# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_mdabconh4i3_
_database_code_depnum_ccdc_archive 'CCDC 1892554'
loop_
_audit_author_name
_audit_author_address
'Gregor Kieslich'
;TU Munich
Germany
;
_audit_update_record             
;
2019-01-21 deposited with the CCDC.	2019-03-04 downloaded from the CCDC.
;
_audit_creation_date             2018-11-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        MDABCONH4I3
_chemical_formula_moiety         '0.6(N), 1.8(I), 0.6(C7 N2)'
_chemical_formula_sum            'C4.20 I1.80 N1.80'
_chemical_formula_weight         304.08
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C7 N3 I3 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -1.1694 0.9355 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0018 0.0014 '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           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   9.7802(13)
_cell_length_b                   9.7802(13)
_cell_length_c                   13.652(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1130.9(4)
_cell_formula_units_Z            5.00004
_cell_measurement_reflns_used    684
_cell_measurement_temperature    300
_cell_measurement_theta_max      20.6870
_cell_measurement_theta_min      2.6150
_shelx_estimated_absorpt_T_max   0.895
_shelx_estimated_absorpt_T_min   0.263
_exptl_absorpt_coefficient_mu    2.277
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             666
_exptl_crystal_preparation       DAC
_exptl_crystal_recrystallization_method 'see experimental'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.1281
_diffrn_reflns_Laue_measured_fraction_full 0.829
_diffrn_reflns_Laue_measured_fraction_max 0.635
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2353
_diffrn_reflns_point_group_measured_fraction_full 0.777
_diffrn_reflns_point_group_measured_fraction_max 0.603
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         22.403
_diffrn_reflns_theta_min         2.620
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.829
_diffrn_measured_fraction_theta_max 0.635
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 -24.23  280
  2  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 155.77  280
  3  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 155.77  155
  4  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 -24.23  155
  5  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00  24.23  330
  6  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00-155.77  200
  7  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00  24.23  200
  8  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00-155.77  330
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0462553000
_diffrn_orient_matrix_UB_12      0.0239801000
_diffrn_orient_matrix_UB_13      -0.0210347000
_diffrn_orient_matrix_UB_21      -0.0203047000
_diffrn_orient_matrix_UB_22      0.0303441000
_diffrn_orient_matrix_UB_23      -0.0163118000
_diffrn_orient_matrix_UB_31      0.0271832000
_diffrn_orient_matrix_UB_32      0.0423628000
_diffrn_orient_matrix_UB_33      0.0236286000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_special_details          -
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.726
_reflns_Friedel_fraction_max     0.570
_reflns_number_gt                787
_reflns_number_total             1237
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.156
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.322
_refine_ls_abs_structure_details 
;
 Flack x determined using 260 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         1237
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0896
_refine_ls_restrained_S_all      1.093
_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)+(0.1261P)²+6.4983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2405
_refine_ls_wR_factor_ref         0.2665
_refine_special_details          -
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(N1)
Uanis(N001) = Uanis(I1)
Uanis(N3) = Uanis(C4) = Uanis(C2) = Uanis(N1) = Uanis(C1)
;
_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
N001 N 0.666667 0.333333 0.299(4) 0.0515(6) Uani 1 3 d S T P . .
I1 I 0.4763(2) 0.4555(2) 0.48161(2) 0.0515(6) Uani 1 1 d . . . . .
N1 N 0.666667 0.333333 0.859(4) 0.051(4) Uani 1 3 d S T P . .
C2 C 0.677(4) 0.483(4) 0.826(3) 0.051(4) Uani 1 1 d . . . . .
N3 N 0.666667 0.333333 0.672(4) 0.051(4) Uani 1 3 d S T P . .
C4 C 0.700(4) 0.489(4) 0.717(3) 0.051(4) Uani 1 1 d . . . . .
C1 C 0.666667 0.333333 0.975(4) 0.051(4) Uani 1 3 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
N001 0.0470(7) 0.0470(7) 0.0607(11) 0.000 0.000 0.0235(4)
I1 0.0470(7) 0.0470(7) 0.0607(11) 0.000 0.000 0.0235(4)
N1 0.049(6) 0.049(6) 0.053(10) 0.000 0.000 0.025(3)
C2 0.049(6) 0.049(6) 0.053(10) 0.000 0.000 0.025(3)
N3 0.049(6) 0.049(6) 0.053(10) 0.000 0.000 0.025(3)
C4 0.049(6) 0.049(6) 0.053(10) 0.000 0.000 0.025(3)
C1 0.049(6) 0.049(6) 0.053(10) 0.000 0.000 0.025(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
N1 C2 1.49(4) 3_665 ?
N1 C2 1.49(4) . ?
N1 C2 1.49(4) 2_655 ?
N1 C1 1.59(8) . ?
C2 C4 1.51(5) . ?
N3 C4 1.52(4) 2_655 ?
N3 C4 1.52(4) . ?
N3 C4 1.52(4) 3_665 ?

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
C2 N1 C2 112(2) 3_665 2_655 ?
C2 N1 C2 112(2) 3_665 . ?
C2 N1 C2 112(2) 2_655 . ?
C2 N1 C1 107(2) 3_665 . ?
C2 N1 C1 107(2) 2_655 . ?
C2 N1 C1 107(2) . . ?
N1 C2 C4 105(3) . . ?
C4 N3 C4 105(3) 2_655 . ?
C4 N3 C4 105(3) 3_665 2_655 ?
C4 N3 C4 105(3) 3_665 . ?
C2 C4 N3 114(3) . . ?

