# Supplementary Information (SI) for Materials Horizons.
# 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_r-3ap-rbi3-465
_database_code_depnum_ccdc_archive 'CCDC 2366228'
loop_
_audit_author_name
_audit_author_address
'Kai Li'
;Jinzhong University
China
;
_audit_update_record             
;
2025-03-26 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;
_audit_creation_date             2025-01-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(I0.75 Rb0.25), 2(C7)'
_chemical_formula_sum            'C14 I3 Rb'
_chemical_formula_weight         634.41
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   7.3138(7)
_cell_length_b                   7.3138(7)
_cell_length_c                   7.3138(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     391.22(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    277
_cell_measurement_temperature    464.99(15)
_cell_measurement_theta_max      67.5700
_cell_measurement_theta_min      8.5220
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    50.651
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.692
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            543
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.650
_diffrn_reflns_theta_min         6.051
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      464.99(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     40.00  65.00   0.50    0.50    --    0.00  57.00-150.00   50
  2  ω     -7.00  22.00   0.50    0.50    --    0.00  57.00-150.00   58
  3  ω     75.00 111.00   0.50    0.74    --   98.20 -61.00-180.00   72
  4  ω     10.00  65.00   0.50    0.74    --   98.20 -61.00-180.00  110
  5  ω     63.00 125.00   0.50    0.74    --   98.20 -61.00  30.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1203323000
_diffrn_orient_matrix_UB_12      -0.1317696000
_diffrn_orient_matrix_UB_13      -0.1120468000
_diffrn_orient_matrix_UB_21      0.1021125000
_diffrn_orient_matrix_UB_22      0.1642278000
_diffrn_orient_matrix_UB_23      -0.0831415000
_diffrn_orient_matrix_UB_31      0.1394348000
_diffrn_orient_matrix_UB_32      -0.0068872000
_diffrn_orient_matrix_UB_33      0.1578253000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                95
_reflns_number_total             110
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.309
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     10
_refine_ls_number_reflns         110
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      1.218
_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)+(0.0785P)²+0.0747P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1282
_refine_special_details          ?
_olex2_refinement_description    
;
;
_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
I1 I 1.000000 0.500000 0.500000 0.1334(11) Uani 1 16 d S T P . .
Rb1 Rb 0.500000 0.500000 0.500000 0.0765(9) Uani 1 48 d S T P . .
C1 C 1.000000 0.320(12) 0.000000 0.37(5) Uani 1 8 d S T P . .
C2 C 1.113(4) 0.113(4) 0.113(4) 0.32(2) Uani 1 6 d S T P . .

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 0.0716(10) 0.1643(14) 0.1643(14) 0.000 0.000 0.000
Rb1 0.0765(9) 0.0765(9) 0.0765(9) 0.000 0.000 0.000
C1 0.24(3) 0.62(17) 0.24(3) 0.000 0.000 0.000
C2 0.32(2) 0.32(2) 0.32(2) -0.053(17) -0.053(17) -0.053(17)

_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
I1 Rb1 3.6569(3) 1_655 ?
I1 Rb1 3.6569(3) . ?
C1 C2 1.91(7) 26 ?
C1 C2 1.91(7) 28_755 ?
C1 C2 1.91(7) . ?
C1 C2 1.91(7) 3_755 ?
C2 C2 1.65(6) 28_755 ?
C2 C2 1.65(6) 27 ?
C2 C2 1.65(6) 26 ?

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
Rb1 I1 Rb1 180.0 1_655 . ?
I1 Rb1 I1 90.0 1_455 5 ?
I1 Rb1 I1 90.0 1_455 5_545 ?
I1 Rb1 I1 90.0 . 5 ?
I1 Rb1 I1 90.0 . 5_545 ?
I1 Rb1 I1 90.0 1_455 9_554 ?
I1 Rb1 I1 180.0 5_545 5 ?
I1 Rb1 I1 90.0 9 . ?
I1 Rb1 I1 90.0 9 5_545 ?
I1 Rb1 I1 180.0 9 9_554 ?
I1 Rb1 I1 90.0 5_545 9_554 ?
I1 Rb1 I1 90.0 9 1_455 ?
I1 Rb1 I1 90.0 9 5 ?
I1 Rb1 I1 90.0 5 9_554 ?
I1 Rb1 I1 180.0 . 1_455 ?
I1 Rb1 I1 90.0 . 9_554 ?
C2 C1 C2 51(4) 3_755 28_755 ?
C2 C1 C2 75(6) 28_755 26 ?
C2 C1 C2 75(6) 3_755 . ?
C2 C1 C2 51(4) 26 . ?
C2 C1 C2 51(4) 3_755 26 ?
C2 C1 C2 51(4) 28_755 . ?
C1 C2 C1 119.8(4) . 5_645 ?
C1 C2 C1 119.8(4) . 9_654 ?
C1 C2 C1 119.8(4) 9_654 5_645 ?
C2 C2 C1 142(3) 26 5_645 ?
C2 C2 C1 64.4(18) 27 9_654 ?
C2 C2 C1 142(3) 27 . ?
C2 C2 C1 64.4(18) 28_755 . ?
C2 C2 C1 142(3) 28_755 9_654 ?
C2 C2 C1 64.4(18) 26 9_654 ?
C2 C2 C1 64.4(18) 28_755 5_645 ?
C2 C2 C1 64.4(18) 26 . ?
C2 C2 C1 64.4(18) 27 5_645 ?
C2 C2 C2 89.999(2) 28_755 27 ?
C2 C2 C2 89.999(2) 28_755 26 ?
C2 C2 C2 89.999(1) 27 26 ?

_shelx_res_file                  
;
TITL r-3ap-rbi3-465_a.res in Pm-3m
    r-3ap-rbi3-465.res
    created by SHELXL-2016/6 at 19:37:15 on 02-Dec-2019
REM Old TITL r-3AP-RbI3-465 in Pm-3m #221
REM SHELXT solution in Pm-3m
REM R1 0.335, Rweak 0.260, Alpha 0.016, Orientation as input
REM Formula found by SHELXT: O6 Rb
CELL 1.54184 7.313763 7.313763 7.313763 90 90 90
ZERR 0.99984 0.000675 0.000675 0.000675 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Z,+X,+Y
SYMM +Z,-X,-Y
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,+Z,+X
SYMM -Y,+Z,-X
SYMM +Y,-Z,-X
SYMM -Y,-Z,+X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM +Y,-X,+Z
SYMM -Y,+X,+Z
SYMM +X,+Z,-Y
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +X,-Z,+Y
SYMM +Z,+Y,-X
SYMM +Z,-Y,+X
SYMM -Z,+Y,+X
SYMM -Z,-Y,-X
SFAC C I Rb
UNIT 14 3 1

L.S. 99
PLAN  20
LIST 6
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\r-3AP-RbI3-465.hkl">
REM </olex2.extras>

WGHT    0.078500    0.074700
FVAR       0.67557
I1    2    1.000000    0.500000    0.500000    10.06250    0.07163    0.16426 =
         0.16426    0.00000    0.00000    0.00000
RB1   3    0.500000    0.500000    0.500000    10.02083    0.07655    0.07655 =
         0.07655    0.00000    0.00000    0.00000
C1    1    1.000000    0.320382    0.000000    10.12500    0.24414    0.62127 =
         0.24414    0.00000    0.00000    0.00000
C2    1    1.112966    0.112966    0.112966    10.16667    0.31722    0.31722 =
         0.31722   -0.05253   -0.05253   -0.05253
HKLF 4




