# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2024

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

data_jmx175_62_fcf
_database_code_depnum_ccdc_archive 'CCDC 2346572'
loop_
_audit_author_name
_audit_author_address
'Jakob Moebs'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2024-04-06 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_audit_creation_date             2023-11-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I3 Pb, C6 N'
_chemical_formula_sum            'C6 I3 N Pb'
_chemical_formula_weight         673.96
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   7.8521(4)
_cell_length_b                   11.3081(8)
_cell_length_c                   15.9901(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1419.80(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4452
_cell_measurement_temperature    230
_cell_measurement_theta_max      31.58
_cell_measurement_theta_min      2.55
_shelx_estimated_absorpt_T_max   0.688
_shelx_estimated_absorpt_T_min   0.289
_exptl_absorpt_coefficient_mu    18.363
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.153
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.022
_exptl_crystal_size_rad          0.034
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13193
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.474
_diffrn_reflns_theta_min         2.548
_diffrn_ambient_temperature      230
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
 550 frames, detector distance = 70 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Stoe_Stadivari_Mo
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'GeniX Mo'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1242
_reflns_number_total             1887
_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       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.423
_refine_diff_density_min         -2.326
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1887
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0421
_refine_ls_restrained_S_all      1.003
_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)+(0.0676P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1181
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Others
 Fixed Sof: N1(0.5) C3(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.57308(6) 0.250000 0.25067(4) 0.03050(17) Uani 1 2 d S T P . .
I1 I 0.32071(8) 0.44550(6) 0.16800(4) 0.0368(2) Uani 1 1 d . . . . .
I2 I 0.32757(13) 0.250000 0.40864(6) 0.0350(2) Uani 1 2 d S T P . .
C1 C 0.538(2) 0.750000 0.2742(11) 0.049(4) Uani 1 2 d S T P . .
C5 C 0.095(2) 0.750000 0.4555(12) 0.048(4) Uani 1 2 d S T P . .
C2 C 0.547(2) 0.750000 0.3691(11) 0.048(4) Uani 1 2 d S T P . .
C4 C 0.313(2) 0.5804(12) 0.4126(8) 0.062(4) Uani 1 1 d . . . . .
N1 N 0.259(2) 0.7057(14) 0.4231(10) 0.030(4) Uiso 0.5 1 d . . P A 1
C3 C 0.371(3) 0.7170(18) 0.4052(13) 0.040(5) Uiso 0.5 1 d . . P A 1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0209(2) 0.0359(3) 0.0347(3) 0.000 0.0003(2) 0.000
I1 0.0334(4) 0.0339(4) 0.0432(4) 0.0065(3) -0.0010(3) 0.0000(3)
I2 0.0344(5) 0.0414(5) 0.0292(4) 0.000 0.0011(4) 0.000
C1 0.032(8) 0.071(13) 0.045(9) 0.000 0.002(8) 0.000
C5 0.034(9) 0.053(11) 0.056(11) 0.000 -0.006(8) 0.000
C2 0.037(9) 0.061(12) 0.045(10) 0.000 0.000(8) 0.000
C4 0.088(11) 0.045(7) 0.052(8) -0.016(6) 0.005(8) -0.002(7)

_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 3.2187(8) 6_656 ?
Pb1 I1 3.2187(8) 4 ?
Pb1 I1 3.2499(8) . ?
Pb1 I1 3.2499(8) 7_565 ?
Pb1 I2 3.1775(11) . ?
Pb1 I2 3.2375(12) 6_656 ?
C1 C2 1.52(2) . ?
C5 N1 1.47(2) 7_575 ?
C5 N1 1.47(2) . ?
C2 C3 1.54(3) . ?
C2 C3 1.54(3) 7_575 ?
C4 N1 1.49(2) . ?
C4 C3 1.62(2) . ?
N1 C3 1.28(2) 7_575 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 86.76(3) 6_656 4 ?
I1 Pb1 I1 93.75(2) 6_656 . ?
I1 Pb1 I1 179.48(2) 4 . ?
I1 Pb1 I1 93.75(2) 4 7_565 ?
I1 Pb1 I1 179.48(2) 6_656 7_565 ?
I1 Pb1 I1 85.73(3) . 7_565 ?
I1 Pb1 I2 86.85(2) 6_656 6_656 ?
I1 Pb1 I2 86.85(2) 4 6_656 ?
I2 Pb1 I1 92.60(2) . 4 ?
I2 Pb1 I1 87.33(2) . 7_565 ?
I2 Pb1 I1 93.23(2) 6_656 . ?
I2 Pb1 I1 87.33(2) . . ?
I2 Pb1 I1 92.60(2) . 6_656 ?
I2 Pb1 I1 93.23(2) 6_656 7_565 ?
I2 Pb1 I2 179.24(4) . 6_656 ?
Pb1 I1 Pb1 74.738(15) 6_556 . ?
Pb1 I2 Pb1 75.46(2) . 6_556 ?
N1 C5 N1 39.8(13) 7_575 . ?
C1 C2 C3 109.5(15) . . ?
C1 C2 C3 109.5(15) . 7_575 ?
C3 C2 C3 28.1(16) . 7_575 ?
N1 C4 C3 34.9(9) . . ?
C5 N1 C4 127.8(14) . . ?
C3 N1 C5 116.8(14) 7_575 . ?
C3 N1 C4 115.3(16) 7_575 . ?
C2 C3 C4 120.9(15) . . ?
N1 C3 C2 122.6(16) 7_575 . ?
N1 C3 C4 116.2(17) 7_575 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 82.1(16) . . . . ?
C1 C2 C3 N1 -91(2) . . . 7_575 ?
N1 C5 N1 C4 179.8(13) 7_575 . . . ?
N1 C5 N1 C3 3.3(19) 7_575 . . 7_575 ?
N1 C4 C3 C2 -174(3) . . . . ?
N1 C4 C3 N1 -1.0(6) . . . 7_575 ?
C3 C2 C3 C4 177.2(13) 7_575 . . . ?
C3 C2 C3 N1 4(2) 7_575 . . 7_575 ?
C3 C4 N1 C5 -176(3) . . . . ?
C3 C4 N1 C3 0.7(5) . . . 7_575 ?

_shelx_res_file                  
;
TITL jmx175_62_a.res in Pnma
    jmx175_62_fcf.res
    created by SHELXL-2018/3 at 16:03:17 on 02-Nov-2023
REM Old TITL jmx175_62 in Pnma
REM SHELXT solution in Pnma: R1 0.119, Rweak 0.002, Alpha 0.012
REM <I/s> 0.351 for 136 systematic absences, Orientation as input
REM Formula found by SHELXT: N3 I3 Pb
CELL 0.71073 7.8521 11.3081 15.9901 90 90 90
ZERR 4 0.0004 0.0008 0.0009 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C I N Pb
UNIT 24 12 4 4
EQIV $1 +X,1.5-Y,+Z

L.S. 10
PLAN  12
SIZE 0.022 0.035 0.09
TEMP -43.15
CONF
FREE N1 N1_$1
FREE C3 N1
FREE C3 C3_$1
list 4
MORE -1
fmap 2 53
acta
OMIT 0 57
REM <olex2.extras>
REM <HklSrc "%.\\jmx175_merged.fcf.hkl">
REM </olex2.extras>