_iucr_refine_instructions_details 
;
TITL mdabconh4i3__b.res in R3
    mdabconh4i3_.res
    created by SHELXL-2016/6 at 19:14:13 on 10-Nov-2018
REM Old TITL MDABCONH4I3_ in R3
REM SHELXT solution in R3
REM R1 0.293, Rweak 0.047, Alpha 0.036, Orientation as input
REM Flack x = 0.281 ( 0.923 ) from Parsons' quotients
REM Formula found by SHELXT: C3 N3 I
CELL 0.4859 9.7802 9.7802 13.6519 90 90 120
ZERR 5.00004 0.0013 0.0013 0.0024 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C I N
DISP C 0.0007 0.0007 6.0677
DISP I -1.1694 0.9355 2837.686
DISP N 0.0018 0.0014 8.9832
UNIT 21 9 9
EADP C1 N1
EADP N001 I1
EADP N3 C4 C2 N1 C1

L.S. 50
PLAN  20
SIZE 0.05 0.4 0.8
TEMP 26.85
LIST 5
fmap 2
acta
OMIT 0 4 -1
REM <olex2.extras>
REM <HklSrc "%.\\MDABCONH4I3_.hkl">
REM </olex2.extras>

WGHT    0.126100    6.498300
FVAR       0.27406
N001  3    0.666667    0.333333    0.299016    10.33333    0.04695    0.04695 =
         0.06069    0.00000    0.00000    0.02348
I1    2    0.476257    0.455536    0.481610    11.00000    0.04695    0.04695 =
         0.06069    0.00000    0.00000    0.02348
N1    3    0.666667    0.333333    0.858521    10.33333    0.04946    0.04946 =
         0.05279    0.00000    0.00000    0.02473
C2    1    0.676626    0.483436    0.826180    11.00000    0.04946    0.04946 =
         0.05279    0.00000    0.00000    0.02473
N3    3    0.666667    0.333333    0.672142    10.33333    0.04946    0.04946 =
         0.05279    0.00000    0.00000    0.02473
C4    1    0.700091    0.489442    0.716779    11.00000    0.04946    0.04946 =
         0.05279    0.00000    0.00000    0.02473
C1    1    0.666667    0.333333    0.974994    10.33333    0.04946    0.04946 =
         0.05279    0.00000    0.00000    0.02473
HKLF 4




REM  mdabconh4i3__b.res in R3
REM R1 =  0.0896 for     787 Fo > 4sig(Fo)  and  0.1242 for all    1237 data
REM     18 parameters refined using      1 restraints

END  
     
WGHT      0.1264      6.6782 

REM Highest difference peak  1.156,  deepest hole -1.606,  1-sigma level  0.322
Q1    1   0.8426  0.6493  0.6469  11.00000  0.05    1.16
Q2    1   0.6445  0.2352  0.4014  11.00000  0.05    1.06
Q3    1   0.5090  0.5328  0.3976  11.00000  0.05    1.03
Q4    1   0.7419  0.4157  0.3086  11.00000  0.05    1.03
Q5    1   0.7683  0.5443  0.8464  11.00000  0.05    0.95
Q6    1   0.5714  0.4422  0.7989  11.00000  0.05    0.93
Q7    1   0.7908  0.7261  0.6732  11.00000  0.05    0.93
Q8    1   0.6667  0.3333  0.2145  10.33333  0.05    0.93
Q9    1   0.7403  0.5846  0.6198  11.00000  0.05    0.88
Q10   1   0.4647  0.4518  0.5819  11.00000  0.05    0.87
Q11   1   0.5897  0.5243  0.8859  11.00000  0.05    0.83
Q12   1   0.5308  0.4743  0.5717  11.00000  0.05    0.83
Q13   1   0.6305  0.5146  0.4965  11.00000  0.05    0.81
Q14   1   0.7576  0.5149  0.7977  11.00000  0.05    0.81
Q15   1   0.7768  0.6224  0.7495  11.00000  0.05    0.79
Q16   1   0.3170  0.4473  0.4924  11.00000  0.05    0.74
Q17   1   0.3906  0.2068  0.4524  11.00000  0.05    0.73
Q18   1   0.7712  0.6720  0.7816  11.00000  0.05    0.72
Q19   1   0.6667  0.3333  0.4329  10.33333  0.05    0.71
Q20   1   0.8959  0.6249  0.8385  11.00000  0.05    0.71

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0896 for 787 Fo > 4sig(Fo) and 0.1242 for all 2354 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.16, deepest hole -1.61
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.1242
  REM R1_gt = 0.0896
  REM wR_ref = 0.2665
  REM GOOF = 1.094
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2354
  REM Reflections_gt = 787
  REM Parameters = n/a
  REM Hole = -1.61
  REM Peak = 1.16
  REM Flack = -0.1(5)

