# Supplementary Information (SI) for Dalton Transactions.
# 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_sb01-05-tm3-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405946'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 N4 O6 Tm'
_chemical_formula_sum            'C36 H21 Br12 N4 O6 Tm'
_chemical_formula_weight         1733.42
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C36 O6 N4 Tm'
_chemical_oxdiff_usercomment     'clear block in oil at 100 K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -8.0393 4.1821 '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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.09160(10)
_cell_length_b                   13.09160(10)
_cell_length_c                   46.0882(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6840.78(13)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    10086
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.9850
_cell_measurement_theta_min      4.3330
_shelx_estimated_absorpt_T_max   0.472
_shelx_estimated_absorpt_T_min   0.320
_exptl_absorpt_coefficient_mu    16.372
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4812
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -6 7 0.0245
2 6 -8 0.0283
5 -2 -24 0.0213
-4 6 22 0.0403
8 -2 -2 0.0291
-8 3 0 0.0370
1 -3 28 0.0272
-3 4 -27 0.0341
-5 7 -12 0.0356
7 -7 4 0.0184
3 -7 19 0.0210
-5 0 22 0.0284
-5 -3 -5 0.0298

_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.054
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.7452 -6.1358 6.7900 -0.1740 -0.7290 -0.6620
1.9829 5.8898 -8.0176 0.1657 0.6941 0.7005
4.8904 -1.8895 -24.3636 -0.0781 -0.3237 0.9429
-4.1809 5.5477 21.9281 0.1834 0.7644 -0.6181
8.2315 -2.3464 -1.9296 -0.7255 0.1744 0.6657
-8.2863 2.5104 0.3734 0.7604 -0.1827 -0.6232
0.9802 -2.9470 27.9804 -0.6268 0.1491 -0.7648
-3.2633 3.5115 -26.5329 0.8105 -0.1933 0.5529
-5.4562 7.4663 -12.4162 0.9007 0.3740 0.2211
7.2721 -7.2994 4.1256 -0.9121 -0.3784 0.1578
2.9609 -6.6109 18.7273 -0.7670 -0.3189 -0.5568
-5.1093 0.0043 21.5465 0.0767 0.0407 -0.9962
-5.2421 -3.0304 -5.2468 0.4109 -0.7548 -0.5113

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            27886
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.962
_diffrn_reflns_theta_min         4.346
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    105.00 165.00   0.50    0.05    --  113.25  45.00-180.00  120
  2  ω     93.00 140.00   0.50    0.05    --  113.25  77.00 -30.00   94
  3  ω    153.00 178.00   0.50    0.05    --  113.25  77.00 -30.00   50
  4  ω    120.00 178.00   0.50    0.05    --  113.25  45.00  30.00  116
  5  ω    120.00 178.00   0.50    0.05    --  113.25  45.00  60.00  116
  6  ω    110.00 158.00   0.50    0.05    --  113.25  77.00 120.00   96
  7  ω    102.00 165.00   0.50    0.05    --  113.25  15.00 -30.00  126
  8  ω    122.00 177.00   0.50    0.05    --  113.25  15.00 -60.00  110
  9  ω    143.00 177.00   0.50    0.05    --  113.25  45.00-120.00   68
 10  ω    109.00 166.00   0.50    0.05    --  113.25  30.00-150.00  114
 11  ω    111.00 137.00   0.50    0.05    --  113.25  45.00-120.00   52
 12  ω     42.00  68.00   0.50    0.05    --  113.25 -61.00  30.00   52
 13  ω     42.00  68.00   0.50    0.05    --  113.25 -61.00 -30.00   52
 14  ω     45.00  91.00   0.50    0.05    --  113.25 -77.00 -60.00   92
 15  ω     42.00  71.00   0.50    0.05    --  113.25 -61.00-120.00   58
 16  ω     42.00  67.00   0.50    0.05    --  113.25 -61.00-180.00   50
 17  ω     45.00  70.00   0.50    0.05    --  113.25 -61.00 -90.00   50
 18  ω     43.00  89.00   0.50    0.05    --  113.25 -77.00  30.00   92
 19  ω     52.00  89.00   0.50    0.05    --  113.25 -77.00  60.00   74
 20  ω     45.00  71.00   0.50    0.05    --  113.25 -61.00  60.00   52
 21  ω     46.00  71.00   0.50    0.05    --  113.25 -61.00  90.00   50
 22  ω     42.00  94.00   0.50    0.05    --  113.25 -77.00 150.00  104
 23  ω     40.00  84.00   0.50    0.05    --   47.51-125.00  30.00   88
 24  ω     82.00 111.00   0.50    0.05    --  113.25-125.00 150.00   58
 25  ω     47.00 109.00   0.50    0.05    --  113.25-125.00  60.00  124
 26  ω     45.00  76.00   0.50    0.05    --  113.25-125.00 150.00   62
 27  ω     60.00 108.00   0.50    0.05    --  113.25-111.00  51.90   96
 28  ω     84.00 110.00   0.50    0.05    --  113.25-125.00   0.00   52
 29  ω     47.00 107.00   0.50    0.05    --  113.25-106.00-117.51  120
 30  ω     78.00 103.00   0.50    0.05    --  113.25 -94.00 -90.00   50
 31  ω     44.00  74.00   0.50    0.05    --  113.25 -94.00 -90.00   60
 32  ω     73.00  98.00   0.50    0.05    --  113.25 -94.00-180.00   50
 33  ω     44.00  70.00   0.50    0.05    --  113.25-125.00-180.00   52
 34  ω     77.00 110.00   0.50    0.05    --  113.25-125.00-180.00   66
 35  ω     56.00 101.00   0.50    0.05    --  113.25 -94.00-120.00   90
 36  ω     67.00 103.00   0.50    0.05    --  113.25 -94.00 -60.00   72
 37  ω     79.00 106.00   0.50    0.05    --  113.25 -94.00  90.00   54
 38  ω    -66.00 -40.00   0.50    0.05    --  -47.51 -38.00   0.00   52
 39  ω   -117.00 -70.00   0.50    0.05    --  -47.51 -38.00   0.00   94
 40  ω    -30.00  25.00   0.50    0.05    --  -47.51  19.00 120.00  110
 41  ω    -26.00  25.00   0.50    0.05    --  -47.51  38.00-120.00  102
 42  ω    -27.00  22.00   0.50    0.05    --  -47.51  19.00-180.00   98
 43  ω    -30.00  19.00   0.50    0.05    --  -47.51  19.00  30.00   98
 44  ω    -70.00  16.00   0.50    0.05    --  -47.51  77.00 120.00  172
 45  ω    -54.00 -27.00   0.50    0.05    --  -91.75 125.00 120.00   54
 46  ω    -83.00 -56.00   0.50    0.05    --  -91.75 125.00 120.00   54
 47  ω    -68.00 -30.00   0.50    0.05    --  -91.75  61.00   0.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0821561000
_diffrn_orient_matrix_UB_12      0.0341014000
_diffrn_orient_matrix_UB_13      -0.0159302000
_diffrn_orient_matrix_UB_21      0.0589941000
_diffrn_orient_matrix_UB_22      0.1195751000
_diffrn_orient_matrix_UB_23      0.0158555000
_diffrn_orient_matrix_UB_31      0.0906699000
_diffrn_orient_matrix_UB_32      0.0547258000
_diffrn_orient_matrix_UB_33      -0.0247464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                3101
_reflns_number_total             3227
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details 
;
 Flack x determined using 1405 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3227
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0384
_refine_ls_restrained_S_all      1.151
_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)+(0.0582P)²+56.0877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1056
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
1.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.666667 0.333333 0.52433(2) 0.0156(2) Uani 1 3 d S T P . .
Br1 Br 0.50862(11) 0.54976(11) 0.52969(2) 0.0197(3) Uani 1 1 d . . . . .
Br4 Br 0.83169(10) 0.71457(11) 0.41184(2) 0.0211(3) Uani 1 1 d . . . . .
Br3 Br 0.75663(12) 0.89863(10) 0.44218(3) 0.0244(3) Uani 1 1 d . . . . .
Br2 Br 0.57902(12) 0.80777(11) 0.49965(3) 0.0244(3) Uani 1 1 d . . . . .
O2 O 0.7567(8) 0.5004(7) 0.44873(18) 0.0223(16) Uani 1 1 d . . . . .
H2 H 0.761967 0.459619 0.462100 0.034 Uiso 1 1 calc R U . . .
O1 O 0.6071(8) 0.4211(7) 0.49438(17) 0.0179(17) Uani 1 1 d . . . . .
C11 C 0.7443(10) 0.6745(10) 0.4466(3) 0.018(2) Uani 1 1 d . . . . .
C12 C 0.7137(10) 0.5676(9) 0.4596(3) 0.016(2) Uani 1 1 d . . . . .
C9 C 0.6333(10) 0.7110(10) 0.4831(2) 0.017(2) Uani 1 1 d . . . . .
N2 N 0.7785(9) 0.5300(10) 0.5450(2) 0.0212(19) Uani 1 1 d . . . . .
C3 C 0.7935(11) 0.6616(12) 0.5833(3) 0.026(3) Uani 1 1 d . . . . .
H3 H 0.772924 0.671561 0.602390 0.031 Uiso 1 1 calc R U . . .
C4 C 0.8673(11) 0.7588(12) 0.5665(3) 0.030(3) Uani 1 1 d . . . . .
H4 H 0.896621 0.836668 0.573636 0.036 Uiso 1 1 calc R U . . .
C10 C 0.7046(11) 0.7479(9) 0.4586(3) 0.018(2) Uani 1 1 d . . . . .
C5 C 0.8978(10) 0.7384(11) 0.5383(3) 0.026(3) Uani 1 1 d . . . . .
H5 H 0.948797 0.802525 0.526215 0.031 Uiso 1 1 calc R U . . .
C7 C 0.6384(10) 0.5280(10) 0.4840(2) 0.018(2) Uani 1 1 d . . . . .
C6 C 0.8527(12) 0.6254(12) 0.5291(3) 0.025(3) Uani 1 1 d . . . . .
H6 H 0.874582 0.612685 0.510425 0.030 Uiso 1 1 calc R U . . .
C8 C 0.6009(10) 0.6011(10) 0.4953(3) 0.017(2) Uani 1 1 d . . . . .
N1 N 0.666667 0.333333 0.5777(4) 0.024(3) Uani 1 3 d S T P . .
C2 C 0.7495(10) 0.5482(11) 0.5716(3) 0.023(2) Uani 1 1 d . . . . .
C1 C 0.6655(12) 0.4396(11) 0.5884(3) 0.028(2) Uani 1 1 d . . . . .
H1A H 0.687563 0.451516 0.609153 0.034 Uiso 1 1 calc R U . . .
H1B H 0.584651 0.427174 0.586637 0.034 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O1 2.174(7) 3_665 ?
Tm1 O1 2.174(7) . ?
Tm1 O1 2.174(7) 2_655 ?
Tm1 N2 2.432(10) 3_665 ?
Tm1 N2 2.432(10) 2_655 ?
Tm1 N2 2.432(11) . ?
Tm1 N1 2.458(19) . ?
Br1 C8 1.900(12) . ?
Br4 C11 1.885(12) . ?
Br3 C10 1.894(11) . ?
Br2 C9 1.895(12) . ?
O2 H2 0.8400 . ?
O2 C12 1.356(14) . ?
O1 C7 1.336(14) . ?
C11 C12 1.385(16) . ?
C11 C10 1.413(16) . ?
C12 C7 1.409(12) . ?
C9 C10 1.391(12) . ?
C9 C8 1.399(16) . ?
N2 C6 1.351(18) . ?
N2 C2 1.338(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.38(2) . ?
C3 C2 1.403(17) . ?
C4 H4 0.9500 . ?
C4 C5 1.42(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.357(18) . ?
C7 C8 1.379(17) . ?
C6 H6 0.9500 . ?
N1 C1 1.484(14) 3_665 ?
N1 C1 1.484(14) . ?
N1 C1 1.484(14) 2_655 ?
C2 C1 1.505(18) . ?
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
O1 Tm1 O1 84.0(3) 3_665 . ?
O1 Tm1 O1 84.0(3) 3_665 2_655 ?
O1 Tm1 O1 84.0(3) . 2_655 ?
O1 Tm1 N2 82.8(3) 3_665 3_665 ?
O1 Tm1 N2 82.8(3) . . ?
O1 Tm1 N2 163.6(3) 2_655 . ?
O1 Tm1 N2 85.0(4) . 2_655 ?
O1 Tm1 N2 82.8(3) 2_655 2_655 ?
O1 Tm1 N2 85.0(4) 3_665 . ?
O1 Tm1 N2 163.6(3) 3_665 2_655 ?
O1 Tm1 N2 163.6(3) . 3_665 ?
O1 Tm1 N2 85.0(4) 2_655 3_665 ?
O1 Tm1 N1 129.4(2) 3_665 . ?
O1 Tm1 N1 129.4(2) . . ?
O1 Tm1 N1 129.4(2) 2_655 . ?
N2 Tm1 N2 105.6(3) 3_665 2_655 ?
N2 Tm1 N2 105.6(3) 2_655 . ?
N2 Tm1 N2 105.6(3) 3_665 . ?
N2 Tm1 N1 66.9(3) 2_655 . ?
N2 Tm1 N1 66.9(3) 3_665 . ?
N2 Tm1 N1 66.9(3) . . ?
C12 O2 H2 109.5 . . ?
C7 O1 Tm1 141.1(8) . . ?
C12 C11 Br4 118.6(9) . . ?
C12 C11 C10 120.0(11) . . ?
C10 C11 Br4 121.4(9) . . ?
O2 C12 C11 119.4(10) . . ?
O2 C12 C7 119.8(11) . . ?
C11 C12 C7 120.8(11) . . ?
C10 C9 Br2 120.4(9) . . ?
C10 C9 C8 119.3(11) . . ?
C8 C9 Br2 120.3(9) . . ?
C6 N2 Tm1 122.7(8) . . ?
C2 N2 Tm1 118.3(9) . . ?
C2 N2 C6 117.9(11) . . ?
C4 C3 H3 120.4 . . ?
C4 C3 C2 119.2(12) . . ?
C2 C3 H3 120.4 . . ?
C3 C4 H4 121.0 . . ?
C3 C4 C5 117.9(12) . . ?
C5 C4 H4 121.1 . . ?
C11 C10 Br3 119.3(9) . . ?
C9 C10 Br3 121.1(9) . . ?
C9 C10 C11 119.5(11) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 C4 118.7(12) . . ?
C6 C5 H5 120.7 . . ?
O1 C7 C12 117.6(11) . . ?
O1 C7 C8 124.1(11) . . ?
C8 C7 C12 118.2(12) . . ?
N2 C6 C5 123.9(12) . . ?
N2 C6 H6 118.0 . . ?
C5 C6 H6 118.0 . . ?
C9 C8 Br1 120.7(9) . . ?
C7 C8 Br1 117.1(9) . . ?
C7 C8 C9 122.1(11) . . ?
C1 N1 Tm1 109.4(9) 2_655 . ?
C1 N1 Tm1 109.4(9) . . ?
C1 N1 Tm1 109.4(9) 3_665 . ?
C1 N1 C1 109.5(9) 2_655 . ?
C1 N1 C1 109.5(9) 3_665 . ?
C1 N1 C1 109.5(9) 3_665 2_655 ?
N2 C2 C3 122.4(12) . . ?
N2 C2 C1 116.1(11) . . ?
C3 C2 C1 121.5(11) . . ?
N1 C1 C2 111.7(10) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84 2.01 2.832(11) 166.6 3_665 yes