WGHT    0.067600
FVAR       0.50970
PB1   4    0.573077    0.250000    0.250666    10.50000    0.02092    0.03586 =
         0.03473    0.00000    0.00026    0.00000
I1    2    0.320708    0.445502    0.167998    11.00000    0.03340    0.03387 =
         0.04320    0.00652   -0.00095    0.00004
I2    2    0.327569    0.250000    0.408636    10.50000    0.03439    0.04137 =
         0.02921    0.00000    0.00107    0.00000
C1    1    0.538404    0.750000    0.274151    10.50000    0.03234    0.07054 =
         0.04535    0.00000    0.00242    0.00000
C5    1    0.094780    0.750000    0.455506    10.50000    0.03437    0.05333 =
         0.05636    0.00000   -0.00611    0.00000
C2    1    0.547020    0.750000    0.369136    10.50000    0.03706    0.06145 =
         0.04485    0.00000   -0.00050    0.00000
C4    1    0.312973    0.580383    0.412616    11.00000    0.08824    0.04502 =
         0.05180   -0.01607    0.00536   -0.00207
PART 1
N1    3    0.258571    0.705666    0.423126    10.50000    0.02975
C3    1    0.371434    0.716950    0.405226    10.50000    0.04013
HKLF 4




REM  jmx175_62_a.res in Pnma
REM wR2 = 0.1181, GooF = S = 1.003, Restrained GooF = 1.003 for all data
REM R1 = 0.0421 for 1242 Fo > 4sig(Fo) and 0.0740 for all 1887 data
REM 57 parameters refined using 0 restraints

END

WGHT      0.0676      0.0000

REM Highest difference peak  1.423,  deepest hole -2.326,  1-sigma level  0.311
Q1    1   0.6357  0.3033  0.2453  11.00000  0.05    1.42
Q2    1   0.5885  0.3140  0.2104  11.00000  0.05    1.28
Q3    1   0.5029  0.3035  0.2513  11.00000  0.05    1.26
Q4    1   0.1849  0.7500  0.5751  10.50000  0.05    1.20
Q5    1   0.3261  0.3777  0.2096  11.00000  0.05    1.19
Q6    1   0.3273  0.7500  0.4807  10.50000  0.05    1.16
Q7    1   0.1827  0.2500  0.5172  10.50000  0.05    1.15
Q8    1   0.3269  0.5187  0.1363  11.00000  0.05    1.14
Q9    1   0.5625  0.1779  0.2910  11.00000  0.05    1.12
Q10   1  -0.0484  0.7500  0.3982  10.50000  0.05    1.05
Q11   1   0.3714  0.3825  0.1403  11.00000  0.05    1.04
Q12   1   0.3991  0.1839  0.3978  11.00000  0.05    0.96
;
_shelx_res_checksum              98873
_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '70.0 mm'
_STOE_detector_pixelsize_x       '0.172 mm'
_STOE_detector_pixelsize_y       '0.172 mm'
_STOE_detector_size_x            '8.4 cm'
_STOE_detector_size_y            '10.6 cm'
_STOE_evaluation_integration_A   6.0
_STOE_evaluation_integration_B   1.5
_STOE_evaluation_integration_EMS 0.012
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 8
_STOE_evaluation_LANA_BOS_l_odd_max 5
_STOE_evaluation_LANA_completeness 97.6
_STOE_evaluation_LANA_DXS_max_order -
_STOE_evaluation_LANA_DYS_max_order -
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 64.9
_STOE_evaluation_LANA_max_2theta_desired 64.9
_STOE_evaluation_LANA_mean_redundancy 3.5
_STOE_evaluation_LANA_number_refls_after_OR 21694
_STOE_evaluation_LANA_number_refls_outliers 4739
_STOE_evaluation_LANA_number_refls_total 26433
_STOE_evaluation_LANA_number_refls_unique 6153
_STOE_evaluation_LANA_number_refls_written 26475
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group mmm
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta           7.8   14.6   21.4   28.2   35.0   41.8   48.6   55.4   62.2
#----------------------------------------------------------------------------
<Resolution>    4.65   2.71   1.88   1.44   1.17   0.99   0.86   0.77   0.70
N(total)         192    691   1429   1691   3819   4800   5467   5964   2380
<Redundancy>     3.9    4.2    4.1    3.1    4.5    4.3    3.9    3.4    2.0
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0  100.0   89.9
<I/sigma>       49.2   53.3   25.2   22.1    9.0    6.3    3.1    1.7    0.8
R(int)         0.039  0.023  0.030  0.037  0.055  0.071  0.129  0.205  0.325
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     jmx175
_STOE_measurement_max_exposure_per_frame '150.0 s'
_STOE_measurement_mean_exposure_per_frame '150.0 s'
_STOE_measurement_min_exposure_per_frame '150.0 s'
_STOE_measurement_total_exposure_time '22.9 h'
_STOE_measurement_total_frame_number 550
_STOE_measurement_total_run_number 8
_STOE_measurement_tube_power     '50.0 W'
####################################################################### 
# 
# 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_jmx114
_database_code_depnum_ccdc_archive 'CCDC 2346573'
loop_
_audit_author_name
_audit_author_address
'Jakob Moebs'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2024-04-06 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_audit_creation_date             2022-04-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I, C5 H12 N'
_chemical_formula_sum            'C5 H12 I N'
_chemical_formula_weight         213.06
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   7.38460(10)
_cell_length_b                   7.38460(10)
_cell_length_c                   7.2299(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     394.263(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    27457
_cell_measurement_temperature    100
_cell_measurement_theta_max      39.03
_cell_measurement_theta_min      3.90
_shelx_estimated_absorpt_T_max   0.867
_shelx_estimated_absorpt_T_min   0.592
_exptl_absorpt_coefficient_mu    3.964
_exptl_absorpt_correction_T_max  0.8036
_exptl_absorpt_correction_T_min  0.2828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.037
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         42.627
_diffrn_reflns_theta_min         3.902
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
 2934 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Stoe_Stadivari_Mo
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'GeniX Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                719
_reflns_number_total             755
_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       
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction        
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.798
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         755
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0172
_refine_ls_restrained_S_all      1.048
_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)+(0.0213P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0375
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1_1-C1_1 \\sim N1_1-C2_1
 with sigma of 0.02
 C3_1-C4_1 \\sim C4_1-C5_1
 with sigma of 0.02
3. Restrained planarity
 C1_1, C2_1, C3_1, C4_1, C5_1, N1_1
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
C1_1 \\sim C2_1 \\sim C3_1 \\sim C4_1 \\sim C5_1 \\sim N1_1: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 C1_1, C2_1, C3_1, C4_1, C5_1, N1_1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C1(0.125) H1A(0.125) H1B(0.125) H1C(0.125) C2(0.125) H2A(0.125)
 H2B(0.125) H2C(0.125) C3(0.125) H3A(0.125) H3B(0.125) H3C(0.125) C4(0.125)
 C5(0.125) H5A(0.125) H5B(0.125) H5C(0.125) N1(0.125)
7.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.500000 0.500000 0.500000 0.02804(5) Uani 1 8 d S T P . .
C1_1 C 0.474(4) 0.236(3) -0.018(5) 0.016(5) Uani 0.125 1 d D U P A -1
H1A_1 H 0.383383 0.165977 0.043542 0.024 Uiso 0.125 1 calc R U P A -1
H1B_1 H 0.590504 0.211912 0.035778 0.024 Uiso 0.125 1 calc R U P A -1
H1C_1 H 0.476644 0.205127 -0.147097 0.024 Uiso 0.125 1 calc R U P A -1
C2_1 C 0.237(3) 0.474(4) 0.015(8) 0.018(5) Uani 0.125 1 d D U P A -1
H2A_1 H 0.184538 0.472485 -0.106605 0.027 Uiso 0.125 1 calc R U P A -1
H2B_1 H 0.222216 0.591802 0.068560 0.027 Uiso 0.125 1 calc R U P A -1
H2C_1 H 0.177960 0.385343 0.091003 0.027 Uiso 0.125 1 calc R U P A -1
C3_1 C 0.751(3) 0.507(6) -0.006(7) 0.015(5) Uani 0.125 1 d D U P A -1
H3A_1 H 0.820324 0.614450 0.013983 0.022 Uiso 0.125 1 calc R U P A -1
H3B_1 H 0.776717 0.458989 -0.126798 0.022 Uiso 0.125 1 calc R U P A -1
H3C_1 H 0.781351 0.418007 0.085903 0.022 Uiso 0.125 1 calc R U P A -1
C4_1 C 0.552(3) 0.551(3) 0.007(5) 0.016(2) Uani 0.125 1 d D U P A -1
C5_1 C 0.507(6) 0.749(3) 0.028(7) 0.019(6) Uani 0.125 1 d D U P A -1
H5A_1 H 0.456268 0.769811 0.147867 0.028 Uiso 0.125 1 calc R U P A -1
H5B_1 H 0.421529 0.783142 -0.065608 0.028 Uiso 0.125 1 calc R U P A -1
H5C_1 H 0.615790 0.818866 0.013860 0.028 Uiso 0.125 1 calc R U P A -1
N1_1 N 0.432(2) 0.431(2) 0.002(5) 0.0165(18) Uani 0.125 1 d D U P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.03223(6) 0.03223(6) 0.01966(7) 0.000 0.000 0.000
C1_1 0.015(5) 0.017(3) 0.018(13) 0.001(4) 0.001(5) -0.005(3)
C2_1 0.017(3) 0.014(5) 0.023(14) -0.004(6) 0.000(5) -0.006(2)
C3_1 0.016(4) 0.016(9) 0.013(11) -0.004(14) -0.003(7) 0.001(5)
C4_1 0.016(3) 0.014(3) 0.018(5) -0.003(4) -0.004(4) 0.000(2)
C5_1 0.017(9) 0.012(3) 0.026(13) 0.002(4) -0.007(9) 0.001(4)
N1_1 0.016(3) 0.016(3) 0.017(3) -0.002(5) -0.002(5) -0.0068(16)