REM  r-3ap-rbi3-465_a.res in Pm-3m
REM R1 =  0.0480 for      95 Fo > 4sig(Fo)  and  0.0499 for all     110 data
REM     10 parameters refined using      0 restraints

END

WGHT      0.0785      0.0747

REM Highest difference peak  0.309,  deepest hole -1.241,  1-sigma level  0.180
Q1    1   0.3963  0.3963  0.3963  10.16667  0.05    0.31
Q2    1   0.5000  0.3489  0.2556  10.50000  0.05    0.27
Q3    1   0.5000  0.3836  0.3836  10.25000  0.05    0.26
Q4    1   1.0000  0.2269  0.0000  10.12500  0.05    0.25
Q5    1   1.1009  0.3810  0.3810  10.50000  0.05    0.22
Q6    1   0.3721  0.2638  0.4360  11.00000  0.05    0.21
Q7    1   0.4094  0.2576  0.4094  10.50000  0.05    0.21
Q8    1   1.1577  0.4393  0.4044  11.00000  0.05    0.20
Q9    1   1.1321  0.2341  0.5000  10.50000  0.05    0.20
Q10   1   1.1167  0.2419  0.2419  10.50000  0.05    0.15
Q11   1   1.1258  0.4347  0.1888  11.00000  0.05    0.15
Q12   1   1.2105  0.2105  0.2105  10.16667  0.05    0.14
Q13   1   1.1738  0.4236  0.5000  10.50000  0.05    0.14
Q14   1   1.2549  0.0000  0.2549  10.25000  0.05    0.13
Q15   1   1.2418  0.2974  0.0000  10.50000  0.05    0.13
Q16   1   1.1658  0.0866  0.0866  10.50000  0.05    0.01
;
_shelx_res_checksum              26532
_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 2.047
_oxdiff_exptl_absorpt_empirical_full_min 0.623
####################################################################### 
# 
# 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_mo_164393_465k_0m
_database_code_depnum_ccdc_archive 'CCDC 2434284'
loop_
_audit_author_name
_audit_author_address
'Kai Li'
;Jinzhong University
China
;
_audit_update_record             
;
2025-03-26 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;
_audit_creation_date             2025-01-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I3 Rb, 2(C7)'
_chemical_formula_sum            'C14 I3 Rb'
_chemical_formula_weight         634.31
_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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   7.3079(2)
_cell_length_b                   7.3079(2)
_cell_length_c                   7.3079(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     390.28(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2941
_cell_measurement_temperature    465.00
_cell_measurement_theta_max      23.64
_cell_measurement_theta_min      2.79
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.083
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.1532
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1044 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.5856.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10343
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         2.787
_diffrn_ambient_temperature      465.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.6
_diffrn_source_power             0.08
_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                108
_reflns_number_total             127
_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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8
_refine_ls_number_reflns         127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.210
_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)+(0.0969P)²+0.0420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1452
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 1.000000 0.500000 0.500000 0.1379(10) Uani 1 16 d S T P . .
Rb1 Rb 0.500000 0.500000 0.500000 0.0824(8) Uani 1 48 d S T P . .
C1 C 1.000000 0.248(7) 0.000000 0.31(2) Uiso 1 8 d S . P . .
C2 C 1.139(5) 0.139(5) 0.139(5) 0.47(4) Uiso 1 6 d S . P . .

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 0.0768(9) 0.1685(13) 0.1685(13) 0.000 0.000 0.000
Rb1 0.0824(8) 0.0824(8) 0.0824(8) 0.000 0.000 0.000

_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
I1 Rb1 3.65395(9) 1_655 ?
I1 Rb1 3.65395(10) . ?
C1 C2 1.641(14) 28_755 ?
C1 C2 1.641(14) 3_755 ?
C1 C2 1.641(14) 26 ?
C1 C2 1.641(14) . ?
C2 C2 2.03(7) 28_755 ?
C2 C2 2.03(7) 26 ?
C2 C2 2.03(7) 27 ?

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
Rb1 I1 Rb1 180.0 1_655 . ?
I1 Rb1 I1 90.0 1_455 5 ?
I1 Rb1 I1 90.0 1_455 5_545 ?
I1 Rb1 I1 90.0 . 5 ?
I1 Rb1 I1 90.0 . 5_545 ?
I1 Rb1 I1 90.0 1_455 9_554 ?
I1 Rb1 I1 180.0 5_545 5 ?
I1 Rb1 I1 90.0 9 . ?
I1 Rb1 I1 90.0 9 5_545 ?
I1 Rb1 I1 180.0 9 9_554 ?
I1 Rb1 I1 90.0 5_545 9_554 ?
I1 Rb1 I1 90.0 9 1_455 ?
I1 Rb1 I1 90.0 9 5 ?
I1 Rb1 I1 90.0 5 9_554 ?
I1 Rb1 I1 180.0 . 1_455 ?
I1 Rb1 I1 90.0 . 9_554 ?
C2 C1 C2 122(7) . 3_755 ?
C2 C1 C2 76(3) 3_755 28_755 ?
C2 C1 C2 76(3) . 26 ?
C2 C1 C2 122(7) 28_755 26 ?
C2 C1 C2 76(3) . 28_755 ?
C2 C1 C2 76(3) 3_755 26 ?
C1 C2 C1 103(4) 9_654 5_645 ?
C1 C2 C1 103(4) 9_654 . ?
C1 C2 C1 103(4) 5_645 . ?
C1 C2 C2 51.8(16) . 26 ?
C1 C2 C2 119(4) 5_645 26 ?
C1 C2 C2 51.8(16) 5_645 28_755 ?
C1 C2 C2 51.8(16) 5_645 27 ?
C1 C2 C2 51.8(16) 9_654 26 ?
C1 C2 C2 51.8(16) . 28_755 ?
C1 C2 C2 119(4) . 27 ?
C1 C2 C2 51.8(16) 9_654 27 ?
C1 C2 C2 119(4) 9_654 28_755 ?
C2 C2 C2 90.000(1) 26 27 ?
C2 C2 C2 90.000(5) 28_755 27 ?
C2 C2 C2 90.000(3) 28_755 26 ?

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
C2 C1 C2 C1 53(4) 3_755 . . 9_654 ?
C2 C1 C2 C1 -11(6) 26 . . 9_654 ?
C2 C1 C2 C1 117.2(10) 28_755 . . 9_654 ?
C2 C1 C2 C1 11(6) 28_755 . . 5_645 ?
C2 C1 C2 C1 -53(4) 3_755 . . 5_645 ?
C2 C1 C2 C1 -117.2(10) 26 . . 5_645 ?
C2 C1 C2 C2 -64(3) 3_755 . . 28_755 ?
C2 C1 C2 C2 64(3) 28_755 . . 27 ?
C2 C1 C2 C2 -128(5) 26 . . 28_755 ?
C2 C1 C2 C2 0.000(3) 3_755 . . 27 ?
C2 C1 C2 C2 64(3) 3_755 . . 26 ?
C2 C1 C2 C2 128(5) 28_755 . . 26 ?
C2 C1 C2 C2 -64(3) 26 . . 27 ?

