_reflns_Laue_measured_fraction_max 0.136
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            1668
_diffrn_reflns_point_group_measured_fraction_full 0.175
_diffrn_reflns_point_group_measured_fraction_max 0.136
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.419
_diffrn_reflns_theta_min         1.564
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.175
_diffrn_measured_fraction_theta_max 0.136
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   60.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   60.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   60.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   60.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   60.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   60.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   60.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   60.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   60.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   60.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   60.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   60.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   60.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   60.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   60.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   60.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0016753000
_diffrn_orient_matrix_UB_12      0.0610300000
_diffrn_orient_matrix_UB_13      -0.0148987000
_diffrn_orient_matrix_UB_21      0.0389133000
_diffrn_orient_matrix_UB_22      0.0046503000
_diffrn_orient_matrix_UB_23      -0.0470842000
_diffrn_orient_matrix_UB_31      -0.0677951000
_diffrn_orient_matrix_UB_32      0.0055582000
_diffrn_orient_matrix_UB_33      -0.0230064000
_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                890
_reflns_number_total             1668
_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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.347
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.330
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1668
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0615
_refine_ls_restrained_S_all      1.097
_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)+(0.0824P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1749
_refine_special_details          
;
 Refined as a 3-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.44(11)
 0.31(4) 0.25(10)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
3. Restrained distances
 C19-N1
 1.3 with sigma of 0.02
 C39-N25
 1.3 with sigma of 0.02
4. Others
 Uiso(N3)=Uiso(N10)=Uiso(N17)=FVAR(1)
 Uiso(C39)=Uiso(C3)=Uiso(C30)=Uiso(C19)=FVAR(2)
5.a X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N34(H34A,H34B), N10(H10A,H10B), N11(H11A,H11B), N25(H25A,H25B),
 N6(H6A,H6B), N14(H14A,H14B), N19(H19A,H19B), N1(H1A,H1B), N17(H17A,H17B),
 N39(H39A,H39B), N20(H20A,H20B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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
Pb01 Pb 0.2054(3) 0.6637(7) 0.1828(2) 0.025(6) Uani 1 1 d . . . . .
Pb02 Pb 0.2480(3) 0.1681(7) 0.1660(2) 0.030(6) Uani 1 1 d . . . . .
I003 I 0.0111(5) 0.2002(12) 0.0010(4) 0.044(9) Uani 1 1 d . . . . .
I004 I 0.0112(5) 0.1049(11) 0.3415(4) 0.0391(18) Uiso 1 1 d . . . . .
I005 I 0.5107(6) 0.1134(12) 0.3137(4) 0.042(9) Uani 1 1 d . . . . .
I006 I 0.1812(6) 0.4344(12) 0.1402(4) 0.041(11) Uani 1 1 d . . . . .
I007 I 0.4318(5) 0.5613(11) 0.3476(4) 0.043(9) Uani 1 1 d . . . . .
I008 I 0.2711(6) -0.0948(14) 0.2003(5) 0.043(11) Uani 1 1 d . . . . .
I00A I 0.5122(5) 0.2576(11) -0.0185(4) 0.047(9) Uani 1 1 d . . . . .
I2 I -0.0601(5) 0.5881(11) 0.3491(4) 0.039(9) Uani 1 1 d . . . . .
N3 N 0.138(6) 0.103(12) 0.784(5) 0.049(14) Uiso 1 1 d . U . . .
H3A H 0.104574 0.155568 0.729744 0.059 Uiso 1 1 calc R U . . .
H3B H 0.091135 0.040004 0.814926 0.059 Uiso 1 1 calc R U . . .
N34 N 0.793(6) 0.551(12) 0.125(4) 0.027(19) Uiso 1 1 d . . . . .
H34A H 0.886350 0.561172 0.114220 0.032 Uiso 1 1 calc R U . . .
H34B H 0.734741 0.607219 0.126090 0.032 Uiso 1 1 calc R U . . .
N10 N 0.307(7) 0.028(12) 0.896(5) 0.049(14) Uiso 1 1 d . U . . .
H10A H 0.391197 0.033699 0.917620 0.059 Uiso 1 1 calc R U . . .
H10B H 0.257761 -0.034279 0.925034 0.059 Uiso 1 1 calc R U . . .
N11 N 0.215(5) 0.301(11) 0.416(4) 0.023(17) Uiso 1 1 d . . . . .
H11A H 0.232096 0.374407 0.393280 0.028 Uiso 1 1 calc R U . . .
H11B H 0.152312 0.275867 0.387381 0.028 Uiso 1 1 calc R U . . .
N25 N 0.803(7) 0.338(10) 0.145(4) 0.05(2) Uiso 1 1 d D . . . .
H25A H 0.758475 0.278054 0.146650 0.060 Uiso 1 1 calc R U . . .
H25B H 0.897811 0.337039 0.144381 0.060 Uiso 1 1 calc R U . . .
N6 N 0.862(6) 0.266(14) 0.539(5) 0.06(3) Uiso 1 1 d . . . . .
H6A H 0.899858 0.333639 0.517574 0.074 Uiso 1 1 calc R U . . .
H6B H 0.888792 0.213041 0.594981 0.074 Uiso 1 1 calc R U . . .
N14 N 0.722(7) 0.327(14) 0.396(5) 0.06(2) Uiso 1 1 d . . . . .
H14A H 0.759019 0.394801 0.374770 0.072 Uiso 1 1 calc R U . . .
H14B H 0.657804 0.311686 0.361949 0.072 Uiso 1 1 calc R U . . .
N19 N 0.572(5) 0.414(10) 0.146(4) 0.032(19) Uiso 1 1 d . . . . .
H19A H 0.539685 0.349539 0.147418 0.038 Uiso 1 1 calc R U . . .
H19B H 0.510857 0.468927 0.145646 0.038 Uiso 1 1 calc R U . . .
C39 C 0.728(9) 0.429(11) 0.144(6) 0.038(14) Uiso 1 1 d D U . . .
N1 N 0.380(6) 0.267(11) 0.536(4) 0.04(2) Uiso 1 1 d D . . . .
H1A H 0.397885 0.340121 0.514218 0.053 Uiso 1 1 calc R U . . .
H1B H 0.424606 0.218954 0.586285 0.053 Uiso 1 1 calc R U . . .
N17 N 0.331(7) 0.201(13) 0.781(5) 0.049(14) Uiso 1 1 d . U . . .
H17A H 0.308482 0.258717 0.727107 0.059 Uiso 1 1 calc R U . . .
H17B H 0.409732 0.201684 0.810403 0.059 Uiso 1 1 calc R U . . .
N39 N 0.712(8) 0.128(16) 0.516(6) 0.07(3) Uiso 1 1 d . . . . .
H39A H 0.744677 0.073831 0.569294 0.088 Uiso 1 1 calc R U . . .
H39B H 0.648254 0.113189 0.481617 0.088 Uiso 1 1 calc R U . . .
C3 C 0.253(8) 0.119(17) 0.815(7) 0.038(14) Uiso 1 1 d . U . . .
C30 C 0.764(9) 0.243(17) 0.486(7) 0.038(14) Uiso 1 1 d . U . . .
C19 C 0.284(8) 0.231(12) 0.491(6) 0.038(14) Uiso 1 1 d D U . . .
N20 N 0.228(6) 0.122(13) 0.555(5) 0.04(2) Uiso 1 1 d . . . . .
H20A H 0.144586 0.100877 0.544606 0.049 Uiso 1 1 calc R U . . .
H20B H 0.277034 0.077301 0.605279 0.049 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
Pb01 I003 3.267(7) 2_565 ?
Pb01 I006 3.156(16) . ?
Pb01 I007 3.093(6) . ?
Pb01 I008 3.200(18) 1_565 ?
Pb01 I00A 3.237(6) 2_665 ?
Pb01 I2 3.137(6) . ?
Pb02 I003 3.205(6) . ?
Pb02 I004 3.032(6) . ?
Pb02 I005 3.180(6) . ?
Pb02 I006 3.233(17) . ?
Pb02 I008 3.125(16) . ?
Pb02 I00A 3.291(6) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 C3 1.22(10) . ?
N34 H34A 0.8600 . ?
N34 H34B 0.8600 . ?
N34 C39 1.57(15) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
N10 C3 1.37(14) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N11 C19 1.29(11) . ?
N25 H25A 0.8600 . ?
N25 H25B 0.8600 . ?
N25 C39 1.30(3) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
N6 C30 1.32(13) . ?
N14 H14A 0.8600 . ?
N14 H14B 0.8600 . ?
N14 C30 1.37(13) . ?
N19 H19A 0.8600 . ?
N19 H19B 0.8600 . ?
N19 C39 1.44(9) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C19 1.31(3) . ?
N17 H17A 0.8600 . ?
N17 H17B 0.8600 . ?
N17 C3 1.19(19) . ?
N39 H39A 0.8600 . ?
N39 H39B 0.8600 . ?
N39 C30 1.4(3) . ?
C19 N20 1.40(16) . ?
N20 H20A 0.8600 . ?
N20 H20B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I006 Pb01 I003 90.2(3) . 2_565 ?
I006 Pb01 I008 171.31(17) . 1_565 ?
I006 Pb01 I00A 90.9(3) . 2_665 ?
I007 Pb01 I003 173.3(4) . 2_565 ?
I007 Pb01 I006 94.9(3) . . ?
I007 Pb01 I008 84.7(3) . 1_565 ?
I007 Pb01 I00A 86.10(16) . 2_665 ?
I007 Pb01 I2 91.79(17) . . ?
I008 Pb01 I003 89.5(3) 1_565 2_565 ?
I008 Pb01 I00A 80.4(3) 1_565 2_665 ?
I00A Pb01 I003 89.46(17) 2_665 2_565 ?
I2 Pb01 I003 92.54(16) . 2_565 ?
I2 Pb01 I006 90.4(3) . . ?
I2 Pb01 I008 98.3(3) . 1_565 ?
I2 Pb01 I00A 177.6(2) . 2_665 ?
I003 Pb02 I006 88.1(3) . . ?
I003 Pb02 I00A 90.74(15) . . ?
I004 Pb02 I003 92.00(16) . . ?
I004 Pb02 I005 93.74(16) . . ?
I004 Pb02 I006 86.4(3) . . ?
I004 Pb02 I008 87.5(3) . . ?
I004 Pb02 I00A 174.5(4) . . ?
I005 Pb02 I003 171.4(4) . . ?
I005 Pb02 I006 98.6(3) . . ?
I005 Pb02 I00A 84.08(15) . . ?
I006 Pb02 I00A 88.9(3) . . ?
I008 Pb02 I003 88.4(3) . . ?
I008 Pb02 I005 85.5(3) . . ?
I008 Pb02 I006 172.85(18) . . ?
I008 Pb02 I00A 97.3(3) . . ?
Pb02 I003 Pb01 157.9(5) . 2_565 ?
Pb01 I006 Pb02 157.3(2) . . ?
Pb02 I008 Pb01 160.2(2) . 1_545 ?
Pb01 I00A Pb02 174.4(2) 2_665 . ?
H3A N3 H3B 120.0 . . ?
C3 N3 H3A 120.0 . . ?
C3 N3 H3B 120.0 . . ?
H34A N34 H34B 120.0 . . ?
C39 N34 H34A 120.0 . . ?
C39 N34 H34B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C3 N10 H10A 120.0 . . ?
C3 N10 H10B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C19 N11 H11A 120.0 . . ?
C19 N11 H11B 120.0 . . ?
H25A N25 H25B 120.0 . . ?
C39 N25 H25A 120.0 . . ?
C39 N25 H25B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C30 N6 H6A 120.0 . . ?
C30 N6 H6B 120.0 . . ?
H14A N14 H14B 120.0 . . ?
C30 N14 H14A 120.0 . . ?
C30 N14 H14B 120.0 . . ?
H19A N19 H19B 120.0 . . ?
C39 N19 H19A 120.0 . . ?
C39 N19 H19B 120.0 . . ?
N25 C39 N34 126(8) . . ?
N25 C39 N19 112(9) . . ?
N19 C39 N34 122(9) . . ?
H1A N1 H1B 120.0 . . ?
C19 N1 H1A 120.0 . . ?
C19 N1 H1B 120.0 . . ?
H17A N17 H17B 120.0 . . ?
C3 N17 H17A 120.0 . . ?
C3 N17 H17B 120.0 . . ?
H39A N39 H39B 120.0 . . ?
C30 N39 H39A 120.0 . . ?
C30 N39 H39B 120.0 . . ?
N3 C3 N10 117(10) . . ?
N17 C3 N3 128(10) . . ?
N17 C3 N10 114(8) . . ?
N6 C30 N14 120(10) . . ?
N6 C30 N39 120(10) . . ?
N14 C30 N39 120(10) . . ?
N11 C19 N1 121(10) . . ?
N11 C19 N20 123(7) . . ?
N1 C19 N20 112(8) . . ?
C19 N20 H20A 120.0 . . ?
C19 N20 H20B 120.0 . . ?
H20A N20 H20B 120.0 . . ?

_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 2.328
_oxdiff_exptl_absorpt_empirical_full_min 0.685
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.44(11)
2 0.31(4)
3 0.25(10)

_twin_special_details            
;
Component 2 rotated by 179.9887° 
 around [0.00 -0.00 1.00] (reciprocal) or [-0.09 -0.39 0.92] (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_G2PbI4_0_15
_database_code_depnum_ccdc_archive 'CCDC 2428384'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_systematic        'Guanidinium lead(II) tetraiodide'
_chemical_formula_sum            'C2 H12 I4 N6 Pb'
_chemical_formula_weight         834.97
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.742(6)
_cell_length_b                   26.9140(17)
_cell_length_c                   9.2472(4)
_cell_angle_alpha                90
_cell_angle_beta                 88.992(11)
_cell_angle_gamma                90
_cell_volume                     3170.9(14)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2037
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       150000(30000)
_cell_measurement_theta_max      23.3780
_cell_measurement_theta_min      2.6540
_exptl_absorpt_coefficient_mu    18.410
_exptl_absorpt_correction_T_max  0.23279
_exptl_absorpt_correction_T_min  0.21238
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 0.15(3) GPa
(150000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.498
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.032
_exptl_crystal_size_rad          0.04
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.301
_diffrn_reflns_Laue_measured_fraction_max 0.235
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14294
_diffrn_reflns_point_group_measured_fraction_full 0.301
_diffrn_reflns_point_group_measured_fraction_max 0.235
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_min         1.513
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.301
_diffrn_measured_fraction_theta_max 0.235
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   60.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   60.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   60.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   60.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   60.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   60.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   60.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   60.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   60.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   60.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   60.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   60.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   60.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   60.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   60.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   60.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0019354000
_diffrn_orient_matrix_UB_12      -0.0071520000
_diffrn_orient_matrix_UB_13      -0.0534815000
_diffrn_orient_matrix_UB_21      0.0334159000
_diffrn_orient_matrix_UB_22      -0.0227661000
_diffrn_orient_matrix_UB_23      0.0146055000
_diffrn_orient_matrix_UB_31      -0.0690819000
_diffrn_orient_matrix_UB_32      -0.0112041000
_diffrn_orient_matrix_UB_33      0.0044831000
_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                1094
_reflns_number_total             1864
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       0.000097(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1864
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0612
_refine_ls_restrained_S_all      1.099
_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)+(0.0228P)²+130.6049P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1323
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Restrained distances
 C3-N58
 1.3 with sigma of 0.02
 C17-N11
 1.3 with sigma of 0.02
3. Others
 Uiso(N4)=Uiso(N5)=Uiso(N11)=Uiso(N19)=Uiso(N25)=Uiso(N26)=Uiso(N28)=Uiso(N30)=
 Uiso(N33)=Uiso(N48)=Uiso(N54)=Uiso(N58)=FVAR(1)
 Uiso(C3)=Uiso(C17)=Uiso(C38)=Uiso(C47)=FVAR(2)
4.a X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), N11(H11A,H11B), N19(H19A,H19B), N25(H25A,H25B),
 N26(H26A,H26B), N28(H28A,H28B), N30(H30A,H30B), N33(H33A,H33B), N48(H48A,H48B),
  N54(H54A,H54B), N58(H58A,H58B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.2418(3) 0.08449(5) 0.25166(16) 0.041(2) Uani 1 1 d . . . . .
Pb2 Pb 0.7445(3) 0.08989(5) 0.24156(16) 0.044(2) Uani 1 1 d . . . . .
I3 I 0.4964(6) 0.07477(10) 0.1925(3) 0.046(5) Uani 1 1 d . . . . .
I4 I 0.6989(5) 0.16786(9) 0.4760(3) 0.060(4) Uani 1 1 d . . . . .
I5 I -0.0074(5) 0.10367(10) 0.3017(3) 0.051(4) Uani 1 1 d . . . . .
I6 I 0.2048(5) 0.00107(8) -0.0001(3) 0.048(4) Uani 1 1 d . . . . .
I7 I 0.2416(5) 0.16780(9) 0.0224(3) 0.054(4) Uani 1 1 d . . . . .
I8 I 0.2458(5) -0.00489(8) 0.5017(3) 0.049(4) Uani 1 1 d . . . . .
I9 I 0.2755(5) 0.15692(9) 0.5125(3) 0.069(4) Uani 1 1 d . . . . .
I10 I 0.7613(5) 0.17118(9) 0.0014(3) 0.058(4) Uani 1 1 d . . . . .
C3 C 0.501(6) 0.2553(15) 0.193(4) 0.051(7) Uiso 1 1 d D U . . .
N4 N 0.502(6) 0.9336(12) 0.408(4) 0.094(4) Uiso 1 1 d . U . . .
H4A H 0.447424 0.937097 0.462850 0.113 Uiso 1 1 calc R U . . .
H4B H 0.562954 0.930375 0.444934 0.113 Uiso 1 1 calc R U . . .
N5 N 0.493(7) 0.8110(13) 0.185(4) 0.094(4) Uiso 1 1 d . U . . .
H5A H 0.448034 0.823864 0.127306 0.113 Uiso 1 1 calc R U . . .
H5B H 0.544616 0.828349 0.214799 0.113 Uiso 1 1 calc R U . . .
N11 N 0.551(6) 0.7464(14) 0.304(4) 0.094(4) Uiso 1 1 d D U . . .
H11A H 0.543957 0.715580 0.326474 0.113 Uiso 1 1 calc R U . . .
H11B H 0.604265 0.762876 0.334736 0.113 Uiso 1 1 calc R U . . .
C17 C 0.482(6) 0.7682(15) 0.225(4) 0.051(7) Uiso 1 1 d D U . . .
N19 N 0.574(7) 0.2766(14) 0.242(4) 0.094(4) Uiso 1 1 d . U . . .
H19A H 0.603979 0.265235 0.318410 0.113 Uiso 1 1 calc R U . . .
H19B H 0.597427 0.303223 0.201771 0.113 Uiso 1 1 calc R U . . .
N25 N 0.415(7) 0.7412(14) 0.193(4) 0.094(4) Uiso 1 1 d . U . . .
H25A H 0.367001 0.751001 0.135400 0.113 Uiso 1 1 calc R U . . .
H25B H 0.413557 0.711421 0.226808 0.113 Uiso 1 1 calc R U . . .
N26 N 0.516(6) 0.4514(13) 0.197(4) 0.094(4) Uiso 1 1 d . U . . .
H26A H 0.488746 0.462714 0.118491 0.113 Uiso 1 1 calc R U . . .
H26B H 0.569795 0.465557 0.232326 0.113 Uiso 1 1 calc R U . . .
N28 N 0.506(7) 0.4062(12) 0.388(4) 0.094(4) Uiso 1 1 d . U . . .
H28A H 0.470337 0.385596 0.439773 0.113 Uiso 1 1 calc R U . . .
H28B H 0.560430 0.420494 0.422649 0.113 Uiso 1 1 calc R U . . .
N30 N 0.472(6) 0.2156(13) 0.262(4) 0.094(4) Uiso 1 1 d . U . . .
H30A H 0.504645 0.206246 0.337362 0.113 Uiso 1 1 calc R U . . .
H30B H 0.419020 0.198621 0.232023 0.113 Uiso 1 1 calc R U . . .
N33 N 0.408(8) 0.9377(13) 0.195(5) 0.094(4) Uiso 1 1 d . U . . .
H33A H 0.351440 0.941232 0.246137 0.113 Uiso 1 1 calc R U . . .
H33B H 0.404996 0.937267 0.102117 0.113 Uiso 1 1 calc R U . . .
C38 C 0.491(9) 0.9333(14) 0.253(4) 0.051(7) Uiso 1 1 d . U . . .
C47 C 0.478(8) 0.4160(15) 0.255(4) 0.051(7) Uiso 1 1 d . U . . .
N48 N 0.602(7) 0.9295(12) 0.203(5) 0.094(4) Uiso 1 1 d . U . . .
H48A H 0.617616 0.930411 0.112003 0.113 Uiso 1 1 calc R U . . .
H48B H 0.651672 0.926475 0.264848 0.113 Uiso 1 1 calc R U . . .
N54 N 0.403(7) 0.3968(15) 0.205(4) 0.094(4) Uiso 1 1 d . U . . .
H54A H 0.376366 0.408292 0.126945 0.113 Uiso 1 1 calc R U . . .
H54B H 0.374909 0.371268 0.246698 0.113 Uiso 1 1 calc R U . . .
N58 N 0.435(6) 0.2774(14) 0.110(4) 0.094(4) Uiso 1 1 d D U . . .
H58A H 0.443356 0.308227 0.088593 0.113 Uiso 1 1 calc R U . . .
H58B H 0.382392 0.261246 0.076089 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 I3 3.291(8) . ?
Pb1 I5 3.242(8) . ?
Pb1 I6 3.275(3) . ?
Pb1 I7 3.086(3) . ?
Pb1 I8 3.338(3) . ?
Pb1 I9 3.137(3) . ?
Pb2 I3 3.228(8) . ?
Pb2 I4 3.066(3) . ?
Pb2 I5 3.240(8) 1_655 ?
Pb2 I6 3.368(3) 3_655 ?
Pb2 I8 3.300(3) 3_656 ?
Pb2 I10 3.122(3) . ?
C3 N19 1.20(9) . ?
C3 N30 1.29(5) . ?
C3 N58 1.29(2) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C38 1.44(5) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N5 C17 1.22(4) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N11 C17 1.30(2) . ?
C17 N25 1.16(8) . ?
N19 H19A 0.8600 . ?
N19 H19B 0.8600 . ?
N25 H25A 0.8600 . ?
N25 H25B 0.8600 . ?
N26 H26A 0.8600 . ?
N26 H26B 0.8600 . ?
N26 C47 1.20(6) . ?
N28 H28A 0.8600 . ?
N28 H28B 0.8600 . ?
N28 C47 1.31(6) . ?
N30 H30A 0.8600 . ?
N30 H30B 0.8600 . ?
N33 H33A 0.8600 . ?
N33 H33B 0.8600 . ?
N33 C38 1.20(14) . ?
C38 N48 1.49(13) . ?
C47 N54 1.19(11) . ?
N48 H48A 0.8600 . ?
N48 H48B 0.8600 . ?
N54 H54A 0.8600 . ?
N54 H54B 0.8600 . ?
N58 H58A 0.8600 . ?
N58 H58B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3 Pb1 I8 91.75(13) . . ?
I5 Pb1 I3 175.22(8) . . ?
I5 Pb1 I6 93.32(14) . . ?
I5 Pb1 I8 92.47(13) . . ?
I6 Pb1 I3 88.91(13) . . ?
I6 Pb1 I8 90.15(7) . . ?
I7 Pb1 I3 87.50(14) . . ?
I7 Pb1 I5 88.26(14) . . ?
I7 Pb1 I6 90.45(8) . . ?
I7 Pb1 I8 179.03(19) . . ?
I7 Pb1 I9 94.50(8) . . ?
I9 Pb1 I3 91.68(16) . . ?
I9 Pb1 I5 86.47(15) . . ?
I9 Pb1 I6 175.03(8) . . ?
I9 Pb1 I8 84.90(8) . . ?
I3 Pb2 I5 178.10(9) . 1_655 ?
I3 Pb2 I6 89.54(13) . 3_655 ?
I3 Pb2 I8 93.59(13) . 3_656 ?
I4 Pb2 I3 90.66(16) . . ?
I4 Pb2 I5 88.51(15) . 1_655 ?
I4 Pb2 I6 176.48(8) . 3_655 ?
I4 Pb2 I8 88.55(8) . 3_656 ?
I4 Pb2 I10 91.90(8) . . ?
I5 Pb2 I6 91.19(14) 1_655 3_655 ?
I5 Pb2 I8 84.68(13) 1_655 3_656 ?
I8 Pb2 I6 87.93(7) 3_656 3_655 ?
I10 Pb2 I3 92.49(14) . . ?
I10 Pb2 I5 89.25(15) . 1_655 ?
I10 Pb2 I6 91.60(8) . 3_655 ?
I10 Pb2 I8 173.9(2) . 3_656 ?
Pb2 I3 Pb1 158.71(10) . . ?
Pb2 I5 Pb1 155.95(10) 1_455 . ?
Pb1 I6 Pb2 160.3(2) . 3_655 ?
Pb2 I8 Pb1 177.47(14) 3_656 . ?
N19 C3 N30 115(5) . . ?
N19 C3 N58 122(5) . . ?
N30 C3 N58 119(6) . . ?
H4A N4 H4B 120.0 . . ?
C38 N4 H4A 120.0 . . ?
C38 N4 H4B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C17 N5 H5A 120.0 . . ?
C17 N5 H5B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C17 N11 H11A 120.0 . . ?
C17 N11 H11B 120.0 . . ?
N5 C17 N11 122(6) . . ?
N25 C17 N5 126(7) . . ?
N25 C17 N11 112(5) . . ?
C3 N19 H19A 120.0 . . ?
C3 N19 H19B 120.0 . . ?
H19A N19 H19B 120.0 . . ?
C17 N25 H25A 120.0 . . ?
C17 N25 H25B 120.0 . . ?
H25A N25 H25B 120.0 . . ?
H26A N26 H26B 120.0 . . ?
C47 N26 H26A 120.0 . . ?
C47 N26 H26B 120.0 . . ?
H28A N28 H28B 120.0 . . ?
C47 N28 H28A 120.0 . . ?
C47 N28 H28B 120.0 . . ?
C3 N30 H30A 120.0 . . ?
C3 N30 H30B 120.0 . . ?
H30A N30 H30B 120.0 . . ?
H33A N33 H33B 120.0 . . ?
C38 N33 H33A 120.0 . . ?
C38 N33 H33B 120.0 . . ?
N4 C38 N48 102(8) . . ?
N33 C38 N4 123(10) . . ?
N33 C38 N48 135(5) . . ?
N26 C47 N28 118(7) . . ?
N54 C47 N26 119(6) . . ?
N54 C47 N28 121(6) . . ?
C38 N48 H48A 120.0 . . ?
C38 N48 H48B 120.0 . . ?
H48A N48 H48B 120.0 . . ?
C47 N54 H54A 120.0 . . ?
C47 N54 H54B 120.0 . . ?
H54A N54 H54B 120.0 . . ?
C3 N58 H58A 120.0 . . ?
C3 N58 H58B 120.0 . . ?
H58A N58 H58B 120.0 . . ?