_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
C1_1 H1A_1 0.9600 . ?
C1_1 H1B_1 0.9600 . ?
C1_1 H1C_1 0.9600 . ?
C1_1 N1_1 1.475(18) . ?
C2_1 H2A_1 0.9600 . ?
C2_1 H2B_1 0.9600 . ?
C2_1 H2C_1 0.9600 . ?
C2_1 N1_1 1.477(18) . ?
C3_1 H3A_1 0.9600 . ?
C3_1 H3B_1 0.9600 . ?
C3_1 H3C_1 0.9600 . ?
C3_1 C4_1 1.508(18) . ?
C4_1 C5_1 1.505(17) . ?
C4_1 N1_1 1.252(9) . ?
C5_1 H5A_1 0.9600 . ?
C5_1 H5B_1 0.9600 . ?
C5_1 H5C_1 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A_1 C1_1 H1B_1 109.5 . . ?
H1A_1 C1_1 H1C_1 109.5 . . ?
H1B_1 C1_1 H1C_1 109.5 . . ?
N1_1 C1_1 H1A_1 109.5 . . ?
N1_1 C1_1 H1B_1 109.5 . . ?
N1_1 C1_1 H1C_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
N1_1 C2_1 H2A_1 109.5 . . ?
N1_1 C2_1 H2B_1 109.5 . . ?
N1_1 C2_1 H2C_1 109.5 . . ?
H3A_1 C3_1 H3B_1 109.5 . . ?
H3A_1 C3_1 H3C_1 109.5 . . ?
H3B_1 C3_1 H3C_1 109.5 . . ?
C4_1 C3_1 H3A_1 109.5 . . ?
C4_1 C3_1 H3B_1 109.5 . . ?
C4_1 C3_1 H3C_1 109.5 . . ?
C5_1 C4_1 C3_1 115(3) . . ?
N1_1 C4_1 C3_1 122.2(19) . . ?
N1_1 C4_1 C5_1 122.4(19) . . ?
C4_1 C5_1 H5A_1 109.5 . . ?
C4_1 C5_1 H5B_1 109.5 . . ?
C4_1 C5_1 H5C_1 109.5 . . ?
H5A_1 C5_1 H5B_1 109.5 . . ?
H5A_1 C5_1 H5C_1 109.5 . . ?
H5B_1 C5_1 H5C_1 109.5 . . ?
C1_1 N1_1 C2_1 115(2) . . ?
C4_1 N1_1 C1_1 122.8(13) . . ?
C4_1 N1_1 C2_1 122.2(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3_1 C4_1 N1_1 C1_1 0.0(11) . . . . ?
C3_1 C4_1 N1_1 C2_1 -180.0(5) . . . . ?
C5_1 C4_1 N1_1 C1_1 180.0(6) . . . . ?
C5_1 C4_1 N1_1 C2_1 0.0(11) . . . . ?

_shelx_res_file                  
;
TITL jmx114_a.res in I4/m
    jmx114.res
    created by SHELXL-2018/3 at 15:51:10 on 04-Apr-2022
REM Old TITL jmx114 in I-4
REM SHELXT solution in I4/m: R1 0.066, Rweak 0.413, Alpha 0.023
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C4 N4 I
rem SADI_MEIM 0.04 N1 C3 N1 C5
rem SADI_MEIM 0.04 C1 C4 C2 C4
CELL 0.71073 7.3846 7.3846 7.2299 90 90 90
ZERR 2 0.0001 0.0001 0.0002 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SFAC C H I N
UNIT 10 24 2 2
FLAT_MEIM 0.05 C1 C2 C3 C4 C5 N1
SADI_MEIM N1 C1 N1 C2
SADI_MEIM C3 C4 C4 C5
SIMU_MEIM 0.01 0.02 2 C1 C2 C3 C4 C5 N1
RIGU_1 0.002 0.002 C1 C2 C3 C4 C5 N1

L.S. 10 0 0
PLAN  1
SIZE 0.037 0.055 0.148
TEMP 0
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\jmx114.hkl">
REM </olex2.extras>

WGHT    0.021300
FVAR       0.67645
I1    3    0.500000    0.500000    0.500000    10.12500    0.03223    0.03223 =
         0.01966    0.00000    0.00000    0.00000
RESI MEIM 1
PART -1
C1    1    0.474322    0.236473   -0.018255    10.12500    0.01470    0.01677 =
         0.01750    0.00075    0.00102   -0.00453
AFIX 137
H1A   2    0.383383    0.165977    0.043542    10.12500   -1.50000
H1B   2    0.590504    0.211912    0.035778    10.12500   -1.50000
H1C   2    0.476644    0.205127   -0.147097    10.12500   -1.50000
AFIX   0
C2    1    0.237127    0.473864    0.014819    10.12500    0.01655    0.01413 =
         0.02292   -0.00390   -0.00049   -0.00579
AFIX 137
H2A   2    0.184538    0.472485   -0.106605    10.12500   -1.50000
H2B   2    0.222216    0.591802    0.068560    10.12500   -1.50000
H2C   2    0.177960    0.385343    0.091003    10.12500   -1.50000
AFIX   0
C3    1    0.750581    0.506522   -0.006127    10.12500    0.01590    0.01575 =
         0.01309   -0.00358   -0.00262    0.00056
AFIX 137
H3A   2    0.820324    0.614450    0.013983    10.12500   -1.50000
H3B   2    0.776717    0.458989   -0.126798    10.12500   -1.50000
H3C   2    0.781351    0.418007    0.085903    10.12500   -1.50000
AFIX   0
C4    1    0.551697    0.550680    0.007270    10.12500    0.01556    0.01421 =
         0.01844   -0.00304   -0.00370    0.00012
C5    1    0.507304    0.748528    0.027695    10.12500    0.01746    0.01249 =
         0.02634    0.00192   -0.00736    0.00149
AFIX 137
H5A   2    0.456268    0.769811    0.147867    10.12500   -1.50000
H5B   2    0.421529    0.783142   -0.065608    10.12500   -1.50000
H5C   2    0.615790    0.818866    0.013860    10.12500   -1.50000
AFIX   0
N1    4    0.431957    0.430738    0.001745    10.12500    0.01638    0.01583 =
         0.01726   -0.00186   -0.00209   -0.00677
HKLF 4