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
Tm1 O1 C7 C12 86.8(13) . . . . ?
Tm1 O1 C7 C8 -93.8(15) . . . . ?
Tm1 N2 C6 C5 166.3(10) . . . . ?
Tm1 N2 C2 C3 -168.2(9) . . . . ?
Tm1 N2 C2 C1 11.2(13) . . . . ?
Tm1 N1 C1 C2 -43.4(11) . . . . ?
Br4 C11 C12 O2 6.4(15) . . . . ?
Br4 C11 C12 C7 -173.5(8) . . . . ?
Br4 C11 C10 Br3 -8.0(14) . . . . ?
Br4 C11 C10 C9 175.4(7) . . . . ?
Br2 C9 C10 Br3 3.5(11) . . . . ?
Br2 C9 C10 C11 179.9(10) . . . . ?
Br2 C9 C8 Br1 -3.1(14) . . . . ?
Br2 C9 C8 C7 179.9(9) . . . . ?
O2 C12 C7 O1 -3.7(14) . . . . ?
O2 C12 C7 C8 176.9(12) . . . . ?
O1 C7 C8 Br1 4.9(16) . . . . ?
O1 C7 C8 C9 -178.0(11) . . . . ?
C11 C12 C7 O1 176.2(11) . . . . ?
C11 C12 C7 C8 -3.2(15) . . . . ?
C12 C11 C10 Br3 175.4(9) . . . . ?
C12 C11 C10 C9 -1.1(16) . . . . ?
C12 C7 C8 Br1 -175.8(7) . . . . ?
C12 C7 C8 C9 1.4(17) . . . . ?
N2 C2 C1 N1 22.5(15) . . . . ?
C3 C4 C5 C6 0.6(18) . . . . ?
C3 C2 C1 N1 -158.1(11) . . . . ?
C4 C3 C2 N2 1.7(18) . . . . ?
C4 C3 C2 C1 -177.7(12) . . . . ?
C4 C5 C6 N2 1.0(19) . . . . ?
C10 C11 C12 O2 -177.0(11) . . . . ?
C10 C11 C12 C7 3.1(17) . . . . ?
C10 C9 C8 Br1 177.6(7) . . . . ?
C10 C9 C8 C7 0.6(17) . . . . ?
C6 N2 C2 C3 -0.2(16) . . . . ?
C6 N2 C2 C1 179.3(10) . . . . ?
C8 C9 C10 Br3 -177.2(10) . . . . ?
C8 C9 C10 C11 -0.7(13) . . . . ?
C2 N2 C6 C5 -1.2(17) . . . . ?
C2 C3 C4 C5 -1.8(18) . . . . ?
C1 N1 C1 C2 -163.4(11) 2_655 . . . ?
C1 N1 C1 C2 76.6(18) 3_665 . . . ?

_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 1.295
_oxdiff_exptl_absorpt_empirical_full_min 0.829
_exptl_crystal_recrystallization_method 'From reaction'
####################################################################### 
# 
# 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_sb01-05-tb2-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405948'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 N4 O6 Tb'
_chemical_formula_sum            'C36 H21 Br12 N4 O6 Tb'
_chemical_formula_weight         1723.41
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Gd C36 Br12 O6 N4'
_chemical_oxdiff_usercomment     'clear cube in oil at 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 '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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.11280(10)
_cell_length_b                   13.11280(10)
_cell_length_c                   46.3988(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6909.21(15)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    17954
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      78.4390
_cell_measurement_theta_min      3.9970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.153
_exptl_absorpt_correction_T_max  0.369
_exptl_absorpt_correction_T_min  0.150
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4788
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 1 -13 0.0491
-7 0 14 0.0488
3 -1 28 0.0432
7 -1 17 0.0388
7 0 -6 0.0491
4 0 -24 0.0589
-5 1 -24 0.0472
-4 -3 -15 0.0547
-8 4 13 0.0393
-6 6 20 0.0364
4 3 15 0.0235
6 -5 -19 0.0546
-2 -6 6 0.0440
-8 3 -6 0.0432
-7 7 -10 0.0478
2 6 -6 0.0592
7 0 2 0.0456
8 -6 8 0.0446
4 -8 10 0.0479

_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.078
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.9806 0.7731 -13.1665 0.1028 -0.3481 0.9318
-6.5126 0.0618 14.3295 -0.1569 0.5264 0.8356
3.3347 -0.8954 27.5163 -0.2507 0.8452 -0.4720
6.5066 -0.8301 16.6901 -0.1377 0.4658 -0.8741
7.4019 -0.3343 -5.6283 0.0771 -0.2574 -0.9632
4.1865 0.3334 -24.2642 0.2438 -0.8198 -0.5181
-4.6710 0.9056 -24.4770 0.2176 -0.7340 0.6433
-4.3255 -3.0036 -15.0735 0.5351 -0.2555 0.8052
-7.6440 4.3425 13.0774 -0.6124 0.2909 0.7351
-5.6134 5.6051 19.5471 -0.8398 0.3995 0.3676
4.4859 2.8865 14.6920 -0.5180 0.2474 -0.8188
5.9805 -5.4905 -18.8454 0.8171 -0.3886 -0.4259
-2.3667 -5.7595 5.7149 0.5788 0.4939 0.6490
-8.2818 3.1165 -5.5336 -0.2458 -0.2120 0.9459
-6.7578 7.1953 -9.6197 -0.6546 -0.5608 0.5069
1.9341 6.0539 -6.1485 -0.6044 -0.5159 -0.6070
7.4169 -0.1284 2.0343 -0.0397 -0.0322 -0.9987
7.9311 -5.7110 8.2907 0.5015 0.4303 -0.7506
4.4254 -8.0244 9.9340 0.7520 0.6434 -0.1433

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            28311
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.418
_diffrn_reflns_theta_min         4.335
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00 -36.00   0.50    0.05    --  -47.51  77.00-180.00   56
  2  ω    -33.00  24.00   0.50    0.05    --  -47.51  77.00-180.00  114
  3  ω    -37.00  15.00   0.50    0.05    --  -47.51  38.00 -30.00  104
  4  ω    -61.00  13.00   0.50    0.05    --  -47.51  57.00  90.00  148
  5  ω    -25.00   1.00   0.50    0.05    --   47.51 -19.00 -90.00   52
  6  ω     -4.00  23.00   0.50    0.05    --   47.51 -19.00-120.00   54
  7  ω    -27.00  30.00   0.50    0.05    --   47.51 -19.00  30.00  114
  8  ω    -21.00  27.00   0.50    0.05    --   47.51 -19.00 150.00   96
  9  ω     98.00 124.00   0.50    0.05    --  113.25 125.00 120.00   52
 10  ω    151.00 176.00   0.50    0.05    --  113.25 125.00 120.00   50
 11  ω     63.00 106.00   0.50    0.05    --  113.25 -94.00  90.00   86
 12  ω     46.00  81.00   0.50    0.05    --  113.25-132.00 124.47   70
 13  ω     86.00 117.00   0.50    0.05    --  113.25-132.00 124.47   62
 14  ω     86.00 111.00   0.50    0.05    --  113.25-125.00   0.00   50
 15  ω     44.00  75.00   0.50    0.05    --  113.25-125.00   0.00   62
 16  ω     81.00 111.00   0.50    0.05    --  113.25-125.00  30.00   60
 17  ω     66.00 106.00   0.50    0.05    --  113.25-125.00  90.00   80
 18  ω     63.00 101.00   0.50    0.05    --  113.25-125.00  60.00   76
 19  ω     69.00 105.00   0.50    0.05    --  113.25-102.00 -80.70   72
 20  ω     58.00  96.00   0.50    0.05    --  113.25 -94.00 -60.00   76
 21  ω     45.00  89.00   0.50    0.05    --  113.25-125.00 -90.00   88
 22  ω     48.00  78.00   0.50    0.05    --  113.25-125.00-150.00   60
 23  ω     46.00 107.00   0.50    0.05    --  113.25-125.00-180.00  122
 24  ω     76.00 106.00   0.50    0.05    --  113.25 -94.00-180.00   60
 25  ω     61.00 103.00   0.50    0.05    --  113.25 -94.00-150.00   84
 26  ω     79.00 104.00   0.50    0.05    --  113.25 -94.00 150.00   50
 27  ω     44.00  70.00   0.50    0.05    --  113.25 -61.00   0.00   52
 28  ω     44.00  69.00   0.50    0.05    --  113.25 -61.00  90.00   50
 29  ω     42.00  67.00   0.50    0.05    --  113.25 -61.00  30.00   50
 30  ω     45.00  70.00   0.50    0.05    --  113.25 -61.00 120.00   50
 31  ω     45.00  70.00   0.50    0.05    --  113.25 -61.00 -30.00   50
 32  ω     44.00  70.00   0.50    0.05    --  113.25 -61.00 -60.00   52
 33  ω     53.00  94.00   0.50    0.05    --  113.25 -77.00-120.00   82
 34  ω     45.00  70.00   0.50    0.05    --  113.25 -61.00-180.00   50
 35  ω    111.00 175.00   0.50    0.05    --  113.25  15.00 -90.00  128
 36  ω    153.00 178.00   0.50    0.05    --  113.25  77.00  30.00   50
 37  ω     96.00 140.00   0.50    0.05    --  113.25  77.00  30.00   88
 38  ω    105.00 175.00   0.50    0.05    --  113.25  45.00   0.00  140
 39  ω    146.00 176.00   0.50    0.05    --  113.25  45.00 -30.00   60
 40  ω    101.00 142.00   0.50    0.05    --  113.25  45.00 -30.00   82
 41  ω    102.00 134.00   0.50    0.05    --  113.25  61.00-180.00   64
 42  ω    140.00 166.00   0.50    0.05    --  113.25  61.00-180.00   52
 43  ω    102.00 154.00   0.50    0.05    --  113.25  45.00-120.00  104
 44  ω    101.00 177.00   0.50    0.05    --  113.25  45.00 -60.00  152
 45  ω    101.00 145.00   0.50    0.05    --  113.25  45.00 120.00   88
 46  ω    103.00 143.00   0.50    0.05    --  113.25  30.00 120.00   80
 47  ω   -111.00 -47.00   0.50    0.05    --  -47.51 -57.00  30.00  128
 48  ω    -50.00 -20.00   0.50    0.05    --  -91.75  45.00  30.00   60
 49  ω    -80.00 -36.00   0.50    0.05    --  -91.75 125.00-120.00   88
 50  ω    -48.00 -23.00   0.50    0.05    --  -91.75  45.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0039137000
_diffrn_orient_matrix_UB_12      -0.1110330000
_diffrn_orient_matrix_UB_13      -0.0122494000
_diffrn_orient_matrix_UB_21      -0.0136315000
_diffrn_orient_matrix_UB_22      -0.0496287000
_diffrn_orient_matrix_UB_23      0.0307536000
_diffrn_orient_matrix_UB_31      -0.1349336000
_diffrn_orient_matrix_UB_32      -0.0599599000
_diffrn_orient_matrix_UB_33      -0.0027519000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                3276
_reflns_number_total             3324
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.626
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 
;
 Flack x determined using 1572 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3324
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0365
_refine_ls_restrained_S_all      1.165
_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)+(0.0560P)²+74.5090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1037
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
1.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.666667 0.333333 0.52421(2) 0.0221(2) Uani 1 3 d S T P . .
Br1 Br 0.51072(10) 0.55191(10) 0.52900(2) 0.0258(3) Uani 1 1 d . . . . .
Br2 Br 0.58142(12) 0.80997(10) 0.49924(2) 0.0311(3) Uani 1 1 d . . . . .
Br3 Br 0.75643(11) 0.89920(10) 0.44165(2) 0.0308(3) Uani 1 1 d . . . . .
Br4 Br 0.83102(10) 0.71535(10) 0.41162(2) 0.0271(3) Uani 1 1 d . . . . .
O1 O 0.6076(7) 0.4230(6) 0.49379(15) 0.0223(15) Uani 1 1 d . . . . .
O2 O 0.7570(8) 0.5025(7) 0.44839(16) 0.0291(15) Uani 1 1 d . . . . .
H2 H 0.755354 0.456583 0.461232 0.044 Uiso 1 1 calc R U . . .
N1 N 0.666667 0.333333 0.5786(4) 0.034(3) Uani 1 3 d S T P . .
N2 N 0.7809(8) 0.5326(9) 0.5459(2) 0.0271(18) Uani 1 1 d . . . . .
C1 C 0.6658(12) 0.4398(11) 0.5888(2) 0.037(2) Uani 1 1 d . . . . .
H1A H 0.685623 0.451084 0.609527 0.044 Uiso 1 1 calc R U . . .
H1B H 0.585516 0.427924 0.586477 0.044 Uiso 1 1 calc R U . . .
C2 C 0.7503(10) 0.5472(11) 0.5729(3) 0.032(2) Uani 1 1 d . . . . .
C3 C 0.7929(10) 0.6615(11) 0.5836(2) 0.031(2) Uani 1 1 d . . . . .
H3 H 0.771150 0.671877 0.602438 0.037 Uiso 1 1 calc R U . . .
C4 C 0.8654(11) 0.7581(11) 0.5674(3) 0.038(3) Uani 1 1 d . . . . .
H4 H 0.893072 0.835312 0.574641 0.046 Uiso 1 1 calc R U . . .
C5 C 0.8978(10) 0.7411(10) 0.5399(3) 0.032(2) Uani 1 1 d . . . . .
H5 H 0.949044 0.806141 0.528118 0.038 Uiso 1 1 calc R U . . .
C6 C 0.8533(11) 0.6270(11) 0.5303(3) 0.032(2) Uani 1 1 d . . . . .
H6 H 0.875133 0.614947 0.511590 0.038 Uiso 1 1 calc R U . . .
C7 C 0.6396(9) 0.5300(10) 0.4831(2) 0.024(2) Uani 1 1 d . . . . .
C8 C 0.6022(9) 0.6040(9) 0.4948(2) 0.024(2) Uani 1 1 d . . . . .
C9 C 0.6338(10) 0.7123(10) 0.4825(2) 0.026(2) Uani 1 1 d . . . . .
C10 C 0.7050(9) 0.7491(9) 0.4581(2) 0.023(2) Uani 1 1 d . . . . .
C11 C 0.7436(9) 0.6757(10) 0.4463(2) 0.023(2) Uani 1 1 d . . . . .
C12 C 0.7138(9) 0.5693(9) 0.4591(2) 0.0222(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.210(7) 3_665 ?
Tb1 O1 2.210(7) 2_655 ?
Tb1 O1 2.210(6) . ?
Tb1 N1 2.522(19) . ?
Tb1 N2 2.484(10) 2_655 ?
Tb1 N2 2.484(10) . ?
Tb1 N2 2.484(9) 3_665 ?
Br1 C8 1.900(11) . ?
Br2 C9 1.898(11) . ?
Br3 C10 1.893(10) . ?
Br4 C11 1.892(11) . ?
O1 C7 1.342(13) . ?
O2 H2 0.8400 . ?
O2 C12 1.354(13) . ?
N1 C1 1.479(14) 2_655 ?
N1 C1 1.479(14) . ?
N1 C1 1.479(14) 3_665 ?
N2 C2 1.354(15) . ?
N2 C6 1.338(17) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.481(18) . ?
C2 C3 1.403(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.37(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.399(19) . ?
C5 H5 0.9500 . ?
C5 C6 1.380(16) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(16) . ?
C7 C12 1.396(12) . ?
C8 C9 1.387(15) . ?
C9 C10 1.388(12) . ?
C10 C11 1.405(15) . ?
C11 C12 1.381(15) . ?