  
;
_olex2_exptl_crystal_mounting_method DAC
_olex2_submission_original_sample_id MDABCONH4I3-p01
_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 2.267
_oxdiff_exptl_absorpt_empirical_full_min 0.542
####################################################################### 
# 
# 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_mdbachonh4i3_
_database_code_depnum_ccdc_archive 'CCDC 1892555'
loop_
_audit_author_name
_audit_author_address
'Gregor Kieslich'
;TU Munich
Germany
;
_audit_update_record             
;
2019-01-21 deposited with the CCDC.	2019-03-04 downloaded from the CCDC.
;
_audit_creation_date             2018-11-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1.8(I), 0.6(N), 0.6(C7 N2)'
_chemical_formula_sum            'C4.20 I1.80 N1.80'
_chemical_formula_weight         304.08
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C7N3I3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -1.1694 0.9355 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0018 0.0014 '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           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   9.7267(16)
_cell_length_b                   9.7267(16)
_cell_length_c                   13.569(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1111.8(4)
_cell_formula_units_Z            5.00004
_cell_measurement_reflns_used    564
_cell_measurement_temperature    300
_cell_measurement_theta_max      16.0170
_cell_measurement_theta_min      2.6060
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.259
_exptl_absorpt_coefficient_mu    2.316
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             666
_exptl_crystal_preparation       'cut from plate like crystal'
_exptl_crystal_recrystallization_method 'see supporting information'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_unetI/netI     0.1753
_diffrn_reflns_Laue_measured_fraction_full 0.834
_diffrn_reflns_Laue_measured_fraction_max 0.635
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2340
_diffrn_reflns_point_group_measured_fraction_full 0.792
_diffrn_reflns_point_group_measured_fraction_max 0.608
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         22.444
_diffrn_reflns_theta_min         2.635
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.834
_diffrn_measured_fraction_theta_max 0.635
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 -24.23  280
  2  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 155.77  280
  3  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 155.77  155
  4  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 -24.23  155
  5  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00  24.23  330
  6  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00-155.77  200
  7  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00  24.23  200
  8  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00-155.77  330
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0224529000
_diffrn_orient_matrix_UB_12      -0.0465322000
_diffrn_orient_matrix_UB_13      -0.0211758000
_diffrn_orient_matrix_UB_21      0.0509169000
_diffrn_orient_matrix_UB_22      0.0204424000
_diffrn_orient_matrix_UB_23      -0.0164778000
_diffrn_orient_matrix_UB_31      0.0152996000
_diffrn_orient_matrix_UB_32      -0.0273119000
_diffrn_orient_matrix_UB_33      0.0237039000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_special_details          synchrotron
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.750
_reflns_Friedel_fraction_max     0.581
_reflns_number_gt                699
_reflns_number_total             1233
_reflns_odcompleteness_completeness 81.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     17.68
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.024
_refine_diff_density_min         -1.652
_refine_diff_density_rms         0.530
_refine_ls_abs_structure_details 
;
 Flack x determined using 210 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(8)
_refine_ls_extinction_coef       0.034(11)
_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   1.073
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         1233
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1616
_refine_ls_R_factor_gt           0.1113
_refine_ls_restrained_S_all      1.073
_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)+(0.1649P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2922
_refine_ls_wR_factor_ref         0.3367
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(N4) = Uanis(C3) = Uanis(C2) = Uanis(N0AA) = Uanis(C19)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.2113(3) 0.3549(3) 0.41021(2) 0.0638(12) Uani 1 1 d . . . . .
N1 N 0.333333 0.666667 0.233(5) 0.075(17) Uani 1 3 d S T P . .
N0AA N 0.666667 0.333333 0.455(5) 0.068(5) Uani 1 3 d S T P . .
C2 C 0.678(6) 0.480(6) 0.418(4) 0.068(5) Uani 1 1 d . . . . .
C3 C 0.704(6) 0.488(6) 0.319(3) 0.068(5) Uani 1 1 d . . . . .
N4 N 0.666667 0.333333 0.272(5) 0.068(5) Uani 1 3 d S T P . .
C19 C 0.666667 0.333333 0.572(6) 0.068(5) Uani 1 3 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 0.0613(17) 0.0587(16) 0.0747(18) 0.0039(12) 0.0075(12) 0.0323(12)
N1 0.09(3) 0.09(3) 0.04(3) 0.000 0.000 0.045(15)
N0AA 0.066(8) 0.066(8) 0.070(12) 0.000 0.000 0.033(4)
C2 0.066(8) 0.066(8) 0.070(12) 0.000 0.000 0.033(4)
C3 0.066(8) 0.066(8) 0.070(12) 0.000 0.000 0.033(4)
N4 0.066(8) 0.066(8) 0.070(12) 0.000 0.000 0.033(4)
C19 0.066(8) 0.066(8) 0.070(12) 0.000 0.000 0.033(4)

_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
N0AA C2 1.46(6) 3_665 ?
N0AA C2 1.46(6) 2_655 ?
N0AA C2 1.46(6) . ?
N0AA C19 1.60(12) . ?
C2 C3 1.37(7) . ?
C3 N4 1.50(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N0AA C2 109(3) 3_665 2_655 ?
C2 N0AA C2 109(3) 3_665 . ?
C2 N0AA C2 109(3) 2_655 . ?
C2 N0AA C19 110(3) 3_665 . ?
C2 N0AA C19 110(3) 2_655 . ?
C2 N0AA C19 110(3) . . ?
C3 C2 N0AA 108(5) . . ?
C2 C3 N4 115(5) . . ?
C3 N4 C3 103(4) 2_655 . ?
C3 N4 C3 103(4) 3_665 . ?
C3 N4 C3 103(4) 3_665 2_655 ?

_iucr_refine_instructions_details 
;
TITL MDBACHONH4I3_ in R3 #146
    mdbachonh4i3_.res
    created by SHELXL-2016/6 at 12:14:24 on 13-Nov-2018
REM reset to R3 #146
CELL 0.4859 9.726672 9.726672 13.569202 90 90 120
ZERR 5.00004 0.001572 0.001572 0.002984 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C I N
DISP C 0.0007 0.0007 6.0677
DISP I -1.1694 0.9355 2837.686
DISP N 0.0018 0.0014 8.9832
UNIT 21 9 9
EADP N4 C3 C2 N0AA C19

L.S. 10
PLAN  20
SIZE 0.05 0.14 0.8
TEMP 26.85
LIST 5
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\MDBACHONH4I3_.hkl">
REM </olex2.extras>

WGHT    0.164900
EXTI    0.034387
FVAR       0.90886
I1    2    0.211290    0.354939    0.410210    11.00000    0.06128    0.05867 =
         0.07468    0.00390    0.00749    0.03232
N1    3    0.333333    0.666667    0.232530    10.33333    0.09069    0.09069 =
         0.04341    0.00000    0.00000    0.04534
N0AA  3    0.666667    0.333333    0.454551    10.33333    0.06626    0.06626 =
         0.07047    0.00000    0.00000    0.03313
C2    1    0.678384    0.480309    0.418395    11.00000    0.06626    0.06626 =
         0.07047    0.00000    0.00000    0.03313
C3    1    0.703822    0.488074    0.318807    11.00000    0.06626    0.06626 =
         0.07047    0.00000    0.00000    0.03313
N4    3    0.666667    0.333333    0.271616    10.33333    0.06626    0.06626 =
         0.07047    0.00000    0.00000    0.03313
C19   1    0.666667    0.333333    0.572293    10.33333    0.06626    0.06626 =
         0.07047    0.00000    0.00000    0.03313
HKLF 4




REM  MDBACHONH4I3_ in R3 #146
REM R1 =  0.1113 for     699 Fo > 4sig(Fo)  and  0.1616 for all    1233 data
REM     25 parameters refined using      1 restraints