REM  jmx114_a.res in I4/m
REM wR2 = 0.0375, GooF = S = 1.092, Restrained GooF = 1.048 for all data
REM R1 = 0.0172 for 719 Fo > 4sig(Fo) and 0.0205 for all 755 data
REM 61 parameters refined using 68 restraints

END

WGHT      0.0213      0.0000

REM Highest difference peak  0.798,  deepest hole -1.563,  1-sigma level  0.080
Q1    1   0.4339  0.5008  0.5000  10.50000  0.05    0.80
;
_shelx_res_checksum              41336
_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_jmx116a_176
_database_code_depnum_ccdc_archive 'CCDC 2346574'
loop_
_audit_author_name
_audit_author_address
'Jakob Moebs'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2024-04-06 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_audit_creation_date             2022-04-11
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(I Pb0.333), C5 H12 N'
_chemical_formula_sum            'C5 H12 I3 N Pb'
_chemical_formula_weight         674.05
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   16.745(4)
_cell_length_b                   16.745(4)
_cell_length_c                   8.387(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2036.5(12)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    1977
_cell_measurement_temperature    273.00
_cell_measurement_theta_max      23.01
_cell_measurement_theta_min      2.43
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.202
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1075 before and 0.0811 after correction.
The Ratio of minimum to maximum transmission is 0.7866.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.298
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1740
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.027
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1402
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21901
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.433
_diffrn_ambient_temperature      273.00
_diffrn_detector                 'PHOTON III C14'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                845
_reflns_number_total             1438
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.666
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1438
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0406
_refine_ls_restrained_S_all      1.037
_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)+(0.0071P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0981
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.3 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1_1-C1_1 \\sim N1_1-C2_1
 N1_2-C1_2 \\sim N1_2-C2_2
 with sigma of 0.02
 C3_1-C4_1 \\sim C4_1-C5_1
 C3_2-C4_2 \\sim C4_2-C5_2
 with sigma of 0.02
 N1_1-C3_1 \\sim N1_1-C5_1
 N1_2-C3_2 \\sim N1_2-C5_2
 with sigma of 0.04
 C1_1-C4_1 \\sim C2_1-C4_1
 C1_2-C4_2 \\sim C2_2-C4_2
 with sigma of 0.04
3. Restrained planarity
 C1_1, C2_1, C3_1, C4_1, C5_1, N1_1
 C1_2, C2_2, C3_2, C4_2, C5_2, N1_2
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
C1_1 \\sim C2_1 \\sim C3_1 \\sim C4_1 \\sim C5_1 \\sim N1_1 \\sim C1_2 \\sim
C2_2 \\sim C3_2 \\sim C4_2 \\sim C5_2 \\sim N1_2: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
5. Others
 Fixed Sof: C1(0.25) H1A(0.25) H1B(0.25) H1C(0.25) C2(0.25) H2A(0.25)
 H2B(0.25) H2C(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) C4(0.25) C5(0.25)
 H5A(0.25) H5B(0.25) H5C(0.25) N1(0.25) C1(0.25) H1A(0.25) H1B(0.25) H1C(0.25)
 C2(0.25) H2A(0.25) H2B(0.25) H2C(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25)
 C4(0.25) C5(0.25) H5A(0.25) H5B(0.25) H5C(0.25) N1(0.25)
6.a Free rotating group:
 C1(C2,C3,C4,C5,N1)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C1(H1A,
 H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.000000 1.000000 0.500000 0.0476(3) Uani 1 6 d S T P . .
Pb2 Pb 0.333333 0.666667 0.49961(8) 0.0505(2) Uani 1 3 d S T P . .
I1 I 0.82979(7) 0.90339(8) 0.750000 0.0618(4) Uani 1 2 d S T P . .
I3 I 0.38159(9) 0.54864(8) 0.250000 0.0675(4) Uani 1 2 d S T P . .
I2 I 0.48873(8) 0.68409(9) 0.750000 0.0700(4) Uani 1 2 d S T P . .
C1_1 C 0.644(3) 0.984(3) 0.954(4) 0.11(3) Uiso 0.25 1 d DG U P A -1
H1A_1 H 0.604266 1.006069 0.994086 0.148 Uiso 0.25 1 calc R U P A -1
H1B_1 H 0.698609 1.008988 1.016937 0.148 Uiso 0.25 1 calc R U P A -1
H1C_1 H 0.611774 0.918163 0.958314 0.148 Uiso 0.25 1 calc R U P A -1
C2_1 C 0.597(3) 0.953(3) 0.659(5) 0.11(3) Uiso 0.25 1 d DG U P A -1
H2A_1 H 0.609639 0.905083 0.626487 0.147 Uiso 0.25 1 calc R U P A -1
H2B_1 H 0.599033 0.988037 0.566886 0.147 Uiso 0.25 1 calc R U P A -1
H2C_1 H 0.536973 0.925375 0.706302 0.147 Uiso 0.25 1 calc R U P A -1
C3_1 C 0.807(2) 1.139(3) 0.869(5) 0.043(16) Uiso 0.25 1 d DG U P A -1
H3A_1 H 0.867981 1.150404 0.844851 0.056 Uiso 0.25 1 calc R U P A -1
H3B_1 H 0.787261 1.106988 0.969039 0.056 Uiso 0.25 1 calc R U P A -1
H3C_1 H 0.808498 1.197114 0.877430 0.056 Uiso 0.25 1 calc R U P A -1
C4_1 C 0.744(2) 1.084(2) 0.744(4) 0.053(12) Uiso 0.25 1 d DG U P A -1
C5_1 C 0.761(3) 1.111(4) 0.577(4) 0.16(5) Uiso 0.25 1 d DG U P A -1
H5A_1 H 0.819954 1.166641 0.566717 0.214 Uiso 0.25 1 calc R U P A -1
H5B_1 H 0.713647 1.121652 0.536956 0.214 Uiso 0.25 1 calc R U P A -1
H5C_1 H 0.762081 1.062839 0.515892 0.214 Uiso 0.25 1 calc R U P A -1
N1_1 N 0.6694(19) 1.0158(19) 0.779(4) 0.067(13) Uiso 0.25 1 d DG U P A -1
C1_2 C 0.786(3) 1.123(3) 0.907(6) 0.026(11) Uiso 0.25 1 d D U P B -2
H1A_2 H 0.847001 1.132162 0.897119 0.033 Uiso 0.25 1 calc R U P B -2
H1B_2 H 0.757972 1.088740 1.003129 0.033 Uiso 0.25 1 calc R U P B -2
H1C_2 H 0.788217 1.181027 0.911101 0.033 Uiso 0.25 1 calc R U P B -2
C2_2 C 0.785(3) 1.094(3) 0.606(7) 0.062(18) Uiso 0.25 1 d D U P B -2
H2A_2 H 0.810726 1.158983 0.587046 0.081 Uiso 0.25 1 calc R U P B -2
H2B_2 H 0.745326 1.060035 0.518803 0.081 Uiso 0.25 1 calc R U P B -2
H2C_2 H 0.833440 1.079948 0.615774 0.081 Uiso 0.25 1 calc R U P B -2
C3_2 C 0.591(3) 0.982(3) 0.906(5) 0.037(13) Uiso 0.25 1 d D U P B -2
H3A_2 H 0.558468 1.015083 0.912426 0.048 Uiso 0.25 1 calc R U P B -2
H3B_2 H 0.630389 0.995732 0.997748 0.048 Uiso 0.25 1 calc R U P B -2
H3C_2 H 0.548255 0.916910 0.902413 0.048 Uiso 0.25 1 calc R U P B -2
C4_2 C 0.648(2) 1.0092(19) 0.763(5) 0.070(14) Uiso 0.25 1 d D U P B -2
C5_2 C 0.607(3) 0.966(3) 0.610(6) 0.032(13) Uiso 0.25 1 d D U P B -2
H5A_2 H 0.542337 0.921979 0.624925 0.041 Uiso 0.25 1 calc R U P B -2
H5B_2 H 0.637400 0.934506 0.569820 0.041 Uiso 0.25 1 calc R U P B -2
H5C_2 H 0.613198 1.011985 0.535181 0.041 Uiso 0.25 1 calc R U P B -2
N1_2 N 0.728(2) 1.067(2) 0.763(5) 0.097(16) Uiso 0.25 1 d D U P B -2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0542(4) 0.0542(4) 0.0345(6) 0.000 0.000 0.0271(2)
Pb2 0.0569(3) 0.0569(3) 0.0378(5) 0.000 0.000 0.02845(16)
I1 0.0508(7) 0.0759(9) 0.0477(7) 0.000 0.000 0.0233(6)
I3 0.0978(10) 0.0771(9) 0.0505(7) 0.000 0.000 0.0609(8)
I2 0.0602(8) 0.1024(10) 0.0514(8) 0.000 0.000 0.0436(8)