_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 1.685
_oxdiff_exptl_absorpt_empirical_full_min 0.755
####################################################################### 
# 
# 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_CsGPbI4_1_21
_database_code_depnum_ccdc_archive 'CCDC 2428394'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   18.217(6)
_cell_length_b                   12.3881(3)
_cell_length_c                   11.9171(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2689.4(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3652
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       1210000(30000)
_cell_measurement_theta_max      27.9620
_cell_measurement_theta_min      1.7360
_shelx_estimated_absorpt_T_max   0.442
_shelx_estimated_absorpt_T_min   0.097
_exptl_absorpt_coefficient_mu    24.354
_exptl_absorpt_correction_T_max  0.158
_exptl_absorpt_correction_T_min  0.058
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 1.21(3) GPa
(1210000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.484
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -1 -17 0.0746
3 1 17 0.0636
5 -17 2 0.0679
-5 17 -4 0.1066
-1 14 10 0.0858
-5 10 -13 0.0855
25 3 -2 0.0220
-25 -3 2 0.0220

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.044
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.406     0.454
         range of gasket transmission (min-max)           0.446     1.000
         range of P media transmission (min-max)          1.000     1.000

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

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

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 161.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
-3.3691 -1.0036 -16.6177 -0.0062 -0.8403 -0.5420
3.2766 1.3534 16.6027 0.0061 0.8291 0.5590
4.7185 -17.0672 1.6715 0.0057 0.5966 -0.8025
-5.0396 16.7074 -3.5641 -0.0063 -0.6850 0.7286
-1.2926 13.8133 10.2276 -0.0001 0.1236 0.9923
-5.4216 9.7166 -13.4900 -0.0082 -0.9963 0.0857
25.0479 3.0337 -2.4534 -1.0000 0.0000 0.0000
-25.0479 -3.0337 2.4534 1.0000 0.0000 0.0000

_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.360
_diffrn_reflns_Laue_measured_fraction_max 0.288
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11151
_diffrn_reflns_point_group_measured_fraction_full 0.360
_diffrn_reflns_point_group_measured_fraction_max 0.288
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.476
_diffrn_reflns_theta_min         2.371
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.360
_diffrn_measured_fraction_theta_max 0.288
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   70.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   70.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   70.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   70.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0378701000
_diffrn_orient_matrix_UB_12      -0.0099552000
_diffrn_orient_matrix_UB_13      0.0086542000
_diffrn_orient_matrix_UB_21      0.0083077000
_diffrn_orient_matrix_UB_22      -0.0277059000
_diffrn_orient_matrix_UB_23      0.0505584000
_diffrn_orient_matrix_UB_31      -0.0029905000
_diffrn_orient_matrix_UB_32      0.0491585000
_diffrn_orient_matrix_UB_33      0.0302537000
_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                651
_reflns_number_total             1025
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.000076(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1025
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0304
_refine_ls_restrained_S_all      1.229
_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)+(0.0172P)²+24.7942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0708
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5)
 Fixed X: H22(0.55893)
 Fixed Y: H22(0.12215)
 Fixed Z: H22(0.062429)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_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 0.25062(8) 0.87487(6) 0.25108(4) 0.0266(10) Uani 1 1 d . . . . .
Cs1 Cs 0.4078(2) 0.62474(13) 0.500000 0.039(2) Uani 1 2 d S T P . .
I1 I 0.41982(15) 0.87798(9) 0.30944(8) 0.0374(18) Uani 1 1 d . . . . .
I2 I 0.07940(14) 0.87256(9) 0.19569(8) 0.0350(17) Uani 1 1 d . . . . .
Cs2 Cs 0.3903(2) 1.12546(13) 0.500000 0.044(2) Uani 1 2 d S T P . .
I3 I 0.24881(15) 1.12495(7) 0.20690(10) 0.0435(16) Uani 1 1 d . . . . .
I4B I 0.2186(3) 0.92997(14) 0.500000 0.048(3) Uani 1 2 d S T P . .
I5A I 0.2784(3) 0.82167(14) 0.000000 0.047(3) Uani 1 2 d S T P . .
C1 C -0.037(4) 0.8831(19) 0.500000 0.021(6) Uiso 1 2 d S . P . .
N11 N -0.0773(16) 0.8849(9) 0.4026(10) 0.039(4) Uiso 1 1 d . . . . .
H11A H -0.055470 0.883651 0.338590 0.047 Uiso 1 1 calc R U . . .
H11B H -0.124428 0.887396 0.405641 0.047 Uiso 1 1 calc R U . . .
N12 N 0.035(3) 0.8794(17) 0.500000 0.052(9) Uiso 1 2 d S . P . .
H12A H 0.058244 0.877986 0.437503 0.062 Uiso 0.5 1 calc R U P . .
H12B H 0.058251 0.878290 0.562497 0.062 Uiso 0.5 1 calc R U P . .
C2 C 0.462(4) 0.117(2) 0.000000 0.032(8) Uiso 1 2 d S . P . .
N21 N 0.4293(18) 0.1123(10) 0.0949(12) 0.056(5) Uiso 1 1 d . . . . .
H21A H 0.382367 0.105257 0.097212 0.067 Uiso 1 1 calc R U . . .
H21B H 0.454065 0.115952 0.156264 0.067 Uiso 1 1 calc R U . . .
N22 N 0.534(4) 0.1184(18) 0.000000 0.046(8) Uiso 1 2 d S . P . .
H22 H 0.558930 0.122150 0.062429 0.055 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.160(3) . ?
Pb1 I2 3.188(3) . ?
Pb1 I3 3.1426(12) . ?
Pb1 I3 3.1363(12) 3_545 ?
Pb1 I4B 3.0994(11) 6_556 ?
Pb1 I4B 3.0994(11) . ?
Pb1 I5A 3.1055(10) . ?
I4B I4B 0.000(10) 6_556 ?
C1 N11 1.38(4) . ?
C1 N11 1.38(4) 6_556 ?
C1 N12 1.30(8) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C2 N21 1.28(4) 6 ?
C2 N21 1.28(4) . ?
C2 N22 1.31(9) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22 0.87(3) . ?
N22 H22 0.87(3) 6 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 179.21(3) . . ?
I3 Pb1 I1 92.01(6) . . ?
I3 Pb1 I1 88.49(6) 3_545 . ?
I3 Pb1 I2 91.57(6) 3_545 . ?
I3 Pb1 I2 87.93(6) . . ?
I3 Pb1 I3 179.38(4) 3_545 . ?
I4B Pb1 I1 88.31(9) . . ?
I4B Pb1 I1 88.31(9) 6_556 . ?
I4B Pb1 I2 90.91(9) . . ?
I4B Pb1 I2 90.91(9) 6_556 . ?
I4B Pb1 I3 86.63(4) . . ?
I4B Pb1 I3 86.63(4) 6_556 . ?
I4B Pb1 I3 93.74(4) 6_556 3_545 ?
I4B Pb1 I3 93.74(4) . 3_545 ?
I4B Pb1 I4B 0.00(19) 6_556 . ?
I4B Pb1 I5A 178.44(14) 6_556 . ?
I4B Pb1 I5A 178.44(14) . . ?
I5A Pb1 I1 93.18(9) . . ?
I5A Pb1 I2 87.61(9) . . ?
I5A Pb1 I3 86.78(4) . 3_545 ?
I5A Pb1 I3 92.84(4) . . ?
Pb1 I2 Cs1 93.32(7) . 3 ?
Pb1 I2 Cs1 155.21(5) . 7_575 ?
Cs1 I2 Cs1 71.58(8) 7_575 3 ?
Pb1 I3 Pb1 161.15(4) 3 . ?
Pb1 I3 Cs1 96.17(6) 3 3 ?
Pb1 I3 Cs1 96.71(5) . 3 ?
Pb1 I4B Pb1 146.31(12) 6_556 . ?
I4B I4B Pb1 0(10) 6_556 . ?
I4B I4B Pb1 0(10) 6_556 6_556 ?
Pb1 I5A Pb1 148.95(12) . 6 ?
N11 C1 N11 115(5) . 6_556 ?
N12 C1 N11 122(3) . 6_556 ?
N12 C1 N11 122(3) . . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N21 C2 N21 124(7) . 6 ?
N21 C2 N22 118(3) . . ?
N21 C2 N22 118(3) 6 . ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22 121(4) . . ?
C2 N22 H22 121(4) . 6 ?
H22 N22 H22 118(7) . 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 1.605
_oxdiff_exptl_absorpt_empirical_full_min 0.534
####################################################################### 
# 
# 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_CsGPbI4_4
_database_code_depnum_ccdc_archive 'CCDC 2428393'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   17.69(5)
_cell_length_b                   11.8898(10)
_cell_length_c                   11.5310(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2426(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2580
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       4000000(30000)
_cell_measurement_theta_max      28.5040
_cell_measurement_theta_min      2.4180
_shelx_estimated_absorpt_T_max   0.411
_shelx_estimated_absorpt_T_min   0.085
_exptl_absorpt_coefficient_mu    27.002
_exptl_absorpt_correction_T_max  0.432
_exptl_absorpt_correction_T_min  0.101
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 4.00(3) GPa
(4000000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.971
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -17 0 0.0767
-1 17 0 0.0783
1 0 -16 0.1136
25 1 1 0.0097
-25 -1 -1 0.0097
-1 0 16 0.1115

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.259     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 174.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
1.1367 -16.7465 -0.1067 0.0083 -0.9366 -0.3503
-1.1459 16.7453 0.2226 -0.0084 0.9391 0.3435
1.2948 0.0270 -16.2089 0.0045 -0.3548 0.9349
24.9033 0.8923 0.9683 -1.0000 0.0000 0.0000
-24.9033 -0.8923 -0.9683 1.0000 0.0000 0.0000
-1.2849 -0.1727 16.2080 -0.0044 0.3467 -0.9380

_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.240
_diffrn_reflns_Laue_measured_fraction_max 0.195
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9566
_diffrn_reflns_point_group_measured_fraction_full 0.240
_diffrn_reflns_point_group_measured_fraction_max 0.195
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.549
_diffrn_reflns_theta_min         2.461
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.240
_diffrn_measured_fraction_theta_max 0.195
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.99   0.47   60.00   0.00 -30.00   0.00    --   117
  2  φ    140.00 199.69   0.47   60.00   0.00 -30.00   0.00    --   127
  3  φ    160.00 216.87   0.47   60.00   0.00  30.00   0.00    --   121
  4  φ    -20.00  34.99   0.47   60.00   0.00  30.00   0.00    --   117
  5  ω    -24.00  23.94   0.47   60.00    --   30.00  39.46 -12.90  102
  6  ω    -24.00  23.94   0.47   60.00    --   30.00  39.46 167.10  102
  7  ω    -50.00   9.69   0.47   60.00    --  -30.00  39.46 167.10  127
  8  ω    -50.00   9.69   0.47   60.00    --  -30.00  39.46 -12.90  127
  9  ω    -64.00  -8.07   0.47   60.00    --  -30.00  81.40 -28.90  119
 10  ω    -64.00  -8.07   0.47   60.00    --  -30.00  81.40 151.10  119
 11  ω    -19.00   7.79   0.47   60.00    --   30.00  81.40 151.10   57
 12  ω    -19.00   7.79   0.47   60.00    --   30.00  81.40 -28.90   57
 13  ω    -43.00 -21.38   0.47   60.00    --   30.00 134.60 -56.90   46
 14  ω    -43.00 -21.38   0.47   60.00    --   30.00 134.60 123.10   46
 15  ω    -90.00 -36.42   0.47   60.00    --  -30.00 134.60 123.10  114
 16  ω    -90.00 -36.42   0.47   60.00    --  -30.00 134.60 -56.90  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0399064000
_diffrn_orient_matrix_UB_12      -0.0031839000
_diffrn_orient_matrix_UB_13      -0.0034693000
_diffrn_orient_matrix_UB_21      -0.0028380000
_diffrn_orient_matrix_UB_22      0.0555978000
_diffrn_orient_matrix_UB_23      0.0217582000
_diffrn_orient_matrix_UB_31      0.0014706000
_diffrn_orient_matrix_UB_32      0.0213816000
_diffrn_orient_matrix_UB_33      -0.0575259000
_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                420
_reflns_number_total             634
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0472
_refine_ls_restrained_S_all      1.231
_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)+(0.0180P)²+114.9495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1084
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2. Others
 Fixed X: H12(0.06548) H22(0.56654)
 Fixed Y: H12(0.884589) H22(0.11618)
 Fixed Z: H12(0.4358) H22(0.06425)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N21(H21A,H21B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_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 0.2520(3) 0.87429(15) 0.25174(10) 0.025(5) Uani 1 1 d . . . . .
Cs1 Cs 0.4125(6) 0.6228(3) 0.500000 0.026(10) Uani 1 2 d S T P . .
I1 I 0.4227(5) 0.8767(2) 0.31270(17) 0.034(8) Uani 1 1 d . . . . .
I2 I 0.0788(5) 0.87233(19) 0.19552(17) 0.032(8) Uani 1 1 d . . . . .
Cs2 Cs 0.3930(7) 1.1255(3) 0.500000 0.035(10) Uani 1 2 d S T P . .
I3 I 0.2473(5) 1.12449(18) 0.1921(2) 0.044(9) Uani 1 1 d . . . . .
I4A I 0.2206(8) 0.9422(3) 0.500000 0.040(13) Uani 1 2 d S T P . .
I5A I 0.2760(8) 0.8084(3) 0.000000 0.060(12) Uani 1 2 d S T P . .
C1 C -0.046(12) 0.872(4) 0.500000 0.008(11) Uiso 1 2 d S . P . .
N11 N -0.080(5) 0.873(2) 0.401(2) 0.038(7) Uiso 1 1 d . . . . .
H11A H -0.128195 0.874830 0.398391 0.046 Uiso 1 1 calc R U . . .
H11B H -0.053750 0.871848 0.338141 0.046 Uiso 1 1 calc R U . . .
N12 N 0.053(11) 0.886(4) 0.500000 0.040(18) Uiso 1 2 d S . P . .
H12 H 0.065480 0.884589 0.435800 0.049 Uiso 1 1 d . U . . .
C2 C 0.458(13) 0.121(5) 0.000000 0.03(2) Uiso 1 2 d S . P . .
N21 N 0.426(6) 0.123(3) 0.098(2) 0.059(10) Uiso 1 1 d . . . . .
H21A H 0.377124 0.126814 0.102441 0.071 Uiso 1 1 calc R U . . .
H21B H 0.452189 0.121459 0.160669 0.071 Uiso 1 1 calc R U . . .
N22 N 0.555(10) 0.117(3) 0.000000 0.019(14) Uiso 1 2 d S . P . .
H22 H 0.566540 0.116180 0.064250 0.023 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.133(13) . ?
Pb1 I3 3.040(3) 3_545 ?
Pb1 I3 3.054(3) . ?
Pb1 I4A 3.026(3) . ?
Pb1 I4A 3.026(3) 6_556 ?
Pb1 I5A 3.036(2) . ?
Cs1 Cs2 4.561(15) 5_676 ?
Cs1 Cs2 4.561(15) 2_675 ?
I1 Cs2 3.913(14) 5_676 ?
I1 Cs2 3.913(14) 2_675 ?
I2 Cs2 3.735(4) 3_545 ?
I4A I4A 0.00(3) 6_556 ?
C1 N11 1.29(10) 6_556 ?
C1 N11 1.29(10) . ?
C1 N12 1.8(3) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12 0.77(6) . ?
N12 H12 0.77(6) 6_556 ?
C2 N21 1.27(11) . ?
C2 N21 1.27(11) 6 ?
C2 N22 1.7(3) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22 0.77(5) . ?
N22 H22 0.77(5) 6 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3 Pb1 I2 86.2(2) . . ?
I3 Pb1 I2 92.33(19) 3_545 . ?
I3 Pb1 I3 178.47(18) 3_545 . ?
I4A Pb1 I2 91.0(3) . . ?
I4A Pb1 I2 91.0(3) 6_556 . ?
I4A Pb1 I3 93.44(9) 6_556 3_545 ?
I4A Pb1 I3 87.02(9) . . ?
I4A Pb1 I3 87.02(9) 6_556 . ?
I4A Pb1 I3 93.44(9) . 3_545 ?
I4A Pb1 I4A 0.0(5) . 6_556 ?
I4A Pb1 I5A 177.4(4) . . ?
I4A Pb1 I5A 177.4(4) 6_556 . ?
I5A Pb1 I2 86.4(3) . . ?
I5A Pb1 I3 92.28(8) . . ?
I5A Pb1 I3 87.20(9) . 3_545 ?
Cs2 Cs1 Cs2 0.0 5_676 2_675 ?
Cs2 I1 Cs2 0.00(9) 5_676 2_675 ?
Pb1 I2 Cs1 94.5(2) . 3 ?
Pb1 I2 Cs1 154.45(18) . 7_575 ?
Pb1 I2 Cs2 90.0(2) . 3_545 ?
Cs1 I2 Cs1 69.7(2) 7_575 3 ?
Cs1 I2 Cs2 75.6(2) 7_575 3_545 ?
Cs2 I2 Cs1 104.86(7) 3_545 3 ?
Pb1 I3 Pb1 154.62(9) 3 . ?
Pb1 I3 Cs1 98.04(17) 3 3 ?
Pb1 I3 Cs1 98.91(18) . 3 ?
Pb1 I4A Pb1 142.2(3) 6_556 . ?
I4A I4A Pb1 0(10) 6_556 . ?
I4A I4A Pb1 0(10) 6_556 6_556 ?
Pb1 I5A Pb1 145.9(3) . 6 ?
Pb1 I5A Cs2 92.2(3) . 3_545 ?
Pb1 I5A Cs2 92.2(3) 6 3_545 ?
N11 C1 N11 124(10) 6_556 . ?
N11 C1 N12 118(8) 6_556 . ?
N11 C1 N12 118(8) . . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12 106(10) . . ?
C1 N12 H12 107(10) . 6_556 ?
H12 N12 H12 147(10) . 6_556 ?
N21 C2 N21 126(10) . 6 ?
N21 C2 N22 117(10) . . ?
N21 C2 N22 117(10) 6 . ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22 105(10) . . ?
C2 N22 H22 105(10) . 6 ?
H22 N22 H22 150(10) . 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 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.478
####################################################################### 
# 
# 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_CsGPbI4_3_79
_database_code_depnum_ccdc_archive 'CCDC 2428396'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   17.738(15)
_cell_length_b                   11.9435(8)
_cell_length_c                   11.5372(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2444(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2999
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       3790000(30000)
_cell_measurement_theta_max      28.4140
_cell_measurement_theta_min      1.7830
_shelx_estimated_absorpt_T_max   0.385
_shelx_estimated_absorpt_T_min   0.085
_exptl_absorpt_coefficient_mu    26.799
_exptl_absorpt_correction_T_max  0.226
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 3.79(3) GPa
(3790000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.934
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -1 16 0.0689
4 2 -16 0.0653
4 17 1 0.0798
-4 -17 1 0.0997
-5 -11 11 0.0788
0 -12 -12 0.0727
25 -3 2 0.0220
-25 3 -2 0.0220