_shelx_res_file                  
;
TITL mo_164393_465k_0m_a.res in Pm-3m
    mo_164393_465k_0m.res
    created by SHELXL-2016/6 at 15:41:59 on 13-Nov-2024
REM Old TITL mo_164393_465k_0m_a.res in Pm-3m
REM SHELXT solution in Pm-3m
REM R1 0.325, Rweak 0.028, Alpha 0.039, Orientation as input
REM Formula found by SHELXT: I
CELL 0.71073 7.3079 7.3079 7.3079 90 90 90
ZERR 1 0.0002 0.0002 0.0002 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Z,+X,+Y
SYMM +Z,-X,-Y
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,+Z,+X
SYMM -Y,+Z,-X
SYMM +Y,-Z,-X
SYMM -Y,-Z,+X
SYMM +Y,+X,-Z
SYMM -Y,-X,-Z
SYMM +Y,-X,+Z
SYMM -Y,+X,+Z
SYMM +X,+Z,-Y
SYMM -X,+Z,+Y
SYMM -X,-Z,-Y
SYMM +X,-Z,+Y
SYMM +Z,+Y,-X
SYMM +Z,-Y,+X
SYMM -Z,+Y,+X
SYMM -Z,-Y,-X
SFAC C I Rb
UNIT 14 3 1

L.S. 10
PLAN  5
TEMP 191.85
CONF
LIST 6
fmap 2
MORE -1
ACTA
REM <olex2.extras>
REM <HklSrc "%.\\mo_164393_465K_0m.hkl">
REM </olex2.extras>

WGHT    0.096900    0.042000
FVAR       0.70390
I1    2    1.000000    0.500000    0.500000    10.06250    0.07676    0.16847 =
         0.16847    0.00000    0.00000    0.00000
RB1   3    0.500000    0.500000    0.500000    10.02083    0.08240    0.08240 =
         0.08240    0.00000    0.00000    0.00000
C1    1    1.000000    0.247774    0.000000    10.12500    0.31108
C2    1    1.138889    0.138889    0.138889    10.16667    0.47129
HKLF 4




REM  mo_164393_465k_0m_a.res in Pm-3m
REM R1 =  0.0403 for     108 Fo > 4sig(Fo)  and  0.0438 for all     127 data
REM      8 parameters refined using      0 restraints

END

WGHT      0.0961      0.0444

REM Highest difference peak  0.488,  deepest hole -0.846,  1-sigma level  0.136
Q1    1   1.1059  0.1058  0.1058  10.16667  0.05    0.49
Q2    1   1.2373  0.5000  0.5000  10.12500  0.05    0.20
Q3    1   1.0000  0.3583  0.0000  10.12500  0.05    0.18
Q4    1   0.5000  0.3183  0.4143  10.50000  0.05    0.16
Q5    1   0.3863  0.3863  0.3863  10.16667  0.05    0.15
;
_shelx_res_checksum              63598
_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_lk_auto
_database_code_depnum_ccdc_archive 'CCDC 2434215'
loop_
_audit_author_name
_audit_author_address
'Kai Li'
;Jinzhong University
China
;
_audit_update_record             
;
2025-03-26 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H16 I3 N2 Rb'
_chemical_formula_weight         594.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_H-M_alt        'P 31 2 1'
_space_group_name_Hall           'P 31 2"'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'

_cell_length_a                   10.07490(10)
_cell_length_b                   10.07490(10)
_cell_length_c                   25.0784(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2204.51(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9524
_cell_measurement_theta_min      2.2220
_cell_measurement_theta_max      27.2120

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.686
_exptl_crystal_F_000             1608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    53.858
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26994
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         5.069
_diffrn_reflns_theta_max         76.805
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3082
_reflns_number_gt                3053
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.705
_reflns_Friedel_fraction_max     0.985
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0604P)²+1.7571P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.007(9)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3082
_refine_ls_number_parameters     120
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0831
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.00585(5) 0.16615(5) 0.41707(2) 0.01258(15) Uani 1 1 d . . . . .
I3 I 0.48728(5) 0.66259(5) 0.41188(2) 0.01357(16) Uani 1 1 d . . . . .
I2 I 0.22979(5) 0.57658(5) 0.57811(2) 0.01192(15) Uani 1 1 d . . . . .
Rb2 Rb 0.66944(9) 1.000000 0.333333 0.0113(2) Uani 1 2 d S T P . .
Rb1 Rb 0.34374(9) 0.34374(9) 0.500000 0.0108(2) Uani 1 2 d S T P . .
N2 N 0.1146(7) 0.5240(6) 0.3598(2) 0.0156(12) Uani 1 1 d . . . . .
H2A H 0.107358 0.536203 0.324124 0.019 Uiso 1 1 calc R U . . .
H2B H 0.092379 0.426161 0.366393 0.019 Uiso 1 1 calc R U . . .
H2C H 0.211604 0.590485 0.370975 0.019 Uiso 1 1 calc R U . . .
N1 N 0.0652(7) 0.7075(7) 0.4720(2) 0.0135(12) Uani 1 1 d . . . . .
H1 H 0.081949 0.706012 0.511286 0.016 Uiso 1 1 calc R U . . .
C3 C 0.0227(8) 0.7104(8) 0.3727(3) 0.0122(13) Uani 1 1 d . . . . .
H3 H 0.005483 0.711374 0.333494 0.015 Uiso 1 1 calc R U . . .
C7 C 0.1799(8) 0.8431(8) 0.3874(3) 0.0133(13) Uani 1 1 d . . . . .
H7A H 0.183136 0.941661 0.380986 0.016 Uiso 1 1 calc R U . . .
H7B H 0.259404 0.840469 0.364927 0.016 Uiso 1 1 calc R U . . .
C5 C 0.0210(9) 0.5522(8) 0.4493(3) 0.0173(15) Uani 1 1 d . . . . .
H5A H -0.076834 0.473310 0.465232 0.021 Uiso 1 1 calc R U . . .
H5B H 0.100903 0.525752 0.457820 0.021 Uiso 1 1 calc R U . . .
C4 C 0.0035(8) 0.5554(8) 0.3890(3) 0.0109(12) Uani 1 1 d . . . . .
H4 H -0.102674 0.473741 0.379331 0.013 Uiso 1 1 calc R U . . .
C6 C 0.2117(7) 0.8297(8) 0.4468(3) 0.0144(14) Uani 1 1 d . U . . .
H6A H 0.292727 0.801846 0.450070 0.017 Uiso 1 1 calc R U . . .
H6B H 0.247224 0.928997 0.464978 0.017 Uiso 1 1 calc R U . . .
C2 C -0.1015(8) 0.7249(9) 0.4034(3) 0.0154(14) Uani 1 1 d . . . . .
H2D H -0.107224 0.814566 0.390294 0.019 Uiso 1 1 calc R U . . .
H2E H -0.202614 0.631946 0.397886 0.019 Uiso 1 1 calc R U . . .
C1 C -0.0608(8) 0.7444(9) 0.4629(3) 0.0173(14) Uani 1 1 d . . . . .
H1A H -0.026111 0.851062 0.474097 0.021 Uiso 1 1 calc R U . . .
H1B H -0.152062 0.674737 0.484275 0.021 Uiso 1 1 calc R U . . .