_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 3.2443(11) . ?
Pb1 I1 3.2444(11) 7_776 ?
Pb1 I1 3.2444(11) 8_566 ?
Pb1 I1 3.2444(11) 9_656 ?
Pb1 I1 3.2444(11) 3_675 ?
Pb1 I1 3.2444(11) 2_765 ?
Pb2 I3 3.2462(12) 3_565 ?
Pb2 I3 3.2462(12) . ?
Pb2 I3 3.2462(12) 2_665 ?
Pb2 I2 3.2414(12) 2_665 ?
Pb2 I2 3.2414(12) . ?
Pb2 I2 3.2414(12) 3_565 ?
C1_1 H1A_1 0.9600 . ?
C1_1 H1B_1 0.9600 . ?
C1_1 H1C_1 0.9600 . ?
C1_1 N1_1 1.5419 . ?
C2_1 H2A_1 0.9600 . ?
C2_1 H2B_1 0.9600 . ?
C2_1 H2C_1 0.9600 . ?
C2_1 N1_1 1.5255 . ?
C3_1 H3A_1 0.9600 . ?
C3_1 H3B_1 0.9600 . ?
C3_1 H3C_1 0.9600 . ?
C3_1 C4_1 1.4533 . ?
C4_1 C5_1 1.4585 . ?
C4_1 N1_1 1.2337 . ?
C5_1 H5A_1 0.9600 . ?
C5_1 H5B_1 0.9600 . ?
C5_1 H5C_1 0.9600 . ?
C1_2 H1A_2 0.9600 . ?
C1_2 H1B_2 0.9600 . ?
C1_2 H1C_2 0.9600 . ?
C1_2 N1_2 1.537(16) . ?
C2_2 H2A_2 0.9600 . ?
C2_2 H2B_2 0.9600 . ?
C2_2 H2C_2 0.9600 . ?
C2_2 N1_2 1.552(16) . ?
C3_2 H3A_2 0.9600 . ?
C3_2 H3B_2 0.9600 . ?
C3_2 H3C_2 0.9600 . ?
C3_2 C4_2 1.452(16) . ?
C4_2 C5_2 1.462(16) . ?
C4_2 N1_2 1.20(3) . ?
C5_2 H5A_2 0.9600 . ?
C5_2 H5B_2 0.9600 . ?
C5_2 H5C_2 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 97.26(3) . 9_656 ?
I1 Pb1 I1 180.0 2_765 8_566 ?
I1 Pb1 I1 97.26(3) 2_765 7_776 ?
I1 Pb1 I1 82.74(3) . 3_675 ?
I1 Pb1 I1 82.74(3) 9_656 7_776 ?
I1 Pb1 I1 180.0 9_656 3_675 ?
I1 Pb1 I1 82.74(3) 9_656 8_566 ?
I1 Pb1 I1 82.74(3) . 2_765 ?
I1 Pb1 I1 180.0 . 7_776 ?
I1 Pb1 I1 97.26(3) 9_656 2_765 ?
I1 Pb1 I1 97.26(3) 3_675 7_776 ?
I1 Pb1 I1 82.74(3) 3_675 2_765 ?
I1 Pb1 I1 82.74(3) 8_566 7_776 ?
I1 Pb1 I1 97.26(3) . 8_566 ?
I1 Pb1 I1 97.26(3) 3_675 8_566 ?
I3 Pb2 I3 82.89(3) 3_565 . ?
I3 Pb2 I3 82.89(3) 2_665 . ?
I3 Pb2 I3 82.89(3) 3_565 2_665 ?
I2 Pb2 I3 102.92(3) 2_665 3_565 ?
I2 Pb2 I3 171.98(3) 3_565 2_665 ?
I2 Pb2 I3 171.98(3) 2_665 . ?
I2 Pb2 I3 92.27(3) 3_565 3_565 ?
I2 Pb2 I3 102.92(3) . 2_665 ?
I2 Pb2 I3 171.98(3) . 3_565 ?
I2 Pb2 I3 102.92(3) 3_565 . ?
I2 Pb2 I3 92.27(3) 2_665 2_665 ?
I2 Pb2 I3 92.27(3) . . ?
I2 Pb2 I2 82.56(3) 2_665 3_565 ?
I2 Pb2 I2 82.56(3) 3_565 . ?
I2 Pb2 I2 82.55(3) 2_665 . ?
Pb1 I1 Pb1 80.52(3) 4_775 . ?
Pb2 I3 Pb2 80.31(4) . 10_556 ?
Pb2 I2 Pb2 80.76(4) . 10_557 ?
H1A_1 C1_1 H1B_1 109.5 . . ?
H1A_1 C1_1 H1C_1 109.5 . . ?
H1B_1 C1_1 H1C_1 109.5 . . ?
N1_1 C1_1 H1A_1 109.5 . . ?
N1_1 C1_1 H1B_1 109.5 . . ?
N1_1 C1_1 H1C_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
N1_1 C2_1 H2A_1 109.5 . . ?
N1_1 C2_1 H2B_1 109.5 . . ?
N1_1 C2_1 H2C_1 109.5 . . ?
H3A_1 C3_1 H3B_1 109.5 . . ?
H3A_1 C3_1 H3C_1 109.5 . . ?
H3B_1 C3_1 H3C_1 109.5 . . ?
C4_1 C3_1 H3A_1 109.5 . . ?
C4_1 C3_1 H3B_1 109.5 . . ?
C4_1 C3_1 H3C_1 109.5 . . ?
C3_1 C4_1 C5_1 122.0 . . ?
N1_1 C4_1 C3_1 119.6 . . ?
N1_1 C4_1 C5_1 118.2 . . ?
C4_1 C5_1 H5A_1 109.5 . . ?
C4_1 C5_1 H5B_1 109.5 . . ?
C4_1 C5_1 H5C_1 109.5 . . ?
H5A_1 C5_1 H5B_1 109.5 . . ?
H5A_1 C5_1 H5C_1 109.5 . . ?
H5B_1 C5_1 H5C_1 109.5 . . ?
C2_1 N1_1 C1_1 113.7 . . ?
C4_1 N1_1 C1_1 121.7 . . ?
C4_1 N1_1 C2_1 124.5 . . ?
H1A_2 C1_2 H1B_2 109.5 . . ?
H1A_2 C1_2 H1C_2 109.5 . . ?
H1B_2 C1_2 H1C_2 109.5 . . ?
N1_2 C1_2 H1A_2 109.5 . . ?
N1_2 C1_2 H1B_2 109.5 . . ?
N1_2 C1_2 H1C_2 109.5 . . ?
H2A_2 C2_2 H2B_2 109.5 . . ?
H2A_2 C2_2 H2C_2 109.5 . . ?
H2B_2 C2_2 H2C_2 109.5 . . ?
N1_2 C2_2 H2A_2 109.5 . . ?
N1_2 C2_2 H2B_2 109.5 . . ?
N1_2 C2_2 H2C_2 109.5 . . ?
H3A_2 C3_2 H3B_2 109.5 . . ?
H3A_2 C3_2 H3C_2 109.5 . . ?
H3B_2 C3_2 H3C_2 109.5 . . ?
C4_2 C3_2 H3A_2 109.5 . . ?
C4_2 C3_2 H3B_2 109.5 . . ?
C4_2 C3_2 H3C_2 109.5 . . ?
C3_2 C4_2 C5_2 120(3) . . ?
N1_2 C4_2 C3_2 123(2) . . ?
N1_2 C4_2 C5_2 117(2) . . ?
C4_2 C5_2 H5A_2 109.5 . . ?
C4_2 C5_2 H5B_2 109.5 . . ?
C4_2 C5_2 H5C_2 109.5 . . ?
H5A_2 C5_2 H5B_2 109.5 . . ?
H5A_2 C5_2 H5C_2 109.5 . . ?
H5B_2 C5_2 H5C_2 109.5 . . ?
C1_2 N1_2 C2_2 112(3) . . ?
C4_2 N1_2 C1_2 127(2) . . ?
C4_2 N1_2 C2_2 121(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3_1 C4_1 N1_1 C1_1 -3.4 . . . . ?
C3_1 C4_1 N1_1 C2_1 179.8 . . . . ?
C5_1 C4_1 N1_1 C1_1 -177.8 . . . . ?
C5_1 C4_1 N1_1 C2_1 5.3 . . . . ?
C3_2 C4_2 N1_2 C1_2 0.2(11) . . . . ?
C3_2 C4_2 N1_2 C2_2 -180.0(4) . . . . ?
C5_2 C4_2 N1_2 C1_2 180.0(5) . . . . ?
C5_2 C4_2 N1_2 C2_2 -0.2(10) . . . . ?