END  
     
WGHT      0.1650      0.0000 

REM Highest difference peak  2.024,  deepest hole -1.652,  1-sigma level  0.530
Q1    1   0.3359  0.4252  0.3854  11.00000  0.05    1.64
Q2    1   0.1392  0.2285  0.3867  11.00000  0.05    1.56
Q3    1   0.8194  0.6553  0.2640  11.00000  0.05    1.52
Q4    1   0.2276  0.3258  0.3235  11.00000  0.05    1.41
Q5    1   0.0650  0.2892  0.4222  11.00000  0.05    1.41
Q6    1   0.2659  0.4914  0.4327  11.00000  0.05    1.37
Q7    1   0.2592  0.3333  0.4918  11.00000  0.05    1.32
Q8    1   0.2722  0.2957  0.4351  11.00000  0.05    1.31
Q9    1   0.3062  0.4191  0.3329  11.00000  0.05    1.30
Q10   1   0.2451  0.4570  0.4899  11.00000  0.05    1.26
Q11   1   0.6718  0.3999  0.4060  11.00000  0.05    1.23
Q12   1   0.8633  0.4407  0.2092  11.00000  0.05    1.22
Q13   1   0.7569  0.5275  0.4372  11.00000  0.05    1.22
Q14   1   0.6667  0.3333  0.3785  10.33333  0.05    1.21
Q15   1   0.1507  0.4144  0.3684  11.00000  0.05    1.11
Q16   1   0.3333  0.6667  0.3318  10.33333  0.05    1.07
Q17   1   0.6200  0.4558  0.3124  11.00000  0.05    1.04
Q18   1   0.3232  0.4234  0.2511  11.00000  0.05    1.00
Q19   1   0.7496  0.5303  0.5153  11.00000  0.05    0.97
Q20   1   0.7250  0.4552  0.6023  11.00000  0.05    0.96

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.1113 for 699 Fo > 4sig(Fo) and 0.1616 for all 2340 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 2.02, deepest hole -1.65
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.1616
  REM R1_gt = 0.1113
  REM wR_ref = 0.3367
  REM GOOF = 1.073
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2340
  REM Reflections_gt = 699
  REM Parameters = n/a
  REM Hole = -1.65
  REM Peak = 2.02
  REM Flack = -0.2(8)

  
;
_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 4.722
_oxdiff_exptl_absorpt_empirical_full_min 0.280
####################################################################### 
# 
# 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_dabconh5i3_
_database_code_depnum_ccdc_archive 'CCDC 1892558'
loop_
_audit_author_name
_audit_author_address
'Gregor Kieslich'
;TU Munich
Germany
;
_audit_update_record             
;
2019-01-21 deposited with the CCDC.	2019-03-04 downloaded from the CCDC.
;
_audit_creation_date             2018-11-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        MDABCONH4I3
_chemical_formula_moiety         '1.8(I), 0.6(N), 0.2(C21 N6)'
_chemical_formula_sum            'C4.20 I1.80 N1.80'
_chemical_formula_weight         304.08
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C7N3I3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -1.1694 0.9355 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0018 0.0014 '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           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   9.5718(15)
_cell_length_b                   9.5718(15)
_cell_length_c                   13.380(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1061.6(4)
_cell_formula_units_Z            5.00004
_cell_measurement_reflns_used    522
_cell_measurement_temperature    300
_cell_measurement_theta_max      16.3910
_cell_measurement_theta_min      2.6570
_shelx_estimated_absorpt_T_max   0.888
_shelx_estimated_absorpt_T_min   0.247
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.378
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             666
_exptl_crystal_preparation       'cut from plate like crystal'
_exptl_crystal_recrystallization_method 'see supporting information'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_unetI/netI     0.2016
_diffrn_reflns_Laue_measured_fraction_full 0.836
_diffrn_reflns_Laue_measured_fraction_max 0.612
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2233
_diffrn_reflns_point_group_measured_fraction_full 0.787
_diffrn_reflns_point_group_measured_fraction_max 0.583
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         22.818
_diffrn_reflns_theta_min         2.675
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.836
_diffrn_measured_fraction_theta_max 0.612
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 -24.23  280
  2  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 155.77  280
  3  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 155.77  155
  4  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 -24.23  155
  5  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00  24.23  330
  6  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00-155.77  200
  7  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00  24.23  200
  8  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00-155.77  330
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0471470000
_diffrn_orient_matrix_UB_12      -0.0228539000
_diffrn_orient_matrix_UB_13      0.0215690000
_diffrn_orient_matrix_UB_21      0.0206366000
_diffrn_orient_matrix_UB_22      0.0517142000
_diffrn_orient_matrix_UB_23      0.0167301000
_diffrn_orient_matrix_UB_31      -0.0279551000
_diffrn_orient_matrix_UB_32      0.0153933000
_diffrn_orient_matrix_UB_33      -0.0239992000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_source                   synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_special_details          synchrotron
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.737
_reflns_Friedel_fraction_max     0.554
_reflns_number_gt                570
_reflns_number_total             1180
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.436
_refine_diff_density_min         -1.784
_refine_diff_density_rms         0.572
_refine_ls_abs_structure_details 
;
 Flack x determined using 151 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_coef       0.050(18)
_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   1.068
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         1180
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2050
_refine_ls_R_factor_gt           0.1391
_refine_ls_restrained_S_all      1.068
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3412
_refine_ls_wR_factor_ref         0.4089
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(C16) = Uanis(N3) = Uanis(C4) = Uanis(C5) = Uanis(N2)
2. Others
 Fixed X: C16(0.66667)
 Fixed Y: C16(0.33333)
 Fixed Z: C16(0.51533)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.1883(4) 0.3088(4) 0.664(8) 0.0711(18) Uani 1 1 d . . . . .
N1 N 0.000000 0.000000 0.857(9) 0.046(12) Uani 1 3 d S T P . .
N2 N 0.000000 0.000000 0.459(10) 0.071(7) Uani 1 3 d S T P . .
N3 N 0.666667 0.333333 0.620(11) 0.071(7) Uani 1 3 d S T P . .
C4 C 0.656(7) 0.466(7) 0.651(9) 0.071(7) Uani 1 1 d . . . . .
C5 C -0.031(7) 0.121(7) 0.422(9) 0.071(7) Uani 1 1 d . . . . .
C16 C 0.666670 0.333330 0.515330 0.071(7) Uani 1 3 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 0.061(2) 0.063(2) 0.086(3) 0.0070(18) -0.0001(16) 0.0284(19)
N1 0.05(2) 0.05(2) 0.03(3) 0.000 0.000 0.027(10)
N2 0.061(10) 0.061(10) 0.092(19) 0.000 0.000 0.030(5)
N3 0.061(10) 0.061(10) 0.092(19) 0.000 0.000 0.030(5)
C4 0.061(10) 0.061(10) 0.092(19) 0.000 0.000 0.030(5)
C5 0.061(10) 0.061(10) 0.092(19) 0.000 0.000 0.030(5)
C16 0.061(10) 0.061(10) 0.092(19) 0.000 0.000 0.030(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
N2 C5 1.42(7) . ?
N2 C5 1.42(7) 2 ?
N2 C5 1.42(7) 3 ?
N3 C4 1.39(7) 2_655 ?
N3 C4 1.39(7) . ?
N3 C4 1.39(7) 3_665 ?
N3 C16 1.40(15) . ?
C4 C5 1.40(10) 4 ?