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
O1 Tb1 O1 83.6(3) 3_665 2_655 ?
O1 Tb1 O1 83.6(3) 3_665 . ?
O1 Tb1 O1 83.6(3) 2_655 . ?
O1 Tb1 N1 129.69(19) 3_665 . ?
O1 Tb1 N1 129.69(19) . . ?
O1 Tb1 N1 129.69(19) 2_655 . ?
O1 Tb1 N2 164.2(3) 3_665 2_655 ?
O1 Tb1 N2 83.5(3) 2_655 2_655 ?
O1 Tb1 N2 164.2(3) . 3_665 ?
O1 Tb1 N2 85.9(3) . 2_655 ?
O1 Tb1 N2 83.5(3) . . ?
O1 Tb1 N2 164.2(3) 2_655 . ?
O1 Tb1 N2 85.9(3) 2_655 3_665 ?
O1 Tb1 N2 85.9(3) 3_665 . ?
O1 Tb1 N2 83.5(3) 3_665 3_665 ?
N2 Tb1 N1 66.0(2) . . ?
N2 Tb1 N1 66.1(2) 3_665 . ?
N2 Tb1 N1 66.1(2) 2_655 . ?
N2 Tb1 N2 104.6(3) 2_655 . ?
N2 Tb1 N2 104.6(3) 3_665 2_655 ?
N2 Tb1 N2 104.6(3) 3_665 . ?
C7 O1 Tb1 141.5(7) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Tb1 108.6(8) 2_655 . ?
C1 N1 Tb1 108.6(8) 3_665 . ?
C1 N1 Tb1 108.6(8) . . ?
C1 N1 C1 110.3(8) 2_655 . ?
C1 N1 C1 110.3(8) 3_665 . ?
C1 N1 C1 110.3(8) 3_665 2_655 ?
C2 N2 Tb1 117.2(8) . . ?
C6 N2 Tb1 121.9(7) . . ?
C6 N2 C2 119.6(10) . . ?
N1 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
N1 C1 C2 112.5(10) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
N2 C2 C1 117.3(11) . . ?
N2 C2 C3 119.4(12) . . ?
C3 C2 C1 123.2(11) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(11) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.7(11) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 121.0 . . ?
C6 C5 C4 118.1(12) . . ?
C6 C5 H5 121.0 . . ?
N2 C6 C5 123.2(11) . . ?
N2 C6 H6 118.4 . . ?
C5 C6 H6 118.4 . . ?
O1 C7 C8 123.3(10) . . ?
O1 C7 C12 118.4(10) . . ?
C12 C7 C8 118.3(11) . . ?
C7 C8 Br1 116.8(8) . . ?
C9 C8 Br1 121.6(8) . . ?
C9 C8 C7 121.5(11) . . ?
C8 C9 Br2 119.9(8) . . ?
C8 C9 C10 119.7(11) . . ?
C10 C9 Br2 120.4(9) . . ?
C9 C10 Br3 121.2(9) . . ?
C9 C10 C11 119.3(10) . . ?
C11 C10 Br3 119.4(8) . . ?
C10 C11 Br4 121.4(8) . . ?
C12 C11 Br4 118.1(8) . . ?
C12 C11 C10 120.5(10) . . ?
O2 C12 C7 119.6(10) . . ?
O2 C12 C11 119.7(9) . . ?
C11 C12 C7 120.6(11) . . ?

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
Tb1 O1 C7 C8 -93.5(13) . . . . ?
Tb1 O1 C7 C12 86.7(12) . . . . ?
Tb1 N1 C1 C2 -44.9(11) . . . . ?
Tb1 N2 C2 C1 10.0(13) . . . . ?
Tb1 N2 C2 C3 -165.9(8) . . . . ?
Tb1 N2 C6 C5 165.5(9) . . . . ?
Br1 C8 C9 Br2 -1.9(14) . . . . ?
Br1 C8 C9 C10 177.3(7) . . . . ?
Br2 C9 C10 Br3 2.2(10) . . . . ?
Br2 C9 C10 C11 179.3(9) . . . . ?
Br3 C10 C11 Br4 -7.4(12) . . . . ?
Br3 C10 C11 C12 175.5(8) . . . . ?
Br4 C11 C12 O2 6.5(14) . . . . ?
Br4 C11 C12 C7 -173.6(7) . . . . ?
O1 C7 C8 Br1 4.5(15) . . . . ?
O1 C7 C8 C9 -177.6(10) . . . . ?
O1 C7 C12 O2 -3.9(13) . . . . ?
O1 C7 C12 C11 176.1(10) . . . . ?
N1 C1 C2 N2 24.6(15) . . . . ?
N1 C1 C2 C3 -159.6(11) . . . . ?
N2 C2 C3 C4 -0.4(17) . . . . ?
C1 N1 C1 C2 -163.8(11) 2_655 . . . ?
C1 N1 C1 C2 74.1(18) 3_665 . . . ?
C1 C2 C3 C4 -176.1(12) . . . . ?
C2 N2 C6 C5 -1.4(17) . . . . ?
C2 C3 C4 C5 -0.9(18) . . . . ?
C3 C4 C5 C6 1.1(18) . . . . ?
C4 C5 C6 N2 0.1(18) . . . . ?
C6 N2 C2 C1 177.4(11) . . . . ?
C6 N2 C2 C3 1.5(16) . . . . ?
C7 C8 C9 Br2 -179.6(8) . . . . ?
C7 C8 C9 C10 -0.5(16) . . . . ?
C8 C7 C12 O2 176.2(11) . . . . ?
C8 C7 C12 C11 -3.8(14) . . . . ?
C8 C9 C10 Br3 -177.0(10) . . . . ?
C8 C9 C10 C11 0.2(13) . . . . ?
C9 C10 C11 Br4 175.3(7) . . . . ?
C9 C10 C11 C12 -1.7(15) . . . . ?
C10 C11 C12 O2 -176.4(10) . . . . ?
C10 C11 C12 C7 3.5(15) . . . . ?
C12 C7 C8 Br1 -175.6(7) . . . . ?
C12 C7 C8 C9 2.2(16) . . . . ?

_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 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.698
_exptl_crystal_recrystallization_method 'From reaction'
####################################################################### 
# 
# 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_sb01-05-dy2-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405953'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 Dy N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Dy N4 O6'
_chemical_formula_weight         1726.99
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Dy Br12 O6 N4 C36'
_chemical_oxdiff_usercomment     'colourless cube in oil 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.11740(10)
_cell_length_b                   13.11740(10)
_cell_length_c                   46.3156(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6901.66(14)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    22606
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      79.3170
_cell_measurement_theta_min      4.0670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.305
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4794
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -6 19 0.0098
-2 3 -28 0.0208
1 -7 -10 0.0117
2 -7 13 0.0174
-2 8 -4 0.0159
-3 -4 -19 0.0135
-6 -2 5 0.0199
1 4 25 0.0064
2 -5 -24 0.0251
-7 7 9 0.0098
8 -5 4 0.0165

_exptl_crystal_size_max          0.056
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.026
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.6641 -5.6994 19.1565 -0.9097 -0.1688 -0.3795
-1.9721 3.3381 -27.6187 0.5963 0.5089 0.6209
0.7532 -7.3031 -10.0043 -0.4793 -0.4113 0.7753
1.9248 -7.4372 12.7082 -0.7564 -0.6471 0.0959
-1.5792 7.9714 -4.0510 0.6985 0.5982 -0.3927
-2.7338 -3.7341 -19.4423 0.0645 -0.3390 0.9386
-6.0998 -1.9267 5.3264 0.1767 -0.9477 0.2658
0.7096 3.6187 25.1943 -0.0032 0.0088 -1.0000
2.0471 -5.2065 -23.6794 -0.2867 0.1378 0.9481
-7.4788 6.5499 8.6905 0.8349 -0.3980 -0.3803
8.3724 -5.2026 3.5617 -0.8983 0.4276 -0.1009