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 0.0096(2) 0.0096(2) 0.0167(3) -0.00015(13) -0.00195(16) 0.00347(16)
I3 0.0097(2) 0.0114(3) 0.0198(2) 0.00526(16) 0.00325(14) 0.00545(16)
I2 0.0113(2) 0.0097(2) 0.0154(2) -0.00201(13) -0.00040(14) 0.0057(2)
Rb2 0.0107(3) 0.0067(4) 0.0153(5) -0.0003(3) -0.00016(16) 0.0033(2)
Rb1 0.0087(3) 0.0087(3) 0.0152(5) 0.00064(16) -0.00064(16) 0.0045(3)
N2 0.016(3) 0.013(3) 0.022(3) -0.001(2) 0.001(2) 0.011(2)
N1 0.009(3) 0.009(3) 0.016(3) -0.001(2) -0.001(2) 0.000(2)
C3 0.015(3) 0.009(3) 0.017(3) -0.001(3) -0.002(3) 0.009(3)
C7 0.012(3) 0.008(3) 0.017(3) 0.002(3) 0.005(3) 0.002(3)
C5 0.022(4) 0.005(3) 0.023(4) 0.001(3) -0.003(3) 0.005(3)
C4 0.009(3) 0.006(3) 0.017(3) 0.000(3) -0.002(3) 0.003(2)
C6 0.003(3) 0.012(3) 0.022(3) -0.005(3) 0.000(3) -0.002(3)
C2 0.008(3) 0.020(3) 0.024(3) -0.003(3) -0.004(3) 0.011(3)
C1 0.009(3) 0.024(4) 0.021(3) -0.003(3) 0.006(3) 0.010(3)

_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
I1 Rb1 3.6090(8) . ?
I1 Rb2 3.6092(8) 1_445 ?
I3 Rb2 3.5449(4) . ?
I3 Rb1 3.5564(7) . ?
I2 Rb2 3.6515(7) 2_665 ?
I2 Rb1 3.6539(4) . ?
N2 C4 1.499(8) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N1 C1 1.508(9) . ?
N1 C5 1.508(9) . ?
N1 C6 1.510(8) . ?
N1 H1 1.0000 . ?
C3 C7 1.521(9) . ?
C3 C4 1.531(9) . ?
C3 C2 1.537(9) . ?
C3 H3 1.0000 . ?
C7 C6 1.544(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C5 C4 1.523(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C4 H4 1.0000 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C2 C1 1.533(9) . ?
C2 H2D 0.9900 . ?
C2 H2E 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?

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
Rb1 I1 Rb2 178.247(17) . 1_445 ?
Rb2 I3 Rb1 173.32(2) . . ?
Rb2 I2 Rb1 158.99(2) 2_665 . ?
I3 Rb2 I3 175.62(3) 5_675 . ?
I3 Rb2 I1 92.137(14) 5_675 5_665 ?
I3 Rb2 I1 90.962(15) . 5_665 ?
I3 Rb2 I1 90.961(15) 5_675 1_665 ?
I3 Rb2 I1 92.138(14) . 1_665 ?
I1 Rb2 I1 89.99(2) 5_665 1_665 ?
I3 Rb2 I2 95.513(14) 5_675 3_564 ?
I3 Rb2 I2 81.957(12) . 3_564 ?
I1 Rb2 I2 80.264(11) 5_665 3_564 ?
I1 Rb2 I2 168.47(2) 1_665 3_564 ?
I3 Rb2 I2 81.957(12) 5_675 4_566 ?
I3 Rb2 I2 95.514(14) . 4_566 ?
I1 Rb2 I2 168.47(2) 5_665 4_566 ?
I1 Rb2 I2 80.265(11) 1_665 4_566 ?
I2 Rb2 I2 110.05(3) 3_564 4_566 ?
I3 Rb1 I3 98.17(3) . 4_556 ?
I3 Rb1 I1 86.932(9) . . ?
I3 Rb1 I1 174.87(2) 4_556 . ?
I3 Rb1 I1 174.87(2) . 4_556 ?
I3 Rb1 I1 86.931(9) 4_556 4_556 ?
I1 Rb1 I1 87.97(2) . 4_556 ?
I3 Rb1 I2 82.506(13) . . ?
I3 Rb1 I2 85.164(15) 4_556 . ?
I1 Rb1 I2 96.081(12) . . ?
I1 Rb1 I2 97.466(14) 4_556 . ?
I3 Rb1 I2 85.165(15) . 4_556 ?
I3 Rb1 I2 82.506(13) 4_556 4_556 ?
I1 Rb1 I2 97.466(14) . 4_556 ?
I1 Rb1 I2 96.081(12) 4_556 4_556 ?
I2 Rb1 I2 161.13(3) . 4_556 ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C1 N1 C5 110.5(5) . . ?
C1 N1 C6 109.6(5) . . ?
C5 N1 C6 110.4(6) . . ?
C1 N1 H1 108.8 . . ?
C5 N1 H1 108.8 . . ?
C6 N1 H1 108.8 . . ?
C7 C3 C4 112.2(6) . . ?
C7 C3 C2 109.6(6) . . ?
C4 C3 C2 105.6(6) . . ?
C7 C3 H3 109.8 . . ?
C4 C3 H3 109.8 . . ?
C2 C3 H3 109.8 . . ?
C3 C7 C6 109.1(5) . . ?
C3 C7 H7A 109.9 . . ?
C6 C7 H7A 109.9 . . ?
C3 C7 H7B 109.9 . . ?
C6 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N1 C5 C4 109.3(5) . . ?
N1 C5 H5A 109.8 . . ?
C4 C5 H5A 109.8 . . ?
N1 C5 H5B 109.8 . . ?
C4 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
N2 C4 C5 112.0(6) . . ?
N2 C4 C3 111.0(6) . . ?
C5 C4 C3 109.2(5) . . ?
N2 C4 H4 108.2 . . ?
C5 C4 H4 108.2 . . ?
C3 C4 H4 108.2 . . ?
N1 C6 C7 108.4(5) . . ?
N1 C6 H6A 110.0 . . ?
C7 C6 H6A 110.0 . . ?
N1 C6 H6B 110.0 . . ?
C7 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
C1 C2 C3 108.7(5) . . ?
C1 C2 H2D 109.9 . . ?
C3 C2 H2D 109.9 . . ?
C1 C2 H2E 109.9 . . ?
C3 C2 H2E 109.9 . . ?
H2D C2 H2E 108.3 . . ?
N1 C1 C2 108.7(5) . . ?
N1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
N1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.3 . . ?