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
C5 N2 C5 108(5) . 2 ?
C5 N2 C5 108(5) . 3 ?
C5 N2 C5 108(5) 2 3 ?
C4 N3 C4 111(4) 3_665 2_655 ?
C4 N3 C4 111(4) 3_665 . ?
C4 N3 C4 111(4) 2_655 . ?
C4 N3 C16 107(5) 3_665 . ?
C4 N3 C16 107(5) 2_655 . ?
C4 N3 C16 107(5) . . ?
N3 C4 C5 107(6) . 4 ?
C4 C5 N2 110(6) 7_444 . ?

_iucr_refine_instructions_details 
;
TITL DABCONH5I3_ in R3 #146
    dabconh5i3_.res
    created by SHELXL-2016/6 at 09:25:46 on 15-Nov-2018
REM reset to R3 #146
CELL 0.4859 9.571837 9.571837 13.379994 90 90 120
ZERR 5.00004 0.001529 0.001529 0.002785 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C I N
DISP C 0.0007 0.0007 6.0677
DISP I -1.1694 0.9355 2837.686
DISP N 0.0018 0.0014 8.9832
UNIT 21 9 9
EADP C16 N3 C4 C5 N2

L.S. 40 0 0
PLAN  20
SIZE 0.05 0.14 0.8
TEMP 26.85
LIST 5
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\DABCONH5I3_.hkl">
REM </olex2.extras>

WGHT    0.200000
EXTI    0.049505
FVAR       0.93774
I1    2    0.188288    0.308778    0.663902    11.00000    0.06075    0.06301 =
         0.08622    0.00701   -0.00009    0.02845
N1    3    0.000000    0.000000    0.857116    10.33333    0.05392    0.05392 =
         0.03075    0.00000    0.00000    0.02696
N2    3    0.000000    0.000000    0.459470    10.33333    0.06097    0.06097 =
         0.09176    0.00000    0.00000    0.03049
N3    3    0.666667    0.333333    0.620045    10.33333    0.06097    0.06097 =
         0.09176    0.00000    0.00000    0.03049
C4    1    0.655672    0.466374    0.651129    11.00000    0.06097    0.06097 =
         0.09176    0.00000    0.00000    0.03049
C5    1   -0.030946    0.120922    0.421999    11.00000    0.06097    0.06097 =
         0.09176    0.00000    0.00000    0.03049
C16   1   10.666670   10.333330   10.515330    10.33333    0.06097    0.06097 =
         0.09176    0.00000    0.00000    0.03049
HKLF 4




REM  DABCONH5I3_ in R3 #146
REM R1 =  0.1391 for     570 Fo > 4sig(Fo)  and  0.2050 for all    1180 data
REM     24 parameters refined using      0 restraints

END  
     
WGHT      0.2000      0.0000 

REM Highest difference peak  2.436,  deepest hole -1.784,  1-sigma level  0.572
Q1    1   0.0000  0.0000  0.8055  10.33333  0.05    2.44
Q2    1  -0.1441  0.1799  0.5245  11.00000  0.05    1.64
Q3    1   0.2052  0.3117  0.7491  11.00000  0.05    1.61
Q4    1   0.0288  0.2404  0.6488  11.00000  0.05    1.55
Q5    1   0.1183  0.4002  0.6717  11.00000  0.05    1.52
Q6    1   0.1986  0.3029  0.5789  11.00000  0.05    1.52
Q7    1  -0.1577  0.1440  0.4648  11.00000  0.05    1.49
Q8    1   0.5719  0.4295  0.6229  11.00000  0.05    1.41
Q9    1   0.7533  0.4265  0.6469  11.00000  0.05    1.40
Q10   1   0.2963  0.3691  0.6045  11.00000  0.05    1.34
Q11   1   0.2476  0.2326  0.6986  11.00000  0.05    1.32
Q12   1   0.0958  0.1670  0.6266  11.00000  0.05    1.25
Q13   1   0.2322  0.2549  0.7402  11.00000  0.05    1.25
Q14   1   0.2513  0.4258  0.7046  11.00000  0.05    1.22
Q15   1   0.5997  0.4383  0.4952  11.00000  0.05    1.21
Q16   1  -0.1279 -0.0118  0.3664  11.00000  0.05    1.19
Q17   1   0.0691  0.1592  0.4586  11.00000  0.05    1.08
Q18   1   0.6667  0.3333  0.6900  10.33333  0.05    1.08
Q19   1  -0.0364  0.2470  0.7392  11.00000  0.05    1.06
Q20   1   0.6717  0.3859  0.6825  11.00000  0.05    1.03

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.1391 for 570 Fo > 4sig(Fo) and 0.2050 for all 2233 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 2.44, deepest hole -1.78
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.2050
  REM R1_gt = 0.1391
  REM wR_ref = 0.4089
  REM GOOF = 1.068
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2233
  REM Reflections_gt = 570
  REM Parameters = n/a
  REM Hole = -1.78
  REM Peak = 2.44
  REM Flack = -0.2(10)