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            27533
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.217
_diffrn_reflns_theta_min         4.335
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -51.00 -26.00   0.50    0.20    --  -47.51  57.00  90.00   50
  2  ω    -22.00  25.00   0.50    0.20    --  -47.51  57.00  90.00   94
  3  ω    -18.00  26.00   0.50    0.20    --  -47.51  19.00  90.00   88
  4  ω    106.00 149.00   0.50    0.80    --  113.25  45.00   0.00   86
  5  ω    101.00 151.00   0.50    0.80    --  113.25  61.00 -30.00  100
  6  ω    140.00 176.00   0.50    0.80    --  113.25  45.00  30.00   72
  7  ω    101.00 173.00   0.50    0.80    --  113.25  45.00 120.00  144
  8  ω    106.00 172.00   0.50    0.80    --  113.25  30.00  60.00  132
  9  ω    107.00 133.00   0.50    0.80    --  113.25  45.00  30.00   52
 10  ω    126.00 173.00   0.50    0.80    --  113.25  15.00 -60.00   94
 11  ω    107.00 174.00   0.50    0.80    --  113.25  30.00 -90.00  134
 12  ω    108.00 157.00   0.50    0.80    --  113.25  30.00-150.00   98
 13  ω      6.00  44.00   0.50    0.20    --   47.51 -38.00-120.00   76
 14  ω     43.00  75.00   0.50    0.80    --  113.25 -77.00 -60.00   64
 15  ω     42.00  90.00   0.50    0.80    --  113.25 -77.00 -30.00   96
 16  ω     52.00  80.00   0.50    0.80    --  113.25 -77.00  30.00   56
 17  ω     54.00  79.00   0.50    0.80    --  113.25 -77.00   0.00   50
 18  ω     42.00  68.00   0.50    0.80    --  113.25 -61.00  60.00   52
 19  ω     42.00  67.00   0.50    0.80    --  113.25 -61.00 120.00   50
 20  ω     43.00  68.00   0.50    0.80    --  113.25 -61.00  30.00   50
 21  ω    116.00 165.00   0.50    0.80    --  113.25 125.00  30.00   98
 22  ω    122.00 170.00   0.50    0.80    --  113.25 125.00 -90.00   96
 23  ω     52.00  84.00   0.50    0.80    --  113.25 -77.00-180.00   64
 24  ω     46.00  73.00   0.50    0.80    --  113.25-125.00-150.00   54
 25  ω     78.00 103.00   0.50    0.80    --  113.25-125.00-150.00   50
 26  ω     63.00 111.00   0.50    0.80    --  113.25-125.00-120.00   96
 27  ω     45.00 111.00   0.50    0.80    --  113.25-125.00 -90.00  132
 28  ω     45.00  82.00   0.50    0.80    --  113.25-125.00 -30.00   74
 29  ω     44.00  70.00   0.50    0.80    --  113.25-125.00 120.00   52
 30  ω     80.00 107.00   0.50    0.80    --  113.25-125.00 120.00   54
 31  ω     86.00 111.00   0.50    0.80    --  113.25-125.00 150.00   50
 32  ω     54.00 106.00   0.50    0.80    --  113.25 -94.00 120.00  104
 33  ω     43.00 100.00   0.50    0.80    --  113.25 -94.00  90.00  114
 34  ω     74.00 106.00   0.50    0.80    --  113.25 -94.00 -30.00   64
 35  ω     71.00 106.00   0.50    0.80    --  113.25 -94.00   0.00   70
 36  ω     71.00 104.00   0.50    0.80    --  113.25 -94.00 -60.00   66
 37  ω     81.00 106.00   0.50    0.80    --  113.25 -94.00 -90.00   50
 38  ω     51.00  76.00   0.50    0.80    --  113.25 -94.00 -90.00   50
 39  ω     81.00 106.00   0.50    0.80    --  113.25 -94.00-120.00   50
 40  ω    -83.00 -14.00   0.50    0.20    --  -47.51 125.00-180.00  138
 41  ω    -85.00 -13.00   0.50    0.20    --  -47.51 125.00   0.00  144
 42  ω    -76.00 -29.00   0.50    0.80    --  -91.75 125.00 150.00   94
 43  ω   -115.00 -79.00   0.50    0.80    --  -91.75 -45.00   0.00   72
 44  ω   -163.00-120.00   0.50    0.80    --  -91.75 -45.00   0.00   86
 45  ω   -119.00 -28.00   0.50    0.20    --  -47.51 -77.00 -30.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0591708000
_diffrn_orient_matrix_UB_12      0.0714759000
_diffrn_orient_matrix_UB_13      -0.0087253000
_diffrn_orient_matrix_UB_21      0.1133760000
_diffrn_orient_matrix_UB_22      0.0895209000
_diffrn_orient_matrix_UB_23      -0.0157013000
_diffrn_orient_matrix_UB_31      -0.0451556000
_diffrn_orient_matrix_UB_32      -0.0724465000
_diffrn_orient_matrix_UB_33      -0.0280124000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.848
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                3046
_reflns_number_total             3084
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 
;
 Flack x determined using 1337 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3084
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0269
_refine_ls_restrained_S_all      1.183
_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)+(0.0259P)²+67.0449P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0721
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.333333 0.666667 0.47585(2) 0.01909(16) Uani 1 3 d S T P . .
Br1 Br 0.55156(8) 0.51044(8) 0.47091(2) 0.02400(19) Uani 1 1 d . . . . .
Br2 Br 0.80938(8) 0.58108(9) 0.50076(2) 0.0295(2) Uani 1 1 d . . . . .
Br3 Br 0.89884(8) 0.75648(9) 0.55836(2) 0.0293(2) Uani 1 1 d . . . . .
Br4 Br 0.71505(8) 0.83141(7) 0.58839(2) 0.0255(2) Uani 1 1 d . . . . .
O1 O 0.4231(5) 0.6078(5) 0.50600(12) 0.0214(12) Uani 1 1 d . . . . .
O2 O 0.5016(5) 0.7566(6) 0.55170(13) 0.0271(12) Uani 1 1 d . . . . .
H2 H 0.459796 0.760315 0.538479 0.041 Uiso 1 1 calc R U . . .
N1 N 0.333333 0.666667 0.4214(3) 0.031(3) Uani 1 3 d S T P . .
N2 N 0.5321(7) 0.7802(6) 0.45457(16) 0.0252(14) Uani 1 1 d . . . . .
C1 C 0.4398(8) 0.6658(8) 0.41149(19) 0.0331(18) Uani 1 1 d . . . . .
H1A H 0.451835 0.685954 0.390703 0.040 Uiso 1 1 calc R U . . .
H1B H 0.427505 0.585293 0.413707 0.040 Uiso 1 1 calc R U . . .
C2 C 0.5476(8) 0.7498(7) 0.4277(2) 0.0273(17) Uani 1 1 d . . . . .
C3 C 0.6613(8) 0.7931(8) 0.4166(2) 0.0303(19) Uani 1 1 d . . . . .
H3 H 0.671565 0.771628 0.397680 0.036 Uiso 1 1 calc R U . . .
C4 C 0.7580(9) 0.8662(8) 0.4329(3) 0.037(2) Uani 1 1 d . . . . .
H4 H 0.835383 0.894739 0.425658 0.044 Uiso 1 1 calc R U . . .
C5 C 0.7398(8) 0.8977(7) 0.4606(2) 0.031(2) Uani 1 1 d . . . . .
H5 H 0.804549 0.948932 0.472418 0.037 Uiso 1 1 calc R U . . .
C6 C 0.6265(8) 0.8529(8) 0.4701(2) 0.0287(18) Uani 1 1 d . . . . .
H6 H 0.614481 0.874789 0.488796 0.034 Uiso 1 1 calc R U . . .
C7 C 0.5297(7) 0.6389(7) 0.51680(18) 0.0203(15) Uani 1 1 d . . . . .
C8 C 0.6032(7) 0.6021(7) 0.50520(19) 0.0203(15) Uani 1 1 d . . . . .
C9 C 0.7121(7) 0.6344(8) 0.51752(19) 0.0234(16) Uani 1 1 d . . . . .
C10 C 0.7487(7) 0.7047(7) 0.5420(2) 0.0215(16) Uani 1 1 d . . . . .
C11 C 0.6754(7) 0.7441(7) 0.55367(19) 0.0203(15) Uani 1 1 d . . . . .
C12 C 0.5689(7) 0.7140(7) 0.54087(19) 0.0221(16) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.201(5) 3_565 ?
Dy1 O1 2.201(5) . ?
Dy1 O1 2.201(5) 2_665 ?
Dy1 N1 2.521(14) . ?
Dy1 N2 2.471(7) . ?
Dy1 N2 2.471(7) 2_665 ?
Dy1 N2 2.471(7) 3_565 ?
Br1 C8 1.900(9) . ?
Br2 C9 1.901(9) . ?
Br3 C10 1.892(8) . ?
Br4 C11 1.890(9) . ?
O1 C7 1.341(10) . ?
O2 H2 0.8400 . ?
O2 C12 1.355(11) . ?
N1 C1 1.476(10) 2_665 ?
N1 C1 1.476(10) 3_565 ?
N1 C1 1.476(10) . ?
N2 C2 1.355(12) . ?
N2 C6 1.334(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.488(13) . ?
C2 C3 1.401(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.373(16) . ?
C4 H4 0.9500 . ?
C4 C5 1.403(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.370(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(12) . ?
C7 C12 1.404(10) . ?
C8 C9 1.392(12) . ?
C9 C10 1.385(10) . ?
C10 C11 1.408(12) . ?
C11 C12 1.382(12) . ?

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
O1 Dy1 O1 84.0(2) 3_565 2_665 ?
O1 Dy1 O1 84.0(2) 3_565 . ?
O1 Dy1 O1 84.0(2) 2_665 . ?
O1 Dy1 N1 129.38(15) 3_565 . ?
O1 Dy1 N1 129.39(15) . . ?
O1 Dy1 N1 129.39(15) 2_665 . ?
O1 Dy1 N2 82.9(2) 3_565 3_565 ?
O1 Dy1 N2 82.9(2) . . ?
O1 Dy1 N2 85.5(2) 3_565 2_665 ?
O1 Dy1 N2 164.0(2) 2_665 3_565 ?
O1 Dy1 N2 164.0(2) . 2_665 ?
O1 Dy1 N2 85.5(2) 2_665 . ?
O1 Dy1 N2 85.5(2) . 3_565 ?
O1 Dy1 N2 164.0(2) 3_565 . ?
O1 Dy1 N2 82.9(2) 2_665 2_665 ?
N2 Dy1 N1 66.49(18) 3_565 . ?
N2 Dy1 N1 66.49(18) 2_665 . ?
N2 Dy1 N1 66.50(18) . . ?
N2 Dy1 N2 105.2(2) . 3_565 ?
N2 Dy1 N2 105.2(2) 2_665 3_565 ?
N2 Dy1 N2 105.2(2) 2_665 . ?
C7 O1 Dy1 142.1(5) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Dy1 108.2(6) 3_565 . ?
C1 N1 Dy1 108.2(6) 2_665 . ?
C1 N1 Dy1 108.2(6) . . ?
C1 N1 C1 110.7(6) 2_665 3_565 ?
C1 N1 C1 110.7(6) 3_565 . ?
C1 N1 C1 110.7(6) 2_665 . ?
C2 N2 Dy1 117.2(6) . . ?
C6 N2 Dy1 122.6(6) . . ?
C6 N2 C2 119.0(8) . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
N1 C1 C2 112.9(8) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
N2 C2 C1 117.0(8) . . ?
N2 C2 C3 120.2(9) . . ?
C3 C2 C1 122.7(8) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.5(9) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.8 . . ?
C3 C4 C5 118.3(8) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.4(9) . . ?
C6 C5 H5 120.8 . . ?
N2 C6 C5 123.6(9) . . ?
N2 C6 H6 118.2 . . ?
C5 C6 H6 118.2 . . ?
O1 C7 C8 123.4(8) . . ?
O1 C7 C12 118.1(8) . . ?
C8 C7 C12 118.5(9) . . ?
C7 C8 Br1 117.0(6) . . ?
C7 C8 C9 121.4(8) . . ?
C9 C8 Br1 121.5(6) . . ?
C8 C9 Br2 119.7(7) . . ?
C10 C9 Br2 120.3(7) . . ?
C10 C9 C8 120.0(9) . . ?
C9 C10 Br3 121.3(7) . . ?
C9 C10 C11 119.1(8) . . ?
C11 C10 Br3 119.5(6) . . ?
C10 C11 Br4 121.3(6) . . ?
C12 C11 Br4 118.1(6) . . ?
C12 C11 C10 120.5(8) . . ?
O2 C12 C7 119.8(8) . . ?
O2 C12 C11 119.8(8) . . ?
C11 C12 C7 120.4(8) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84 2.05 2.871(8) 164.8 2_665 yes
C1 H1B Br3 0.99 3.00 3.726(9) 131.3 12_454 yes

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
Dy1 O1 C7 C8 -93.4(10) . . . . ?
Dy1 O1 C7 C12 85.7(10) . . . . ?
Dy1 N1 C1 C2 -44.5(8) . . . . ?
Dy1 N2 C2 C1 10.4(9) . . . . ?
Dy1 N2 C2 C3 -167.0(6) . . . . ?
Dy1 N2 C6 C5 166.0(7) . . . . ?
Br1 C8 C9 Br2 -2.6(10) . . . . ?
Br1 C8 C9 C10 177.8(5) . . . . ?
Br2 C9 C10 Br3 3.2(8) . . . . ?
Br2 C9 C10 C11 179.2(7) . . . . ?
Br3 C10 C11 Br4 -8.2(10) . . . . ?
Br3 C10 C11 C12 175.6(6) . . . . ?
Br4 C11 C12 O2 6.4(11) . . . . ?
Br4 C11 C12 C7 -173.3(6) . . . . ?
O1 C7 C8 Br1 3.8(11) . . . . ?
O1 C7 C8 C9 -178.5(8) . . . . ?
O1 C7 C12 O2 -2.8(10) . . . . ?
O1 C7 C12 C11 176.9(8) . . . . ?
N1 C1 C2 N2 24.4(11) . . . . ?
N1 C1 C2 C3 -158.4(8) . . . . ?
N2 C2 C3 C4 0.2(13) . . . . ?
C1 N1 C1 C2 -162.9(8) 3_565 . . . ?
C1 N1 C1 C2 73.9(14) 2_665 . . . ?
C1 C2 C3 C4 -177.0(9) . . . . ?
C2 N2 C6 C5 -1.2(13) . . . . ?
C2 C3 C4 C5 -1.1(14) . . . . ?
C3 C4 C5 C6 0.8(14) . . . . ?
C4 C5 C6 N2 0.4(13) . . . . ?
C6 N2 C2 C1 178.3(8) . . . . ?
C6 N2 C2 C3 0.9(12) . . . . ?
C7 C8 C9 Br2 179.9(6) . . . . ?
C7 C8 C9 C10 0.2(12) . . . . ?
C8 C7 C12 O2 176.4(8) . . . . ?
C8 C7 C12 C11 -3.9(10) . . . . ?
C8 C9 C10 Br3 -177.1(7) . . . . ?
C8 C9 C10 C11 -1.2(10) . . . . ?
C9 C10 C11 Br4 175.8(5) . . . . ?
C9 C10 C11 C12 -0.4(11) . . . . ?
C10 C11 C12 O2 -177.3(8) . . . . ?
C10 C11 C12 C7 3.0(12) . . . . ?
C12 C7 C8 Br1 -175.3(5) . . . . ?
C12 C7 C8 C9 2.3(12) . . . . ?

_olex2_exptl_crystal_mounting_method mounted
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.355
_oxdiff_exptl_absorpt_empirical_full_min 0.826
_exptl_crystal_recrystallization_method 'From reaction'
####################################################################### 
# 
# 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_sb01-05-yb3-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405947'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 N4 O6 Yb'
_chemical_formula_sum            'C36 H21 Br12 N4 O6 Yb'
_chemical_formula_weight         1737.53
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C36 O6 N4 Yb'
_chemical_oxdiff_usercomment     'clear block in oil at 100 K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -7.2108 4.4329 '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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.10280(10)
_cell_length_b                   13.10280(10)
_cell_length_c                   45.9960(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6838.78(16)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    24662
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      80.0150
_cell_measurement_theta_min      4.3420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.526
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.531
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4818
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8 6 6 0.0401
4 3 16 0.0171
-5 -2 -15 0.0442
4 -7 -16 0.0283
-5 -3 -8 0.0424
-1 8 10 0.0412
1 -7 -10 0.0323
-5 1 22 0.0383
-8 5 0 0.0310
-6 6 -18 0.0296
5 0 -23 0.0263
8 -5 -1 0.0264
5 -6 20 0.0226

_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.054
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7.7749 6.4556 6.2701 -0.0674 -0.2788 0.9580
4.4893 2.6251 15.8879 -0.2113 -0.8838 -0.4174
-5.4762 -1.6071 -14.5257 0.1962 0.8164 0.5432
3.6540 -7.2202 -15.7593 0.1952 0.8190 -0.5396
-4.7203 -3.4088 -8.3145 -0.0705 0.8961 0.4382
-1.4508 7.5757 9.6596 0.0760 -0.9507 0.3008
1.2095 -7.4856 -9.7102 -0.0766 0.9589 -0.2733
-5.4210 0.8528 21.7526 -0.7792 0.0205 0.6264
-8.4227 5.2750 0.0692 0.0390 0.0001 0.9992
-5.7822 5.7923 -18.4900 0.7137 -0.0174 0.7003
4.8917 -0.3801 -22.9549 0.8264 -0.0217 -0.5627
8.4339 -5.1890 -0.8637 -0.0096 -0.0008 -1.0000
5.2363 -5.6391 20.1058 -0.7708 0.0190 -0.6368