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
C4 C3 C7 C6 -51.5(7) . . . . ?
C2 C3 C7 C6 65.5(7) . . . . ?
C1 N1 C5 C4 63.7(8) . . . . ?
C6 N1 C5 C4 -57.7(8) . . . . ?
N1 C5 C4 N2 118.4(6) . . . . ?
N1 C5 C4 C3 -5.0(8) . . . . ?
C7 C3 C4 N2 -63.1(7) . . . . ?
C2 C3 C4 N2 177.5(5) . . . . ?
C7 C3 C4 C5 60.8(8) . . . . ?
C2 C3 C4 C5 -58.5(8) . . . . ?
C1 N1 C6 C7 -55.1(7) . . . . ?
C5 N1 C6 C7 66.8(7) . . . . ?
C3 C7 C6 N1 -10.4(7) . . . . ?
C7 C3 C2 C1 -52.0(7) . . . . ?
C4 C3 C2 C1 69.0(7) . . . . ?
C5 N1 C1 C2 -53.0(7) . . . . ?
C6 N1 C1 C2 68.9(7) . . . . ?
C3 C2 C1 N1 -12.5(8) . . . . ?

_refine_diff_density_max         1.035
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.327

_shelx_res_file                  
;
TITL lk_auto_a.res in P3(1)21
    lk_auto.res
    created by SHELXL-2016/6 at 11:00:29 on 26-Mar-2025
REM Old TITL LK_auto in P3121 #152
REM SHELXT solution in P3(1)21
REM R1 0.065, Rweak 0.010, Alpha 0.003, Orientation as input
REM Flack x = -0.023 ( 0.010 ) from Parsons' quotients
REM Formula found by SHELXT: C7 N2 I3 Rb
CELL 1.54184 10.0749 10.0749 25.0784 90 90 120
ZERR 6 0.0001 0.0001 0.0004 0 0 0
LATT -1
SYMM -Y,+X-Y,0.333+Z
SYMM +Y-X,-X,0.667+Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,0.667-Z
SYMM -X,-X+Y,0.333-Z
SFAC C H I N Rb
UNIT 42 96 18 12 6
ISOR 0.01 0.02 C6

L.S. 99
PLAN  10
TEMP -173
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\LK_auto.hkl">
REM </olex2.extras>

WGHT    0.060400    1.757100
FVAR       0.09944
I1    3    0.005849    0.166153    0.417069    11.00000    0.00962    0.00961 =
         0.01674   -0.00015   -0.00195    0.00347
I3    3    0.487275    0.662586    0.411885    11.00000    0.00966    0.01143 =
         0.01984    0.00526    0.00325    0.00545
I2    3    0.229794    0.576585    0.578106    11.00000    0.01127    0.00970 =
         0.01541   -0.00201   -0.00040    0.00571
RB2   5    0.669436    1.000000    0.333333    10.50000    0.01068    0.00667 =
         0.01527   -0.00031   -0.00016    0.00334
RB1   5    0.343741    0.343741    0.500000    10.50000    0.00874    0.00874 =
         0.01520    0.00064   -0.00064    0.00452
N2    4    0.114626    0.523969    0.359757    11.00000    0.01643    0.01346 =
         0.02229   -0.00065    0.00054    0.01150
AFIX 137
H2A   2    0.107358    0.536203    0.324124    11.00000   -1.20000
H2B   2    0.092379    0.426161    0.366393    11.00000   -1.20000
H2C   2    0.211604    0.590485    0.370975    11.00000   -1.20000
AFIX   0
N1    4    0.065214    0.707481    0.472037    11.00000    0.00872    0.00931 =
         0.01615   -0.00089   -0.00075   -0.00026
AFIX  13
H1    2    0.081949    0.706012    0.511286    11.00000   -1.20000
AFIX   0
C3    1    0.022718    0.710437    0.372728    11.00000    0.01455    0.00898 =
         0.01707   -0.00118   -0.00178    0.00887
AFIX  13
H3    2    0.005483    0.711374    0.333494    11.00000   -1.20000
AFIX   0
C7    1    0.179923    0.843124    0.387369    11.00000    0.01172    0.00753 =
         0.01729    0.00234    0.00533    0.00235
AFIX  23
H7A   2    0.183136    0.941661    0.380986    11.00000   -1.20000
H7B   2    0.259404    0.840469    0.364927    11.00000   -1.20000
AFIX   0
C5    1    0.020982    0.552210    0.449262    11.00000    0.02201    0.00472 =
         0.02292    0.00083   -0.00267    0.00498
AFIX  23
H5A   2   -0.076834    0.473310    0.465232    11.00000   -1.20000
H5B   2    0.100903    0.525752    0.457820    11.00000   -1.20000
AFIX   0
C4    1    0.003488    0.555366    0.389042    11.00000    0.00916    0.00581 =
         0.01653   -0.00023   -0.00209    0.00289
AFIX  13
H4    2   -0.102674    0.473741    0.379331    11.00000   -1.20000
AFIX   0
C6    1    0.211729    0.829668    0.446765    11.00000    0.00306    0.01166 =
         0.02162   -0.00536    0.00014   -0.00152
AFIX  23
H6A   2    0.292727    0.801846    0.450070    11.00000   -1.20000
H6B   2    0.247224    0.928997    0.464978    11.00000   -1.20000
AFIX   0
C2    1   -0.101512    0.724902    0.403444    11.00000    0.00822    0.01965 =
         0.02371   -0.00273   -0.00418    0.01093
AFIX  23
H2D   2   -0.107224    0.814566    0.390294    11.00000   -1.20000
H2E   2   -0.202614    0.631946    0.397886    11.00000   -1.20000
AFIX   0
C1    1   -0.060766    0.744404    0.462912    11.00000    0.00917    0.02367 =
         0.02097   -0.00293    0.00566    0.00975
AFIX  23
H1A   2   -0.026111    0.851062    0.474097    11.00000   -1.20000
H1B   2   -0.152062    0.674737    0.484275    11.00000   -1.20000
AFIX   0
HKLF 4




REM  lk_auto_a.res in P3(1)21
REM R1 =  0.0310 for    3053 Fo > 4sig(Fo)  and  0.0312 for all    3082 data
REM    120 parameters refined using      6 restraints

END

WGHT      0.0604      1.7658

REM Highest difference peak  1.035,  deepest hole -1.727,  1-sigma level  0.327
Q1    1   0.0737  1.0753  0.4761  11.00000  0.05    1.04
Q2    1   0.1892  0.6636  0.5797  11.00000  0.05    1.02
Q3    1   0.1893  0.7561  0.5551  11.00000  0.05    0.98
Q4    1  -0.1745  0.5117  0.3765  11.00000  0.05    0.97
Q5    1   0.2365  0.4121  0.3764  11.00000  0.05    0.96
Q6    1   0.1183  0.6570  0.3772  11.00000  0.05    0.95
Q7    1   0.3376  0.6783  0.5794  11.00000  0.05    0.94
Q8    1  -0.1003  0.7585  0.5499  11.00000  0.05    0.92
Q9    1  -0.1403  0.4969  0.4546  11.00000  0.05    0.91
Q10   1  -0.0916  0.2514  0.3549  11.00000  0.05    0.89
;
_shelx_res_checksum              54397
####################################################################### 
# 
# 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_k-s_auto
_database_code_depnum_ccdc_archive 'CCDC 2434285'
loop_
_audit_author_name
_audit_author_address
'Kai Li'
;Jinzhong University
China
;
_audit_update_record             
;
2025-03-26 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;
_audit_creation_date             2025-01-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I3 Rb, C7 H16 N2'
_chemical_formula_sum            'C7 H16 I3 N2 Rb'
_chemical_formula_weight         594.39
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N K I '
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'
Rb Rb -0.9393 2.9676 '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      trigonal
_space_group_IT_number           152
_space_group_name_H-M_alt        'P 31 2 1'
_space_group_name_Hall           'P 31 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -z'