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.044
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.632     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 182.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
-3.7626 -1.4796 15.9628 -0.0079 -0.9105 -0.4135
3.7938 1.6175 -15.9472 0.0079 0.9139 0.4059
3.8271 16.5340 1.4747 0.0024 0.4321 -0.9018
-4.3151 -16.5270 0.8299 -0.0035 -0.5567 0.8307
-5.2815 -11.4756 11.3310 -0.0075 -0.9691 0.2466
-0.4062 -11.5861 -11.7423 0.0034 0.2773 0.9608
24.5395 -2.8255 2.2803 -1.0000 0.0000 0.0000
-24.5395 2.8255 -2.2803 1.0000 0.0000 0.0000

_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.355
_diffrn_reflns_Laue_measured_fraction_max 0.288
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9979
_diffrn_reflns_point_group_measured_fraction_full 0.355
_diffrn_reflns_point_group_measured_fraction_max 0.288
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.456
_diffrn_reflns_theta_min         2.454
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.355
_diffrn_measured_fraction_theta_max 0.288
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   70.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   70.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   70.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   70.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0387999896
_diffrn_orient_matrix_UB_12      0.0099030426
_diffrn_orient_matrix_UB_13      -0.0087216191
_diffrn_orient_matrix_UB_21      0.0082000917
_diffrn_orient_matrix_UB_22      0.0289099384
_diffrn_orient_matrix_UB_23      -0.0524246181
_diffrn_orient_matrix_UB_31      -0.0029675696
_diffrn_orient_matrix_UB_32      -0.0510626981
_diffrn_orient_matrix_UB_33      -0.0313358039
_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                566
_reflns_number_total             934
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         934
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0404
_refine_ls_restrained_S_all      1.168
_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)+(0.0215P)²+83.3946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0986
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H22A(0.5) H22B(0.5)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B), N22(H22A,H22B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.25180(13) 0.87468(11) 0.25164(7) 0.0273(16) Uani 1 1 d . . . . .
Cs1 Cs 0.4134(3) 0.6234(2) 0.500000 0.029(3) Uani 1 2 d S T P . .
I1 I 0.4223(2) 0.87721(14) 0.31294(12) 0.030(3) Uani 1 1 d . . . . .
I2 I 0.0795(2) 0.87288(14) 0.19494(11) 0.025(3) Uani 1 1 d . . . . .
Cs2 Cs 0.3930(3) 1.1256(2) 0.500000 0.032(3) Uani 1 2 d S T P . .
I3 I 0.2478(2) 1.12441(12) 0.19156(14) 0.039(3) Uani 1 1 d . . . . .
I4A I 0.2197(4) 0.9435(2) 0.500000 0.041(4) Uani 1 2 d S T P . .
I5A I 0.2763(4) 0.8075(2) 0.000000 0.033(4) Uani 1 2 d S T P . .
C1 C -0.034(6) 0.875(4) 0.500000 0.017(9) Uiso 1 2 d S . P . .
N11 N -0.076(3) 0.8766(16) 0.4009(15) 0.032(5) Uiso 1 1 d . . . . .
H11A H -0.054883 0.884023 0.334475 0.039 Uiso 1 1 calc R U . . .
H11B H -0.124507 0.869991 0.405189 0.039 Uiso 1 1 calc R U . . .
N12 N 0.035(5) 0.884(3) 0.500000 0.050(15) Uiso 1 2 d S . P . .
H12A H 0.058944 0.891790 0.564387 0.060 Uiso 0.5 1 calc R U P . .
H12B H 0.059473 0.882844 0.435613 0.060 Uiso 0.5 1 calc R U P . .
C2 C 0.474(6) 0.123(4) 0.000000 0.020(10) Uiso 1 2 d S . P . .
N21 N 0.429(3) 0.1210(19) 0.0999(18) 0.052(7) Uiso 1 1 d . . . . .
H21A H 0.449533 0.114058 0.167005 0.062 Uiso 1 1 calc R U . . .
H21B H 0.380830 0.126609 0.093904 0.062 Uiso 1 1 calc R U . . .
N22 N 0.543(5) 0.116(3) 0.000000 0.037(12) Uiso 1 2 d S . P . .
H22A H 0.567050 0.108591 0.064385 0.044 Uiso 0.5 1 calc R U P . .
H22B H 0.567490 0.117595 -0.064385 0.044 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.106(5) . ?
Pb1 I2 3.125(5) . ?
Pb1 I3 3.060(2) 3_545 ?
Pb1 I3 3.063(2) . ?
Pb1 I4A 3.0349(17) . ?
Pb1 I5A 3.0434(15) . ?
C1 N11 1.37(7) . ?
C1 N11 1.37(7) 6_556 ?
C1 N12 1.22(14) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 6_556 ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 6_556 ?
N12 H12B 0.8600 . ?
C2 N21 1.40(7) 6 ?
C2 N21 1.40(7) . ?
C2 N22 1.23(13) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22A 0.8600 6 ?
N22 H22A 0.8600 . ?
N22 H22B 0.8600 6 ?
N22 H22B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 178.91(5) . . ?
I3 Pb1 I1 87.64(10) 3_545 . ?
I3 Pb1 I1 93.69(10) . . ?
I3 Pb1 I2 86.38(10) . . ?
I3 Pb1 I2 92.30(10) 3_545 . ?
I3 Pb1 I3 178.60(8) 3_545 . ?
I4A Pb1 I1 87.99(14) . . ?
I4A Pb1 I2 90.92(14) . . ?
I4A Pb1 I3 93.61(6) . 3_545 ?
I4A Pb1 I3 86.87(6) . . ?
I4A Pb1 I5A 177.3(2) . . ?
I5A Pb1 I1 94.63(14) . . ?
I5A Pb1 I2 86.46(14) . . ?
I5A Pb1 I3 86.93(6) . 3_545 ?
I5A Pb1 I3 92.53(6) . . ?
Pb1 I3 Pb1 154.51(6) 3 . ?
Pb1 I4A Pb1 141.51(17) 6_556 . ?
Pb1 I5A Pb1 145.09(15) . 6 ?
N11 C1 N11 113(8) 6_556 . ?
N12 C1 N11 123(4) . 6_556 ?
N12 C1 N11 123(4) . . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0(3) . 6_556 ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
C1 N12 H12B 120.0(2) . 6_556 ?
H12A N12 H12A 119.5 . 6_556 ?
H12A N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 6_556 6_556 ?
H12A N12 H12B 7.1 . 6_556 ?
H12B N12 H12A 7.1 . 6_556 ?
H12B N12 H12B 119.5 . 6_556 ?
N21 C2 N21 110(8) . 6 ?
N22 C2 N21 125(4) . . ?
N22 C2 N21 125(4) . 6 ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22A 120.0 . . ?
C2 N22 H22A 120.0(2) . 6 ?
C2 N22 H22B 120.0 . . ?
C2 N22 H22B 120.0(2) . 6 ?
H22A N22 H22A 119.5 . 6 ?
H22A N22 H22B 120.0 . . ?
H22A N22 H22B 7.2 . 6 ?
H22A N22 H22B 120.0 6 6 ?
H22B N22 H22A 7.2 . 6 ?
H22B N22 H22B 119.5 . 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 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.769
####################################################################### 
# 
# 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_CsGPbI4_4_74
_database_code_depnum_ccdc_archive 'CCDC 2428387'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2025-02-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   17.29(3)
_cell_length_b                   11.9193(6)
_cell_length_c                   11.5884(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2388(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1786
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       4740000(30000)
_cell_measurement_theta_max      27.8870
_cell_measurement_theta_min      2.4480
_shelx_estimated_absorpt_T_max   0.407
_shelx_estimated_absorpt_T_min   0.083
_exptl_absorpt_coefficient_mu    27.432
_exptl_absorpt_correction_T_max  0.431
_exptl_absorpt_correction_T_min  0.172
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 4.74(3) GPa
(4740000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    5.051
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 0 16 0.1111
25 -1 1 0.0097
-25 1 -1 0.0097
7 16 0 0.0576
3 -1 -16 0.1125
-7 -16 0 0.0716

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.447     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 174.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
-3.3002 -0.1260 16.0605 -0.0867 -0.3671 0.9261
24.6382 -0.8651 0.8976 1.0000 0.0000 0.0000
-24.6382 0.8651 -0.8976 -1.0000 0.0000 0.0000
6.5838 16.0794 -0.0236 0.2192 0.9170 0.3332
2.9642 -0.7008 -16.0771 0.0755 0.3204 -0.9443
-6.5778 -16.0806 -0.0079 -0.2190 -0.9164 -0.3350

_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.226
_diffrn_reflns_Laue_measured_fraction_max 0.178
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9329
_diffrn_reflns_point_group_measured_fraction_full 0.226
_diffrn_reflns_point_group_measured_fraction_max 0.178
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.777
_diffrn_reflns_theta_min         2.451
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.226
_diffrn_measured_fraction_theta_max 0.178
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.60   0.65   60.00   0.00 -30.00   0.00    --    84
  2  φ    140.00 199.80   0.65   60.00   0.00 -30.00   0.00    --    92
  3  φ    160.00 216.55   0.65   60.00   0.00  30.00   0.00    --    87
  4  φ    -20.00  34.60   0.65   60.00   0.00  30.00   0.00    --    84
  5  ω    -24.00  23.45   0.65   60.00    --   30.00  39.46 -12.90   73
  6  ω    -24.00  23.45   0.65   60.00    --   30.00  39.46 167.10   73
  7  ω    -50.00   9.80   0.65   60.00    --  -30.00  39.46 167.10   92
  8  ω    -50.00   9.80   0.65   60.00    --  -30.00  39.46 -12.90   92
  9  ω    -64.00  -8.10   0.65   60.00    --  -30.00  81.40 -28.90   86
 10  ω    -64.00  -8.10   0.65   60.00    --  -30.00  81.40 151.10   86
 11  ω    -19.00   7.65   0.65   60.00    --   30.00  81.40 151.10   41
 12  ω    -19.00   7.65   0.65   60.00    --   30.00  81.40 -28.90   41
 13  ω    -43.00 -21.55   0.65   60.00    --   30.00 134.60 -56.90   33
 14  ω    -43.00 -21.55   0.65   60.00    --   30.00 134.60 123.10   33
 15  ω    -90.00 -36.05   0.65   60.00    --  -30.00 134.60 123.10   83
 16  ω    -90.00 -36.05   0.65   60.00    --  -30.00 134.60 -56.90   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0403808000
_diffrn_orient_matrix_UB_12      -0.0028982000
_diffrn_orient_matrix_UB_13      0.0028749000
_diffrn_orient_matrix_UB_21      0.0027580000
_diffrn_orient_matrix_UB_22      0.0558701000
_diffrn_orient_matrix_UB_23      -0.0218551000
_diffrn_orient_matrix_UB_31      -0.0013469000
_diffrn_orient_matrix_UB_32      0.0213568000
_diffrn_orient_matrix_UB_33      0.0575546000
_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                370
_reflns_number_total             582
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.107
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.314
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         582
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0950
_refine_ls_restrained_S_all      1.075
_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)+(0.0681P)²+707.8647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2201
_refine_ls_wR_factor_ref         0.2413
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Restrained distances
 C2-N22
 1.3 with sigma of 0.02
 C2-N21
 1.3 with sigma of 0.02
 C1-N11
 1.3 with sigma of 0.02
 C1-N12
 1.3 with sigma of 0.02
3. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H22A(0.5) H22B(0.5)
4.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B), N22(H22A,H22B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.2524(6) 0.8747(2) 0.2518(2) 0.0355(9) Uiso 1 1 d . . . . .
Cs1 Cs 0.4097(15) 0.6210(5) 0.500000 0.0365(16) Uiso 1 2 d S . P . .
I1 I 0.4232(10) 0.8766(3) 0.3136(4) 0.039(17) Uani 1 1 d . . . . .
I4 I 0.0779(10) 0.8724(3) 0.1959(3) 0.0363(12) Uiso 1 1 d . . . . .
Cs2 Cs 0.3917(15) 1.1242(5) 0.500000 0.0373(16) Uiso 1 2 d S . P . .
C1 C -0.047(9) 0.875(8) 0.500000 0.02(3) Uiso 1 2 d DS . P . .
N11 N -0.077(9) 0.876(4) 0.397(4) 0.037(14) Uiso 1 1 d D . . . .
H11A H -0.048167 0.877349 0.337335 0.045 Uiso 1 1 calc R U . . .
H11B H -0.126807 0.874860 0.389822 0.045 Uiso 1 1 calc R U . . .
N12 N 0.029(9) 0.877(9) 0.500000 0.07(5) Uiso 1 2 d DS . P . .
H12A H 0.053606 0.878143 0.564262 0.081 Uiso 0.5 1 calc R U P . .
H12B H 0.053625 0.876269 0.435738 0.081 Uiso 0.5 1 calc R U P . .
C2 C 0.462(9) 0.121(9) 0.000000 0.03(3) Uiso 1 2 d DS . P . .
N21 N 0.424(9) 0.122(4) 0.096(4) 0.045(16) Uiso 1 1 d D . . . .
H21A H 0.447656 0.117288 0.161125 0.054 Uiso 1 1 calc R U . . .
H21B H 0.374076 0.127906 0.095125 0.054 Uiso 1 1 calc R U . . .
N22 N 0.538(9) 0.113(8) 0.000000 0.05(4) Uiso 1 2 d DS . P . .
H22A H 0.562186 0.107970 0.064225 0.063 Uiso 0.5 1 calc R U P . .
H22B H 0.562431 0.112582 -0.064225 0.063 Uiso 0.5 1 calc R U P . .
I2 I 0.2196(16) 0.9407(5) 0.500000 0.045(2) Uiso 1 2 d S . P . .
I5 I 0.2766(17) 0.8111(6) 0.000000 0.049(2) Uiso 1 2 d S . P . .
I6 I 0.2480(11) 1.1255(4) 0.1940(4) 0.0504(16) Uiso 1 1 d . . . . .