_shelx_res_file                  
;
TITL jmx116a_176_a.res in P6(3)/m
    jmx116a_176.res
    created by SHELXL-2018/3 at 14:17:04 on 11-Apr-2022
REM Old TITL jmx116a_176 in P6(3)/m
REM SHELXT solution in P6(3)/m: R1 0.188, Rweak 0.009, Alpha 0.024
REM <I/s> 0.487 for 5 systematic absences, Orientation as input
REM Formula found by SHELXT: I3 Pb
CELL 0.71073 16.745 16.745 8.3866 90 90 120
ZERR 6 0.004 0.004 0.0031 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,+X,0.5+Z
SFAC C H I N Pb
UNIT 30 72 18 6 6
SADI_MEIM N1 C1 N1 C2
SADI_MEIM C3 C4 C4 C5
SADI_MEIM 0.04 N1 C3 N1 C5
SADI_MEIM 0.04 C1 C4 C2 C4
FLAT_MEIM 0.05 C1 C2 C3 C4 C5 N1
SIMU_MEIM C1 C2 C3 C4 C5 N1

L.S. 20 0 0
PLAN  6
TEMP -0.15
CONF
list 4
MORE -1
fmap 2 53
acta
BOND $H
OMIT 0 52
REM <olex2.extras>
REM <HklSrc "%.\\jmx116a_0m.hkl">
REM </olex2.extras>

WGHT    0.007100
FVAR       0.03246
PB1   5    1.000000    1.000000    0.500000    10.16667    0.05422    0.05422 =
         0.03448    0.00000    0.00000    0.02711
PB2   5    0.333333    0.666667    0.499607    10.33333    0.05691    0.05691 =
         0.03780    0.00000    0.00000    0.02845
I1    3    0.829790    0.903386    0.750000    10.50000    0.05084    0.07588 =
         0.04770    0.00000    0.00000    0.02334
I3    3    0.381591    0.548645    0.250000    10.50000    0.09780    0.07714 =
         0.05049    0.00000    0.00000    0.06089
I2    3    0.488728    0.684093    0.750000    10.50000    0.06018    0.10236 =
         0.05140    0.00000    0.00000    0.04363
RESI MEIM 1
PART -1
AFIX   6
C1    1    0.643571    0.984290    0.953580    10.25000    0.11407
AFIX 137
H1A   2    0.604266    1.006069    0.994086    10.25000   -1.30000
H1B   2    0.698609    1.008988    1.016937    10.25000   -1.30000
H1C   2    0.611774    0.918163    0.958314    10.25000   -1.30000
AFIX   5
C2    1    0.597052    0.952738    0.658530    10.25000    0.11280
AFIX 137
H2A   2    0.609639    0.905083    0.626487    10.25000   -1.30000
H2B   2    0.599033    0.988037    0.566886    10.25000   -1.30000
H2C   2    0.536973    0.925375    0.706302    10.25000   -1.30000
AFIX   5
C3    1    0.807278    1.139323    0.869450    10.25000    0.04281
AFIX 137
H3A   2    0.867981    1.150404    0.844851    10.25000   -1.30000
H3B   2    0.787261    1.106988    0.969039    10.25000   -1.30000
H3C   2    0.808498    1.197114    0.877430    10.25000   -1.30000
AFIX   5
C4    1    0.743839    1.084011    0.743850    10.25000    0.05262
C5    1    0.761379    1.111100    0.576560    10.25000    0.16459
AFIX 137
H5A   2    0.819954    1.166641    0.566717    10.25000   -1.30000
H5B   2    0.713647    1.121652    0.536956    10.25000   -1.30000
H5C   2    0.762081    1.062839    0.515892    10.25000   -1.30000
AFIX   5
N1    4    0.669370    1.015850    0.779160    10.25000    0.06658
AFIX   0

RESI MEIM 2
PART -2
C1    1    0.785673    1.122502    0.907066    10.25000    0.02553
AFIX 137
H1A   2    0.847001    1.132162    0.897119    10.25000   -1.30000
H1B   2    0.757972    1.088740    1.003129    10.25000   -1.30000
H1C   2    0.788217    1.181027    0.911101    10.25000   -1.30000
AFIX   0
C2    1    0.784745    1.094138    0.606161    10.25000    0.06209
AFIX 137
H2A   2    0.810726    1.158983    0.587046    10.25000   -1.30000
H2B   2    0.745326    1.060035    0.518803    10.25000   -1.30000
H2C   2    0.833440    1.079948    0.615774    10.25000   -1.30000
AFIX   0
C3    1    0.591405    0.981927    0.905931    10.25000    0.03656
AFIX 137
H3A   2    0.558468    1.015083    0.912426    10.25000   -1.30000
H3B   2    0.630389    0.995732    0.997748    10.25000   -1.30000
H3C   2    0.548255    0.916910    0.902413    10.25000   -1.30000
AFIX   0
C4    1    0.647512    1.009231    0.762590    10.25000    0.06970
C5    1    0.606598    0.965685    0.610026    10.25000    0.03177
AFIX 137
H5A   2    0.542337    0.921979    0.624925    10.25000   -1.30000
H5B   2    0.637400    0.934506    0.569820    10.25000   -1.30000
H5C   2    0.613198    1.011985    0.535181    10.25000   -1.30000
AFIX   0
N1    4    0.727758    1.067385    0.762714    10.25000    0.09713
HKLF 4