  
;
_olex2_submission_original_sample_id MDABCNH4I3
_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 2.829
_oxdiff_exptl_absorpt_empirical_full_min 0.442
####################################################################### 
# 
# 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_mdabconh4i3_final
_database_code_depnum_ccdc_archive 'CCDC 1892557'
loop_
_audit_author_name
_audit_author_address
'Gregor Kieslich'
;TU Munich
Germany
;
_audit_update_record             
;
2019-01-21 deposited with the CCDC.	2019-03-04 downloaded from the CCDC.
;
_audit_creation_date             2018-10-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        MDABCONH4I3
_chemical_formula_moiety         '3(I), 1(N), 1(C7 N2)'
_chemical_formula_sum            'C7 I3 N3'
_chemical_formula_weight         506.80
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C7 N3 I3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -1.1694 0.9355 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0018 0.0014 '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           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   9.8206(5)
_cell_length_b                   9.8206(5)
_cell_length_c                   13.6904(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1143.47(12)
_cell_formula_units_Z            2.99997
_cell_measurement_reflns_used    2484
_cell_measurement_temperature    300
_cell_measurement_theta_max      22.4600
_cell_measurement_theta_min      2.5970
_shelx_estimated_absorpt_T_max   0.896
_shelx_estimated_absorpt_T_min   0.266
_exptl_absorpt_coefficient_mu    2.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             666
_exptl_crystal_preparation       'cut from plate like crystal'
_exptl_crystal_recrystallization_method 'see supporting information'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3003
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         22.524
_diffrn_reflns_theta_min         2.611
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 -24.23  280
  2  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 155.77  280
  3  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 155.77  155
  4  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 -24.23  155
  5  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00  24.23  330
  6  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00-155.77  200
  7  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00  24.23  200
  8  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00-155.77  330
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0193838000
_diffrn_orient_matrix_UB_12      0.0548602000
_diffrn_orient_matrix_UB_13      0.0080531000
_diffrn_orient_matrix_UB_21      -0.0057415000
_diffrn_orient_matrix_UB_22      0.0106670000
_diffrn_orient_matrix_UB_23      -0.0339549000
_diffrn_orient_matrix_UB_31      -0.0534529000
_diffrn_orient_matrix_UB_32      -0.0117844000
_diffrn_orient_matrix_UB_33      0.0065631000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_source                   synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_special_details          synchrotron
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.889
_reflns_number_gt                1618
_reflns_number_total             1655
_reflns_odcompleteness_completeness 95.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     17.68
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.274
_refine_ls_abs_structure_details 
;
 Flack x determined using 659 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1655
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0455
_refine_ls_restrained_S_all      1.047
_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)+(0.0712P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1176
_refine_special_details          synchrotron
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.600(4)
 0.400(4)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.45556(11) 0.47628(11) 0.33572(2) 0.04788(19) Uani 1 1 d . . . . .
N1 N 0.333333 0.666667 0.5159(12) 0.041(3) Uani 1 3 d S T P . .
C2 C 0.6553(16) 0.4709(16) 0.6613(12) 0.045(2) Uani 1 1 d . . . . .
N3 N 0.666667 0.333333 0.6251(12) 0.039(3) Uani 1 3 d S T P . .
C4 C 0.624(2) 0.452(2) 0.7707(12) 0.058(4) Uani 1 1 d . . . . .
N0AA N 0.666667 0.333333 0.8068(15) 0.058(5) Uani 1 3 d S T P . .
C1 C 0.666667 0.333333 0.513(2) 0.089(12) Uani 1 3 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 0.0486(4) 0.0451(4) 0.0509(3) 0.0027(3) 0.0049(3) 0.0242(5)
N1 0.040(5) 0.040(5) 0.042(8) 0.000 0.000 0.020(2)
C2 0.046(5) 0.037(5) 0.062(7) 0.004(5) -0.002(5) 0.027(4)
N3 0.040(5) 0.040(5) 0.037(7) 0.000 0.000 0.020(2)
C4 0.064(9) 0.061(8) 0.055(7) -0.024(6) 0.002(6) 0.034(8)
N0AA 0.070(8) 0.070(8) 0.034(8) 0.000 0.000 0.035(4)
C1 0.12(2) 0.12(2) 0.028(10) 0.000 0.000 0.060(10)

_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
C2 N3 1.494(15) . ?
C2 C4 1.52(2) . ?
N3 C1 1.53(3) . ?
C4 N0AA 1.51(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C2 C4 108.6(12) . . ?
C2 N3 C2 109.6(9) 3_665 . ?
C2 N3 C2 109.6(9) 2_655 . ?
C2 N3 C2 109.6(9) 3_665 2_655 ?
C2 N3 C1 109.4(9) 3_665 . ?
C2 N3 C1 109.3(9) . . ?
C2 N3 C1 109.4(9) 2_655 . ?
N0AA C4 C2 107.4(12) . . ?
C4 N0AA C4 109.8(9) 2_655 . ?
C4 N0AA C4 109.8(9) 3_665 2_655 ?
C4 N0AA C4 109.8(9) 3_665 . ?

_iucr_refine_instructions_details 
;
TITL MDABCONH4I3_final in R3 #146
    mdabconh4i3_final.res
    created by SHELXL-2016/6 at 20:39:17 on 06-Oct-2018
REM reset to R3 #146
CELL 0.4859 9.820625 9.820625 13.690428 90 90 120
ZERR 2.99997 0.00046 0.00046 0.000719 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C I N
DISP C 0.0007 0.0007 6.0677
DISP I -1.1694 0.9355 2837.686
DISP N 0.0018 0.0014 8.9832
UNIT 21 9 9

L.S. 10
PLAN  20
SIZE 0.05 0.14 0.8
TEMP 26.85
fmap 2
ACTA
TWIN 0 1 0 1 0 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\MDABCONH4I3_final.hkl">
REM </olex2.extras>

WGHT    0.071200
BASF   0.39961
FVAR       2.37254
I1    2    0.455562    0.476284    0.335720    11.00000    0.04865    0.04506 =
         0.05091    0.00269    0.00490    0.02417
N1    3    0.333333    0.666667    0.515899    10.33333    0.04032    0.04032 =
         0.04212    0.00000    0.00000    0.02016
C2    1    0.655280    0.470850    0.661287    11.00000    0.04632    0.03666 =
         0.06231    0.00416   -0.00168    0.02747
N3    3    0.666667    0.333333    0.625128    10.33333    0.04029    0.04029 =
         0.03679    0.00000    0.00000    0.02015
C4    1    0.623820    0.451995    0.770678    11.00000    0.06353    0.06093 =
         0.05523   -0.02387    0.00175    0.03427
N0AA  3    0.666667    0.333333    0.806764    10.33333    0.06953    0.06953 =
         0.03390    0.00000    0.00000    0.03476
C1    1    0.666667    0.333333    0.513150    10.33333    0.11985    0.11985 =
         0.02823    0.00000    0.00000    0.05993
HKLF 4




REM  MDABCONH4I3_final in R3 #146
REM R1 =  0.0455 for    1618 Fo > 4sig(Fo)  and  0.0460 for all    1655 data
REM     41 parameters refined using      1 restraints