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            27280
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.262
_diffrn_reflns_theta_min         4.345
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  22.00   0.50    0.06    --  -47.51  19.00 -90.00  104
  2  ω    -64.00 -30.00   0.50    0.22    --  -91.75  61.00 -90.00   68
  3  ω    -44.00  24.00   0.50    0.06    --  -47.51  38.00  30.00  136
  4  ω    -61.00 -30.00   0.50    0.22    --  -91.75  61.00  60.00   62
  5  ω    -51.00 -23.00   0.50    0.22    --  -91.75  45.00 150.00   56
  6  ω    -86.00 -50.00   0.50    0.06    --  -47.51 125.00 150.00   72
  7  ω   -120.00 -48.00   0.50    0.06    --  -47.51 -38.00  90.00  144
  8  ω   -120.00 -35.00   0.50    0.06    --  -47.51 -19.00-120.00  170
  9  ω     46.00  80.00   0.50    0.22    --  113.25 -77.00  90.00   68
 10  ω     75.00 101.00   0.50    0.22    --  113.25 -77.00 -30.00   52
 11  ω     53.00  93.00   0.50    0.22    --  113.25 -77.00 -60.00   80
 12  ω     46.00  71.00   0.50    0.22    --  113.25 -77.00 -30.00   50
 13  ω     44.00  71.00   0.50    0.22    --  113.25 -61.00-180.00   54
 14  ω     43.00  68.00   0.50    0.22    --  113.25 -61.00  30.00   50
 15  ω     42.00  67.00   0.50    0.22    --  113.25 -61.00 -30.00   50
 16  ω     45.00  71.00   0.50    0.22    --  113.25 -61.00-120.00   52
 17  ω    127.00 158.00   0.50    0.22    --  113.25 125.00 150.00   62
 18  ω     43.00  68.00   0.50    0.22    --  113.25 -61.00 150.00   50
 19  ω     44.00  70.00   0.50    0.22    --  113.25 -61.00 120.00   52
 20  ω     58.00  96.00   0.50    0.22    --  113.25 -77.00 120.00   76
 21  ω     44.00  73.00   0.50    0.22    --  113.25 -94.00  90.00   58
 22  ω     44.00  81.00   0.50    0.22    --  113.25-125.00   0.00   74
 23  ω     86.00 111.00   0.50    0.22    --  113.25-125.00   0.00   50
 24  ω     86.00 111.00   0.50    0.22    --  113.25-125.00 -30.00   50
 25  ω     48.00  76.00   0.50    0.22    --  113.25-125.00 -30.00   56
 26  ω     82.00 111.00   0.50    0.22    --  113.25-125.00-120.00   58
 27  ω     42.00  70.00   0.50    0.22    --  113.25 -94.00-150.00   56
 28  ω     51.00  98.00   0.50    0.22    --  113.25 -94.00 -90.00   94
 29  ω     38.00  76.00   0.50    0.06    --   47.51-125.00 -30.00   76
 30  ω     71.00 101.00   0.50    0.22    --  113.25 -94.00  30.00   60
 31  ω     60.00 104.00   0.50    0.22    --  113.25 -94.00  60.00   88
 32  ω     79.00 106.00   0.50    0.22    --  113.25 -94.00  90.00   54
 33  ω     78.00 104.00   0.50    0.22    --  113.25 -94.00 120.00   52
 34  ω     81.00 106.00   0.50    0.22    --  113.25 -94.00 150.00   50
 35  ω      4.00  75.00   0.50    0.06    --   47.51 -99.00 150.00  142
 36  ω     79.00 104.00   0.50    0.22    --  113.25 -94.00   0.00   50
 37  ω     45.00  70.00   0.50    0.22    --  113.25 -94.00-120.00   50
 38  ω     78.00 103.00   0.50    0.22    --  113.25 -94.00-150.00   50
 39  ω     81.00 106.00   0.50    0.22    --  113.25 -94.00-120.00   50
 40  ω    101.00 151.00   0.50    0.22    --  113.25  45.00  30.00  100
 41  ω    114.00 172.00   0.50    0.22    --  113.25  30.00  60.00  116
 42  ω    121.00 177.00   0.50    0.22    --  113.25  45.00 -30.00  112
 43  ω    103.00 165.00   0.50    0.22    --  113.25  45.00 -60.00  124
 44  ω    103.00 129.00   0.50    0.22    --  113.25  30.00 -90.00   52
 45  ω    104.00 130.00   0.50    0.22    --  113.25  45.00-180.00   52
 46  ω    135.00 162.00   0.50    0.22    --  113.25  45.00-180.00   54
 47  ω    115.00 167.00   0.50    0.22    --  113.25  15.00-120.00  104
 48  ω    133.00 160.00   0.50    0.22    --  113.25  30.00 -90.00   54
 49  ω    103.00 164.00   0.50    0.22    --  113.25  15.00 120.00  122
 50  ω    108.00 178.00   0.50    0.22    --  113.25  30.00 150.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0293914000
_diffrn_orient_matrix_UB_12      0.0547277000
_diffrn_orient_matrix_UB_13      -0.0306438000
_diffrn_orient_matrix_UB_21      -0.0772141000
_diffrn_orient_matrix_UB_22      -0.1230953000
_diffrn_orient_matrix_UB_23      -0.0134728000
_diffrn_orient_matrix_UB_31      -0.1076910000
_diffrn_orient_matrix_UB_32      0.0174607000
_diffrn_orient_matrix_UB_33      0.0012736000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                3275
_reflns_number_total             3294
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.701
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 
;
 Flack x determined using 1587 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0264
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0356P)²+64.6134P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0765
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
1.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.666667 0.333333 0.52394(2) 0.01748(15) Uani 1 3 d S T P . .
Br1 Br 0.50835(8) 0.54891(8) 0.52933(2) 0.0219(2) Uani 1 1 d . . . . .
Br2 Br 0.57857(9) 0.80659(8) 0.49926(2) 0.0270(2) Uani 1 1 d . . . . .
Br3 Br 0.75651(9) 0.89782(8) 0.44175(2) 0.0269(2) Uani 1 1 d . . . . .
Br4 Br 0.83229(8) 0.71442(8) 0.41150(2) 0.0231(2) Uani 1 1 d . . . . .
O1 O 0.6070(5) 0.4210(5) 0.49409(12) 0.0190(12) Uani 1 1 d . . . . .
O2 O 0.7569(6) 0.5001(6) 0.44826(13) 0.0232(12) Uani 1 1 d . . . . .
H2 H 0.760094 0.457521 0.461477 0.035 Uiso 1 1 calc R U . . .
N1 N 0.666667 0.333333 0.5774(3) 0.030(3) Uani 1 3 d S T P . .
N2 N 0.7784(7) 0.5298(7) 0.54459(16) 0.0237(14) Uani 1 1 d . . . . .
C1 C 0.6647(9) 0.4390(9) 0.58784(19) 0.0318(19) Uani 1 1 d . . . . .
H1A H 0.685588 0.450934 0.608739 0.038 Uiso 1 1 calc R U . . .
H1B H 0.584098 0.426625 0.585743 0.038 Uiso 1 1 calc R U . . .
C2 C 0.7491(8) 0.5465(8) 0.5713(2) 0.0254(18) Uani 1 1 d . . . . .
C3 C 0.7923(8) 0.6606(8) 0.5827(2) 0.0268(18) Uani 1 1 d . . . . .
H3 H 0.770546 0.671077 0.601676 0.032 Uiso 1 1 calc R U . . .
C4 C 0.8666(8) 0.7571(9) 0.5660(3) 0.033(2) Uani 1 1 d . . . . .
H4 H 0.895693 0.834769 0.573187 0.039 Uiso 1 1 calc R U . . .
C5 C 0.8987(8) 0.7380(8) 0.5381(2) 0.0279(19) Uani 1 1 d . . . . .
H5 H 0.951124 0.802289 0.526212 0.034 Uiso 1 1 calc R U . . .
C6 C 0.8519(9) 0.6240(9) 0.5286(2) 0.0271(18) Uani 1 1 d . . . . .
H6 H 0.872720 0.611040 0.509768 0.033 Uiso 1 1 calc R U . . .
C7 C 0.6390(7) 0.5278(7) 0.48348(18) 0.0180(15) Uani 1 1 d . . . . .
C8 C 0.6011(8) 0.6020(8) 0.49503(19) 0.0200(16) Uani 1 1 d . . . . .
C9 C 0.6326(8) 0.7099(8) 0.48269(18) 0.0220(17) Uani 1 1 d . . . . .
C10 C 0.7042(8) 0.7476(7) 0.45820(19) 0.0199(16) Uani 1 1 d . . . . .
C11 C 0.7438(8) 0.6739(7) 0.4463(2) 0.0194(16) Uani 1 1 d . . . . .
C12 C 0.7141(8) 0.5671(7) 0.45931(18) 0.0194(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O1 2.171(5) . ?
Yb1 O1 2.171(5) 3_665 ?
Yb1 O1 2.171(5) 2_655 ?
Yb1 N1 2.458(15) . ?
Yb1 N2 2.430(8) 2_655 ?
Yb1 N2 2.430(8) . ?
Yb1 N2 2.430(8) 3_665 ?
Br1 C8 1.899(9) . ?
Br2 C9 1.893(9) . ?
Br3 C10 1.888(8) . ?
Br4 C11 1.891(9) . ?
O1 C7 1.337(10) . ?
O2 H2 0.8400 . ?
O2 C12 1.355(11) . ?
N1 C1 1.479(11) 2_655 ?
N1 C1 1.479(11) 3_665 ?
N1 C1 1.479(11) . ?
N2 C2 1.337(12) . ?
N2 C6 1.342(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.493(14) . ?
C2 C3 1.409(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.379(16) . ?
C4 H4 0.9500 . ?
C4 C5 1.411(15) . ?
C5 H5 0.9500 . ?
C5 C6 1.371(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.399(12) . ?
C7 C12 1.401(10) . ?
C8 C9 1.381(13) . ?
C9 C10 1.389(10) . ?
C10 C11 1.416(12) . ?
C11 C12 1.387(12) . ?

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
O1 Yb1 O1 84.3(2) . 3_665 ?
O1 Yb1 O1 84.3(2) . 2_655 ?
O1 Yb1 O1 84.3(2) 3_665 2_655 ?
O1 Yb1 N1 129.23(16) . . ?
O1 Yb1 N1 129.23(16) 2_655 . ?
O1 Yb1 N1 129.23(16) 3_665 . ?
O1 Yb1 N2 84.8(3) . 2_655 ?
O1 Yb1 N2 163.7(2) 3_665 2_655 ?
O1 Yb1 N2 84.8(3) 2_655 3_665 ?
O1 Yb1 N2 82.7(2) 2_655 2_655 ?
O1 Yb1 N2 163.7(2) 2_655 . ?
O1 Yb1 N2 84.8(3) 3_665 . ?
O1 Yb1 N2 82.7(2) 3_665 3_665 ?
O1 Yb1 N2 82.7(2) . . ?
O1 Yb1 N2 163.7(2) . 3_665 ?
N2 Yb1 N1 67.00(19) . . ?
N2 Yb1 N1 67.00(19) 3_665 . ?
N2 Yb1 N1 67.00(19) 2_655 . ?
N2 Yb1 N2 105.7(2) 2_655 . ?
N2 Yb1 N2 105.7(2) 3_665 2_655 ?
N2 Yb1 N2 105.7(2) 3_665 . ?
C7 O1 Yb1 141.0(5) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Yb1 109.0(7) 2_655 . ?
C1 N1 Yb1 109.0(7) 3_665 . ?
C1 N1 Yb1 109.0(7) . . ?
C1 N1 C1 109.9(6) 2_655 . ?
C1 N1 C1 109.9(6) 3_665 . ?
C1 N1 C1 109.9(6) 3_665 2_655 ?
C2 N2 Yb1 117.5(7) . . ?
C2 N2 C6 119.0(8) . . ?
C6 N2 Yb1 122.4(6) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C2 111.5(8) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
N2 C2 C1 116.9(8) . . ?
N2 C2 C3 121.3(9) . . ?
C3 C2 C1 121.8(8) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(8) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.7(9) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 120.9 . . ?
C6 C5 C4 118.1(10) . . ?
C6 C5 H5 120.9 . . ?
N2 C6 C5 123.5(9) . . ?
N2 C6 H6 118.2 . . ?
C5 C6 H6 118.2 . . ?
O1 C7 C8 123.7(8) . . ?
O1 C7 C12 118.0(8) . . ?
C8 C7 C12 118.3(9) . . ?
C7 C8 Br1 116.5(7) . . ?
C9 C8 Br1 121.7(7) . . ?
C9 C8 C7 121.8(8) . . ?
C8 C9 Br2 120.0(7) . . ?
C8 C9 C10 120.0(9) . . ?
C10 C9 Br2 120.0(7) . . ?
C9 C10 Br3 121.7(7) . . ?
C9 C10 C11 118.9(8) . . ?
C11 C10 Br3 119.4(6) . . ?
C10 C11 Br4 121.2(6) . . ?
C12 C11 Br4 118.1(6) . . ?
C12 C11 C10 120.6(8) . . ?
O2 C12 C7 120.1(8) . . ?
O2 C12 C11 119.6(8) . . ?
C11 C12 C7 120.3(8) . . ?

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
Yb1 O1 C7 C8 -94.7(11) . . . . ?
Yb1 O1 C7 C12 85.7(10) . . . . ?
Yb1 N1 C1 C2 -44.3(8) . . . . ?
Yb1 N2 C2 C1 10.1(10) . . . . ?
Yb1 N2 C2 C3 -167.4(7) . . . . ?
Yb1 N2 C6 C5 167.2(7) . . . . ?
Br1 C8 C9 Br2 -2.2(11) . . . . ?
Br1 C8 C9 C10 177.6(6) . . . . ?
Br2 C9 C10 Br3 3.2(8) . . . . ?
Br2 C9 C10 C11 179.7(7) . . . . ?
Br3 C10 C11 Br4 -7.9(10) . . . . ?
Br3 C10 C11 C12 175.0(7) . . . . ?
Br4 C11 C12 O2 5.4(11) . . . . ?
Br4 C11 C12 C7 -173.7(6) . . . . ?
O1 C7 C8 Br1 4.6(11) . . . . ?
O1 C7 C8 C9 -177.4(8) . . . . ?
O1 C7 C12 O2 -3.3(11) . . . . ?
O1 C7 C12 C11 175.8(8) . . . . ?
N1 C1 C2 N2 23.9(12) . . . . ?
N1 C1 C2 C3 -158.6(9) . . . . ?
N2 C2 C3 C4 -0.2(13) . . . . ?
C1 N1 C1 C2 -163.7(8) 2_655 . . . ?
C1 N1 C1 C2 75.1(14) 3_665 . . . ?
C1 C2 C3 C4 -177.6(9) . . . . ?
C2 N2 C6 C5 -0.6(13) . . . . ?
C2 C3 C4 C5 -1.1(14) . . . . ?
C3 C4 C5 C6 1.5(14) . . . . ?
C4 C5 C6 N2 -0.7(14) . . . . ?
C6 N2 C2 C1 178.5(8) . . . . ?
C6 N2 C2 C3 1.0(13) . . . . ?
C7 C8 C9 Br2 180.0(6) . . . . ?
C7 C8 C9 C10 -0.2(12) . . . . ?
C8 C7 C12 O2 177.1(8) . . . . ?
C8 C7 C12 C11 -3.7(11) . . . . ?
C8 C9 C10 Br3 -176.6(8) . . . . ?
C8 C9 C10 C11 -0.1(10) . . . . ?
C9 C10 C11 Br4 175.6(6) . . . . ?
C9 C10 C11 C12 -1.5(12) . . . . ?
C10 C11 C12 O2 -177.4(8) . . . . ?
C10 C11 C12 C7 3.5(13) . . . . ?
C12 C7 C8 Br1 -175.8(6) . . . . ?
C12 C7 C8 C9 2.1(12) . . . . ?