REM  jmx116a_176_a.res in P6(3)/m
REM wR2 = 0.0981, GooF = S = 1.029, Restrained GooF = 1.037 for all data
REM R1 = 0.0406 for 845 Fo > 4sig(Fo) and 0.0917 for all 1438 data
REM 68 parameters refined using 40 restraints

END

WGHT      0.0071      0.0000

REM Highest difference peak  1.666,  deepest hole -0.869,  1-sigma level  0.210
Q1    1   0.3174  0.5166  0.2500  10.50000  0.05    1.67
Q2    1   0.8611  0.8822  0.7500  10.50000  0.05    1.11
Q3    1   0.3402  0.7391  0.4909  11.00000  0.05    1.01
Q4    1   0.7998  0.8228  0.7500  10.50000  0.05    1.00
Q5    1   0.9412  1.0161  0.4908  11.00000  0.05    0.92
Q6    1   0.7436  1.2446  0.7500  10.50000  0.05    0.81
;
_shelx_res_checksum              59604
_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_jmx112
_database_code_depnum_ccdc_archive 'CCDC 2346575'
loop_
_audit_author_name
_audit_author_address
'Jakob Moebs'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2024-04-06 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_audit_creation_date             2022-03-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(I Pb0.333), C5 H12 N'
_chemical_formula_sum            'C5 H12 I3 N Pb'
_chemical_formula_weight         674.05
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   16.4064(4)
_cell_length_b                   16.4064(4)
_cell_length_c                   8.3883(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1955.38(12)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    19527
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.05
_cell_measurement_theta_min      2.48
_shelx_estimated_absorpt_T_max   0.604
_shelx_estimated_absorpt_T_min   0.395
_exptl_absorpt_coefficient_mu    19.999
_exptl_absorpt_correction_T_max  0.3179
_exptl_absorpt_correction_T_min  0.1337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1740
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 -23 -3 0.0034
-15 11 0 0.0031
-30 -18 -7 0.0090
30 14 7 0.0077
-10 3 -15 0.0064
30 -8 27 0.0061
-29 -20 30 0.0084

_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.028
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            38204
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.341
_diffrn_reflns_theta_min         2.483
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
 816 frames, detector distance = 50 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'GeniX Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1825
_reflns_number_total             2586
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction        
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.843
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.365
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         2586
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.026
_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)+(0.0243P)²+0.8555P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0610
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6111(11)
 0.3889(11)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{N1, C1}
{C2, N2}
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C1)
Uanis(C2) = Uanis(N2)
5. Others
 Sof(C1)=Sof(N2)=0.5*(1-FVAR(2))
 Sof(N1)=Sof(C2)=0.5*FVAR(2)
6.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.000000 1.000000 1.000000 0.01454(13) Uani 1 6 d S T P . .
Pb2 Pb 0.333333 0.666667 0.99983(4) 0.01530(9) Uani 1 3 d S T P . .
I1 I 0.82724(5) 0.92264(6) 0.750000 0.01923(15) Uani 1 2 d S T P . .
I3 I 0.38231(5) 0.83517(5) 1.250000 0.02050(15) Uani 1 2 d S T P . .
I2 I 0.31735(5) 0.50879(5) 0.750000 0.01929(16) Uani 1 2 d S T P . .
N1 N 0.6605(7) 0.9197(7) 1.250000 0.021(2) Uani 0.61(9) 2 d S T P A 1
C2 C 0.6434(6) 0.9880(6) 1.250000 0.018(3) Uani 0.61(9) 2 d S T P A 1
C1 C 0.6605(7) 0.9197(7) 1.250000 0.021(2) Uani 0.39(9) 2 d S T P A 2
N2 N 0.6434(6) 0.9880(6) 1.250000 0.018(3) Uani 0.39(9) 2 d S T P A 2
C3 C 0.6712(7) 0.8776(6) 1.1010(8) 0.0322(18) Uani 1 1 d . . . . .
H3A H 0.722457 0.863832 1.113261 0.048 Uiso 1 1 calc R U . A 1
H3B H 0.685628 0.921939 1.012731 0.048 Uiso 1 1 calc R U . A 1
H3C H 0.612399 0.819189 1.078152 0.048 Uiso 1 1 calc R U . A 1
C4 C 0.6347(7) 1.0308(6) 1.3979(9) 0.043(2) Uani 1 1 d . . . . .
H4A H 0.619060 0.986228 1.486100 0.064 Uiso 1 1 calc R U . A 1
H4B H 0.584783 1.046593 1.385858 0.064 Uiso 1 1 calc R U . A 1
H4C H 0.694474 1.088170 1.420552 0.064 Uiso 1 1 calc R U . A 1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.01568(19) 0.01568(19) 0.0123(3) 0.000 0.000 0.00784(10)
Pb2 0.01566(12) 0.01566(12) 0.01458(17) 0.000 0.000 0.00783(6)
I1 0.0146(3) 0.0243(4) 0.0162(3) 0.000 0.000 0.0078(3)
I3 0.0293(4) 0.0146(4) 0.0172(3) 0.000 0.000 0.0106(3)
I2 0.0257(4) 0.0160(4) 0.0174(3) 0.000 0.000 0.0114(3)
N1 0.012(5) 0.026(6) 0.018(4) 0.000 0.000 0.004(5)
C2 0.012(5) 0.012(5) 0.023(4) 0.000 0.000 0.002(4)
C1 0.012(5) 0.026(6) 0.018(4) 0.000 0.000 0.004(5)
N2 0.012(5) 0.012(5) 0.023(4) 0.000 0.000 0.002(4)
C3 0.033(5) 0.040(5) 0.029(3) -0.015(4) -0.007(4) 0.022(5)
C4 0.051(6) 0.034(5) 0.035(4) -0.014(4) 0.004(4) 0.015(5)