_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 3.04(2) . ?
Pb1 I4 3.09(2) . ?
Pb1 I2 3.035(6) . ?
Pb1 I5 3.044(5) . ?
Pb1 I6 3.064(5) . ?
Pb1 I6 3.036(5) 3_545 ?
C1 N11 1.30(2) . ?
C1 N11 1.30(2) 6_556 ?
C1 N12 1.30(2) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C2 N21 1.30(2) 6 ?
C2 N21 1.30(2) . ?
C2 N22 1.30(2) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22A 0.8600 . ?
N22 H22B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I4 178.5(2) . . ?
I1 Pb1 I5 95.4(6) . . ?
I1 Pb1 I6 93.9(4) . . ?
I2 Pb1 I1 87.5(5) . . ?
I2 Pb1 I4 91.1(6) . . ?
I2 Pb1 I5 177.0(8) . . ?
I2 Pb1 I6 93.27(18) . 3_545 ?
I2 Pb1 I6 87.13(17) . . ?
I5 Pb1 I4 86.0(6) . . ?
I5 Pb1 I6 92.10(17) . . ?
I6 Pb1 I1 87.8(4) 3_545 . ?
I6 Pb1 I4 91.9(4) 3_545 . ?
I6 Pb1 I4 86.5(4) . . ?
I6 Pb1 I5 87.42(17) 3_545 . ?
I6 Pb1 I6 178.3(4) 3_545 . ?
N11 C1 N11 132(10) 6_556 . ?
N12 C1 N11 114(5) . . ?
N12 C1 N11 114(5) . 6_556 ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N21 C2 N21 118(9) . 6 ?
N22 C2 N21 121(5) . . ?
N22 C2 N21 121(5) . 6 ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22A 120.0 . . ?
C2 N22 H22B 120.0 . . ?
H22A N22 H22B 120.0 . . ?
Pb1 I2 Pb1 142.8(7) 6_556 . ?
Pb1 I5 Pb1 147.0(6) . 6 ?
Pb1 I6 Pb1 155.40(19) 3 . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.569
####################################################################### 
# 
# 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_g2pbi4_0_43
_database_code_depnum_ccdc_archive 'CCDC 2428385'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_systematic        'Guanidinium lead(II) tetraiodide'
_chemical_formula_sum            'C2 H12 I4 N6 Pb'
_chemical_formula_weight         834.97
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.673(4)
_cell_length_b                   26.7036(12)
_cell_length_c                   9.1630(3)
_cell_angle_alpha                90
_cell_angle_beta                 88.468(8)
_cell_angle_gamma                90
_cell_volume                     3099.7(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2462
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       430000(30000)
_cell_measurement_theta_max      27.7590
_cell_measurement_theta_min      2.6810
_exptl_absorpt_coefficient_mu    18.832
_exptl_absorpt_correction_T_max  0.22680
_exptl_absorpt_correction_T_min  0.20524
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 0.43(3) GPa
(430000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.578
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.032
_exptl_crystal_size_rad          0.04
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.300
_diffrn_reflns_Laue_measured_fraction_max 0.222
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13873
_diffrn_reflns_point_group_measured_fraction_full 0.300
_diffrn_reflns_point_group_measured_fraction_max 0.222
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.009
_diffrn_reflns_theta_min         2.351
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.300
_diffrn_measured_fraction_theta_max 0.222
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   73.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   73.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   73.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   73.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   73.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   73.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   73.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   73.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   73.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   73.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   73.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   73.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   73.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   73.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   73.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   73.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0019572000
_diffrn_orient_matrix_UB_12      -0.0076248000
_diffrn_orient_matrix_UB_13      -0.0535696000
_diffrn_orient_matrix_UB_21      0.0338890000
_diffrn_orient_matrix_UB_22      -0.0227927000
_diffrn_orient_matrix_UB_23      0.0156606000
_diffrn_orient_matrix_UB_31      -0.0695974000
_diffrn_orient_matrix_UB_32      -0.0113079000
_diffrn_orient_matrix_UB_33      0.0044980000
_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                1137
_reflns_number_total             1836
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         1836
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0570
_refine_ls_restrained_S_all      1.086
_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)+(0.0415P)²+106.3283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1426
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Restrained distances
 C3-N58
 1.3 with sigma of 0.02
 N25-N11
 2.13 with sigma of 0.02
3. Others
 Uiso(N4)=Uiso(N5)=Uiso(N11)=Uiso(N19)=Uiso(N25)=Uiso(N26)=Uiso(N28)=Uiso(N30)=
 Uiso(N33)=Uiso(N48)=Uiso(N54)=Uiso(N58)=FVAR(1)
 Uiso(C3)=Uiso(C17)=Uiso(C38)=Uiso(C47)=FVAR(2)
4.a X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), N11(H11A,H11B), N19(H19A,H19B), N25(H25A,H25B),
 N26(H26A,H26B), N28(H28A,H28B), N30(H30A,H30B), N33(H33A,H33B), N48(H48A,H48B),
  N54(H54A,H54B), N58(H58A,H58B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.2401(3) 0.08398(4) 0.25311(14) 0.030(2) Uani 1 1 d . . . . .
Pb2 Pb 0.7439(3) 0.09089(4) 0.24004(15) 0.038(2) Uani 1 1 d . . . . .
I3 I 0.4950(5) 0.07413(9) 0.1923(3) 0.040(4) Uani 1 1 d . . . . .
I4 I 0.6946(5) 0.16870(8) 0.4782(3) 0.053(3) Uani 1 1 d . . . . .
I5 I -0.0086(5) 0.10465(9) 0.3019(3) 0.040(4) Uani 1 1 d . . . . .
I6 I 0.2009(4) 0.00053(7) 0.0007(2) 0.047(4) Uani 1 1 d . . . . .
I7 I 0.2409(4) 0.16806(8) 0.0233(3) 0.051(4) Uani 1 1 d . . . . .
I8 I 0.2446(4) -0.00540(8) 0.5033(2) 0.045(3) Uani 1 1 d . . . . .
I9 I 0.2708(5) 0.15547(9) 0.5196(3) 0.063(4) Uani 1 1 d . . . . .
I10 I 0.7618(5) 0.17319(8) 0.0006(3) 0.058(4) Uani 1 1 d . . . . .
C3 C 0.493(5) 0.2558(14) 0.204(4) 0.047(6) Uiso 1 1 d D U . . .
N4 N 0.503(6) 0.9361(11) 0.412(3) 0.082(4) Uiso 1 1 d . U . . .
H4A H 0.445498 0.938736 0.462162 0.098 Uiso 1 1 calc R U . . .
H4B H 0.562762 0.934750 0.454927 0.098 Uiso 1 1 calc R U . . .
N5 N 0.505(6) 0.8130(12) 0.175(3) 0.082(4) Uiso 1 1 d . U . . .
H5A H 0.557327 0.831123 0.202715 0.098 Uiso 1 1 calc R U . . .
H5B H 0.458884 0.825379 0.119045 0.098 Uiso 1 1 calc R U . . .
N11 N 0.562(5) 0.7494(13) 0.297(4) 0.082(4) Uiso 1 1 d D U . . .
H11A H 0.615324 0.766010 0.327705 0.098 Uiso 1 1 calc R U . . .
H11B H 0.553113 0.718736 0.323059 0.098 Uiso 1 1 calc R U . . .
C17 C 0.498(7) 0.7699(13) 0.216(4) 0.047(6) Uiso 1 1 d . U . . .
N19 N 0.589(7) 0.2780(13) 0.255(4) 0.082(4) Uiso 1 1 d . U . . .
H19A H 0.624156 0.263544 0.322331 0.098 Uiso 1 1 calc R U . . .
H19B H 0.612066 0.305724 0.217723 0.098 Uiso 1 1 calc R U . . .
N25 N 0.415(5) 0.7409(13) 0.194(4) 0.082(4) Uiso 1 1 d D U . . .
H25A H 0.361949 0.752431 0.147869 0.098 Uiso 1 1 calc R U . . .
H25B H 0.414333 0.710598 0.225424 0.098 Uiso 1 1 calc R U . . .
N26 N 0.515(6) 0.4533(12) 0.198(4) 0.082(4) Uiso 1 1 d . U . . .
H26A H 0.484280 0.467029 0.125178 0.098 Uiso 1 1 calc R U . . .
H26B H 0.571343 0.466126 0.231191 0.098 Uiso 1 1 calc R U . . .
N28 N 0.509(6) 0.4041(12) 0.385(4) 0.082(4) Uiso 1 1 d . U . . .
H28A H 0.554621 0.422783 0.426813 0.098 Uiso 1 1 calc R U . . .
H28B H 0.484929 0.377858 0.428053 0.098 Uiso 1 1 calc R U . . .
N30 N 0.463(6) 0.2143(12) 0.263(3) 0.082(4) Uiso 1 1 d . U . . .
H30A H 0.404660 0.200539 0.236922 0.098 Uiso 1 1 calc R U . . .
H30B H 0.500268 0.200296 0.328014 0.098 Uiso 1 1 calc R U . . .
N33 N 0.409(7) 0.9363(11) 0.195(4) 0.082(4) Uiso 1 1 d . U . . .
H33A H 0.353761 0.938865 0.250667 0.098 Uiso 1 1 calc R U . . .
H33B H 0.403238 0.935175 0.101759 0.098 Uiso 1 1 calc R U . . .
C38 C 0.501(8) 0.9340(13) 0.251(4) 0.047(6) Uiso 1 1 d . U . . .
C47 C 0.477(7) 0.4158(14) 0.253(4) 0.047(6) Uiso 1 1 d . U . . .
N48 N 0.614(7) 0.9295(11) 0.198(4) 0.082(4) Uiso 1 1 d . U . . .
H48A H 0.628275 0.927735 0.106417 0.098 Uiso 1 1 calc R U . . .
H48B H 0.663434 0.928714 0.260216 0.098 Uiso 1 1 calc R U . . .
N54 N 0.392(7) 0.3961(14) 0.204(4) 0.082(4) Uiso 1 1 d . U . . .
H54A H 0.361272 0.409612 0.131816 0.098 Uiso 1 1 calc R U . . .
H54B H 0.366212 0.369536 0.244502 0.098 Uiso 1 1 calc R U . . .
N58 N 0.439(5) 0.2783(12) 0.105(3) 0.082(4) Uiso 1 1 d D U . . .
H58A H 0.381004 0.265623 0.076593 0.098 Uiso 1 1 calc R U . . .
H58B H 0.462020 0.306001 0.067780 0.098 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I3 3.274(7) . ?
Pb1 I5 3.219(7) . ?
Pb1 I6 3.259(3) . ?
Pb1 I7 3.078(2) . ?
Pb1 I8 3.311(2) . ?
Pb1 I9 3.132(3) . ?
Pb2 I3 3.228(7) . ?
Pb2 I4 3.066(3) . ?
Pb2 I5 3.222(7) 1_655 ?
Pb2 I6 3.351(3) 3_655 ?
Pb2 I8 3.284(3) 3_656 ?
Pb2 I10 3.110(3) . ?
C3 N19 1.45(9) . ?
C3 N30 1.29(5) . ?
C3 N58 1.30(2) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C38 1.47(5) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N5 C17 1.21(4) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N11 C17 1.24(8) . ?
C17 N25 1.32(9) . ?
N19 H19A 0.8600 . ?
N19 H19B 0.8600 . ?
N25 H25A 0.8600 . ?
N25 H25B 0.8600 . ?
N26 H26A 0.8600 . ?
N26 H26B 0.8600 . ?
N26 C47 1.21(5) . ?
N28 H28A 0.8600 . ?
N28 H28B 0.8600 . ?
N28 C47 1.32(6) . ?
N30 H30A 0.8600 . ?
N30 H30B 0.8600 . ?
N33 H33A 0.8600 . ?
N33 H33B 0.8600 . ?
N33 C38 1.29(12) . ?
C38 N48 1.50(11) . ?
C47 N54 1.29(11) . ?
N48 H48A 0.8600 . ?
N48 H48B 0.8600 . ?
N54 H54A 0.8600 . ?
N54 H54B 0.8600 . ?
N58 H58A 0.8600 . ?
N58 H58B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3 Pb1 I8 91.41(12) . . ?
I5 Pb1 I3 174.46(7) . . ?
I5 Pb1 I6 92.79(13) . . ?
I5 Pb1 I8 93.58(12) . . ?
I6 Pb1 I3 89.58(12) . . ?
I6 Pb1 I8 90.24(6) . . ?
I7 Pb1 I3 87.52(13) . . ?
I7 Pb1 I5 87.45(13) . . ?
I7 Pb1 I6 90.62(7) . . ?
I7 Pb1 I8 178.62(17) . . ?
I7 Pb1 I9 95.20(7) . . ?
I9 Pb1 I3 92.23(15) . . ?
I9 Pb1 I5 85.93(14) . . ?
I9 Pb1 I6 173.97(9) . . ?
I9 Pb1 I8 83.96(7) . . ?
I3 Pb2 I6 89.85(12) . 3_655 ?
I3 Pb2 I8 93.60(12) . 3_656 ?
I4 Pb2 I3 90.52(14) . . ?
I4 Pb2 I5 88.75(14) . 1_655 ?
I4 Pb2 I6 175.75(8) . 3_655 ?
I4 Pb2 I8 88.47(7) . 3_656 ?
I4 Pb2 I10 91.89(7) . . ?
I5 Pb2 I3 177.28(8) 1_655 . ?
I5 Pb2 I6 90.68(13) 1_655 3_655 ?
I5 Pb2 I8 83.76(12) 1_655 3_656 ?
I8 Pb2 I6 87.28(6) 3_656 3_655 ?
I10 Pb2 I3 93.18(13) . . ?
I10 Pb2 I5 89.46(14) . 1_655 ?
I10 Pb2 I6 92.31(7) . 3_655 ?
I10 Pb2 I8 173.20(19) . 3_656 ?
Pb2 I3 Pb1 158.34(9) . . ?
Pb1 I5 Pb2 155.47(10) . 1_455 ?
Pb1 I6 Pb2 158.8(2) . 3_655 ?
Pb2 I8 Pb1 177.43(15) 3_656 . ?
N30 C3 N19 118(5) . . ?
N30 C3 N58 122(5) . . ?
N58 C3 N19 120(4) . . ?
H4A N4 H4B 120.0 . . ?
C38 N4 H4A 120.0 . . ?
C38 N4 H4B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C17 N5 H5A 120.0 . . ?
C17 N5 H5B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C17 N11 H11A 120.0 . . ?
C17 N11 H11B 120.0 . . ?
N5 C17 N11 124(7) . . ?
N5 C17 N25 124(7) . . ?
N11 C17 N25 112(3) . . ?
C3 N19 H19A 120.0 . . ?
C3 N19 H19B 120.0 . . ?
H19A N19 H19B 120.0 . . ?
C17 N25 H25A 120.0 . . ?
C17 N25 H25B 120.0 . . ?
H25A N25 H25B 120.0 . . ?
H26A N26 H26B 120.0 . . ?
C47 N26 H26A 120.0 . . ?
C47 N26 H26B 120.0 . . ?
H28A N28 H28B 120.0 . . ?
C47 N28 H28A 120.0 . . ?
C47 N28 H28B 120.0 . . ?
C3 N30 H30A 120.0 . . ?
C3 N30 H30B 120.0 . . ?
H30A N30 H30B 120.0 . . ?
H33A N33 H33B 120.0 . . ?
C38 N33 H33A 120.0 . . ?
C38 N33 H33B 120.0 . . ?
N4 C38 N48 106(7) . . ?
N33 C38 N4 116(8) . . ?
N33 C38 N48 138(5) . . ?
N26 C47 N28 117(6) . . ?
N26 C47 N54 121(6) . . ?
N54 C47 N28 120(6) . . ?
C38 N48 H48A 120.0 . . ?
C38 N48 H48B 120.0 . . ?
H48A N48 H48B 120.0 . . ?
C47 N54 H54A 120.0 . . ?
C47 N54 H54B 120.0 . . ?
H54A N54 H54B 120.0 . . ?
C3 N58 H58A 120.0 . . ?
C3 N58 H58B 120.0 . . ?
H58A N58 H58B 120.0 . . ?

_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 1.307
_oxdiff_exptl_absorpt_empirical_full_min 0.811
####################################################################### 
# 
# 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_CsGPbI4_atm
_database_code_depnum_ccdc_archive 'CCDC 2428388'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   18.5595(4)
_cell_length_b                   12.7464(3)
_cell_length_c                   12.2365(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2894.76(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4120
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5290
_cell_measurement_theta_min      2.2160
_exptl_absorpt_coefficient_mu    22.627
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.166
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 3 -17 0.0331
-1 14 -11 0.1014
0 -2 17 0.0366
1 -17 -5 0.1820
-26 3 1 0.0150
26 -3 -1 0.0080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
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
-0.0033 2.9998 -16.9807 0.2637 -0.9535 -0.1355
-1.0022 13.9854 -10.9898 0.2415 -0.8061 0.5527
0.0032 -2.0010 16.9806 -0.2609 0.9370 0.1885
0.9998 -16.9786 -4.9909 -0.0097 0.0049 -0.9890
-25.9679 2.9944 1.0005 0.9502 0.2644 0.2065
25.9679 -2.9944 -1.0005 -0.9502 -0.2644 -0.2065

_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15731
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.697
_diffrn_reflns_theta_min         1.938
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  20.00   1.00   70.00    --  -19.52 101.00 -22.00   91
  2  ω    -94.00 -10.00   1.00   70.00    --  -19.52 139.00  45.00   84
  3  ω    -60.00  69.00   1.00   70.00    --  -19.52  57.00-180.00  129
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0368440000
_diffrn_orient_matrix_UB_12      0.0028202000
_diffrn_orient_matrix_UB_13      -0.0150232000
_diffrn_orient_matrix_UB_21      -0.0100350000
_diffrn_orient_matrix_UB_22      -0.0165254000
_diffrn_orient_matrix_UB_23      0.0532331000
_diffrn_orient_matrix_UB_31      -0.0011649000
_diffrn_orient_matrix_UB_32      0.0530769000
_diffrn_orient_matrix_UB_33      0.0173558000
_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                2039
_reflns_number_total             3543
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.405
_refine_diff_density_min         -2.564
_refine_diff_density_rms         0.509
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         3543
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0459
_refine_ls_restrained_S_all      1.105
_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)+(0.0678P)²+0.0411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1563
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H22A(0.5) H22B(0.5)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B), N22(H22A,H22B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.25009(2) 0.87521(5) 0.25058(2) 0.02705(18) Uani 1 1 d . . . . .
Cs1 Cs 0.40243(8) 0.62541(10) 0.500000 0.0549(3) Uani 1 2 d S T P . .
I1 I 0.41761(4) 0.87769(7) 0.30631(7) 0.0439(2) Uani 1 1 d . . . . .
I2 I 0.08010(4) 0.87232(7) 0.19685(6) 0.0421(2) Uani 1 1 d . . . . .
Cs2 Cs 0.38723(8) 1.12471(9) 0.500000 0.0555(3) Uani 1 2 d S T P . .
I3 I 0.24940(4) 1.12513(7) 0.22321(10) 0.0477(3) Uani 1 1 d . . . . .
I4A I 0.21815(7) 0.91177(12) 0.500000 0.0576(4) Uani 1 2 d S T P . .
I5B I 0.28074(7) 0.84005(13) 0.000000 0.0615(4) Uani 1 2 d S T P . .
C1 C -0.0442(9) 0.8740(14) 0.500000 0.035(3) Uiso 1 2 d S . P . .
N11 N -0.0772(5) 0.8744(7) 0.4060(9) 0.047(3) Uani 1 1 d . . . . .
H11A H -0.123549 0.874842 0.403703 0.056 Uiso 1 1 calc R U . . .
H11B H -0.052752 0.874110 0.346367 0.056 Uiso 1 1 calc R U . . .
N12 N 0.0279(7) 0.8837(10) 0.500000 0.043(3) Uani 1 2 d S T P . .
H12A H 0.050741 0.889926 0.439220 0.052 Uiso 0.5 1 calc R U P . .
H12B H 0.051133 0.883765 0.560780 0.052 Uiso 0.5 1 calc R U P . .
C2 C 0.4578(9) 0.1255(15) 0.000000 0.035(3) Uiso 1 2 d S . P . .
N21 N 0.4257(7) 0.1260(8) 0.0949(11) 0.075(4) Uani 1 1 d . . . . .
H21A H 0.379381 0.126596 0.098402 0.091 Uiso 1 1 calc R U . . .
H21B H 0.450779 0.125616 0.153994 0.091 Uiso 1 1 calc R U . . .
N22 N 0.5282(8) 0.1160(11) 0.000000 0.054(4) Uani 1 2 d S T P . .
H22A H 0.551123 0.110463 0.060811 0.064 Uiso 0.5 1 calc R U P . .
H22B H 0.551437 0.115400 -0.060811 0.064 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1832(8) . ?
Pb1 I2 3.2229(8) . ?
Pb1 I3 3.2032(11) . ?
Pb1 I3 3.2037(11) 3_545 ?
Pb1 I4A 3.1438(4) . ?
Pb1 I5B 3.1506(4) . ?
C1 N11 1.303(13) . ?
C1 N11 1.303(13) 6_556 ?
C1 N12 1.34(2) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C2 N21 1.306(14) . ?
C2 N21 1.306(14) 6 ?
C2 N22 1.31(2) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22A 0.8600 . ?
N22 H22B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 179.393(19) . . ?
I1 Pb1 I3 89.17(3) . 3_545 ?
I1 Pb1 I3 90.94(3) . . ?
I3 Pb1 I2 89.20(2) . . ?
I3 Pb1 I2 90.69(3) 3_545 . ?
I3 Pb1 I3 179.739(12) . 3_545 ?
I4A Pb1 I1 88.55(3) . . ?
I4A Pb1 I2 90.87(3) . . ?
I4A Pb1 I3 92.91(3) . 3_545 ?
I4A Pb1 I3 87.33(3) . . ?
I4A Pb1 I5B 179.41(4) . . ?
I5B Pb1 I1 91.92(3) . . ?
I5B Pb1 I2 88.66(3) . . ?
I5B Pb1 I3 92.32(3) . . ?
I5B Pb1 I3 87.44(3) . 3_545 ?
Pb1 I3 Pb1 168.24(4) . 3 ?
Pb1 I4A Pb1 152.25(5) 6_556 . ?
Pb1 I5B Pb1 153.42(5) . 6 ?
N11 C1 N11 123.8(15) . 6_556 ?
N11 C1 N12 117.9(8) . . ?
N11 C1 N12 117.9(8) 6_556 . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N21 C2 N21 125.7(17) . 6 ?
N21 C2 N22 117.1(9) . . ?
N21 C2 N22 117.1(9) 6 . ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22A 120.0 . . ?
C2 N22 H22B 120.0 . . ?
H22A N22 H22B 120.0 . . ?