_cell_length_a                   10.0809(2)
_cell_length_b                   10.0809(2)
_cell_length_c                   25.1213(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2210.91(11)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    12377
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.1470
_cell_measurement_theta_min      2.3270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.131a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.679
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16906
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.266
_diffrn_reflns_theta_min         2.333
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  35.00   0.50    1.87    --   10.49  81.00-145.00  102
  2  ω    -15.00  42.00   0.50    1.87    --   10.49  78.00 -32.00  114
  3  ω     52.00  77.00   0.50    1.87    --   10.49  38.00  60.00   50
  4  ω    -14.00  50.00   0.50    1.87    --   10.49  75.00  84.00  128
  5  ω     -5.00  20.00   0.50    1.87    --   10.49  38.00  60.00   50
  6  ω     31.00  56.00   0.50    1.87    --  -11.74  19.00 150.00   50
  7  ω     13.00  55.00   0.50    1.87    --   10.49-125.00 -60.00   84
  8  ω    -23.00   3.00   0.50    1.87    --   10.49 -99.00 -60.00   52
  9  ω    -19.00   6.00   0.50    1.87    --  -11.74  19.00 150.00   50
 10  ω    -18.00  18.00   0.50    1.87    --  -11.74 -99.00  30.00   72
 11  ω    -20.00   5.00   0.50    1.87    --  -11.74 -99.00 -30.00   50
 12  ω    -19.00   6.00   0.50    1.87    --  -11.74 -99.00  90.00   50
 13  ω    -10.00  15.00   0.50    1.87    --  -11.74 -99.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0129426000
_diffrn_orient_matrix_UB_12      0.0757211000
_diffrn_orient_matrix_UB_13      0.0020374000
_diffrn_orient_matrix_UB_21      -0.0440470000
_diffrn_orient_matrix_UB_22      -0.0201681000
_diffrn_orient_matrix_UB_23      0.0237188000
_diffrn_orient_matrix_UB_31      0.0670345000
_diffrn_orient_matrix_UB_32      0.0213299000
_diffrn_orient_matrix_UB_33      0.0151969000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.688
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                2864
_reflns_number_total             3136
_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 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.694
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 
;
 Flack x determined using 1064 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.016(13)
_refine_ls_extinction_coef       0.00127(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0426
_refine_ls_restrained_S_all      1.074
_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)+(0.0770P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1203
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 N007(H007), C1(H1), C2(H2)
1.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C5(H5A,H5B), C7(H7A,H7B), C3(H3A,H3B), C4(H4A,H4B)
1.c Idealised Me refined as rotating group:
 N006(H00A,H00B,H00C)
;
_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
I1 I 0.16034(9) 0.99346(8) 0.58374(2) 0.0172(2) Uani 1 1 d . . . . .
I3 I 0.42224(9) 0.65295(8) 0.41142(2) 0.0161(2) Uani 1 1 d . . . . .
I2 I 0.17526(10) 0.51265(9) 0.57833(2) 0.0179(2) Uani 1 1 d . . . . .
Rb1 Rb 0.000000 0.65572(16) 0.666667 0.0160(4) Uani 1 2 d S T P . .
Rb2 Rb 0.33049(17) 0.33049(17) 0.500000 0.0170(4) Uani 1 2 d S T P . .
N006 N 0.4091(10) 0.8842(9) 0.5266(3) 0.016(2) Uani 1 1 d . . . . .
H00A H 0.427866 0.891281 0.491004 0.019 Uiso 1 1 calc R U . . .
H00B H 0.333591 0.906417 0.533446 0.019 Uiso 1 1 calc R U . . .
H00C H 0.378920 0.787419 0.537854 0.019 Uiso 1 1 calc R U . . .
N007 N 0.6415(11) 0.9326(11) 0.6386(3) 0.016(2) Uani 1 1 d . . . . .
H007 H 0.623108 0.914488 0.677742 0.019 Uiso 1 1 calc R U . . .
C6 C 0.6614(14) 0.8193(13) 0.5543(4) 0.020(3) Uani 1 1 d . . . . .
H6A H 0.755724 0.814581 0.547490 0.024 Uiso 1 1 calc R U . . .
H6B H 0.577994 0.740005 0.532244 0.024 Uiso 1 1 calc R U . . .
C5 C 0.8248(13) 1.1000(13) 0.5701(4) 0.019(3) Uani 1 1 d . . . . .
H5A H 0.833770 1.201185 0.564001 0.022 Uiso 1 1 calc R U . . .
H5B H 0.920048 1.104723 0.557355 0.022 Uiso 1 1 calc R U . . .
C1 C 0.6874(12) 0.9766(13) 0.5395(4) 0.014(2) Uani 1 1 d . . . . .
H1 H 0.705695 0.993613 0.500348 0.017 Uiso 1 1 calc R U . . .
C7 C 0.6189(13) 0.7893(13) 0.6129(4) 0.019(3) Uani 1 1 d . . . . .
H7A H 0.510553 0.707514 0.616464 0.023 Uiso 1 1 calc R U . . .
H7B H 0.683742 0.754594 0.630711 0.023 Uiso 1 1 calc R U . . .
C3 C 0.5293(15) 0.9762(16) 0.6160(4) 0.024(3) Uani 1 1 d . . . . .
H3A H 0.546712 1.073012 0.632320 0.029 Uiso 1 1 calc R U . . .
H3B H 0.423062 0.895166 0.624030 0.029 Uiso 1 1 calc R U . . .
C2 C 0.5525(14) 0.9960(14) 0.5557(4) 0.016(3) Uani 1 1 d . . . . .
H2 H 0.576990 1.102215 0.546135 0.020 Uiso 1 1 calc R U . . .
C4 C 0.8026(13) 1.0610(13) 0.6297(4) 0.022(3) Uani 1 1 d . . . . .
H4A H 0.876470 1.029559 0.641681 0.026 Uiso 1 1 calc R U . . .
H4B H 0.821075 1.152094 0.650514 0.026 Uiso 1 1 calc R U . . .