_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 1.430
_oxdiff_exptl_absorpt_empirical_full_min 0.779
####################################################################### 
# 
# 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_sb01-05-ho1-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405949'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 Ho N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Ho N4 O6'
_chemical_formula_weight         1729.42
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ho Br12 O6 N4 C36'
_chemical_oxdiff_usercomment     'colourless cube in oil 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.12110(10)
_cell_length_b                   13.12110(10)
_cell_length_c                   46.2179(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6890.98(14)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    23073
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.7810
_cell_measurement_theta_min      4.1370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.853
_exptl_absorpt_correction_T_max  0.572
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 -2 3 0.0139
2 -7 -18 0.0225
-8 3 -2 0.0367
-3 7 18 0.0230
3 2 23 0.0263
5 -3 -23 0.0286
-4 4 26 0.0283
3 -2 28 0.0275
-6 0 -21 0.0400
-7 -1 1 0.0315
-4 -2 18 0.0266
5 3 7 0.0265
-2 8 -7 0.0349
-7 2 -13 0.0372
-4 -4 -5 0.0322
3 -8 9 0.0219

_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.046
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8.2009 -2.2786 3.3845 -0.3633 0.1721 0.9157
2.4986 -6.6534 -18.4126 -0.8378 0.3992 -0.3726
-8.3181 2.6613 -2.2905 0.4112 -0.1949 -0.8905
-2.9114 6.7505 18.1850 0.8539 -0.4069 0.3245
3.1542 2.4233 22.6159 0.5458 0.0424 0.8369
5.2833 -3.4384 -23.3023 -0.9855 -0.0784 0.1506
-4.0635 3.5842 25.5903 0.9960 0.0791 0.0410
2.8594 -1.7437 28.2236 0.5659 0.5960 0.5696
-5.6037 0.4923 -20.5492 -0.2776 -0.2911 -0.9155
-6.5168 -1.4906 0.6215 0.2636 0.2800 -0.9231
-4.2923 -2.4551 17.9192 0.5924 0.6262 -0.5069
5.3079 2.8190 7.4215 0.0533 -0.2786 0.9589
-1.8336 7.9279 -6.7126 0.1774 -0.9513 0.2520
-7.3606 1.7584 -12.9331 0.0508 -0.2807 -0.9585
-4.3893 -3.9872 -5.3653 -0.0805 0.4252 -0.9015
3.1169 -8.0658 8.8887 -0.1825 0.9804 -0.0738

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            28061
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.273
_diffrn_reflns_theta_min         4.336
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  23.00   0.50    0.08    --  -47.51  38.00 150.00  134
  2  ω    -44.00  25.00   0.50    0.08    --  -47.51  38.00  30.00  138
  3  ω    -28.00  13.00   0.50    0.08    --  -47.51  19.00   0.00   82
  4  ω    -44.00  25.00   0.50    0.08    --  -47.51  38.00 -90.00  138
  5  ω   -122.00 -53.00   0.50    0.30    --  -91.75   0.00-180.00  138
  6  ω   -157.00-131.00   0.50    0.30    --  -91.75   0.00-180.00   52
  7  ω    -53.00 -14.00   0.50    0.08    --  -47.51 125.00-120.00   78
  8  ω    -85.00 -22.00   0.50    0.08    --  -47.51 125.00  90.00  126
  9  ω    148.00 173.00   0.50    0.30    --  113.25  77.00   0.00   50
 10  ω    143.00 168.00   0.50    0.30    --  113.25  61.00  30.00   50
 11  ω     98.00 137.00   0.50    0.30    --  113.25  77.00   0.00   78
 12  ω    101.00 162.00   0.50    0.30    --  113.25  45.00 -30.00  122
 13  ω    101.00 127.00   0.50    0.30    --  113.25  61.00  30.00   52
 14  ω    102.00 167.00   0.50    0.30    --  113.25  30.00 120.00  130
 15  ω    153.00 178.00   0.50    0.30    --  113.25  45.00 150.00   50
 16  ω    121.00 149.00   0.50    0.30    --  113.25  45.00 150.00   56
 17  ω    114.00 163.00   0.50    0.30    --  113.25  15.00  90.00   98
 18  ω    106.00 132.00   0.50    0.30    --  113.25  30.00 -90.00   52
 19  ω    100.00 176.00   0.50    0.30    --  113.25  15.00-150.00  152
 20  ω    136.00 165.00   0.50    0.30    --  113.25  30.00 -90.00   58
 21  ω     68.00  93.00   0.50    0.30    --  113.25 -94.00 120.00   50
 22  ω     66.00  92.00   0.50    0.08    --   47.51-125.00 120.00   52
 23  ω     74.00 104.00   0.50    0.30    --  113.25 -94.00   0.00   60
 24  ω     44.00  82.00   0.50    0.30    --  113.25-125.00 -30.00   76
 25  ω     51.00 102.00   0.50    0.30    --  113.25 -94.00 -90.00  102
 26  ω     73.00 103.00   0.50    0.30    --  113.25 -94.00-150.00   60
 27  ω     46.00 106.00   0.50    0.30    --  113.25 -94.00-120.00  120
 28  ω     45.00 111.00   0.50    0.30    --  113.25-125.00-180.00  132
 29  ω     47.00  92.00   0.50    0.08    --   47.51-125.00 -90.00   90
 30  ω     80.00 105.00   0.50    0.30    --  113.25 -94.00 -30.00   50
 31  ω     42.00  68.00   0.50    0.30    --  113.25 -94.00   0.00   52
 32  ω     66.00 105.00   0.50    0.30    --  113.25 -94.00 150.00   78
 33  ω     76.00 105.00   0.50    0.30    --  113.25 -94.00  90.00   58
 34  ω     52.00 103.00   0.50    0.30    --  113.25 -94.00  60.00  102
 35  ω     44.00  69.00   0.50    0.30    --  113.25 -94.00  90.00   50
 36  ω     76.00 103.00   0.50    0.30    --  113.25 -94.00  30.00   54
 37  ω     43.00  70.00   0.50    0.30    --  113.25 -94.00-180.00   54
 38  ω     78.00 103.00   0.50    0.30    --  113.25 -94.00-180.00   50
 39  ω     81.00 106.00   0.50    0.30    --  113.25 -94.00 -60.00   50
 40  ω     68.00  94.00   0.50    0.30    --  113.25 -77.00 -60.00   52
 41  ω     48.00  74.00   0.50    0.30    --  113.25 -77.00-180.00   52
 42  ω     45.00  73.00   0.50    0.30    --  113.25 -77.00   0.00   56
 43  ω     43.00  70.00   0.50    0.30    --  113.25 -61.00  30.00   54
 44  ω     42.00  67.00   0.50    0.30    --  113.25 -61.00  90.00   50
 45  ω     43.00  68.00   0.50    0.30    --  113.25 -77.00 120.00   50
 46  ω     44.00  70.00   0.50    0.30    --  113.25 -61.00   0.00   52
 47  ω     45.00  70.00   0.50    0.30    --  113.25 -61.00 150.00   50
 48  ω     43.00  71.00   0.50    0.30    --  113.25 -61.00 -60.00   56
 49  ω     46.00  71.00   0.50    0.30    --  113.25 -61.00 -90.00   50
 50  ω     42.00  67.00   0.50    0.30    --  113.25 -61.00-120.00   50
 51  ω     42.00  68.00   0.50    0.30    --  113.25 -61.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0457814000
_diffrn_orient_matrix_UB_12      0.0344972000
_diffrn_orient_matrix_UB_13      0.0268207000
_diffrn_orient_matrix_UB_21      -0.0162332000
_diffrn_orient_matrix_UB_22      -0.1102454000
_diffrn_orient_matrix_UB_23      0.0159524000
_diffrn_orient_matrix_UB_31      0.1265302000
_diffrn_orient_matrix_UB_32      0.0709955000
_diffrn_orient_matrix_UB_33      0.0117492000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                3282
_reflns_number_total             3308
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.622
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 
;
 Flack x determined using 1585 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.046(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3308
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0306
_refine_ls_restrained_S_all      1.164
_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)+(0.0515P)²+44.5980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0903
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
1.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.666667 0.333333 0.52411(2) 0.0204(2) Uani 1 3 d S T P . .
Br1 Br 0.50996(8) 0.55084(8) 0.52914(2) 0.0247(2) Uani 1 1 d . . . . .
Br2 Br 0.58041(9) 0.80855(8) 0.49923(2) 0.0304(2) Uani 1 1 d . . . . .
Br3 Br 0.75645(9) 0.89839(8) 0.44164(2) 0.0302(2) Uani 1 1 d . . . . .
Br4 Br 0.83183(8) 0.71493(8) 0.41159(2) 0.0263(2) Uani 1 1 d . . . . .
O1 O 0.6080(5) 0.4227(5) 0.49404(12) 0.0220(12) Uani 1 1 d . . . . .
O2 O 0.7573(6) 0.5019(5) 0.44839(13) 0.0267(12) Uani 1 1 d . . . . .
H2 H 0.760926 0.460068 0.461674 0.040 Uiso 1 1 calc R U . . .
N1 N 0.666667 0.333333 0.5782(3) 0.033(3) Uani 1 3 d S T P . .
N2 N 0.7798(6) 0.5316(7) 0.54537(16) 0.0261(14) Uani 1 1 d . . . . .
C1 C 0.6657(9) 0.4397(9) 0.58847(19) 0.0350(19) Uani 1 1 d . . . . .
H1A H 0.686416 0.451549 0.609267 0.042 Uiso 1 1 calc R U . . .
H1B H 0.585301 0.427631 0.586372 0.042 Uiso 1 1 calc R U . . .
C2 C 0.7499(8) 0.5472(9) 0.5721(2) 0.0296(18) Uani 1 1 d . . . . .
C3 C 0.7927(8) 0.6614(9) 0.5832(2) 0.0314(19) Uani 1 1 d . . . . .
H3 H 0.770176 0.671850 0.602029 0.038 Uiso 1 1 calc R U . . .
C4 C 0.8667(8) 0.7575(9) 0.5669(3) 0.038(2) Uani 1 1 d . . . . .
H4 H 0.896273 0.834871 0.574217 0.045 Uiso 1 1 calc R U . . .
C5 C 0.8984(8) 0.7395(9) 0.5389(2) 0.0311(19) Uani 1 1 d . . . . .
H5 H 0.949767 0.803950 0.527029 0.037 Uiso 1 1 calc R U . . .
C6 C 0.8522(9) 0.6257(9) 0.5297(2) 0.0307(19) Uani 1 1 d . . . . .
H6 H 0.872955 0.612953 0.510874 0.037 Uiso 1 1 calc R U . . .
C7 C 0.6397(7) 0.5291(7) 0.48334(18) 0.0217(15) Uani 1 1 d . . . . .
C8 C 0.6017(7) 0.6031(7) 0.49494(19) 0.0214(15) Uani 1 1 d . . . . .
C9 C 0.6339(8) 0.7116(8) 0.48251(19) 0.0246(17) Uani 1 1 d . . . . .
C10 C 0.7050(8) 0.7487(7) 0.45812(19) 0.0225(16) Uani 1 1 d . . . . .
C11 C 0.7441(8) 0.6750(7) 0.44623(19) 0.0229(16) Uani 1 1 d . . . . .
C12 C 0.7145(7) 0.5689(7) 0.45913(19) 0.0212(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O1 2.191(5) 2_655 ?
Ho1 O1 2.191(5) 3_665 ?
Ho1 O1 2.191(5) . ?
Ho1 N1 2.499(14) . ?
Ho1 N2 2.465(8) . ?
Ho1 N2 2.465(8) 2_655 ?
Ho1 N2 2.465(7) 3_665 ?
Br1 C8 1.895(9) . ?
Br2 C9 1.897(9) . ?
Br3 C10 1.889(8) . ?
Br4 C11 1.887(9) . ?
O1 C7 1.337(10) . ?
O2 H2 0.8400 . ?
O2 C12 1.352(11) . ?
N1 C1 1.481(11) 2_655 ?
N1 C1 1.481(10) . ?
N1 C1 1.481(10) 3_665 ?
N2 C2 1.343(12) . ?
N2 C6 1.334(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.491(14) . ?
C2 C3 1.408(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(17) . ?
C4 H4 0.9500 . ?
C4 C5 1.411(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.370(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.401(12) . ?
C7 C12 1.406(10) . ?
C8 C9 1.390(12) . ?
C9 C10 1.387(9) . ?
C10 C11 1.413(12) . ?
C11 C12 1.380(12) . ?

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
O1 Ho1 O1 84.1(2) 2_655 3_665 ?
O1 Ho1 O1 84.1(2) 2_655 . ?
O1 Ho1 O1 84.1(2) 3_665 . ?
O1 Ho1 N1 129.36(15) 2_655 . ?
O1 Ho1 N1 129.36(15) . . ?
O1 Ho1 N1 129.36(15) 3_665 . ?
O1 Ho1 N2 164.0(2) 2_655 . ?
O1 Ho1 N2 85.5(2) 3_665 . ?
O1 Ho1 N2 164.0(2) . 3_665 ?
O1 Ho1 N2 82.9(2) . . ?
O1 Ho1 N2 85.5(2) . 2_655 ?
O1 Ho1 N2 164.0(2) 3_665 2_655 ?
O1 Ho1 N2 82.9(2) 3_665 3_665 ?
O1 Ho1 N2 82.9(2) 2_655 2_655 ?
O1 Ho1 N2 85.5(2) 2_655 3_665 ?
N2 Ho1 N1 66.50(18) 2_655 . ?
N2 Ho1 N1 66.50(18) 3_665 . ?
N2 Ho1 N1 66.51(19) . . ?
N2 Ho1 N2 105.2(2) . 2_655 ?
N2 Ho1 N2 105.2(2) 3_665 . ?
N2 Ho1 N2 105.2(2) 3_665 2_655 ?
C7 O1 Ho1 141.7(5) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Ho1 108.7(6) 2_655 . ?
C1 N1 Ho1 108.7(6) 3_665 . ?
C1 N1 Ho1 108.7(6) . . ?
C1 N1 C1 110.2(6) 2_655 . ?
C1 N1 C1 110.2(6) 3_665 . ?
C1 N1 C1 110.2(6) 3_665 2_655 ?
C2 N2 Ho1 117.4(6) . . ?
C6 N2 Ho1 122.3(6) . . ?
C6 N2 C2 119.1(8) . . ?
N1 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
N1 C1 C2 112.2(8) . . ?
H1A C1 H1B 107.9 . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
N2 C2 C1 117.2(8) . . ?
N2 C2 C3 120.4(10) . . ?
C3 C2 C1 122.3(8) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0(9) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.9(9) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 121.3 . . ?
C6 C5 C4 117.5(10) . . ?
C6 C5 H5 121.3 . . ?
N2 C6 C5 124.1(9) . . ?
N2 C6 H6 117.9 . . ?
C5 C6 H6 117.9 . . ?
O1 C7 C8 123.3(8) . . ?
O1 C7 C12 118.5(8) . . ?
C8 C7 C12 118.2(9) . . ?
C7 C8 Br1 116.7(6) . . ?
C9 C8 Br1 121.9(7) . . ?
C9 C8 C7 121.3(8) . . ?
C8 C9 Br2 119.5(7) . . ?
C10 C9 Br2 120.3(7) . . ?
C10 C9 C8 120.1(9) . . ?
C9 C10 Br3 121.4(7) . . ?
C9 C10 C11 119.1(9) . . ?
C11 C10 Br3 119.4(7) . . ?
C10 C11 Br4 121.3(6) . . ?
C12 C11 Br4 118.1(7) . . ?
C12 C11 C10 120.5(8) . . ?
O2 C12 C7 119.4(8) . . ?
O2 C12 C11 119.9(8) . . ?
C11 C12 C7 120.7(9) . . ?