_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 2.348
_oxdiff_exptl_absorpt_empirical_full_min 0.384
####################################################################### 
# 
# 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_G2PbI4_0
_database_code_depnum_ccdc_archive 'CCDC 2428386'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_systematic        'Guanidinium lead(II) tetraiodide'
_chemical_formula_sum            'C2 H12 I4 N6 Pb'
_chemical_formula_weight         834.97
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.843(4)
_cell_length_b                   27.036(4)
_cell_length_c                   9.2962(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.783(11)
_cell_angle_gamma                90
_cell_volume                     3227.6(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1315
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       10000(10000)
_cell_measurement_theta_max      26.7000
_cell_measurement_theta_min      2.6390
_exptl_absorpt_coefficient_mu    18.086
_exptl_absorpt_correction_T_max  0.23786
_exptl_absorpt_correction_T_min  0.21751
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 0.01(1) GPa
(10000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.437
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.041
_exptl_crystal_size_rad          0.05
_diffrn_reflns_av_R_equivalents  0.1593
_diffrn_reflns_av_unetI/netI     0.1306
_diffrn_reflns_Laue_measured_fraction_full 0.321
_diffrn_reflns_Laue_measured_fraction_max 0.250
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14406
_diffrn_reflns_point_group_measured_fraction_full 0.321
_diffrn_reflns_point_group_measured_fraction_max 0.250
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.433
_diffrn_reflns_theta_min         2.187
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.321
_diffrn_measured_fraction_theta_max 0.250
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   60.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   60.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   60.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   60.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   60.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   60.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   60.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   60.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   60.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   60.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   60.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   60.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   60.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   60.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   60.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   60.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0005573000
_diffrn_orient_matrix_UB_12      -0.0132323000
_diffrn_orient_matrix_UB_13      0.0477346000
_diffrn_orient_matrix_UB_21      0.0635443000
_diffrn_orient_matrix_UB_22      0.0124482000
_diffrn_orient_matrix_UB_23      0.0163197000
_diffrn_orient_matrix_UB_31      -0.0422032000
_diffrn_orient_matrix_UB_32      0.0189209000
_diffrn_orient_matrix_UB_33      0.0225517000
_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                965
_reflns_number_total             2027
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.090
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.229
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2027
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1863
_refine_ls_R_factor_gt           0.0772
_refine_ls_restrained_S_all      1.036
_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)+(0.0732P)²+70.9238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.2116
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Restrained distances
 C2-N5
 1.25 with sigma of 0.02
 N2-N6
 2.15 with sigma of 0.02
3. Others
 Uiso(N1)=Uiso(N10)=Uiso(N11)=Uiso(N2)=Uiso(N4)=Uiso(N6)=Uiso(N7)=Uiso(N8)=
 Uiso(N3)=Uiso(N9)=Uiso(N25)=Uiso(N5)=FVAR(1)
 Uiso(C1)=Uiso(C4)=Uiso(C2)=Uiso(C10)=FVAR(2)
4.a X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N10(H10A,H10B), N11(H11A,H11B), N2(H2A,H2B), N4(H4A,H4B), N6(H6A,
 H6B), N7(H7A,H7B), N8(H8A,H8B), N3(H3A,H3B), N9(H9A,H9B), N25(H25A,H25B),
 N5(H5A,H5B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.2542(2) 0.08897(6) 0.24294(19) 0.0464(13) Uani 1 1 d . . . . .
Pb2 Pb 0.7566(2) 0.08513(6) 0.25033(19) 0.0440(13) Uani 1 1 d . . . . .
I3 I 0.5025(5) 0.07581(13) 0.1925(4) 0.061(2) Uani 1 1 d . . . . .
I4 I 0.7213(5) 0.15861(13) 0.5065(4) 0.073(2) Uani 1 1 d . . . . .
I5 I 0.0046(4) 0.10223(13) 0.3015(4) 0.060(2) Uani 1 1 d . . . . .
I6 I 0.2092(4) -0.00146(11) 0.0000(3) 0.054(2) Uani 1 1 d . . . . .
I7 I 0.2378(4) 0.16926(12) 0.0024(3) 0.062(2) Uani 1 1 d . . . . .
I8 I 0.2467(4) 0.00426(11) 0.4989(3) 0.051(2) Uani 1 1 d . . . . .
I9 I 0.2985(5) 0.16732(11) 0.4750(4) 0.063(2) Uani 1 1 d . . . . .
I10 I 0.7592(4) 0.16724(12) 0.0218(3) 0.061(2) Uani 1 1 d . . . . .
C1 C 0.503(8) -0.068(2) 0.253(6) 0.076(11) Uiso 1 1 d . U . . .
N1 N 0.406(7) -0.0712(16) 0.207(6) 0.121(6) Uiso 1 1 d . U . . .
H1A H 0.392009 -0.068964 0.116598 0.145 Uiso 1 1 calc R U . . .
H1B H 0.356651 -0.075709 0.267271 0.145 Uiso 1 1 calc R U . . .
N10 N 0.499(6) -0.0657(17) 0.408(5) 0.121(6) Uiso 1 1 d . U . . .
H10A H 0.555025 -0.060263 0.457211 0.145 Uiso 1 1 calc R U . . .
H10B H 0.440886 -0.069968 0.450996 0.145 Uiso 1 1 calc R U . . .
N11 N 0.582(6) -0.0616(18) 0.199(6) 0.121(6) Uiso 1 1 d . U . . .
H11A H 0.585665 -0.058442 0.107483 0.145 Uiso 1 1 calc R U . . .
H11B H 0.638308 -0.060312 0.251153 0.145 Uiso 1 1 calc R U . . .
N2 N 1.094(5) 0.104(2) -0.305(6) 0.121(6) Uiso 1 1 d D U . . .
H2A H 1.120013 0.094183 -0.384125 0.145 Uiso 1 1 calc R U . . .
H2B H 1.119081 0.130297 -0.263141 0.145 Uiso 1 1 calc R U . . .
N4 N 0.995(6) 0.0933(17) -0.101(5) 0.121(6) Uiso 1 1 d . U . . .
H4A H 1.028631 0.115404 -0.053108 0.145 Uiso 1 1 calc R U . . .
H4B H 0.944090 0.077754 -0.061491 0.145 Uiso 1 1 calc R U . . .
N6 N 0.983(5) 0.0454(18) -0.301(5) 0.121(6) Uiso 1 1 d D U . . .
H6A H 1.005079 0.033239 -0.380283 0.145 Uiso 1 1 calc R U . . .
H6B H 0.932443 0.031350 -0.256850 0.145 Uiso 1 1 calc R U . . .
C4 C 1.023(8) 0.082(2) -0.251(5) 0.076(11) Uiso 1 1 d . U . . .
C2 C 1.010(7) 0.241(2) -0.299(6) 0.076(11) Uiso 1 1 d D U . . .
N7 N 0.935(7) 0.226(2) -0.254(5) 0.121(6) Uiso 1 1 d . U . . .
H7A H 0.908457 0.198796 -0.288714 0.145 Uiso 1 1 calc R U . . .
H7B H 0.904529 0.240667 -0.184782 0.145 Uiso 1 1 calc R U . . .
N8 N 1.023(6) 0.2878(19) -0.257(5) 0.121(6) Uiso 1 1 d . U . . .
H8A H 0.977920 0.301950 -0.204064 0.145 Uiso 1 1 calc R U . . .
H8B H 1.077460 0.303860 -0.284253 0.145 Uiso 1 1 calc R U . . .
N3 N 0.565(6) 0.2520(18) -0.301(5) 0.121(6) Uiso 1 1 d . U . . .
H3A H 0.568358 0.282894 -0.321832 0.145 Uiso 1 1 calc R U . . .
H3B H 0.614928 0.232452 -0.324835 0.145 Uiso 1 1 calc R U . . .
N9 N 0.487(6) 0.190(2) -0.169(5) 0.121(6) Uiso 1 1 d . U . . .
H9A H 0.449142 0.178894 -0.100280 0.145 Uiso 1 1 calc R U . . .
H9B H 0.536848 0.172149 -0.201629 0.145 Uiso 1 1 calc R U . . .
C10 C 0.470(8) 0.231(2) -0.220(6) 0.076(11) Uiso 1 1 d . U . . .
N25 N 0.408(7) 0.262(2) -0.194(5) 0.121(6) Uiso 1 1 d . U . . .
H25A H 0.363214 0.256779 -0.127209 0.145 Uiso 1 1 calc R U . . .
H25B H 0.407075 0.289108 -0.241115 0.145 Uiso 1 1 calc R U . . .
N5 N 1.052(5) 0.2179(19) -0.399(5) 0.121(6) Uiso 1 1 d D U . . .
H5A H 1.024010 0.191252 -0.431905 0.145 Uiso 1 1 calc R U . . .
H5B H 1.108781 0.228832 -0.434316 0.145 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I3 3.248(7) . ?
Pb1 I5 3.279(6) . ?
Pb1 I6 3.373(4) . ?
Pb1 I7 3.121(4) . ?
Pb1 I8 3.305(3) . ?
Pb1 I9 3.071(4) . ?
Pb2 I3 3.310(7) . ?
Pb2 I4 3.139(4) . ?
Pb2 I5 3.247(6) 1_655 ?
Pb2 I6 3.279(4) 3_655 ?
Pb2 I8 3.359(3) 3_656 ?
Pb2 I10 3.073(4) . ?
C1 N1 1.31(10) . ?
C1 N10 1.44(6) . ?
C1 N11 1.16(10) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C4 1.21(8) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C4 1.48(7) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
N6 C4 1.21(6) . ?
C2 N7 1.13(9) . ?
C2 N8 1.34(6) . ?
C2 N5 1.24(2) . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
N8 H8A 0.8600 . ?
N8 H8B 0.8600 . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 C10 1.55(10) . ?
N9 H9A 0.8600 . ?
N9 H9B 0.8600 . ?
N9 C10 1.23(6) . ?
C10 N25 1.17(9) . ?
N25 H25A 0.8600 . ?
N25 H25B 0.8600 . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3 Pb1 I5 178.74(10) . . ?
I3 Pb1 I6 89.05(12) . . ?
I3 Pb1 I8 93.80(11) . . ?
I5 Pb1 I6 91.80(13) . . ?
I5 Pb1 I8 85.30(11) . . ?
I7 Pb1 I3 91.69(13) . . ?
I7 Pb1 I5 89.22(13) . . ?
I7 Pb1 I6 90.87(9) . . ?
I7 Pb1 I8 174.46(16) . . ?
I8 Pb1 I6 88.47(9) . . ?
I9 Pb1 I3 90.25(14) . . ?
I9 Pb1 I5 88.85(14) . . ?
I9 Pb1 I6 177.14(11) . . ?
I9 Pb1 I7 91.92(10) . . ?
I9 Pb1 I8 88.81(10) . . ?
I3 Pb2 I8 92.07(11) . 3_656 ?
I4 Pb2 I3 91.09(14) . . ?
I4 Pb2 I5 87.15(14) . 1_655 ?
I4 Pb2 I6 175.65(11) . 3_655 ?
I4 Pb2 I8 85.72(10) . 3_656 ?
I5 Pb2 I3 176.08(10) 1_655 . ?
I5 Pb2 I6 93.54(12) 1_655 3_655 ?
I5 Pb2 I8 91.29(11) 1_655 3_656 ?
I6 Pb2 I3 88.48(12) 3_655 . ?
I6 Pb2 I8 89.96(9) 3_655 3_656 ?
I10 Pb2 I3 87.87(13) . . ?
I10 Pb2 I4 94.03(11) . . ?
I10 Pb2 I5 88.76(13) . 1_655 ?
I10 Pb2 I6 90.28(10) . 3_655 ?
I10 Pb2 I8 179.75(13) . 3_656 ?
Pb1 I3 Pb2 159.35(13) . . ?
Pb2 I5 Pb1 156.85(13) 1_455 . ?
Pb2 I6 Pb1 162.15(19) 3_655 . ?
Pb1 I8 Pb2 177.67(13) . 3_656 ?
N1 C1 N10 107(8) . . ?
N11 C1 N1 135(7) . . ?
N11 C1 N10 118(9) . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C1 N10 H10A 120.0 . . ?
C1 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C4 N2 H2A 120.0 . . ?
C4 N2 H2B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C4 N4 H4A 120.0 . . ?
C4 N4 H4B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C4 N6 H6A 120.0 . . ?
C4 N6 H6B 120.0 . . ?
N2 C4 N4 119(7) . . ?
N2 C4 N6 125(7) . . ?
N6 C4 N4 115(6) . . ?
N7 C2 N8 110(6) . . ?
N7 C2 N5 119(7) . . ?
N5 C2 N8 129(7) . . ?
C2 N7 H7A 120.0 . . ?
C2 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
C2 N8 H8A 120.0 . . ?
C2 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C10 N3 H3A 120.0 . . ?
C10 N3 H3B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C10 N9 H9A 120.0 . . ?
C10 N9 H9B 120.0 . . ?
N9 C10 N3 112(8) . . ?
N25 C10 N3 113(8) . . ?
N25 C10 N9 132(9) . . ?
C10 N25 H25A 120.0 . . ?
C10 N25 H25B 120.0 . . ?
H25A N25 H25B 120.0 . . ?
C2 N5 H5A 120.0 . . ?
C2 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?

_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 1.418
_oxdiff_exptl_absorpt_empirical_full_min 0.863
####################################################################### 
# 
# 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_CsGPbI4_1_92
_database_code_depnum_ccdc_archive 'CCDC 2428389'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   18.043(8)
_cell_length_b                   12.2374(4)
_cell_length_c                   11.7887(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2602.9(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3581
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       1920000(30000)
_cell_measurement_theta_max      28.1200
_cell_measurement_theta_min      1.7300
_shelx_estimated_absorpt_T_max   0.433
_shelx_estimated_absorpt_T_min   0.093
_exptl_absorpt_coefficient_mu    25.164
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.115
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 1.92(3) GPa
(1920000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.633
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -1 16 0.0746
-3 1 -16 0.0636
-5 -17 -2 0.0679
5 17 4 0.1066
1 14 -10 0.0858
5 10 13 0.0855
-25 3 2 0.0220
25 -3 -2 0.0220

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.044
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.558     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 163.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
3.2641 -0.9962 16.4273 -0.0062 -0.8403 -0.5420
-3.1741 1.3417 -16.4119 0.0061 0.8291 0.5590
-4.5900 -16.8606 -1.6746 0.0057 0.5966 -0.8025
4.9008 16.5046 3.5452 -0.0063 -0.6850 0.7286
1.2666 13.6493 -10.0932 -0.0001 0.1236 0.9923
5.2640 9.5955 13.3491 -0.0082 -0.9963 0.0857
-24.8712 2.9548 2.3641 -1.0000 0.0000 0.0000
24.8712 -2.9548 -2.3641 1.0000 0.0000 0.0000

_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.357
_diffrn_reflns_Laue_measured_fraction_max 0.278
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10780
_diffrn_reflns_point_group_measured_fraction_full 0.357
_diffrn_reflns_point_group_measured_fraction_max 0.278
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.825
_diffrn_reflns_theta_min         2.399
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.357
_diffrn_measured_fraction_theta_max 0.278
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   70.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   70.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   70.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   70.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0382172971
_diffrn_orient_matrix_UB_12      -0.0098896138
_diffrn_orient_matrix_UB_13      -0.0085729651
_diffrn_orient_matrix_UB_21      -0.0082031837
_diffrn_orient_matrix_UB_22      -0.0280614035
_diffrn_orient_matrix_UB_23      -0.0512273769
_diffrn_orient_matrix_UB_31      0.0030122268
_diffrn_orient_matrix_UB_32      0.0498149430
_diffrn_orient_matrix_UB_33      -0.0305721696
_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                620
_reflns_number_total             991
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.000074(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         991
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0317
_refine_ls_restrained_S_all      1.259
_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)+(0.0172P)²+24.7927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0726
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5)
 Fixed X: H22(0.55893)
 Fixed Y: H22(0.12215)
 Fixed Z: H22(0.062429)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_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 0.25098(8) 0.87509(7) 0.25135(4) 0.0272(11) Uani 1 1 d . . . . .
Cs1 Cs 0.4098(2) 0.62416(14) 0.500000 0.037(2) Uani 1 2 d S T P . .
I1 I 0.42055(16) 0.87792(9) 0.31069(8) 0.0370(19) Uani 1 1 d . . . . .
I2 I 0.07920(15) 0.87282(9) 0.19543(8) 0.0369(18) Uani 1 1 d . . . . .
Cs2 Cs 0.3917(2) 1.12529(13) 0.500000 0.040(2) Uani 1 2 d S T P . .
I3 I 0.24876(16) 1.12460(8) 0.20094(10) 0.0451(17) Uani 1 1 d . . . . .
I4B I 0.2190(3) 0.93562(14) 0.500000 0.048(3) Uani 1 2 d S T P . .
I5A I 0.2777(3) 0.81574(14) 0.000000 0.042(3) Uani 1 2 d S T P . .
C1 C -0.042(4) 0.884(2) 0.500000 0.029(8) Uiso 1 2 d S . P . .
N11 N -0.0765(16) 0.8832(9) 0.4025(10) 0.035(4) Uiso 1 1 d . . . . .
H11A H -0.051879 0.875900 0.340436 0.042 Uiso 1 1 calc R U . . .
H11B H -0.123900 0.890120 0.400414 0.042 Uiso 1 1 calc R U . . .
N12 N 0.032(3) 0.8727(16) 0.500000 0.034(7) Uiso 1 2 d S . P . .
H12A H 0.055607 0.865524 0.436936 0.040 Uiso 0.5 1 calc R U P . .
H12B H 0.056105 0.872804 0.563064 0.040 Uiso 0.5 1 calc R U P . .
C2 C 0.460(4) 0.116(2) 0.000000 0.034(9) Uiso 1 2 d S . P . .
N21 N 0.4281(19) 0.1135(11) 0.0964(12) 0.055(5) Uiso 1 1 d . . . . .
H21A H 0.380644 0.109390 0.100618 0.066 Uiso 1 1 calc R U . . .
H21B H 0.454261 0.115764 0.157422 0.066 Uiso 1 1 calc R U . . .
N22 N 0.535(4) 0.1239(18) 0.000000 0.037(7) Uiso 1 2 d S . P . .
H22 H 0.558930 0.122150 0.062429 0.044 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.139(3) . ?
Pb1 I2 3.169(3) . ?
Pb1 I3 3.1165(12) 3_545 ?
Pb1 I3 3.1110(12) . ?
Pb1 I4B 3.0778(11) . ?
Pb1 I5A 3.0887(10) . ?
C1 N11 1.31(4) . ?
C1 N11 1.31(4) 6_556 ?
C1 N12 1.34(8) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C2 N21 1.27(4) . ?
C2 N21 1.27(4) 6 ?
C2 N22 1.35(9) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22 0.86(3) . ?
N22 H22 0.86(3) 6 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 179.12(3) . . ?
I3 Pb1 I1 88.23(6) 3_545 . ?
I3 Pb1 I1 92.54(6) . . ?
I3 Pb1 I2 91.74(6) 3_545 . ?
I3 Pb1 I2 87.49(6) . . ?
I3 Pb1 I3 179.10(4) 3_545 . ?
I4B Pb1 I1 88.15(9) . . ?
I4B Pb1 I2 90.98(9) . . ?
I4B Pb1 I3 86.75(4) . . ?
I4B Pb1 I3 93.73(4) . 3_545 ?
I4B Pb1 I5A 178.15(14) . . ?
I5A Pb1 I1 93.68(9) . . ?
I5A Pb1 I2 87.20(9) . . ?
I5A Pb1 I3 92.84(4) . . ?
I5A Pb1 I3 86.65(4) . 3_545 ?
Pb1 I3 Pb1 158.57(4) 3 . ?
Pb1 I4B Pb1 144.49(12) 6_556 . ?
Pb1 I5A Pb1 147.21(11) . 6 ?
N11 C1 N11 123(6) . 6_556 ?
N12 C1 N11 118(3) . 6_556 ?
N12 C1 N11 118(3) . . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N21 C2 N21 127(7) . 6 ?
N21 C2 N22 117(4) . . ?
N21 C2 N22 117(4) 6 . ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22 121(4) . . ?
C2 N22 H22 121(4) . 6 ?
H22 N22 H22 118(7) . 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 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.687
####################################################################### 
# 
# 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_CsGPbI4_2_76
_database_code_depnum_ccdc_archive 'CCDC 2428391'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   17.914(8)
_cell_length_b                   12.0823(4)
_cell_length_c                   11.6499(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2521.5(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3460
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       2760000(30000)
_cell_measurement_theta_max      28.2230
_cell_measurement_theta_min      1.7610
_shelx_estimated_absorpt_T_max   0.423
_shelx_estimated_absorpt_T_min   0.089
_exptl_absorpt_coefficient_mu    25.976
_exptl_absorpt_correction_T_max  0.236
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 2.76(3) GPa
(2760000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.783
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 4 -16 0.0648
4 -4 16 0.0747
3 -16 -4 0.0788
-6 13 -10 0.0771
0 10 13 0.0762
-4 17 3 0.0959
25 3 -2 0.0220
-25 -3 2 0.0220

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.044
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.485     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 161.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
-4.4384 3.6996 -15.7449 -0.0081 -0.9580 -0.2868
4.4895 -3.9529 15.6814 0.0081 0.9623 0.2719
3.3902 -16.4041 -3.7553 0.0012 0.2998 -0.9540
-5.5405 13.3439 -9.5128 -0.0069 -0.9183 0.3958
0.4575 9.7722 13.4240 0.0045 0.4217 0.9067
-3.6195 16.5661 2.9078 -0.0017 -0.3503 0.9367
24.6701 2.9265 -2.4141 -1.0000 0.0000 0.0000
-24.6701 -2.9265 2.4141 1.0000 0.0000 0.0000