END  
     
WGHT      0.0712      0.0000 

REM Highest difference peak  1.498,  deepest hole -0.949,  1-sigma level  0.274
Q1    1   0.4900  0.4609  0.3702  11.00000  0.05    1.50
Q2    1   0.5035  0.4756  0.3070  11.00000  0.05    1.09
Q3    1   0.6704  0.2686  0.6315  11.00000  0.05    0.85
Q4    1   0.6667  0.3333  0.9271  10.33333  0.05    0.71
Q5    1   0.6667  0.3333  0.3997  10.33333  0.05    0.70
Q6    1   0.5420  0.4705  0.5735  11.00000  0.05    0.68
Q7    1   0.5973  0.5687  0.8358  11.00000  0.05    0.64
Q8    1   0.8253  0.2814  0.5018  11.00000  0.05    0.62
Q9    1   0.5640  0.5141  0.6135  11.00000  0.05    0.61
Q10   1   0.5417  0.4188  0.8381  11.00000  0.05    0.60
Q11   1   0.5029  0.5182  0.5996  11.00000  0.05    0.59
Q12   1   0.3546  0.7864  0.4948  11.00000  0.05    0.59
Q13   1   0.6628  0.5790  0.8152  11.00000  0.05    0.58
Q14   1   0.5083  0.5374  0.8225  11.00000  0.05    0.58
Q15   1   0.6667  0.3333  0.4473  10.33333  0.05    0.56
Q16   1   0.8159  0.6738  0.7536  11.00000  0.05    0.56
Q17   1   0.4716  0.5445  0.3825  11.00000  0.05    0.55
Q18   1   0.6112  0.5644  0.5525  11.00000  0.05    0.55
Q19   1   0.6141  0.6059  0.5912  11.00000  0.05    0.55
Q20   1   0.4268  0.5182  0.2877  11.00000  0.05    0.55

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0455 for 1618 Fo > 4sig(Fo) and 0.0460 for all 3003 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.50, deepest hole -0.95
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0460
  REM R1_gt = 0.0455
  REM wR_ref = 0.1176
  REM GOOF = 1.047
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3003
  REM Reflections_gt = 1618
  REM Parameters = n/a
  REM Hole = -0.95
  REM Peak = 1.50
  REM Flack = -0.1(2)

  
;
_olex2_exptl_crystal_mounting_method 'Diamond Anvil Cell experiment'
_olex2_submission_original_sample_id MDABCONH4I3
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.565
_oxdiff_exptl_absorpt_empirical_full_min 0.736
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.600(4)
2 0.400(4)

####################################################################### 
# 
# 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_dabco_i_
_database_code_depnum_ccdc_archive 'CCDC 1892556'
loop_
_audit_author_name
_audit_author_address
'Gregor Kieslich'
;TU Munich
Germany
;
_audit_update_record             
;
2019-01-21 deposited with the CCDC.	2019-03-04 downloaded from the CCDC.
;
_audit_creation_date             2018-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        MDABCONH4I3
_chemical_formula_moiety         '3(I), 1(N), 0.33(C21 N6)'
_chemical_formula_sum            'C7 I3 N3'
_chemical_formula_weight         506.79
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C7N3I3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -1.1694 0.9355 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0018 0.0014 '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           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   9.6748(14)
_cell_length_b                   9.6748(14)
_cell_length_c                   13.517(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1095.7(4)
_cell_formula_units_Z            3.00004
_cell_measurement_reflns_used    592
_cell_measurement_temperature    300
_cell_measurement_theta_max      16.6510
_cell_measurement_theta_min      2.6320
_shelx_estimated_absorpt_T_max   0.892
_shelx_estimated_absorpt_T_min   0.255
_exptl_absorpt_coefficient_mu    2.350
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             666
_exptl_crystal_preparation       'cut from plate like crystal'
_exptl_crystal_recrystallization_method 'see supporting information'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.1921
_diffrn_reflns_Laue_measured_fraction_full 0.833
_diffrn_reflns_Laue_measured_fraction_max 0.632
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2297
_diffrn_reflns_point_group_measured_fraction_full 0.784
_diffrn_reflns_point_group_measured_fraction_max 0.603
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         22.564
_diffrn_reflns_theta_min         1.955
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.833
_diffrn_measured_fraction_theta_max 0.6028
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 -24.23  280
  2  ω   -150.00 -94.00   0.20    0.20    --  -20.00  70.00 155.77  280
  3  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 155.77  155
  4  ω   -105.00 -74.00   0.20    0.20    --   20.00  70.00 -24.23  155
  5  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00  24.23  330
  6  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00-155.77  200
  7  ω   -106.00 -66.00   0.20    0.20    --  -20.00 -70.00  24.23  200
  8  ω    -96.00 -30.00   0.20    0.20    --   20.00 -70.00-155.77  330
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0225769000
_diffrn_orient_matrix_UB_12      -0.0467308000
_diffrn_orient_matrix_UB_13      -0.0212909000
_diffrn_orient_matrix_UB_21      0.0511706000
_diffrn_orient_matrix_UB_22      0.0204502000
_diffrn_orient_matrix_UB_23      -0.0165159000
_diffrn_orient_matrix_UB_31      0.0152838000
_diffrn_orient_matrix_UB_32      -0.0275594000
_diffrn_orient_matrix_UB_33      0.0238138000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_source                   synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_special_details          synchrotron
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.735
_reflns_Friedel_fraction_max     0.573
_reflns_number_gt                649
_reflns_number_total             1220
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.139
_refine_diff_density_min         -1.922
_refine_diff_density_rms         0.551
_refine_ls_abs_structure_details 
;
 Flack x determined using 173 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.7(6)
_refine_ls_extinction_coef       0.030(10)
_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   0.999
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         1220
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1659
_refine_ls_R_factor_gt           0.1149
_refine_ls_restrained_S_all      0.999
_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)+(0.1678P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2889
_refine_ls_wR_factor_ref         0.3383
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(N0AA) = Uanis(C2) = Uanis(C4) = Uanis(N3)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I2 I 0.4775(3) 0.4552(3) 0.37883(2) 0.0646(12) Uani 1 1 d . . . . .
N1 N 0.333333 0.666667 0.531(3) 0.048(11) Uani 1 3 d S T P . .
N0AA N 0.333333 0.666667 0.089(5) 0.068(6) Uani 1 3 d S T P . .
C2 C 0.676(6) 0.482(7) 0.724(3) 0.068(6) Uani 1 1 d . . . . .
N3 N 0.666667 0.333333 0.574(5) 0.068(6) Uani 1 3 d S T P . .
C4 C 0.697(6) 0.482(6) 0.615(3) 0.068(6) Uani 1 1 d . . . . .
C9 C 0.333333 0.666667 0.206(5) 0.068(6) Uani 1 3 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
I2 0.0544(17) 0.0596(17) 0.0787(18) -0.0081(12) -0.0044(12) 0.0278(13)
N1 0.06(2) 0.06(2) 0.015(18) 0.000 0.000 0.032(10)
N0AA 0.075(10) 0.075(10) 0.053(12) 0.000 0.000 0.038(5)
C2 0.075(10) 0.075(10) 0.053(12) 0.000 0.000 0.038(5)
N3 0.075(10) 0.075(10) 0.053(12) 0.000 0.000 0.038(5)
C4 0.075(10) 0.075(10) 0.053(12) 0.000 0.000 0.038(5)
C9 0.075(10) 0.075(10) 0.053(12) 0.000 0.000 0.038(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
N0AA C2 1.46(6) 4_454 ?
N0AA C2 1.46(6) 6_564 ?
N0AA C2 1.46(6) 5_554 ?
N0AA C9 1.57(11) . ?
C2 C4 1.49(6) . ?
N3 C4 1.43(6) 3_665 ?
N3 C4 1.43(6) 2_655 ?
N3 C4 1.43(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N0AA C2 112(3) 4_454 5_554 ?
C2 N0AA C2 112(3) 4_454 6_564 ?
C2 N0AA C2 112(3) 5_554 6_564 ?
C2 N0AA C9 107(3) 4_454 . ?
C2 N0AA C9 107(3) 5_554 . ?
C2 N0AA C9 107(3) 6_564 . ?
N0AA C2 C4 104(5) 7_545 . ?
C4 N3 C4 106(3) 3_665 2_655 ?
C4 N3 C4 106(3) 3_665 . ?
C4 N3 C4 106(3) 2_655 . ?
N3 C4 C2 115(5) . . ?