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
Ho1 O1 C7 C8 -94.3(10) . . . . ?
Ho1 O1 C7 C12 86.0(10) . . . . ?
Ho1 N1 C1 C2 -44.3(8) . . . . ?
Ho1 N2 C2 C1 10.3(10) . . . . ?
Ho1 N2 C2 C3 -166.6(7) . . . . ?
Ho1 N2 C6 C5 166.5(7) . . . . ?
Br1 C8 C9 Br2 -2.3(11) . . . . ?
Br1 C8 C9 C10 177.4(5) . . . . ?
Br2 C9 C10 Br3 2.7(8) . . . . ?
Br2 C9 C10 C11 179.6(7) . . . . ?
Br3 C10 C11 Br4 -7.4(10) . . . . ?
Br3 C10 C11 C12 175.3(7) . . . . ?
Br4 C11 C12 O2 5.9(11) . . . . ?
Br4 C11 C12 C7 -173.7(6) . . . . ?
O1 C7 C8 Br1 4.6(11) . . . . ?
O1 C7 C8 C9 -177.9(8) . . . . ?
O1 C7 C12 O2 -3.6(10) . . . . ?
O1 C7 C12 C11 176.1(8) . . . . ?
N1 C1 C2 N2 24.0(12) . . . . ?
N1 C1 C2 C3 -159.2(9) . . . . ?
N2 C2 C3 C4 -1.0(14) . . . . ?
C1 N1 C1 C2 -163.3(8) 2_655 . . . ?
C1 N1 C1 C2 74.8(14) 3_665 . . . ?
C1 C2 C3 C4 -177.7(9) . . . . ?
C2 N2 C6 C5 -0.6(14) . . . . ?
C2 C3 C4 C5 0.3(14) . . . . ?
C3 C4 C5 C6 0.3(14) . . . . ?
C4 C5 C6 N2 -0.1(14) . . . . ?
C6 N2 C2 C1 178.0(8) . . . . ?
C6 N2 C2 C3 1.1(13) . . . . ?
C7 C8 C9 Br2 -179.7(6) . . . . ?
C7 C8 C9 C10 0.0(12) . . . . ?
C8 C7 C12 O2 176.7(8) . . . . ?
C8 C7 C12 C11 -3.6(11) . . . . ?
C8 C9 C10 Br3 -177.1(8) . . . . ?
C8 C9 C10 C11 -0.1(10) . . . . ?
C9 C10 C11 Br4 175.6(5) . . . . ?
C9 C10 C11 C12 -1.7(12) . . . . ?
C10 C11 C12 O2 -176.7(8) . . . . ?
C10 C11 C12 C7 3.6(13) . . . . ?
C12 C7 C8 Br1 -175.7(6) . . . . ?
C12 C7 C8 C9 1.8(12) . . . . ?

_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 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.776
_exptl_crystal_recrystallization_method 'From reaction'
####################################################################### 
# 
# 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_sb01-05-eu2-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405950'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 Eu N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Eu N4 O6'
_chemical_formula_weight         1716.45
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Eu C36 Br12 O6 N4'
_chemical_oxdiff_usercomment     'clear needle in oil at 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.14720(10)
_cell_length_b                   13.14720(10)
_cell_length_c                   46.5427(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6967.05(15)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    28210
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.7100
_cell_measurement_theta_min      3.9700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.164
_exptl_absorpt_correction_T_max  0.390
_exptl_absorpt_correction_T_min  0.170
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.455
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 0 -11 0.0249
-6 7 -12 0.0399
-6 -2 13 0.0452
7 -7 10 0.0309
6 -5 -20 0.0625
6 1 15 0.0341
-6 5 20 0.0322
-4 -3 -19 0.0588
5 3 4 0.0271
2 -8 -10 0.0477
-4 -4 -5 0.0527
-8 6 8 0.0336
-1 7 9 0.0210

_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.073
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.7303 0.3654 -10.6567 -0.3934 -0.1180 0.9118
-6.4493 7.0491 -12.1729 -0.7828 -0.2317 -0.5776
-5.6502 -1.6910 13.1341 0.5472 0.1635 -0.8208
7.1526 -6.7452 10.2555 0.7000 0.2070 0.6835
6.1053 -5.0210 -19.5388 -0.1963 0.6647 0.7208
5.5726 1.4252 15.0444 0.2079 -0.6964 0.6869
-6.0470 5.0350 19.6911 0.1984 -0.6718 -0.7136
-3.8962 -2.6084 -19.3395 -0.2492 0.8365 -0.4880
4.9839 3.4307 3.7906 -0.2338 -0.6603 0.7137
2.2033 -7.8336 -9.6505 0.3312 0.9377 0.1054
-4.0283 -4.3788 -5.0091 0.2636 0.7449 -0.6129
-7.6637 6.3904 8.3024 -0.1827 -0.5187 -0.8352
-0.5349 7.3077 8.8912 -0.3317 -0.9385 0.0959

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            28401
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.878
_diffrn_reflns_theta_min         4.323
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -62.00 -36.00   0.50    0.19    --  -91.75  61.00  90.00   52
  2  ω    -29.00  27.00   0.50    0.05    --  -47.51  19.00  30.00  112
  3  ω    -29.00  27.00   0.50    0.05    --  -47.51  19.00 -60.00  112
  4  ω    -51.00 -26.00   0.50    0.19    --  -91.75  45.00 -90.00   50
  5  ω   -102.00 -75.00   0.50    0.19    --  -91.75   0.00 -90.00   54
  6  ω      8.00  69.00   0.50    0.05    --   47.51 -77.00  30.00  122
  7  ω    102.00 140.00   0.50    0.19    --  113.25  45.00 -30.00   76
  8  ω     97.00 140.00   0.50    0.19    --  113.25  61.00   0.00   86
  9  ω    130.00 163.00   0.50    0.19    --  113.25  30.00 -60.00   66
 10  ω    104.00 177.00   0.50    0.19    --  113.25  45.00-180.00  146
 11  ω    129.00 155.00   0.50    0.19    --  113.25 125.00 -60.00   52
 12  ω     96.00 122.00   0.50    0.19    --  113.25 125.00 -60.00   52
 13  ω    102.00 147.00   0.50    0.19    --  113.25  15.00-120.00   90
 14  ω    101.00 127.00   0.50    0.19    --  113.25  30.00 -60.00   52
 15  ω    100.00 153.00   0.50    0.19    --  113.25  15.00 -90.00  106
 16  ω    101.00 154.00   0.50    0.19    --  113.25  30.00  60.00  106
 17  ω    104.00 171.00   0.50    0.19    --  113.25  30.00  90.00  134
 18  ω    100.00 173.00   0.50    0.19    --  113.25  15.00 150.00  146
 19  ω     57.00  83.00   0.50    0.05    --   47.51-125.00 -90.00   52
 20  ω     45.00  70.00   0.50    0.19    --  113.25-125.00-150.00   50
 21  ω     78.00 111.00   0.50    0.19    --  113.25-125.00-150.00   66
 22  ω     71.00 106.00   0.50    0.19    --  113.25 -94.00-180.00   70
 23  ω     76.00 102.00   0.50    0.19    --  113.25 -94.00-120.00   52
 24  ω     52.00 106.00   0.50    0.19    --  113.25 -94.00 -60.00  108
 25  ω     48.00 106.00   0.50    0.19    --  113.25 -99.00 -19.35  116
 26  ω     42.00  72.00   0.50    0.19    --  113.25 -94.00-150.00   60
 27  ω     47.00 102.00   0.50    0.19    --  113.25 -94.00  30.00  110
 28  ω     78.00 104.00   0.50    0.19    --  113.25 -94.00  60.00   52
 29  ω     46.00  74.00   0.50    0.19    --  113.25 -94.00  60.00   56
 30  ω     43.00 106.00   0.50    0.19    --  113.25 -94.00 120.00  126
 31  ω     44.00  73.00   0.50    0.19    --  113.25 -94.00   0.00   58
 32  ω     77.00 103.00   0.50    0.19    --  113.25 -94.00   0.00   52
 33  ω     80.00 105.00   0.50    0.19    --  113.25 -94.00-150.00   50
 34  ω     42.00  68.00   0.50    0.19    --  113.25 -94.00-120.00   52
 35  ω     49.00  97.00   0.50    0.19    --  113.25 -94.00 -90.00   96
 36  ω     56.00  99.00   0.50    0.19    --  113.25 -94.00  90.00   86
 37  ω     43.00  99.00   0.50    0.19    --  113.25 -77.00 120.00  112
 38  ω     42.00  71.00   0.50    0.19    --  113.25 -61.00  60.00   58
 39  ω     46.00  72.00   0.50    0.19    --  113.25 -77.00 -30.00   52
 40  ω     42.00  69.00   0.50    0.19    --  113.25 -61.00 -90.00   54
 41  ω     42.00  67.00   0.50    0.19    --  113.25 -61.00-150.00   50
 42  ω     53.00  79.00   0.50    0.19    --  113.25 -77.00-120.00   52
 43  ω     42.00  68.00   0.50    0.19    --  113.25 -61.00 120.00   52
 44  ω   -120.00 -41.00   0.50    0.05    --  -47.51 -38.00  60.00  158
 45  ω   -116.00 -36.00   0.50    0.05    --  -47.51 -57.00 150.00  160
 46  ω    -83.00 -16.00   0.50    0.05    --  -47.51 125.00-150.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0130105000
_diffrn_orient_matrix_UB_12      -0.0780041000
_diffrn_orient_matrix_UB_13      0.0260264000
_diffrn_orient_matrix_UB_21      -0.0434383000
_diffrn_orient_matrix_UB_22      -0.1072258000
_diffrn_orient_matrix_UB_23      -0.0200399000
_diffrn_orient_matrix_UB_31      0.1274189000
_diffrn_orient_matrix_UB_32      0.0274912000
_diffrn_orient_matrix_UB_33      -0.0041423000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                3311
_reflns_number_total             3339
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 
;
 Flack x determined using 1601 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0162(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3339
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.115
_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)+(0.0314P)²+49.3217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0660
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
1.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.666667 0.333333 0.52434(2) 0.01918(14) Uani 1 3 d S T P . .
Br1 Br 0.51186(7) 0.55323(7) 0.52886(2) 0.02472(17) Uani 1 1 d . . . . .
Br2 Br 0.58268(8) 0.81091(7) 0.49923(2) 0.03084(19) Uani 1 1 d . . . . .
Br3 Br 0.75626(8) 0.89942(7) 0.44159(2) 0.03098(19) Uani 1 1 d . . . . .
Br4 Br 0.83098(6) 0.71599(7) 0.41173(2) 0.02601(17) Uani 1 1 d . . . . .
O1 O 0.6086(4) 0.4257(4) 0.49357(10) 0.0234(10) Uani 1 1 d . . . . .
O2 O 0.7572(5) 0.5033(5) 0.44845(11) 0.0286(10) Uani 1 1 d . . . . .
H2 H 0.758264 0.459935 0.461559 0.043 Uiso 1 1 calc R U . . .
N1 N 0.666667 0.333333 0.5793(3) 0.035(2) Uani 1 3 d S T P . .
N2 N 0.7813(6) 0.5330(6) 0.54650(13) 0.0286(12) Uani 1 1 d . . . . .
C1 C 0.6659(8) 0.4395(8) 0.58934(16) 0.0373(17) Uani 1 1 d . . . . .
H1A H 0.685756 0.450897 0.610050 0.045 Uiso 1 1 calc R U . . .
H1B H 0.585722 0.427441 0.587118 0.045 Uiso 1 1 calc R U . . .
C2 C 0.7508(7) 0.5485(8) 0.57334(18) 0.0316(16) Uani 1 1 d . . . . .
C3 C 0.7919(7) 0.6611(8) 0.58450(18) 0.0346(17) Uani 1 1 d . . . . .
H3 H 0.769526 0.671083 0.603233 0.041 Uiso 1 1 calc R U . . .
C4 C 0.8655(7) 0.7580(8) 0.5680(2) 0.041(2) Uani 1 1 d . . . . .
H4 H 0.894046 0.835224 0.575184 0.049 Uiso 1 1 calc R U . . .
C5 C 0.8970(7) 0.7407(7) 0.5405(2) 0.0352(18) Uani 1 1 d . . . . .
H5 H 0.947272 0.805524 0.528730 0.042 Uiso 1 1 calc R U . . .
C6 C 0.8538(7) 0.6280(8) 0.53113(17) 0.0306(16) Uani 1 1 d . . . . .
H6 H 0.876561 0.616473 0.512586 0.037 Uiso 1 1 calc R U . . .
C7 C 0.6396(6) 0.5311(6) 0.48304(15) 0.0209(12) Uani 1 1 d . . . . .
C8 C 0.6025(6) 0.6055(6) 0.49487(15) 0.0206(13) Uani 1 1 d . . . . .
C9 C 0.6352(6) 0.7141(6) 0.48251(15) 0.0229(13) Uani 1 1 d . . . . .
C10 C 0.7049(6) 0.7497(6) 0.45793(16) 0.0226(13) Uani 1 1 d . . . . .
C11 C 0.7437(6) 0.6764(6) 0.44642(15) 0.0214(13) Uani 1 1 d . . . . .
C12 C 0.7149(6) 0.5712(6) 0.45906(16) 0.0233(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.244(5) 3_665 ?
Eu1 O1 2.244(5) 2_655 ?
Eu1 O1 2.244(5) . ?
Eu1 N1 2.558(12) . ?
Eu1 N2 2.504(7) . ?
Eu1 N2 2.504(7) 2_655 ?
Eu1 N2 2.504(6) 3_665 ?
Br1 C8 1.891(7) . ?
Br2 C9 1.893(7) . ?
Br3 C10 1.892(7) . ?
Br4 C11 1.896(7) . ?
O1 C7 1.327(9) . ?
O2 H2 0.8400 . ?
O2 C12 1.359(9) . ?
N1 C1 1.477(9) 2_655 ?
N1 C1 1.477(9) . ?
N1 C1 1.477(9) 3_665 ?
N2 C2 1.358(10) . ?
N2 C6 1.338(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.501(13) . ?
C2 C3 1.397(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.395(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.367(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.405(10) . ?
C7 C12 1.408(8) . ?
C8 C9 1.393(10) . ?
C9 C10 1.392(8) . ?
C10 C11 1.403(10) . ?
C11 C12 1.370(10) . ?