_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.360
_diffrn_reflns_Laue_measured_fraction_max 0.287
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10382
_diffrn_reflns_point_group_measured_fraction_full 0.360
_diffrn_reflns_point_group_measured_fraction_max 0.287
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.569
_diffrn_reflns_theta_min         2.085
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.360
_diffrn_measured_fraction_theta_max 0.287
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   70.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   70.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   70.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   70.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0384594501
_diffrn_orient_matrix_UB_12      -0.0100819421
_diffrn_orient_matrix_UB_13      0.0089879306
_diffrn_orient_matrix_UB_21      0.0084362779
_diffrn_orient_matrix_UB_22      -0.0283911227
_diffrn_orient_matrix_UB_23      0.0517938810
_diffrn_orient_matrix_UB_31      -0.0029623853
_diffrn_orient_matrix_UB_32      0.0504681278
_diffrn_orient_matrix_UB_33      0.0309068008
_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                613
_reflns_number_total             971
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         971
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      1.194
_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)+(0.0382P)²+38.7819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1161
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H22A(0.5) H22B(0.5)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B), N22(H22A,H22B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.25131(10) 0.87507(8) 0.25152(5) 0.0251(17) Uani 1 1 d . . . . .
Cs1 Cs 0.4118(3) 0.62359(16) 0.500000 0.028(3) Uani 1 2 d S T P . .
I1 I 0.4214(2) 0.87749(10) 0.31195(10) 0.032(3) Uani 1 1 d . . . . .
I2 I 0.0794(2) 0.87276(10) 0.19517(10) 0.031(2) Uani 1 1 d . . . . .
Cs2 Cs 0.3927(3) 1.12535(15) 0.500000 0.032(3) Uani 1 2 d S T P . .
I3 I 0.2482(2) 1.12445(9) 0.19580(13) 0.037(2) Uani 1 1 d . . . . .
I4A I 0.2195(3) 0.94037(17) 0.500000 0.043(4) Uani 1 2 d S T P . .
I5A I 0.2772(3) 0.81105(18) 0.000000 0.035(4) Uani 1 2 d S T P . .
C1 C -0.040(5) 0.880(2) 0.500000 0.018(8) Uiso 1 2 d S . P . .
N11 N -0.076(2) 0.8834(10) 0.4015(13) 0.026(4) Uiso 1 1 d . . . . .
H11A H -0.123610 0.888484 0.400259 0.031 Uiso 1 1 calc R U . . .
H11B H -0.051107 0.880805 0.338162 0.031 Uiso 1 1 calc R U . . .
N12 N 0.037(5) 0.8751(19) 0.500000 0.038(9) Uiso 1 2 d S . P . .
H12A H 0.061177 0.874836 0.563920 0.046 Uiso 0.5 1 calc R U P . .
H12B H 0.061119 0.872646 0.436080 0.046 Uiso 0.5 1 calc R U P . .
C2 C 0.465(6) 0.116(3) 0.000000 0.034(12) Uiso 1 2 d S . P . .
N21 N 0.429(2) 0.1139(12) 0.1000(16) 0.047(6) Uiso 1 1 d . . . . .
H21A H 0.452894 0.116264 0.163634 0.056 Uiso 1 1 calc R U . . .
H21B H 0.380648 0.109987 0.100667 0.056 Uiso 1 1 calc R U . . .
N22 N 0.536(5) 0.122(2) 0.000000 0.032(9) Uiso 1 2 d S . P . .
H22A H 0.559459 0.124438 -0.063929 0.039 Uiso 0.5 1 calc R U P . .
H22B H 0.559485 0.123726 0.063929 0.039 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.128(4) . ?
Pb1 I2 3.148(4) . ?
Pb1 I3 3.0826(15) . ?
Pb1 I3 3.0897(15) 3_545 ?
Pb1 I4A 3.0538(14) . ?
Pb1 I5A 3.0659(12) . ?
C1 N11 1.31(5) 6_556 ?
C1 N11 1.31(5) . ?
C1 N12 1.39(11) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C2 N21 1.34(6) . ?
C2 N21 1.34(6) 6 ?
C2 N22 1.26(12) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22A 0.8600 . ?
N22 H22B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 179.03(4) . . ?
I3 Pb1 I1 93.20(8) . . ?
I3 Pb1 I1 87.81(8) 3_545 . ?
I3 Pb1 I2 86.97(8) . . ?
I3 Pb1 I2 92.02(8) 3_545 . ?
I3 Pb1 I3 178.88(6) . 3_545 ?
I4A Pb1 I1 88.04(11) . . ?
I4A Pb1 I2 91.01(11) . . ?
I4A Pb1 I3 93.75(5) . 3_545 ?
I4A Pb1 I3 86.78(5) . . ?
I4A Pb1 I5A 177.91(16) . . ?
I5A Pb1 I1 94.02(11) . . ?
I5A Pb1 I2 86.93(11) . . ?
I5A Pb1 I3 86.68(5) . 3_545 ?
I5A Pb1 I3 92.76(5) . . ?
Pb1 I3 Pb1 156.36(6) . 3 ?
Pb1 I4A Pb1 142.85(14) . 6_556 ?
Pb1 I5A Pb1 145.78(13) 6 . ?
N11 C1 N11 122(8) 6_556 . ?
N11 C1 N12 119(4) 6_556 . ?
N11 C1 N12 119(4) . . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N21 C2 N21 121(9) 6 . ?
N22 C2 N21 120(4) . . ?
N22 C2 N21 120(4) . 6 ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22A 120.0 . . ?
C2 N22 H22B 120.0 . . ?
H22A N22 H22B 120.0 . . ?

_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 1.356
_oxdiff_exptl_absorpt_empirical_full_min 0.712
####################################################################### 
# 
# 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_CsGPbI4_340K
_database_code_depnum_ccdc_archive 'CCDC 2428399'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'

_cell_length_a                   12.2916(3)
_cell_length_b                   6.39616(13)
_cell_length_c                   18.5282(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1456.67(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4868
_cell_measurement_temperature    340.01(10)
_cell_measurement_theta_min      1.9900
_cell_measurement_theta_max      29.9280
_exptl_absorpt_coefficient_mu    22.467
_exptl_absorpt_correction_T_min  0.057
_exptl_absorpt_correction_T_max  0.350
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.139
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -1 26 0.0248
2 1 -26 0.0348
6 -8 -5 0.0955
-6 8 11 0.1019
-17 -1 6 0.0843
17 1 -7 0.0746
2 -9 2 0.0823
8 8 -5 0.1032
-12 -6 6 0.0872
2 -1 -26 0.0281
-3 3 24 0.0551

_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.060
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
-1.9971 -1.3395 25.6581 0.4742 -0.8718 0.1231
1.9421 1.4183 -25.6322 -0.4736 0.8707 -0.1324
6.0025 -8.3100 -4.5682 -0.0931 0.1737 0.9804
-6.1995 7.5973 10.5134 0.2026 -0.3748 -0.9047
-16.7577 -0.6228 6.3837 0.9672 0.0765 -0.2423
16.5742 1.3469 -6.5339 -0.9836 -0.0778 0.1628
1.8277 -8.9396 2.0163 0.2272 0.0191 0.9737
7.5781 7.9089 -5.1837 -0.7191 -0.0578 -0.6925
-12.0080 -6.1275 6.2851 0.9029 0.0721 0.4238
1.5990 -0.9340 -25.8721 -0.3811 0.9182 0.1079
-3.0498 3.2400 23.9414 0.3551 -0.8548 -0.3784

_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8824
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.285
_diffrn_reflns_theta_min         1.988
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      340.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  20.00   1.00   37.50    --  -23.33  99.00  72.00   94
  2  ω    -92.00  -4.00   1.00   37.50    --  -23.33 132.00 144.00   88
  3  ω    -67.00  39.00   1.00   37.50    --  -23.33  77.00 -30.00  106
  4  ω    -67.00  39.00   1.00   37.50    --  -23.33  77.00 -90.00  106
  5  ω    -21.00  39.00   1.00   37.50    --   22.87  77.00-120.00   60
  6  ω   -114.00  23.00   1.00   37.50    --  -23.33 -38.00 -60.00  137
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0516349000
_diffrn_orient_matrix_UB_12      -0.0330957000
_diffrn_orient_matrix_UB_13      0.0127350000
_diffrn_orient_matrix_UB_21      -0.0177921000
_diffrn_orient_matrix_UB_22      -0.0139176000
_diffrn_orient_matrix_UB_23      -0.0360875000
_diffrn_orient_matrix_UB_31      0.0186513000
_diffrn_orient_matrix_UB_32      -0.1049290000
_diffrn_orient_matrix_UB_33      0.0007721000
_diffrn_radiation_type           MoK\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                1084
_reflns_number_total             1168
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       0.00044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         1168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0232
_refine_ls_restrained_S_all      1.147
_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)+(0.0234P)²+3.3326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0539
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H5A(0.25) H5B(0.25) I2(0.25)
3.a X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N3(H3A,H3B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.250000 0.250000 0.250000 0.03029(10) Uani 1 4 d S T P . .
Cs2 Cs 0.000000 -0.250000 0.10642(5) 0.0670(2) Uani 1 4 d S T P . .
I3 I 0.19533(4) 0.250000 0.08091(2) 0.05061(13) Uani 1 2 d S T P . .
N5 N 0.000000 0.250000 0.4727(5) 0.061(2) Uiso 1 4 d S . P . .
H5A H 0.060593 0.250000 0.449443 0.074 Uiso 0.5 2 calc R U P . .
H5B H -0.060593 0.250000 0.449443 0.074 Uiso 0.5 2 calc R U P . .
I1 I 0.250000 -0.250000 0.250000 0.0672(2) Uani 1 4 d S T P . .
N3 N 0.0920(7) 0.250000 0.5756(4) 0.078(2) Uiso 1 2 d S . P . .
H3A H 0.094662 0.250000 0.621968 0.094 Uiso 1 2 calc R U P . .
H3B H 0.151226 0.250000 0.550868 0.094 Uiso 1 2 calc R U P . .
C1 C 0.000000 0.250000 0.5434(5) 0.0407(17) Uiso 1 4 d S . P . .
I2 I 0.000000 0.2989(3) 0.28155(5) 0.0643(6) Uani 0.5 2 d S T 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 I3 3.2043(4) 13 ?
Pb1 I3 3.2042(4) . ?
Pb1 I1 3.19808(6) 1_565 ?
Pb1 I1 3.19808(6) . ?
Pb1 I2 3.1436(3) 14 ?
Pb1 I2 3.1436(3) . ?
Pb1 I2 3.1436(3) 13 ?
Pb1 I2 3.1436(3) 2 ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N5 C1 1.310(12) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 C1 1.279(9) . ?
I2 I2 0.626(3) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3 Pb1 I3 180.0 . 13 ?
I1 Pb1 I3 90.0 . . ?
I1 Pb1 I3 90.0 1_565 13 ?
I1 Pb1 I3 90.0 . 13 ?
I1 Pb1 I3 90.0 1_565 . ?
I1 Pb1 I1 180.0 . 1_565 ?
I2 Pb1 I3 88.671(18) 2 . ?
I2 Pb1 I3 91.329(18) 13 . ?
I2 Pb1 I3 88.670(18) 13 13 ?
I2 Pb1 I3 91.329(18) . 13 ?
I2 Pb1 I3 88.670(18) 14 13 ?
I2 Pb1 I3 91.330(18) 2 13 ?
I2 Pb1 I3 88.672(18) . . ?
I2 Pb1 I3 91.329(18) 14 . ?
I2 Pb1 I1 95.71(3) 14 . ?
I2 Pb1 I1 95.71(3) 2 1_565 ?
I2 Pb1 I1 84.29(3) . 1_565 ?
I2 Pb1 I1 84.29(3) 14 1_565 ?
I2 Pb1 I1 84.29(3) 13 . ?
I2 Pb1 I1 95.71(3) 13 1_565 ?
I2 Pb1 I1 84.29(3) 2 . ?
I2 Pb1 I1 95.71(3) . . ?
I2 Pb1 I2 11.43(6) 2 . ?
I2 Pb1 I2 180.0 14 2 ?
I2 Pb1 I2 180.0 13 . ?
I2 Pb1 I2 168.57(6) 2 13 ?
I2 Pb1 I2 11.43(6) 14 13 ?
I2 Pb1 I2 168.57(6) 14 . ?
H5A N5 H5B 120.0 . . ?
C1 N5 H5A 120.0 . . ?
C1 N5 H5B 120.0 . . ?
Pb1 I1 Pb1 180.0 1_545 . ?
H3A N3 H3B 120.0 . . ?
C1 N3 H3A 120.0 . . ?
C1 N3 H3B 120.0 . . ?
N3 C1 N5 117.8(5) 2 . ?
N3 C1 N5 117.8(5) . . ?
N3 C1 N3 124.4(10) . 2 ?
Pb1 I2 Pb1 155.65(4) 2 . ?
I2 I2 Pb1 84.29(3) 2 . ?
I2 I2 Pb1 84.29(3) 2 2 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CsGPbI4_4_46
_database_code_depnum_ccdc_archive 'CCDC 2428390'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   17.60(2)
_cell_length_b                   11.8686(12)
_cell_length_c                   11.4888(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2399(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1896
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       4460000(30000)
_cell_measurement_theta_max      28.8930
_cell_measurement_theta_min      2.4560
_shelx_estimated_absorpt_T_max   0.408
_shelx_estimated_absorpt_T_min   0.084
_exptl_absorpt_coefficient_mu    27.300
_exptl_absorpt_correction_T_max  0.225
_exptl_absorpt_correction_T_min  0.059
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 4.46(3) GPa
(4460000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    5.026
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 -16 0.0646
2 -1 16 0.0686
-3 -17 0 0.0691
4 16 2 0.1003
1 12 -12 0.0747
4 9 14 0.0803
-24 3 2 0.0220
24 -3 -2 0.0220

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.044
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.328     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 180.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
-2.2328 1.4655 -16.0468 0.0203 0.8170 0.5762
2.3824 -0.7742 16.0835 -0.0209 -0.8404 -0.5416
-3.4484 -16.5666 -0.0132 0.0140 0.5135 -0.8580
3.7248 16.4174 1.9569 -0.0165 -0.6133 0.7896
0.5489 11.5327 -11.6998 0.0059 0.2718 0.9623
3.9615 8.7310 13.5645 -0.0256 -0.9992 0.0295
-24.3493 2.5998 2.0251 -1.0000 0.0000 0.0000
24.3493 -2.5998 -2.0251 1.0000 0.0000 0.0000

_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.331
_diffrn_reflns_Laue_measured_fraction_max 0.270
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9051
_diffrn_reflns_point_group_measured_fraction_full 0.331
_diffrn_reflns_point_group_measured_fraction_max 0.270
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.482
_diffrn_reflns_theta_min         2.467
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.331
_diffrn_measured_fraction_theta_max 0.270
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   70.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   70.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   70.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   70.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0394712487
_diffrn_orient_matrix_UB_12      -0.0090572948
_diffrn_orient_matrix_UB_13      -0.0075826408
_diffrn_orient_matrix_UB_21      -0.0075090117
_diffrn_orient_matrix_UB_22      -0.0293907765
_diffrn_orient_matrix_UB_23      -0.0525546899
_diffrn_orient_matrix_UB_31      0.0028389770
_diffrn_orient_matrix_UB_32      0.0512239699
_diffrn_orient_matrix_UB_33      -0.0316269365
_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                489
_reflns_number_total             861
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.295
_refine_diff_density_min         -1.712
_refine_diff_density_rms         0.353
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         861
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1622
_refine_ls_R_factor_gt           0.0979
_refine_ls_restrained_S_all      1.203
_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)+(0.0467P)²+486.1730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2289
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H2A(0.5) H2B(0.5)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N2(H2A,H2B), N21(H21A,H21B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.2523(4) 0.8766(2) 0.25174(17) 0.055(5) Uani 1 1 d . . . . .
Cs1 Cs 0.4112(9) 0.6223(5) 0.500000 0.064(10) Uani 1 2 d S T P . .
I1 I 0.4234(6) 0.8770(3) 0.3135(3) 0.049(7) Uani 1 1 d . . . . .
I2 I 0.0784(6) 0.8729(3) 0.1953(3) 0.057(8) Uani 1 1 d . . . . .
Cs2 Cs 0.3935(9) 1.1251(4) 0.500000 0.059(10) Uani 1 2 d S T P . .
I3 I 0.2475(7) 1.1253(3) 0.1936(4) 0.076(8) Uani 1 1 d . . . . .
I4B I 0.2217(11) 0.9417(5) 0.500000 0.077(12) Uani 1 2 d S T P . .
I5A I 0.2755(10) 0.8101(5) 0.000000 0.059(11) Uani 1 2 d S T P . .
C1 C -0.039(15) 0.872(6) 0.500000 0.011(18) Uiso 1 2 d S . P . .
N11 N -0.082(6) 0.871(3) 0.401(4) 0.035(12) Uiso 1 1 d . . . . .
H11A H -0.059688 0.871902 0.334179 0.042 Uiso 1 1 calc R U . . .
H11B H -0.130304 0.868545 0.405603 0.042 Uiso 1 1 calc R U . . .
N12 N 0.035(13) 0.875(7) 0.500000 0.05(3) Uiso 1 2 d S . P . .
H12A H 0.059447 0.876088 0.564825 0.063 Uiso 0.5 1 calc R U P . .
H12B H 0.059463 0.875229 0.435175 0.063 Uiso 0.5 1 calc R U P . .
N2 N 0.539(13) 0.127(6) 0.000000 0.04(3) Uiso 1 2 d S . P . .
H2A H 0.562803 0.116842 -0.064197 0.043 Uiso 0.5 1 calc R U P . .
H2B H 0.563420 0.134268 0.064197 0.043 Uiso 0.5 1 calc R U P . .
N21 N 0.422(6) 0.123(3) 0.100(4) 0.034(12) Uiso 1 1 d . . . . .
H21A H 0.439045 0.112217 0.168824 0.040 Uiso 1 1 calc R U . . .
H21B H 0.373577 0.128262 0.088313 0.040 Uiso 1 1 calc R U . . .
C22 C 0.475(18) 0.132(8) 0.000000 0.03(3) Uiso 1 2 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 3.093(13) . ?
Pb1 I2 3.129(13) . ?
Pb1 I3 3.028(4) . ?
Pb1 I3 3.047(4) 3_545 ?
Pb1 I4B 3.004(4) . ?
Pb1 I5A 3.025(4) . ?
C1 N11 1.36(16) . ?
C1 N11 1.36(16) 6_556 ?
C1 N12 1.3(3) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
N2 H2A 0.8600 . ?
N2 H2A 0.8600 6 ?
N2 H2B 0.8600 . ?
N2 H2B 0.8600 6 ?
N2 C22 1.1(4) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N21 C22 1.5(2) . ?