_iucr_refine_instructions_details 
;
TITL DABCO_I_ in R3 #146
    dabco_i_.res
    created by SHELXL-2016/6 at 14:58:07 on 14-Nov-2018
REM reset to R3 #146
CELL 0.4859 9.674831 9.674831 13.516658 90 90 120
ZERR 3.00004 0.0014 0.0014 0.002688 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C I N
DISP C 0.0007 0.0007 6.0677
DISP I -1.1694 0.9355 2837.686
DISP N 0.0018 0.0014 8.9832
UNIT 21 9 9
EADP C9 N0AA C2 C4 N3

L.S. 50
PLAN  20
SIZE 0.05 0.14 0.8
TEMP 26.85
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\DABCO_I_.hkl">
REM </olex2.extras>

WGHT    0.167800
EXTI    0.029552
FVAR       0.91529
I2    2    0.477536    0.455166    0.378830    11.00000    0.05443    0.05965 =
         0.07869   -0.00811   -0.00436    0.02784
N1    3    0.333333    0.666667    0.531045    10.33333    0.06454    0.06454 =
         0.01538    0.00000    0.00000    0.03227
N0AA  3    0.333333    0.666667    0.089395    10.33333    0.07512    0.07512 =
         0.05252    0.00000    0.00000    0.03756
C2    1    0.676433    0.482158    0.724034    11.00000    0.07512    0.07512 =
         0.05252    0.00000    0.00000    0.03756
N3    3    0.666667    0.333333    0.574070    10.33333    0.07512    0.07512 =
         0.05252    0.00000    0.00000    0.03756
C4    1    0.696843    0.481758    0.614916    11.00000    0.07512    0.07512 =
         0.05252    0.00000    0.00000    0.03756
C9    1    0.333333    0.666667    0.205665    10.33333    0.07512    0.07512 =
         0.05252    0.00000    0.00000    0.03756
HKLF 4




REM  DABCO_I_ in R3 #146
REM R1 =  0.1149 for     649 Fo > 4sig(Fo)  and  0.1659 for all    1220 data
REM     25 parameters refined using      1 restraints

END  
     
WGHT      0.1667      0.0000 

REM Highest difference peak  2.139,  deepest hole -1.922,  1-sigma level  0.551
Q1    1   0.8122  0.6446  0.5680  11.00000  0.05    1.82
Q2    1   0.4531  0.3686  0.2985  11.00000  0.05    1.41
Q3    1   0.4483  0.4433  0.2883  11.00000  0.05    1.41
Q4    1   0.7425  0.5136  0.7643  11.00000  0.05    1.37
Q5    1   0.3565  0.3915  0.4016  11.00000  0.05    1.35
Q6    1   0.4170  0.3271  0.3538  11.00000  0.05    1.34
Q7    1   0.6198  0.5383  0.3579  11.00000  0.05    1.29
Q8    1   0.5597  0.4001  0.4008  11.00000  0.05    1.28
Q9    1   0.4023  0.5140  0.3601  11.00000  0.05    1.28
Q10   1   0.4088  0.4289  0.4606  11.00000  0.05    1.25
Q11   1   0.8173  0.6978  0.5178  11.00000  0.05    1.21
Q12   1   0.6838  0.4104  0.7083  11.00000  0.05    1.19
Q13   1   0.5353  0.5904  0.3920  11.00000  0.05    1.17
Q14   1   0.5651  0.4293  0.5398  11.00000  0.05    1.14
Q15   1   0.4076  0.5979  0.3161  11.00000  0.05    1.13
Q16   1   0.1968  0.6005  0.2280  11.00000  0.05    1.10
Q17   1   0.6158  0.4027  0.7205  11.00000  0.05    1.09
Q18   1   0.8965  0.7032  0.7837  11.00000  0.05    1.01
Q19   1   0.6282  0.5218  0.4213  11.00000  0.05    0.93
Q20   1   0.5976  0.4460  0.6113  11.00000  0.05    0.91

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.1149 for 649 Fo > 4sig(Fo) and 0.1659 for all 2297 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 2.14, deepest hole -1.92
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.1659
  REM R1_gt = 0.1149
  REM wR_ref = 0.3383
  REM GOOF = 0.999
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 2297
  REM Reflections_gt = 649
  REM Parameters = n/a
  REM Hole = -1.92
  REM Peak = 2.14
  REM Flack = -0.7(6)

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.219
_oxdiff_exptl_absorpt_empirical_full_min 0.295