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 0.0187(4) 0.0169(4) 0.0175(4) 0.0014(3) 0.0018(3) 0.0100(3)
I3 0.0156(4) 0.0166(4) 0.0154(3) 0.0002(3) 0.0014(3) 0.0075(3)
I2 0.0160(4) 0.0158(4) 0.0203(4) -0.0032(3) 0.0013(3) 0.0068(4)
Rb1 0.0146(8) 0.0159(6) 0.0172(8) 0.0006(3) 0.0012(6) 0.0073(4)
Rb2 0.0191(7) 0.0191(7) 0.0165(8) 0.0002(3) -0.0002(3) 0.0123(8)
N006 0.011(5) 0.019(5) 0.018(4) -0.001(4) -0.001(4) 0.008(4)
N007 0.026(6) 0.014(5) 0.010(5) 0.001(4) 0.001(4) 0.011(5)
C6 0.020(7) 0.021(7) 0.019(6) -0.009(5) -0.006(5) 0.012(6)
C5 0.011(6) 0.019(7) 0.021(6) 0.008(5) 0.003(5) 0.004(5)
C1 0.011(6) 0.015(6) 0.012(6) 0.005(5) 0.004(4) 0.004(5)
C7 0.023(7) 0.013(6) 0.021(5) 0.001(5) -0.007(5) 0.009(5)
C3 0.021(7) 0.031(8) 0.022(6) 0.007(6) 0.007(5) 0.014(6)
C2 0.028(7) 0.015(6) 0.008(5) 0.003(5) 0.003(5) 0.012(6)
C4 0.021(7) 0.021(7) 0.023(6) 0.002(5) -0.007(5) 0.010(6)

_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
I1 Rb1 3.6113(13) . ?
I1 Rb2 3.6170(14) 1_565 ?
I3 Rb1 3.6598(7) 3_564 ?
I3 Rb2 3.6561(12) . ?
I2 Rb1 3.5601(13) . ?
I2 Rb2 3.5449(7) . ?
N006 H00A 0.9100 . ?
N006 H00B 0.9100 . ?
N006 H00C 0.9100 . ?
N006 C2 1.505(13) . ?
N007 H007 1.0000 . ?
N007 C7 1.492(13) . ?
N007 C3 1.514(14) . ?
N007 C4 1.504(14) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C1 1.519(15) . ?
C6 C7 1.521(15) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C1 1.527(14) . ?
C5 C4 1.537(14) . ?
C1 H1 1.0000 . ?
C1 C2 1.522(15) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.532(16) . ?
C2 H2 1.0000 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?

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
Rb1 I1 Rb2 178.34(3) . 1_565 ?
Rb2 I3 Rb1 158.76(4) . 3_564 ?
Rb2 I2 Rb1 173.16(4) . . ?
I1 Rb1 I1 88.06(4) 5_556 . ?
I1 Rb1 I3 97.49(2) 5_556 2_665 ?
I1 Rb1 I3 96.15(2) . 2_665 ?
I1 Rb1 I3 97.49(2) . 6_456 ?
I1 Rb1 I3 96.15(2) 5_556 6_456 ?
I3 Rb1 I3 160.99(6) 2_665 6_456 ?
I2 Rb1 I1 174.79(4) . 5_556 ?
I2 Rb1 I1 174.79(4) 5_556 . ?
I2 Rb1 I1 86.758(15) 5_556 5_556 ?
I2 Rb1 I1 86.759(15) . . ?
I2 Rb1 I3 85.05(3) 5_556 2_665 ?
I2 Rb1 I3 82.55(2) . 2_665 ?
I2 Rb1 I3 82.56(2) 5_556 6_456 ?
I2 Rb1 I3 85.05(3) . 6_456 ?
I2 Rb1 I2 98.43(5) 5_556 . ?
I1 Rb2 I1 90.05(4) 6_456 1_545 ?
I1 Rb2 I3 168.37(4) 1_545 . ?
I1 Rb2 I3 168.37(4) 6_456 6_556 ?
I1 Rb2 I3 80.081(19) 1_545 6_556 ?
I1 Rb2 I3 80.081(19) 6_456 . ?
I3 Rb2 I3 110.35(5) 6_556 . ?
I2 Rb2 I1 90.87(3) . 6_456 ?
I2 Rb2 I1 90.87(3) 6_556 1_545 ?
I2 Rb2 I1 92.23(2) 6_556 6_456 ?
I2 Rb2 I1 92.23(2) . 1_545 ?
I2 Rb2 I3 81.85(2) . . ?
I2 Rb2 I3 95.63(2) 6_556 . ?
I2 Rb2 I3 95.63(2) . 6_556 ?
I2 Rb2 I3 81.85(2) 6_556 6_556 ?
I2 Rb2 I2 175.61(6) . 6_556 ?
H00A N006 H00B 109.5 . . ?
H00A N006 H00C 109.5 . . ?
H00B N006 H00C 109.5 . . ?
C2 N006 H00A 109.5 . . ?
C2 N006 H00B 109.5 . . ?
C2 N006 H00C 109.5 . . ?
C7 N007 H007 108.9 . . ?
C7 N007 C3 110.1(9) . . ?
C7 N007 C4 110.2(9) . . ?
C3 N007 H007 108.9 . . ?
C4 N007 H007 108.9 . . ?
C4 N007 C3 109.7(9) . . ?
H6A C6 H6B 108.3 . . ?
C1 C6 H6A 109.9 . . ?
C1 C6 H6B 109.9 . . ?
C1 C6 C7 109.1(8) . . ?
C7 C6 H6A 109.9 . . ?
C7 C6 H6B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
C1 C5 H5A 109.9 . . ?
C1 C5 H5B 109.9 . . ?
C1 C5 C4 109.0(9) . . ?
C4 C5 H5A 109.9 . . ?
C4 C5 H5B 109.9 . . ?
C6 C1 C5 109.9(9) . . ?
C6 C1 H1 109.9 . . ?
C6 C1 C2 111.8(9) . . ?
C5 C1 H1 109.9 . . ?
C2 C1 C5 105.4(9) . . ?
C2 C1 H1 109.9 . . ?
N007 C7 C6 109.6(8) . . ?
N007 C7 H7A 109.7 . . ?
N007 C7 H7B 109.7 . . ?
C6 C7 H7A 109.7 . . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
N007 C3 H3A 109.9 . . ?
N007 C3 H3B 109.9 . . ?
N007 C3 C2 108.8(9) . . ?
H3A C3 H3B 108.3 . . ?
C2 C3 H3A 109.9 . . ?
C2 C3 H3B 109.9 . . ?
N006 C2 C1 111.1(9) . . ?
N006 C2 C3 110.8(10) . . ?
N006 C2 H2 108.4 . . ?
C1 C2 C3 109.6(9) . . ?
C1 C2 H2 108.4 . . ?
C3 C2 H2 108.4 . . ?
N007 C4 C5 108.7(8) . . ?
N007 C4 H4A 109.9 . . ?
N007 C4 H4B 109.9 . . ?
C5 C4 H4A 109.9 . . ?
C5 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?

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
N007 C3 C2 N006 118.9(10) . . . . ?
N007 C3 C2 C1 -4.0(15) . . . . ?
C6 C1 C2 N006 -62.8(11) . . . . ?
C6 C1 C2 C3 60.0(13) . . . . ?
C5 C1 C2 N006 177.9(8) . . . . ?
C5 C1 C2 C3 -59.4(12) . . . . ?
C1 C6 C7 N007 -9.2(13) . . . . ?
C1 C5 C4 N007 -10.6(13) . . . . ?
C7 N007 C3 C2 -57.8(13) . . . . ?
C7 N007 C4 C5 66.6(11) . . . . ?
C7 C6 C1 C5 64.3(12) . . . . ?
C7 C6 C1 C2 -52.4(13) . . . . ?
C3 N007 C7 C6 66.1(12) . . . . ?
C3 N007 C4 C5 -54.8(12) . . . . ?
C4 N007 C7 C6 -55.0(12) . . . . ?
C4 N007 C3 C2 63.6(13) . . . . ?
C4 C5 C1 C6 -52.4(12) . . . . ?
C4 C5 C1 C2 68.2(11) . . . . ?