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 I2 178.52(14) . . ?
I3 Pb1 I1 87.3(3) 3_545 . ?
I3 Pb1 I1 94.4(3) . . ?
I3 Pb1 I2 91.7(3) 3_545 . ?
I3 Pb1 I2 86.6(3) . . ?
I3 Pb1 I3 178.2(2) . 3_545 ?
I4B Pb1 I1 87.5(4) . . ?
I4B Pb1 I2 91.4(4) . . ?
I4B Pb1 I3 93.23(16) . 3_545 ?
I4B Pb1 I3 87.33(16) . . ?
I4B Pb1 I5A 177.4(6) . . ?
I5A Pb1 I1 95.1(4) . . ?
I5A Pb1 I2 86.0(4) . . ?
I5A Pb1 I3 86.65(16) . 3_545 ?
I5A Pb1 I3 92.71(16) . . ?
Pb1 I3 Pb1 155.32(17) . 3 ?
Pb1 I4B Pb1 143.4(5) . 6_556 ?
Pb1 I5A Pb1 145.9(4) 6 . ?
N11 C1 N11 113(10) 6_556 . ?
N12 C1 N11 123(10) . . ?
N12 C1 N11 123(10) . 6_556 ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
H2A N2 H2A 118.1 . 6 ?
H2A N2 H2B 13.8 . 6 ?
H2A N2 H2B 120.0 6 6 ?
H2A N2 H2B 120.0 . . ?
H2B N2 H2A 13.8 . 6 ?
H2B N2 H2B 118.1 . 6 ?
C22 N2 H2A 120.0 . . ?
C22 N2 H2A 120.0(11) . 6 ?
C22 N2 H2B 120.0 . . ?
C22 N2 H2B 120.0(11) . 6 ?
H21A N21 H21B 120.0 . . ?
C22 N21 H21A 120.0 . . ?
C22 N21 H21B 120.0 . . ?
N2 C22 N21 129(10) . 6 ?
N2 C22 N21 129(10) . . ?
N21 C22 N21 101(10) 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 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.469
####################################################################### 
# 
# 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_CsGPbI4_4_52
_database_code_depnum_ccdc_archive 'CCDC 2428400'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2025-02-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.475(19)
_cell_length_b                   11.8768(5)
_cell_length_c                   11.5309(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2393(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2235
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       4510000(30000)
_cell_measurement_theta_max      27.9670
_cell_measurement_theta_min      2.4440
_shelx_estimated_absorpt_T_max   0.407
_shelx_estimated_absorpt_T_min   0.084
_exptl_absorpt_coefficient_mu    27.369
_exptl_absorpt_correction_T_max  0.431
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
;
Data were collected at room temperature and pressure of 4.51(3) GPa
(4510000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    5.039
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 0 -16 0.1205
25 -1 1 0.0097
-25 1 -1 0.0097
-7 -16 0 0.0788
-4 -1 16 0.1087
7 16 -1 0.0747

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.566     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 174.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
3.6359 0.3143 -16.0069 0.0895 0.3787 -0.9212
24.7392 -0.9617 0.9741 1.0000 0.0000 0.0000
-24.7392 0.9617 -0.9741 -1.0000 0.0000 0.0000
-6.7012 -16.0501 -0.4915 -0.2175 -0.9065 -0.3619
-3.7168 -0.5117 15.9938 -0.0921 -0.3897 0.9163
6.9972 15.9628 -1.0303 0.2244 0.9358 0.2718

_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.238
_diffrn_reflns_Laue_measured_fraction_max 0.192
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9315
_diffrn_reflns_point_group_measured_fraction_full 0.238
_diffrn_reflns_point_group_measured_fraction_max 0.192
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.552
_diffrn_reflns_theta_min         2.462
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.238
_diffrn_measured_fraction_theta_max 0.192
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.80   0.40   65.00   0.00 -30.00   0.00    --   137
  2  φ    140.00 200.00   0.40   65.00   0.00 -30.00   0.00    --   150
  3  φ    160.00 216.80   0.40   65.00   0.00  30.00   0.00    --   142
  4  φ    -20.00  34.80   0.40   65.00   0.00  30.00   0.00    --   137
  5  ω    -24.00  24.00   0.40   65.00    --   30.00  39.46 -12.90  120
  6  ω    -24.00  24.00   0.40   65.00    --   30.00  39.46 167.10  120
  7  ω    -50.00  10.00   0.40   65.00    --  -30.00  39.46 167.10  150
  8  ω    -50.00  10.00   0.40   65.00    --  -30.00  39.46 -12.90  150
  9  ω    -64.00  -8.00   0.40   65.00    --  -30.00  81.40 -28.90  140
 10  ω    -64.00  -8.00   0.40   65.00    --  -30.00  81.40 151.10  140
 11  ω    -19.00   7.80   0.40   65.00    --   30.00  81.40 151.10   67
 12  ω    -19.00   7.80   0.40   65.00    --   30.00  81.40 -28.90   67
 13  ω    -43.00 -21.00   0.40   65.00    --   30.00 134.60 -56.90   55
 14  ω    -43.00 -21.00   0.40   65.00    --   30.00 134.60 123.10   55
 15  ω    -90.00 -36.00   0.40   65.00    --  -30.00 134.60 123.10  135
 16  ω    -90.00 -36.00   0.40   65.00    --  -30.00 134.60 -56.90  135
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0401561000
_diffrn_orient_matrix_UB_12      -0.0033211000
_diffrn_orient_matrix_UB_13      0.0034652000
_diffrn_orient_matrix_UB_21      0.0030335000
_diffrn_orient_matrix_UB_22      0.0558833000
_diffrn_orient_matrix_UB_23      -0.0218710000
_diffrn_orient_matrix_UB_31      -0.0014385000
_diffrn_orient_matrix_UB_32      0.0213809000
_diffrn_orient_matrix_UB_33      0.0576428000
_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                406
_reflns_number_total             613
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.039
_refine_diff_density_min         -1.964
_refine_diff_density_rms         0.269
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         613
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0765
_refine_ls_restrained_S_all      1.056
_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)+(0.0573P)²+466.9149P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.1971
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Restrained distances
 C1-N12
 1.3 with sigma of 0.02
 C2-N21
 1.3 with sigma of 0.02
 C2-N22
 1.3 with sigma of 0.02
 C1-N11
 1.3 with sigma of 0.02
3. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H22A(0.5) H22B(0.5)
4.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B), N22(H22A,H22B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.2523(5) 0.87370(17) 0.25200(17) 0.0339(7) Uiso 1 1 d . . . . .
Cs1 Cs 0.4124(11) 0.6227(4) 0.500000 0.034(16) Uani 1 2 d S T P . .
I1 I 0.4229(7) 0.8772(3) 0.3133(3) 0.040(12) Uani 1 1 d . . . . .
I4 I 0.0789(8) 0.8725(3) 0.1957(3) 0.038(13) Uani 1 1 d . . . . .
Cs2 Cs 0.3931(11) 1.1256(4) 0.500000 0.0371(13) Uiso 1 2 d S . P . .
I3 I 0.2480(8) 1.1249(3) 0.1919(4) 0.038(14) Uani 1 1 d . . . . .
C1 C -0.044(7) 0.872(6) 0.500000 0.016(18) Uiso 1 2 d DS . P . .
N11 N -0.078(6) 0.872(3) 0.400(3) 0.035(11) Uiso 1 1 d D . . . .
H11A H -0.051930 0.880539 0.337256 0.043 Uiso 1 1 calc R U . . .
H11B H -0.126858 0.863931 0.396423 0.043 Uiso 1 1 calc R U . . .
N12 N 0.030(7) 0.885(7) 0.500000 0.07(3) Uiso 1 2 d DS . P . .
H12A H 0.054478 0.893168 0.435532 0.079 Uiso 0.5 1 calc R U P . .
H12B H 0.055093 0.885526 0.564468 0.079 Uiso 0.5 1 calc R U P . .
C2 C 0.458(8) 0.126(9) 0.000000 0.05(4) Uiso 1 2 d DS . P . .
N21 N 0.424(7) 0.126(3) 0.100(4) 0.044(13) Uiso 1 1 d D . . . .
H21A H 0.374474 0.125782 0.102941 0.053 Uiso 1 1 calc R U . . .
H21B H 0.449936 0.126266 0.163013 0.053 Uiso 1 1 calc R U . . .
N22 N 0.532(8) 0.110(6) 0.000000 0.04(3) Uiso 1 2 d DS . P . .
H22A H 0.555861 0.100270 -0.064392 0.051 Uiso 0.5 1 calc R U P . .
H22B H 0.556831 0.109992 0.064392 0.051 Uiso 0.5 1 calc R U P . .
I2 I 0.2193(12) 0.9417(4) 0.500000 0.0452(15) Uiso 1 2 d S . P . .
I5 I 0.2758(12) 0.8083(4) 0.000000 0.0457(16) Uiso 1 2 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 3.064(15) . ?
Pb1 I4 3.098(16) . ?
Pb1 I3 3.025(4) 4_545 ?
Pb1 I3 3.064(4) . ?
Pb1 I2 3.027(5) . ?
Pb1 I5 3.036(4) . ?
C1 N11 1.30(2) 6_556 ?
C1 N11 1.30(2) . ?
C1 N12 1.30(2) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C2 N21 1.30(2) 6 ?
C2 N21 1.30(2) . ?
C2 N22 1.30(2) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22A 0.8600 6 ?
N22 H22A 0.8600 . ?
N22 H22B 0.8600 6 ?
N22 H22B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I4 178.64(15) . . ?
I1 Pb1 I3 93.6(3) . . ?
I3 Pb1 I1 88.0(3) 4_545 . ?
I3 Pb1 I4 86.2(3) . . ?
I3 Pb1 I4 92.2(3) 4_545 . ?
I3 Pb1 I3 178.3(3) 4_545 . ?
I3 Pb1 I2 93.33(14) 4_545 . ?
I3 Pb1 I5 87.43(14) 4_545 . ?
I2 Pb1 I1 87.9(4) . . ?
I2 Pb1 I4 90.7(4) . . ?
I2 Pb1 I3 87.10(14) . . ?
I2 Pb1 I5 176.7(6) . . ?
I5 Pb1 I1 95.3(4) . . ?
I5 Pb1 I4 86.0(4) . . ?
I5 Pb1 I3 92.06(14) . . ?
Pb1 I4 Cs1 154.3(3) . 3_465 ?
Pb1 I4 Cs1 94.8(4) . 7_665 ?
Cs1 I4 Cs1 69.5(4) 3_465 7_665 ?
Pb1 I3 Pb1 154.54(16) 4 . ?
Pb1 I3 Cs1 98.7(3) . 7_665 ?
Pb1 I3 Cs1 97.9(3) 4 7_665 ?
N11 C1 N11 125(8) . 6_556 ?
N11 C1 N12 117(4) . . ?
N12 C1 N11 117(4) . 6_556 ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N21 C2 N21 125(8) 6 . ?
N21 C2 N22 117(4) 6 . ?
N21 C2 N22 117(4) . . ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22A 120.0 . . ?
C2 N22 H22A 120.0(5) . 6 ?
C2 N22 H22B 120.0 . . ?
C2 N22 H22B 120.0(5) . 6 ?
H22A N22 H22A 119.4 . 6 ?
H22A N22 H22B 7.8 . 6 ?
H22A N22 H22B 120.0 . . ?
H22A N22 H22B 120.0 6 6 ?
H22B N22 H22A 7.8 . 6 ?
H22B N22 H22B 119.4 . 6 ?
Pb1 I2 Pb1 141.7(5) 6_556 . ?
Pb1 I5 Pb1 146.3(4) . 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 1.519
_oxdiff_exptl_absorpt_empirical_full_min 0.596
####################################################################### 
# 
# 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_CsGPbI4_0_61
_database_code_depnum_ccdc_archive 'CCDC 2428392'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   18.409(13)
_cell_length_b                   12.5357(7)
_cell_length_c                   12.0511(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2781.0(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2713
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       610000(30000)
_cell_measurement_theta_max      28.4930
_cell_measurement_theta_min      1.6800
_shelx_estimated_absorpt_T_max   0.453
_shelx_estimated_absorpt_T_min   0.101
_exptl_absorpt_coefficient_mu    23.552
_exptl_absorpt_correction_T_max  0.262
_exptl_absorpt_correction_T_min  0.120
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 0.61(3) GPa
(610000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -2 17 0.0682
3 1 -17 0.0696
-5 17 0 0.0714
5 -17 -3 0.0988
1 -14 10 0.0793
5 -9 -14 0.0738
-25 -3 -2 0.0220
25 3 2 0.0220

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.044
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.541     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 167.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Absorption coeff of pressure medium =   0.00 mm-1
;
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
-3.0146 -1.5992 16.8130 0.0061 0.8221 0.5692
3.0787 1.3634 -16.8273 -0.0061 -0.8298 -0.5580
-4.5537 17.4018 0.1779 0.0051 0.5202 -0.8540
4.9861 -17.1285 -2.6454 -0.0060 -0.6397 0.7686
1.4715 -13.8921 10.4651 0.0000 0.1330 0.9911
5.2413 -9.0250 -14.2084 -0.0081 -0.9995 0.0313
-25.2740 -3.1328 -2.3369 -1.0000 0.0000 0.0000
25.2740 3.1328 2.3369 1.0000 0.0000 0.0000

_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.358
_diffrn_reflns_Laue_measured_fraction_max 0.282
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11604
_diffrn_reflns_point_group_measured_fraction_full 0.358
_diffrn_reflns_point_group_measured_fraction_max 0.282
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.779
_diffrn_reflns_theta_min         2.344
_diffrn_ambient_temperature      293(2)

_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.358
_diffrn_measured_fraction_theta_max 0.282
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   90.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   90.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   90.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   90.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   90.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   90.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   90.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   90.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   90.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   90.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   90.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   90.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   90.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   90.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   90.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   90.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0375766000
_diffrn_orient_matrix_UB_12      0.0100450000
_diffrn_orient_matrix_UB_13      0.0080532000
_diffrn_orient_matrix_UB_21      -0.0080105000
_diffrn_orient_matrix_UB_22      0.0272843000
_diffrn_orient_matrix_UB_23      0.0500583000
_diffrn_orient_matrix_UB_31      0.0032577000
_diffrn_orient_matrix_UB_32      -0.0485303000
_diffrn_orient_matrix_UB_33      0.0298254000
_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                671
_reflns_number_total             1068
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1068
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0304
_refine_ls_restrained_S_all      1.281
_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)+(0.0134P)²+32.6835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0701
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H22A(0.5) H22B(0.5)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B), N22(H22A,H22B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.25033(8) 0.87489(7) 0.25092(4) 0.0274(10) Uani 1 1 d . . . . .
Cs1 Cs 0.4052(2) 0.62527(16) 0.500000 0.045(2) Uani 1 2 d S T P . .
I1 I 0.41899(16) 0.87782(11) 0.30815(8) 0.0406(18) Uani 1 1 d . . . . .
I2 I 0.07948(16) 0.87206(11) 0.19619(8) 0.0392(18) Uani 1 1 d . . . . .
Cs2 Cs 0.3882(2) 1.12526(15) 0.500000 0.048(2) Uani 1 2 d S T P . .
I3 I 0.24915(15) 1.12512(9) 0.21331(10) 0.0458(17) Uani 1 1 d . . . . .
I4A I 0.2188(3) 0.92305(16) 0.500000 0.051(3) Uani 1 2 d S T P . .
I5A I 0.2795(3) 0.82899(16) 0.000000 0.057(3) Uani 1 2 d S T P . .
C1 C -0.040(4) 0.879(2) 0.500000 0.025(7) Uiso 1 2 d S . P . .
N11 N -0.0779(18) 0.8843(10) 0.4050(11) 0.04(2) Uani 1 1 d . . . . .
H11A H -0.124383 0.890468 0.406457 0.051 Uiso 1 1 calc R U . . .
H11B H -0.055446 0.881271 0.342449 0.051 Uiso 1 1 calc R U . . .
N12 N 0.036(4) 0.8809(19) 0.500000 0.056(9) Uiso 1 2 d S . P . .
H12A H 0.058822 0.885141 0.561678 0.068 Uiso 0.5 1 calc R U P . .
H12B H 0.058896 0.877609 0.438322 0.068 Uiso 0.5 1 calc R U P . .
C2 C 0.457(4) 0.118(3) 0.000000 0.037(9) Uiso 1 2 d S . P . .
N21 N 0.428(2) 0.1128(12) 0.0936(14) 0.07(3) Uani 1 1 d . . . . .
H21A H 0.381992 0.104106 0.099294 0.081 Uiso 1 1 calc R U . . .
H21B H 0.454499 0.117776 0.152285 0.081 Uiso 1 1 calc R U . . .
N22 N 0.531(4) 0.1172(17) 0.000000 0.043(8) Uiso 1 2 d S . P . .
H22A H 0.554140 0.113065 0.061673 0.051 Uiso 0.5 1 calc R U P . .
H22B H 0.554189 0.120753 -0.061673 0.051 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.181(4) . ?
Pb1 I2 3.214(4) . ?
Pb1 I3 3.1606(14) 3_545 ?
Pb1 I3 3.1694(14) . ?
Pb1 I4A 3.1161(12) . ?
Pb1 I5A 3.1247(12) . ?
C1 N11 1.34(4) 6_556 ?
C1 N11 1.34(4) . ?
C1 N12 1.40(8) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C2 N21 1.25(4) . ?
C2 N21 1.25(4) 6 ?
C2 N22 1.36(9) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22A 0.8600 . ?
N22 H22B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 179.32(3) . . ?
I3 Pb1 I1 88.80(6) 3_545 . ?
I3 Pb1 I1 91.50(6) . . ?
I3 Pb1 I2 91.14(7) 3_545 . ?
I3 Pb1 I2 88.56(6) . . ?
I3 Pb1 I3 179.56(4) 3_545 . ?
I4A Pb1 I1 88.31(11) . . ?
I4A Pb1 I2 91.02(11) . . ?
I4A Pb1 I3 86.83(5) . . ?
I4A Pb1 I3 93.51(5) . 3_545 ?
I4A Pb1 I5A 178.99(15) . . ?
I5A Pb1 I1 92.53(11) . . ?
I5A Pb1 I2 88.14(11) . . ?
I5A Pb1 I3 92.58(5) . . ?
I5A Pb1 I3 87.08(5) . 3_545 ?
Pb1 I3 Pb1 163.93(4) 3 . ?
Pb1 I4A Pb1 148.84(15) 6_556 . ?
Pb1 I5A Pb1 150.82(15) . 6 ?
N11 C1 N11 118(6) 6_556 . ?
N11 C1 N12 121(3) 6_556 . ?
N11 C1 N12 121(3) . . ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N21 C2 N21 129(8) . 6 ?
N21 C2 N22 115(4) . . ?
N21 C2 N22 115(4) 6 . ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22A 120.0 . . ?
C2 N22 H22B 120.0 . . ?
H22A N22 H22B 120.0 . . ?

_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 1.271
_oxdiff_exptl_absorpt_empirical_full_min 0.729
####################################################################### 
# 
# 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_CsGPbI4_325K
_database_code_depnum_ccdc_archive 'CCDC 2428397'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'

_cell_length_a                   12.28699(15)
_cell_length_b                   6.38954(8)
_cell_length_c                   18.5355(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1455.19(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7186
_cell_measurement_temperature    325.00(11)
_cell_measurement_theta_max      29.9790
_cell_measurement_theta_min      1.9870
_exptl_absorpt_coefficient_mu    22.505
_exptl_absorpt_correction_T_max  0.280
_exptl_absorpt_correction_T_min  0.033
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 1 0.2358
-1 9 8 0.2405
1 0 -26 0.0279
-1 0 26 0.0311
-4 -9 -1 0.2395
17 0 4 0.0706
-17 -1 -4 0.0608

_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
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
-0.0000 -1.0000 1.0000 -0.0031 0.0369 0.1114
-1.1976 8.5287 8.2122 0.0072 0.3288 -0.9444
0.9150 -0.0270 -26.1017 -0.0256 -0.9996 -0.0091
-0.9150 0.0270 26.1017 0.0256 0.9996 0.0091
-4.2316 -8.7298 -0.8222 -0.2984 -0.0226 0.9542
17.1038 -0.0496 4.1093 0.9950 0.0790 0.0605
-16.9271 -1.3019 -4.0368 -0.9928 -0.0787 0.0899