_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 3.2319(5) 7_777 ?
Pb1 I1 3.2319(5) 2_765 ?
Pb1 I1 3.2319(5) 8_567 ?
Pb1 I1 3.2319(5) 3_675 ?
Pb1 I1 3.2319(5) 9_657 ?
Pb1 I1 3.2319(5) . ?
Pb2 I3 3.2358(6) 3_565 ?
Pb2 I3 3.2358(6) 2_665 ?
Pb2 I3 3.2358(6) . ?
Pb2 I2 3.2388(6) 3_565 ?
Pb2 I2 3.2388(6) 2_665 ?
Pb2 I2 3.2388(6) . ?
N1 C2 1.286(13) . ?
N1 C3 1.480(9) 10_558 ?
N1 C3 1.480(9) . ?
C2 C4 1.467(9) 10_558 ?
C2 C4 1.467(9) . ?
C1 N2 1.286(13) . ?
C1 C3 1.480(9) 10_558 ?
C1 C3 1.480(9) . ?
N2 C4 1.467(9) 10_558 ?
N2 C4 1.467(9) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 180.000(19) 7_777 . ?
I1 Pb1 I1 97.560(11) 2_765 9_657 ?
I1 Pb1 I1 180.00(2) 9_657 3_675 ?
I1 Pb1 I1 82.440(11) 8_567 9_657 ?
I1 Pb1 I1 82.440(11) . 3_675 ?
I1 Pb1 I1 82.440(11) 2_765 3_675 ?
I1 Pb1 I1 97.560(11) 7_777 2_765 ?
I1 Pb1 I1 82.440(11) 7_777 8_567 ?
I1 Pb1 I1 82.441(11) . 2_765 ?
I1 Pb1 I1 97.560(12) 7_777 3_675 ?
I1 Pb1 I1 180.0 8_567 2_765 ?
I1 Pb1 I1 97.559(11) . 8_567 ?
I1 Pb1 I1 82.440(11) 7_777 9_657 ?
I1 Pb1 I1 97.560(11) . 9_657 ?
I1 Pb1 I1 97.560(11) 8_567 3_675 ?
I3 Pb2 I3 82.478(14) 2_665 . ?
I3 Pb2 I3 82.478(14) 2_665 3_565 ?
I3 Pb2 I3 82.478(14) . 3_565 ?
I3 Pb2 I2 92.169(13) 2_665 3_565 ?
I3 Pb2 I2 92.169(13) 3_565 . ?
I3 Pb2 I2 103.413(15) . 3_565 ?
I3 Pb2 I2 103.413(15) 2_665 . ?
I3 Pb2 I2 171.522(17) 2_665 2_665 ?
I3 Pb2 I2 171.522(17) 3_565 3_565 ?
I3 Pb2 I2 171.522(17) . . ?
I3 Pb2 I2 103.413(15) 3_565 2_665 ?
I3 Pb2 I2 92.168(13) . 2_665 ?
I2 Pb2 I2 82.647(14) 3_565 2_665 ?
I2 Pb2 I2 82.647(14) 2_665 . ?
I2 Pb2 I2 82.646(13) 3_565 . ?
Pb1 I1 Pb1 80.914(15) . 4_774 ?
Pb2 I3 Pb2 80.863(18) 10_558 . ?
Pb2 I2 Pb2 80.637(18) . 10_557 ?
C2 N1 C3 122.3(5) . 10_558 ?
C2 N1 C3 122.3(5) . . ?
C3 N1 C3 115.3(9) 10_558 . ?
N1 C2 C4 122.2(5) . . ?
N1 C2 C4 122.2(5) . 10_558 ?
C4 C2 C4 115.5(10) 10_558 . ?
N2 C1 C3 122.3(5) . . ?
C3 C1 C3 115.3(9) 10_558 . ?
C1 N2 C4 122.2(5) . . ?
C1 N2 C4 122.2(5) . 10_558 ?
C4 N2 C4 115.5(10) 10_558 . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 C2 C4 178.8(9) 10_558 . . 10_558 ?
C3 N1 C2 C4 -1.1(16) . . . 10_558 ?
C3 N1 C2 C4 1.1(16) 10_558 . . . ?
C3 N1 C2 C4 -178.8(9) . . . . ?
C3 C1 N2 C4 178.8(9) 10_558 . . 10_558 ?
C3 C1 N2 C4 -178.8(9) . . . . ?
C3 C1 N2 C4 -1.1(16) . . . 10_558 ?
C3 C1 N2 C4 1.1(16) 10_558 . . . ?

_shelx_res_file                  
;
TITL jmx112_176_a.res in P6(3)/m
    jmx112.res
    created by SHELXL-2018/3 at 15:25:00 on 29-Mar-2022
REM Old TITL jmx112_176 in P6(3)/m
REM SHELXT solution in P6(3)/m
REM R1 0.408, Rweak 0.040, Alpha 0.116, Orientation as input
REM Formula found by SHELXT: C N7 I3 Pb
CELL 0.71073 16.4064 16.4064 8.3883 90 90 120
ZERR 6 0.0004 0.0004 0.0003 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,+X,0.5+Z
SFAC C H I N Pb
UNIT 30 72 18 6 6
EADP N1 C1
EADP C2 N2
EXYZ N1 C1
EXYZ C2 N2

L.S. 10 0 0
PLAN  6
SIZE 0.028 0.033 0.057
TEMP -173.15
CONF
list 8
MORE -1
BOND $H
fmap 2 53
acta
TWIN 0 1 0 1 0 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\jmx112.hkl">
REM </olex2.extras>

WGHT    0.024300    0.855500
BASF   0.38886
FVAR       0.09689   0.61291
PB1   5    1.000000    1.000000    1.000000    10.16667    0.01568    0.01568 =
         0.01226    0.00000    0.00000    0.00784
PB2   5    0.333333    0.666667    0.999828    10.33333    0.01566    0.01566 =
         0.01458    0.00000    0.00000    0.00783
I1    3    0.827240    0.922643    0.750000    10.50000    0.01461    0.02430 =
         0.01624    0.00000    0.00000    0.00782
I3    3    0.382313    0.835166    1.250000    10.50000    0.02930    0.01455 =
         0.01718    0.00000    0.00000    0.01061
I2    3    0.317347    0.508795    0.750000    10.50000    0.02575    0.01602 =
         0.01740    0.00000    0.00000    0.01141
PART 1
N1    4    0.660538    0.919652    1.250000    20.50000    0.01232    0.02627 =
         0.01774    0.00000    0.00000    0.00429
C2    1    0.643416    0.988042    1.250000    20.50000    0.01222    0.01218 =
         0.02264    0.00000    0.00000    0.00185
PART 2
C1    1    0.660538    0.919652    1.250000   -20.50000    0.01232    0.02627 =
         0.01774    0.00000    0.00000    0.00429
N2    4    0.643416    0.988042    1.250000   -20.50000    0.01222    0.01218 =
         0.02264    0.00000    0.00000    0.00185
PART 0
C3    1    0.671152    0.877603    1.100952    11.00000    0.03335    0.03994 =
         0.02882   -0.01451   -0.00689    0.02246
AFIX 137
H3A   2    0.722457    0.863832    1.113261    11.00000   -1.50000
H3B   2    0.685628    0.921939    1.012731    11.00000   -1.50000
H3C   2    0.612399    0.819189    1.078152    11.00000   -1.50000
AFIX   0
C4    1    0.634711    1.030808    1.397902    11.00000    0.05086    0.03450 =
         0.03534   -0.01407    0.00447    0.01518
AFIX 137
H4A   2    0.619060    0.986228    1.486100    11.00000   -1.50000
H4B   2    0.584783    1.046593    1.385858    11.00000   -1.50000
H4C   2    0.694474    1.088170    1.420552    11.00000   -1.50000
AFIX   0
HKLF 4




REM  jmx112_176_a.res in P6(3)/m
REM wR2 = 0.061040, GooF = S = 1.02640, Restrained GooF = 1.02640 for all data
REM R1 = 0.034200 for 1825 Fo > 4sig(Fo) and 0.077193 for all 2586 data
REM 58 parameters refined using 0 restraints

END

WGHT      0.0243      0.8556

REM Highest difference peak  1.843,  deepest hole -1.749,  1-sigma level  0.365
Q1    1   0.3379  0.8262  1.2500  10.50000  0.05    1.84
Q2    1   0.4933  0.8006  1.2500  10.50000  0.05    1.78
Q3    1   0.3621  0.4477  0.7500  10.50000  0.05    1.66
Q4    1   0.4040  0.5690  0.7500  10.50000  0.05    1.61
Q5    1   1.0000  1.0000  1.2500  10.16667  0.05    1.59
Q6    1   1.0611  1.0589  1.0152  11.00000  0.05    1.59
;
_shelx_res_checksum              32281
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6111(11)
2 0.3889(11)