_shelx_res_file                  
;
TITL k-s_auto_a.res in P3(2)21
    k-s_auto.res
    created by SHELXL-2016/6 at 18:17:02 on 05-Nov-2024
REM Old TITL k-s_auto in P3(1)21
REM SHELXT solution in P3(2)21: R1 0.072, Rweak 0.011, Alpha 0.003
REM <I/s> 1.417 for 19 systematic absences, Orientation as input
REM Flack x = -0.005 ( 0.062 ) from 1090 Parsons' quotients
REM Formula found by SHELXT: C7 N2 I4
CELL 0.71073 10.0809 10.0809 25.1213 90 90 120
ZERR 6 0.0002 0.0002 0.0007 0 0 0
LATT -1
SYMM -Y,+X-Y,0.333+Z
SYMM +Y-X,-X,0.667+Z
SYMM -Y+X,-Y,0.667-Z
SYMM -X,-X+Y,0.333-Z
SYMM +Y,+X,-Z
SFAC C H I N Rb
UNIT 42 96 18 12 6

L.S. 10 0 0
PLAN  11
TEMP -123
CONF
BOND
list 4
fmap 2 53
ACTA
MORE -1
BOND $H
OMIT -7 5 6
OMIT -7 6 4
OMIT -7 7 2
OMIT -5 3 8
OMIT -5 5 4
OMIT -5 5 10
OMIT -5 5 16
OMIT -5 7 6
OMIT -4 7 8
OMIT -3 2 20
OMIT -2 3 20
OMIT -2 5 16
OMIT -2 7 6
OMIT -1 1 3
OMIT -1 1 8
OMIT -1 1 20
OMIT 0 3 12
OMIT 0 5 2
OMIT 0 5 8
OMIT 1 6 8
OMIT 2 3 16
OMIT 2 5 0
OMIT 3 4 4
REM <olex2.extras>
REM <HklSrc "%.\\k-s_auto.hkl">
REM </olex2.extras>

WGHT    0.077000
EXTI    0.001268
FVAR       0.12886
I1    3    0.160340    0.993455    0.583736    11.00000    0.01868    0.01687 =
         0.01745    0.00138    0.00182    0.01000
I3    3    0.422236    0.652948    0.411423    11.00000    0.01564    0.01656 =
         0.01540    0.00020    0.00139    0.00753
I2    3    0.175256    0.512655    0.578325    11.00000    0.01597    0.01581 =
         0.02030   -0.00321    0.00127    0.00676
RB1   5    0.000000    0.655720    0.666667    10.50000    0.01464    0.01589 =
         0.01718    0.00061    0.00122    0.00732
RB2   5    0.330488    0.330488    0.500000    10.50000    0.01907    0.01907 =
         0.01653    0.00024   -0.00024    0.01227
N006  4    0.409051    0.884241    0.526621    11.00000    0.01065    0.01920 =
         0.01846   -0.00075   -0.00070    0.00776
AFIX 137
H00A  2    0.427866    0.891281    0.491004    11.00000   -1.20000
H00B  2    0.333591    0.906417    0.533446    11.00000   -1.20000
H00C  2    0.378920    0.787419    0.537854    11.00000   -1.20000
AFIX   0
N007  4    0.641480    0.932587    0.638614    11.00000    0.02557    0.01429 =
         0.01033    0.00113    0.00052    0.01126
AFIX  13
H007  2    0.623108    0.914488    0.677742    11.00000   -1.20000
AFIX   0
C6    1    0.661414    0.819264    0.554279    11.00000    0.02025    0.02147 =
         0.01882   -0.00914   -0.00584    0.01165
AFIX  23
H6A   2    0.755724    0.814581    0.547490    11.00000   -1.20000
H6B   2    0.577994    0.740005    0.532244    11.00000   -1.20000
AFIX   0
C5    1    0.824809    1.099979    0.570064    11.00000    0.01147    0.01874 =
         0.02084    0.00802    0.00307    0.00412
AFIX  23
H5A   2    0.833770    1.201185    0.564001    11.00000   -1.20000
H5B   2    0.920048    1.104723    0.557355    11.00000   -1.20000
AFIX   0
C1    1    0.687372    0.976587    0.539516    11.00000    0.01096    0.01483 =
         0.01182    0.00525    0.00425    0.00363
AFIX  13
H1    2    0.705695    0.993613    0.500348    11.00000   -1.20000
AFIX   0
C7    1    0.618870    0.789324    0.612869    11.00000    0.02295    0.01287 =
         0.02075    0.00078   -0.00746    0.00907
AFIX  23
H7A   2    0.510553    0.707514    0.616464    11.00000   -1.20000
H7B   2    0.683742    0.754594    0.630711    11.00000   -1.20000
AFIX   0
C3    1    0.529302    0.976195    0.616003    11.00000    0.02117    0.03091 =
         0.02163    0.00673    0.00717    0.01402
AFIX  23
H3A   2    0.546712    1.073012    0.632320    11.00000   -1.20000
H3B   2    0.423062    0.895166    0.624030    11.00000   -1.20000
AFIX   0
C2    1    0.552528    0.996021    0.555651    11.00000    0.02767    0.01497 =
         0.00800    0.00327    0.00258    0.01157
AFIX  13
H2    2    0.576990    1.102215    0.546135    11.00000   -1.20000
AFIX   0
C4    1    0.802643    1.060981    0.629731    11.00000    0.02091    0.02100 =
         0.02318    0.00222   -0.00656    0.00982
AFIX  23
H4A   2    0.876470    1.029559    0.641681    11.00000   -1.20000
H4B   2    0.821075    1.152094    0.650514    11.00000   -1.20000
AFIX   0
HKLF 4




REM  k-s_auto_a.res in P3(2)21
REM R1 =  0.0426 for    2864 Fo > 4sig(Fo)  and  0.0471 for all    3136 data
REM    121 parameters refined using      0 restraints

END

WGHT      0.0770      0.0000

REM Highest difference peak  1.408,  deepest hole -1.694,  1-sigma level  0.210
Q1    1   0.1808  0.9452  0.5565  11.00000  0.05    1.27
Q2    1   0.1218  0.9204  0.6135  11.00000  0.05    1.27
Q3    1   0.2085  1.0758  0.5530  11.00000  0.05    1.24
Q4    1   0.2789  0.6209  0.5786  11.00000  0.05    1.16
Q5    1   0.3853  0.3100  0.4736  11.00000  0.05    1.10
Q6    1   0.3560  0.6209  0.3815  11.00000  0.05    1.10
Q7    1   0.1028  0.4813  0.5469  11.00000  0.05    1.09
Q8    1   0.0603  0.6400  0.6408  11.00000  0.05    1.06
Q9    1   0.2115  0.4701  0.5498  11.00000  0.05    1.05
Q10   1   0.4562  0.7257  0.3794  11.00000  0.05    1.05
Q11   1   0.2349  1.0214  0.6148  11.00000  0.05    0.96
;
_shelx_res_checksum              47174
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.049
_oxdiff_exptl_absorpt_empirical_full_min 0.605