_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18773
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.298
_diffrn_reflns_theta_min         1.989
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      325.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00  38.50   0.70   17.50    --   22.87  77.00   0.00   85
  2  ω    -67.00  38.00   0.70   17.50    --  -23.33  77.00 150.00  150
  3  ω    -65.00  68.00   0.70   17.50    --  -23.33  57.00 -90.00  190
  4  ω   -114.00  21.80   0.70   17.50    --  -23.33 -38.00 -30.00  194
  5  ω    -21.00  38.50   0.70   17.50    --   22.87  77.00 -60.00   85
  6  ω    -21.00  38.50   0.70   17.50    --   22.87  77.00 150.00   85
  7  ω      1.00  73.10   0.70   17.50    --   22.87 -99.00  30.00  103
  8  ω     61.00 123.30   0.70   17.50    --   22.87 178.00  90.00   89
  9  ω    -65.00  68.00   0.70   17.50    --  -23.33  57.00  90.00  190
 10  ω   -114.00  21.80   0.70   17.50    --  -23.33 -38.00 150.00  194
 11  ω    -21.00  38.50   0.70   17.50    --   22.87  77.00-180.00   85
 12  ω     61.00 123.30   0.70   17.50    --   22.87 178.00 -90.00   89
 13  ω    -21.00  36.40   0.70   17.50    --   22.87  77.00  60.00   82
 14  ω      1.00  73.10   0.70   17.50    --   22.87 -99.00   0.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0574763000
_diffrn_orient_matrix_UB_12      0.0060420000
_diffrn_orient_matrix_UB_13      0.0029879000
_diffrn_orient_matrix_UB_21      -0.0045399000
_diffrn_orient_matrix_UB_22      0.0011953000
_diffrn_orient_matrix_UB_23      0.0381372000
_diffrn_orient_matrix_UB_31      0.0030759000
_diffrn_orient_matrix_UB_32      -0.1108449000
_diffrn_orient_matrix_UB_33      0.0005700000
_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                1109
_reflns_number_total             1195
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.842
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00121(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         1195
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0194
_refine_ls_restrained_S_all      1.140
_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)+(0.0203P)²+4.6163P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0464
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H5A(0.25) H5B(0.25) I2(0.25)
3.a X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N3(H3A,H3B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.250000 0.250000 0.250000 0.03062(9) Uani 1 4 d S T P . .
Cs2 Cs 0.000000 -0.250000 0.10627(4) 0.06613(17) Uani 1 4 d S T P . .
I3 I 0.19535(3) 0.250000 0.08090(2) 0.04978(12) Uani 1 2 d S T P . .
N5 N 0.000000 0.250000 0.4721(4) 0.0600(19) Uiso 1 4 d S . P . .
H5A H 0.060615 0.250000 0.448876 0.072 Uiso 0.5 2 calc R U P . .
H5B H -0.060615 0.250000 0.448875 0.072 Uiso 0.5 2 calc R U P . .
I1 I 0.250000 -0.250000 0.250000 0.0707(2) Uani 1 4 d S T P . .
N3 N 0.0925(6) 0.250000 0.5763(4) 0.0751(17) Uiso 1 2 d S . P . .
H3A H 0.094670 0.250000 0.622658 0.090 Uiso 1 2 calc R U P . .
H3B H 0.151933 0.250000 0.551825 0.090 Uiso 1 2 calc R U P . .
C1 C 0.000000 0.250000 0.5434(4) 0.0414(15) Uiso 1 4 d S . P . .
I2 I 0.000000 0.19707(19) 0.28149(4) 0.0635(5) Uani 0.5 2 d S T 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 I3 3.2054(3) . ?
Pb1 I3 3.2054(3) 13 ?
Pb1 I1 3.19477(5) 1_565 ?
Pb1 I1 3.19477(4) . ?
Pb1 I2 3.1449(2) 13 ?
Pb1 I2 3.1450(2) . ?
Pb1 I2 3.1449(2) 2 ?
Pb1 I2 3.1449(2) 14 ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N5 C1 1.323(11) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 C1 1.289(8) . ?
I2 I2 0.676(2) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3 Pb1 I3 180.0 13 . ?
I1 Pb1 I3 90.0 . 13 ?
I1 Pb1 I3 90.0 1_565 . ?
I1 Pb1 I3 90.0 . . ?
I1 Pb1 I3 90.0 1_565 13 ?
I1 Pb1 I1 180.0 . 1_565 ?
I2 Pb1 I3 88.675(15) 14 13 ?
I2 Pb1 I3 91.325(15) 2 13 ?
I2 Pb1 I3 88.675(15) 2 . ?
I2 Pb1 I3 88.676(15) . . ?
I2 Pb1 I3 91.325(15) 13 . ?
I2 Pb1 I3 91.325(15) 14 . ?
I2 Pb1 I3 91.324(15) . 13 ?
I2 Pb1 I3 88.675(15) 13 13 ?
I2 Pb1 I1 96.17(2) 13 . ?
I2 Pb1 I1 96.17(2) 14 1_565 ?
I2 Pb1 I1 96.17(2) . 1_565 ?
I2 Pb1 I1 83.83(2) 13 1_565 ?
I2 Pb1 I1 96.17(2) 2 . ?
I2 Pb1 I1 83.83(2) 2 1_565 ?
I2 Pb1 I1 83.83(2) 14 . ?
I2 Pb1 I1 83.83(2) . . ?
I2 Pb1 I2 167.65(5) 14 . ?
I2 Pb1 I2 12.35(5) 13 14 ?
I2 Pb1 I2 12.35(5) 2 . ?
I2 Pb1 I2 180.0 14 2 ?
I2 Pb1 I2 167.65(5) 13 2 ?
I2 Pb1 I2 180.0 13 . ?
H5A N5 H5B 120.0 . . ?
C1 N5 H5A 120.0 . . ?
C1 N5 H5B 120.0 . . ?
Pb1 I1 Pb1 180.0 1_545 . ?
H3A N3 H3B 120.0 . . ?
C1 N3 H3A 120.0 . . ?
C1 N3 H3B 120.0 . . ?
N3 C1 N5 118.2(4) 2 . ?
N3 C1 N5 118.2(4) . . ?
N3 C1 N3 123.6(9) . 2 ?
Pb1 I2 Pb1 155.23(3) 2 . ?
I2 I2 Pb1 83.83(2) 2 . ?
I2 I2 Pb1 83.83(2) 2 2 ?

_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 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.845
####################################################################### 
# 
# 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_CsGPbI4_3_15
_database_code_depnum_ccdc_archive 'CCDC 2428395'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   17.820(11)
_cell_length_b                   12.0233(6)
_cell_length_c                   11.6046(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2486.4(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3256
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       3150000(30000)
_cell_measurement_theta_max      28.6510
_cell_measurement_theta_min      1.7710
_shelx_estimated_absorpt_T_max   0.390
_shelx_estimated_absorpt_T_min   0.090
_exptl_absorpt_coefficient_mu    26.343
_exptl_absorpt_correction_T_max  0.231
_exptl_absorpt_correction_T_min  0.090
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 3.15(3) GPa
(3150000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.850
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -4 -16 0.0648
-4 4 16 0.0747
-3 16 -4 0.0788
5 -13 -9 0.0770
0 -10 13 0.0762
4 -16 3 0.0959
-25 -3 -2 0.0220
25 3 2 0.0220

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.044
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.470     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 161.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
4.3334 -3.6817 -15.6794 -0.0081 -0.9580 -0.2868
-4.3839 3.9338 15.6164 0.0081 0.9623 0.2719
-3.3448 16.3253 -3.7275 0.0012 0.2998 -0.9540
5.4318 -13.2797 -9.4810 -0.0069 -0.9183 0.3958
-0.4207 -9.7254 13.3592 0.0045 0.4217 0.9067
3.5686 -16.4865 2.8836 -0.0017 -0.3503 0.9367
-24.5890 -2.8875 -2.3438 -1.0000 0.0000 0.0000
24.5890 2.8875 2.3438 1.0000 0.0000 0.0000

_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.359
_diffrn_reflns_Laue_measured_fraction_max 0.282
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10302
_diffrn_reflns_point_group_measured_fraction_full 0.359
_diffrn_reflns_point_group_measured_fraction_max 0.282
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.722
_diffrn_reflns_theta_min         2.439
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.359
_diffrn_measured_fraction_theta_max 0.282
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   70.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   70.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   70.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   70.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0386491000
_diffrn_orient_matrix_UB_12      0.0100152000
_diffrn_orient_matrix_UB_13      0.0088476000
_diffrn_orient_matrix_UB_21      -0.0083187000
_diffrn_orient_matrix_UB_22      0.0285559000
_diffrn_orient_matrix_UB_23      0.0520928000
_diffrn_orient_matrix_UB_31      0.0030000000
_diffrn_orient_matrix_UB_32      -0.0507363000
_diffrn_orient_matrix_UB_33      0.0310317000
_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                617
_reflns_number_total             955
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         955
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.216
_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)+(0.0238P)²+37.0116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0854
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5)
 Fixed X: H22(0.55893)
 Fixed Y: H22(0.12215)
 Fixed Z: H22(0.062429)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_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 0.25153(10) 0.87510(8) 0.25158(5) 0.0279(13) Uani 1 1 d . . . . .
Cs1 Cs 0.4125(2) 0.62347(16) 0.500000 0.034(3) Uani 1 2 d S T P . .
I1 I 0.42171(17) 0.87747(10) 0.31235(9) 0.034(2) Uani 1 1 d . . . . .
I2 I 0.07935(17) 0.87287(10) 0.19515(9) 0.0278(19) Uani 1 1 d . . . . .
Cs2 Cs 0.3925(2) 1.12545(15) 0.500000 0.036(3) Uani 1 2 d S T P . .
I3 I 0.24793(18) 1.12449(9) 0.19402(11) 0.0400(19) Uani 1 1 d . . . . .
I4B I 0.2199(3) 0.94191(16) 0.500000 0.045(3) Uani 1 2 d S T P . .
I5A I 0.2772(3) 0.80954(16) 0.000000 0.036(3) Uani 1 2 d S T P . .
C1 C -0.033(5) 0.882(2) 0.500000 0.014(7) Uiso 1 2 d S . P . .
N11 N -0.0756(19) 0.8822(10) 0.4012(11) 0.031(4) Uiso 1 1 d . . . . .
H11A H -0.054341 0.877896 0.334800 0.038 Uiso 1 1 calc R U . . .
H11B H -0.123647 0.886641 0.405986 0.038 Uiso 1 1 calc R U . . .
N12 N 0.038(4) 0.876(2) 0.500000 0.041(9) Uiso 1 2 d S . P . .
H12A H 0.061627 0.871405 0.564133 0.049 Uiso 0.5 1 calc R U P . .
H12B H 0.061816 0.876131 0.435867 0.049 Uiso 0.5 1 calc R U P . .
C2 C 0.476(5) 0.116(2) 0.000000 0.019(8) Uiso 1 2 d S . P . .
N21 N 0.429(2) 0.1148(12) 0.0993(14) 0.049(5) Uiso 1 1 d . . . . .
H21A H 0.448776 0.121043 0.166786 0.059 Uiso 1 1 calc R U . . .
H21B H 0.381426 0.108129 0.091945 0.059 Uiso 1 1 calc R U . . .
N22 N 0.539(4) 0.124(3) 0.000000 0.046(11) Uiso 1 2 d S . P . .
H22 H 0.558930 0.122150 0.062429 0.056 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.114(4) . ?
Pb1 I2 3.137(4) . ?
Pb1 I3 3.0727(14) . ?
Pb1 I3 3.0786(14) 3_545 ?
Pb1 I4B 3.0454(13) . ?
Pb1 I4B 3.0454(13) 6_556 ?
Pb1 I5A 3.0583(11) . ?
I4B I4B 0.000(4) 6_556 ?
C1 N11 1.38(5) 6_556 ?
C1 N11 1.38(5) . ?
C1 N12 1.25(10) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12B 0.8600 . ?
C2 N21 1.42(6) 6 ?
C2 N21 1.42(6) . ?
C2 N22 1.13(11) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22 0.81(3) . ?
N22 H22 0.81(3) 6 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 178.96(4) . . ?
I3 Pb1 I1 93.48(7) . . ?
I3 Pb1 I1 87.68(7) 3_545 . ?
I3 Pb1 I2 92.15(7) 3_545 . ?
I3 Pb1 I2 86.71(7) . . ?
I3 Pb1 I3 178.75(6) . 3_545 ?
I4B Pb1 I1 87.91(10) 6_556 . ?
I4B Pb1 I1 87.91(10) . . ?
I4B Pb1 I2 91.07(10) . . ?
I4B Pb1 I2 91.07(10) 6_556 . ?
I4B Pb1 I3 86.82(5) 6_556 . ?
I4B Pb1 I3 86.82(5) . . ?
I4B Pb1 I3 93.71(5) 6_556 3_545 ?
I4B Pb1 I3 93.71(5) . 3_545 ?
I4B Pb1 I4B 0.0(2) 6_556 . ?
I4B Pb1 I5A 177.87(16) . . ?
I4B Pb1 I5A 177.87(16) 6_556 . ?
I5A Pb1 I1 94.19(10) . . ?
I5A Pb1 I2 86.83(10) . . ?
I5A Pb1 I3 92.70(5) . . ?
I5A Pb1 I3 86.74(5) . 3_545 ?
Pb1 I2 Cs1 154.72(6) . 7_575 ?
Pb1 I2 Cs1 94.64(9) . 3 ?
Cs1 I2 Cs1 69.96(9) 7_575 3 ?
Pb1 I3 Pb1 155.57(5) . 3 ?
Pb1 I3 Cs1 98.49(7) . 3 ?
Pb1 I3 Cs1 97.62(7) 3 3 ?
Pb1 I4B Pb1 142.39(13) . 6_556 ?
I4B I4B Pb1 0(10) 6_556 6_556 ?
I4B I4B Pb1 0(10) 6_556 . ?
Pb1 I5A Pb1 145.34(11) 6 . ?
N11 C1 N11 112(6) 6_556 . ?
N12 C1 N11 124(3) . . ?
N12 C1 N11 124(3) . 6_556 ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
N21 C2 N21 108(6) 6 . ?
N22 C2 N21 126(3) . . ?
N22 C2 N21 126(3) . 6 ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22 116(5) . 6 ?
C2 N22 H22 116(5) . . ?
H22 N22 H22 128(10) . 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 1.421
_oxdiff_exptl_absorpt_empirical_full_min 0.575
####################################################################### 
# 
# 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_CsGPbI4_3_47
_database_code_depnum_ccdc_archive 'CCDC 2428398'
loop_
_audit_author_name
_audit_author_address
'Marek Szafranski'
;Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3


_chemical_name_systematic        'Cesium guanidinium lead tetraiodide'

_chemical_formula_sum            'C H6 Cs I4 N3 Pb'
_chemical_formula_weight         907.79
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   17.799(9)
_cell_length_b                   11.9757(5)
_cell_length_c                   11.5555(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2463.2(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3364
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       3470000(30000)
_cell_measurement_theta_max      28.3340
_cell_measurement_theta_min      1.7780
_shelx_estimated_absorpt_T_max   0.416
_shelx_estimated_absorpt_T_min   0.087
_exptl_absorpt_coefficient_mu    26.591
_exptl_absorpt_correction_T_max  0.234
_exptl_absorpt_correction_T_min  0.109
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_absorpt_special_details   
; 
Data were collected at room temperature and pressure of 3.47(3) GPa
(3470000 kPa). 
Pressure was determined by monitoring the shift of the ruby
R1-fluorescence line.
"_diffrn_measured_fraction_theta_full" value is low, because 
the access to the reciprocal space is restricted due to the use of
the diamond anvil cell.
;

_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.896
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -1 16 0.0689
4 2 -16 0.0653
4 17 1 0.0798
-4 -17 1 0.0997
-5 -11 11 0.0788
0 -12 -12 0.0727
25 -3 2 0.0220
-25 3 -2 0.0220

_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.044
_exptl_oxdiff_absorpt_process_details 
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.694     0.726
         range of gasket transmission (min-max)           0.577     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2:  8.000 mm, mu =  0.0200 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 174.0 microns
    Gasket absorption coeff =        30.30 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
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
-3.8733 -1.4565 16.0063 -0.0079 -0.9105 -0.4135
3.9052 1.5947 -15.9907 0.0079 0.9139 0.4059
3.9156 16.5875 1.4667 0.0024 0.4321 -0.9018
-4.4183 -16.5765 0.8441 -0.0035 -0.5567 0.8307
-5.4219 -11.4913 11.3694 -0.0075 -0.9691 0.2466
-0.3999 -11.6421 -11.7651 0.0034 0.2773 0.9608
24.5336 -2.8740 2.3607 -1.0000 0.0000 0.0000
-24.5336 2.8740 -2.3607 1.0000 0.0000 0.0000

_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.358
_diffrn_reflns_Laue_measured_fraction_max 0.279
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10222
_diffrn_reflns_point_group_measured_fraction_full 0.358
_diffrn_reflns_point_group_measured_fraction_max 0.279
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.844
_diffrn_reflns_theta_min         2.449
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3200
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.358
_diffrn_measured_fraction_theta_max 0.279
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   70.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   70.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   70.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   70.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   70.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   70.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   70.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   70.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   70.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   70.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0387195306
_diffrn_orient_matrix_UB_12      0.0100748944
_diffrn_orient_matrix_UB_13      -0.0089454517
_diffrn_orient_matrix_UB_21      0.0083873861
_diffrn_orient_matrix_UB_22      0.0286870695
_diffrn_orient_matrix_UB_23      -0.0522423996
_diffrn_orient_matrix_UB_31      -0.0029635683
_diffrn_orient_matrix_UB_32      -0.0509119634
_diffrn_orient_matrix_UB_33      -0.0311826490
_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                599
_reflns_number_total             946
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         946
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0346
_refine_ls_restrained_S_all      1.270
_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)+(0.0210P)²+39.8729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0849
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H22A(0.5) H22B(0.5)
3.a X=CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B), N21(H21A,H21B), N22(H22A,H22B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.25168(10) 0.87484(9) 0.25163(5) 0.0264(13) Uani 1 1 d . . . . .
Cs1 Cs 0.4131(2) 0.62335(18) 0.500000 0.030(3) Uani 1 2 d S T P . .
I1 I 0.42202(18) 0.87727(11) 0.31267(9) 0.031(2) Uani 1 1 d . . . . .
I2 I 0.07952(18) 0.87279(11) 0.19510(9) 0.027(2) Uani 1 1 d . . . . .
Cs2 Cs 0.3928(2) 1.12545(18) 0.500000 0.034(3) Uani 1 2 d S T P . .
I3 I 0.24775(19) 1.12428(10) 0.19267(12) 0.038(2) Uani 1 1 d . . . . .
I4A I 0.2196(3) 0.94285(17) 0.500000 0.044(3) Uani 1 2 d S T P . .
I5A I 0.2764(3) 0.80823(17) 0.000000 0.033(3) Uani 1 2 d S T P . .
C1 C -0.031(4) 0.875(2) 0.500000 0.010(6) Uiso 1 2 d S . P . .
N11 N -0.075(2) 0.8768(12) 0.4006(12) 0.033(4) Uiso 1 1 d . . . . .
H11A H -0.054677 0.886075 0.333949 0.039 Uiso 1 1 calc R U . . .
H11B H -0.123154 0.868608 0.405804 0.039 Uiso 1 1 calc R U . . .
N12 N 0.041(4) 0.886(2) 0.500000 0.045(10) Uiso 1 2 d S . P . .
H12A H 0.064633 0.896047 0.435823 0.054 Uiso 0.5 1 calc R U P . .
H12B H 0.065464 0.884615 0.564177 0.054 Uiso 0.5 1 calc R U P . .
C2 C 0.475(5) 0.123(3) 0.000000 0.027(9) Uiso 1 2 d S . P . .
N21 N 0.430(2) 0.1205(15) 0.0999(15) 0.053(5) Uiso 1 1 d . . . . .
H21A H 0.449749 0.112800 0.167040 0.064 Uiso 1 1 calc R U . . .
H21B H 0.381642 0.126867 0.093567 0.064 Uiso 1 1 calc R U . . .
N22 N 0.542(4) 0.114(2) 0.000000 0.031(9) Uiso 1 2 d S . P . .
H22A H 0.565982 0.106359 0.064250 0.037 Uiso 0.5 1 calc R U P . .
H22B H 0.566531 0.116183 -0.064250 0.037 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.113(4) . ?
Pb1 I2 3.133(4) . ?
Pb1 I3 3.0689(16) 3_545 ?
Pb1 I3 3.0647(16) . ?
Pb1 I4A 3.0376(14) . ?
Pb1 I5A 3.0472(12) . ?
C1 N11 1.39(5) 6_556 ?
C1 N11 1.39(5) . ?
C1 N12 1.29(10) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12A 0.8600 . ?
N12 H12A 0.8600 6_556 ?
N12 H12B 0.8600 6_556 ?
N12 H12B 0.8600 . ?
C2 N21 1.41(6) . ?
C2 N21 1.41(6) 6 ?
C2 N22 1.20(11) . ?
N21 H21A 0.8600 . ?
N21 H21B 0.8600 . ?
N22 H22A 0.8600 6 ?
N22 H22A 0.8600 . ?
N22 H22B 0.8600 6 ?
N22 H22B 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I2 178.93(4) . . ?
I3 Pb1 I1 93.64(8) . . ?
I3 Pb1 I1 87.61(8) 3_545 . ?
I3 Pb1 I2 92.25(8) 3_545 . ?
I3 Pb1 I2 86.50(8) . . ?
I3 Pb1 I3 178.66(6) . 3_545 ?
I4A Pb1 I1 88.09(11) . . ?
I4A Pb1 I2 90.86(11) . . ?
I4A Pb1 I3 93.70(5) . 3_545 ?
I4A Pb1 I3 86.81(5) . . ?
I4A Pb1 I5A 177.43(17) . . ?
I5A Pb1 I1 94.46(11) . . ?
I5A Pb1 I2 86.59(11) . . ?
I5A Pb1 I3 92.66(5) . . ?
I5A Pb1 I3 86.77(5) . 3_545 ?
Pb1 I3 Pb1 155.00(5) . 3 ?
Pb1 I4A Pb1 141.76(13) 6_556 . ?
Pb1 I5A Pb1 145.19(12) . 6 ?
N11 C1 N11 111(6) . 6_556 ?
N12 C1 N11 124(3) . . ?
N12 C1 N11 124(3) . 6_556 ?
C1 N11 H11A 120.0 . . ?
C1 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C1 N12 H12A 120.0 . . ?
C1 N12 H12A 120.0(2) . 6_556 ?
C1 N12 H12B 120.0 . . ?
C1 N12 H12B 120.0(2) . 6_556 ?
H12A N12 H12A 119.2 . 6_556 ?
H12A N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 6_556 6_556 ?
H12A N12 H12B 9.2 . 6_556 ?
H12B N12 H12A 9.2 . 6_556 ?
H12B N12 H12B 119.2 . 6_556 ?
N21 C2 N21 110(7) . 6 ?
N22 C2 N21 125(3) . . ?
N22 C2 N21 125(3) . 6 ?
C2 N21 H21A 120.0 . . ?
C2 N21 H21B 120.0 . . ?
H21A N21 H21B 120.0 . . ?
C2 N22 H22A 120.0(2) . 6 ?
C2 N22 H22A 120.0 . . ?
C2 N22 H22B 120.0 . . ?
C2 N22 H22B 120.0(2) . 6 ?
H22A N22 H22A 119.4 . 6 ?
H22A N22 H22B 120.0 6 6 ?
H22A N22 H22B 120.0 . . ?
H22A N22 H22B 7.9 . 6 ?
H22B N22 H22A 7.9 . 6 ?
H22B N22 H22B 119.4 . 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 1.355
_oxdiff_exptl_absorpt_empirical_full_min 0.657