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
O1 Eu1 O1 83.63(19) 3_665 2_655 ?
O1 Eu1 O1 83.63(19) 3_665 . ?
O1 Eu1 O1 83.63(19) 2_655 . ?
O1 Eu1 N1 129.66(13) 3_665 . ?
O1 Eu1 N1 129.65(13) . . ?
O1 Eu1 N1 129.66(13) 2_655 . ?
O1 Eu1 N2 86.6(2) 3_665 . ?
O1 Eu1 N2 164.5(2) 2_655 . ?
O1 Eu1 N2 164.5(2) . 3_665 ?
O1 Eu1 N2 83.4(2) . . ?
O1 Eu1 N2 86.6(2) . 2_655 ?
O1 Eu1 N2 83.4(2) 2_655 2_655 ?
O1 Eu1 N2 86.6(2) 2_655 3_665 ?
O1 Eu1 N2 164.5(2) 3_665 2_655 ?
O1 Eu1 N2 83.4(2) 3_665 3_665 ?
N2 Eu1 N1 65.68(16) 2_655 . ?
N2 Eu1 N1 65.68(16) 3_665 . ?
N2 Eu1 N1 65.68(16) . . ?
N2 Eu1 N2 104.22(18) . 2_655 ?
N2 Eu1 N2 104.22(18) 3_665 . ?
N2 Eu1 N2 104.22(18) 3_665 2_655 ?
C7 O1 Eu1 142.2(5) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Eu1 108.5(6) 2_655 . ?
C1 N1 Eu1 108.5(6) 3_665 . ?
C1 N1 Eu1 108.5(6) . . ?
C1 N1 C1 110.5(5) 2_655 . ?
C1 N1 C1 110.5(5) 3_665 . ?
C1 N1 C1 110.5(5) 3_665 2_655 ?
C2 N2 Eu1 117.9(6) . . ?
C6 N2 Eu1 122.2(5) . . ?
C6 N2 C2 118.6(7) . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
N1 C1 C2 113.1(7) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
N2 C2 C1 116.6(7) . . ?
N2 C2 C3 120.9(8) . . ?
C3 C2 C1 122.4(7) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(8) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(8) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.3(8) . . ?
C6 C5 H5 120.8 . . ?
N2 C6 C5 123.8(7) . . ?
N2 C6 H6 118.1 . . ?
C5 C6 H6 118.1 . . ?
O1 C7 C8 123.4(6) . . ?
O1 C7 C12 118.4(7) . . ?
C8 C7 C12 118.2(7) . . ?
C7 C8 Br1 116.7(5) . . ?
C9 C8 Br1 122.2(5) . . ?
C9 C8 C7 121.0(7) . . ?
C8 C9 Br2 119.4(5) . . ?
C10 C9 Br2 120.8(6) . . ?
C10 C9 C8 119.9(7) . . ?
C9 C10 Br3 120.9(6) . . ?
C9 C10 C11 119.1(7) . . ?
C11 C10 Br3 119.9(5) . . ?
C10 C11 Br4 121.0(5) . . ?
C12 C11 Br4 117.8(5) . . ?
C12 C11 C10 121.2(6) . . ?
O2 C12 C7 118.9(7) . . ?
O2 C12 C11 120.6(6) . . ?
C11 C12 C7 120.4(7) . . ?

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
Eu1 O1 C7 C8 -92.5(9) . . . . ?
Eu1 O1 C7 C12 86.5(8) . . . . ?
Eu1 N1 C1 C2 -44.7(7) . . . . ?
Eu1 N2 C2 C1 10.9(9) . . . . ?
Eu1 N2 C2 C3 -165.6(6) . . . . ?
Eu1 N2 C6 C5 164.7(6) . . . . ?
Br1 C8 C9 Br2 -2.5(9) . . . . ?
Br1 C8 C9 C10 178.2(5) . . . . ?
Br2 C9 C10 Br3 3.4(7) . . . . ?
Br2 C9 C10 C11 179.0(6) . . . . ?
Br3 C10 C11 Br4 -8.1(8) . . . . ?
Br3 C10 C11 C12 175.2(5) . . . . ?
Br4 C11 C12 O2 6.1(9) . . . . ?
Br4 C11 C12 C7 -173.0(5) . . . . ?
O1 C7 C8 Br1 3.9(9) . . . . ?
O1 C7 C8 C9 -178.3(6) . . . . ?
O1 C7 C12 O2 -3.0(9) . . . . ?
O1 C7 C12 C11 176.1(7) . . . . ?
N1 C1 C2 N2 24.2(10) . . . . ?
N1 C1 C2 C3 -159.4(7) . . . . ?
N2 C2 C3 C4 -0.5(12) . . . . ?
C1 N1 C1 C2 -163.4(7) 2_655 . . . ?
C1 N1 C1 C2 74.0(12) 3_665 . . . ?
C1 C2 C3 C4 -176.8(8) . . . . ?
C2 N2 C6 C5 -1.8(11) . . . . ?
C2 C3 C4 C5 -0.2(13) . . . . ?
C3 C4 C5 C6 -0.1(13) . . . . ?
C4 C5 C6 N2 1.1(12) . . . . ?
C6 N2 C2 C1 177.9(7) . . . . ?
C6 N2 C2 C3 1.4(11) . . . . ?
C7 C8 C9 Br2 179.9(5) . . . . ?
C7 C8 C9 C10 0.5(10) . . . . ?
C8 C7 C12 O2 176.0(7) . . . . ?
C8 C7 C12 C11 -4.8(9) . . . . ?
C8 C9 C10 Br3 -177.3(6) . . . . ?
C8 C9 C10 C11 -1.7(8) . . . . ?
C9 C10 C11 Br4 176.3(5) . . . . ?
C9 C10 C11 C12 -0.5(10) . . . . ?
C10 C11 C12 O2 -177.1(7) . . . . ?
C10 C11 C12 C7 3.8(10) . . . . ?
C12 C7 C8 Br1 -175.1(5) . . . . ?
C12 C7 C8 C9 2.7(10) . . . . ?

_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 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.816
_exptl_crystal_recrystallization_method 'From reaction'
####################################################################### 
# 
# 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_sb01-05-sm2-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405951'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 N4 O6 Sm'
_chemical_formula_sum            'C36 H21 Br12 N4 O6 Sm'
_chemical_formula_weight         1714.84
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 Br12 O6 N5 Sm1'
_chemical_oxdiff_usercomment     'clear cube in oil at 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 '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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.17530(10)
_cell_length_b                   13.17530(10)
_cell_length_c                   46.6188(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7008.30(12)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    19245
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      78.9060
_cell_measurement_theta_min      4.0050
_shelx_estimated_absorpt_T_max   0.244
_shelx_estimated_absorpt_T_min   0.143
_exptl_absorpt_coefficient_mu    21.863
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4770
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 0 -20 0.0606
-1 6 -19 0.0690
4 5 3 0.0529
5 -1 24 0.0671
2 -5 23 0.0780
-3 -5 -1 0.0469
-7 5 -18 0.0577
-8 6 -7 0.0567
-5 5 22 0.0614
6 -5 20 0.0712
8 -7 0 0.0665
5 -5 -23 0.0507
-5 7 -15 0.0569
-5 8 -6 0.0549
-2 7 17 0.0519
3 0 27 0.0714
5 -5 22 0.0734
2 -7 -16 0.0376
-8 1 0 0.0624
-6 3 -20 0.0591
7 0 -11 0.0501
6 -3 22 0.0636
-2 -2 26 0.0735
-6 0 13 0.0675

_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.09
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.3201 -0.3533 -20.2403 0.1513 -0.5112 0.8460
-0.9540 6.1284 -19.2637 -0.2091 0.7024 0.6804
3.6948 4.8036 2.5475 -0.2789 0.9396 -0.1984
5.1419 -1.2410 23.5580 -0.0858 0.2912 -0.9528
2.3968 -5.4494 23.2800 0.1458 -0.4889 -0.8600
-3.4818 -5.0185 -1.1589 0.2816 -0.9485 0.1449
-6.6552 4.9958 -17.7355 0.3565 0.1068 0.9282
-7.8846 6.2235 -7.1052 0.6687 0.1993 0.7163
-5.1952 4.6956 22.4598 0.9214 0.2734 -0.2761
6.2384 -4.6139 19.7730 -0.2784 -0.0836 -0.9568
8.0569 -6.5119 0.3065 -0.8065 -0.2400 -0.5403
4.9432 -4.5090 -23.2507 -0.9100 -0.2700 0.3145
-5.4270 7.1503 -14.7705 0.3045 0.4987 0.8115
-5.0784 8.2949 -6.2990 0.4272 0.6990 0.5736
-1.7236 6.8445 16.7614 0.5024 0.8207 -0.2722
2.9519 0.2603 27.4970 0.2024 0.3296 -0.9222
5.1210 -5.0163 22.0560 -0.1338 -0.2200 -0.9663
1.8327 -6.9519 -16.2939 -0.5052 -0.8255 0.2516
-7.8956 1.1005 0.3754 0.7693 -0.4711 0.4316
-6.4201 2.8053 -19.9191 0.2819 -0.1734 0.9436
6.8019 0.1051 -11.4725 -0.8521 0.5214 -0.0451
5.8325 -2.9293 22.1268 -0.1876 0.1158 -0.9754
-1.9771 -2.2081 26.3866 0.6393 -0.3905 -0.6624
-6.4605 -0.3402 13.4418 0.8526 -0.5216 -0.0317

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            29025
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.189
_diffrn_reflns_theta_min         4.314
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      ?
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0957241000
_diffrn_orient_matrix_UB_12      0.0062417000
_diffrn_orient_matrix_UB_13      0.0175787000
_diffrn_orient_matrix_UB_21      0.0784559000
_diffrn_orient_matrix_UB_22      0.1340414000
_diffrn_orient_matrix_UB_23      0.0022962000
_diffrn_orient_matrix_UB_31      -0.0539082000
_diffrn_orient_matrix_UB_32      0.0149623000
_diffrn_orient_matrix_UB_33      -0.0278911000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.923
_reflns_Friedel_fraction_max     0.889
_reflns_number_gt                3181
_reflns_number_total             3222
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.716
_refine_diff_density_min         -1.249
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 
;
 Flack x determined using 1447 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0289
_refine_ls_restrained_S_all      1.124
_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)+(0.0464P)²+39.1781P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0803
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.333333 0.666667 0.47558(2) 0.01807(16) Uani 1 3 d S T P . .
Br1 Br 0.55365(7) 0.51246(8) 0.47134(2) 0.02237(19) Uani 1 1 d . . . . .
Br2 Br 0.81097(8) 0.58337(9) 0.50087(2) 0.0293(2) Uani 1 1 d . . . . .
Br3 Br 0.89883(8) 0.75595(9) 0.55854(2) 0.0300(2) Uani 1 1 d . . . . .
Br4 Br 0.71604(7) 0.83121(7) 0.58824(2) 0.0240(2) Uani 1 1 d . . . . .
O1 O 0.4262(5) 0.6097(5) 0.50642(12) 0.0220(12) Uani 1 1 d . . . . .
O2 O 0.5040(5) 0.7579(6) 0.55160(13) 0.0265(12) Uani 1 1 d . . . . .
H2 H 0.453303 0.749315 0.539433 0.040 Uiso 1 1 calc R U . . .
N1 N 0.333333 0.666667 0.4205(3) 0.034(3) Uani 1 3 d S T P . .
N2 N 0.5339(7) 0.7821(7) 0.45298(17) 0.0282(15) Uani 1 1 d . . . . .
C1 C 0.4402(10) 0.6664(11) 0.4106(2) 0.044(2) Uani 1 1 d . . . . .
H1A H 0.451778 0.686164 0.389926 0.052 Uiso 1 1 calc R U . . .
H1B H 0.428417 0.586477 0.412853 0.052 Uiso 1 1 calc R U . . .
C2 C 0.5481(9) 0.7509(8) 0.4265(2) 0.033(2) Uani 1 1 d . . . . .
C3 C 0.6607(10) 0.7920(8) 0.4152(2) 0.036(2) Uani 1 1 d . . . . .
H3 H 0.670396 0.769803 0.396446 0.044 Uiso 1 1 calc R U . . .
C4 C 0.7567(10) 0.8647(8) 0.4315(3) 0.042(3) Uani 1 1 d . . . . .
H4 H 0.833470 0.892911 0.424214 0.051 Uiso 1 1 calc R U . . .
C5 C 0.7405(9) 0.8973(8) 0.4594(2) 0.034(2) Uani 1 1 d . . . . .
H5 H 0.805259 0.947273 0.471174 0.041 Uiso 1 1 calc R U . . .
C6 C 0.6284(9) 0.8541(8) 0.4684(2) 0.0297(19) Uani 1 1 d . . . . .
H6 H 0.616351 0.876534 0.486878 0.036 Uiso 1 1 calc R U . . .
C7 C 0.5316(7) 0.6398(7) 0.51705(17) 0.0186(14) Uani 1 1 d . . . . .
C8 C 0.6060(6) 0.6031(7) 0.50527(17) 0.0176(14) Uani 1 1 d . . . . .
C9 C 0.7143(7) 0.6361(7) 0.51764(17) 0.0219(15) Uani 1 1 d . . . . .
C10 C 0.7491(7) 0.7051(7) 0.54206(18) 0.0194(14) Uani 1 1 d . . . . .
C11 C 0.6766(7) 0.7444(7) 0.55374(17) 0.0201(15) Uani 1 1 d . . . . .
C12 C 0.5720(7) 0.7153(7) 0.54072(18) 0.0201(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.246(5) 2_665 ?
Sm1 O1 2.246(5) 3_565 ?
Sm1 O1 2.246(5) . ?
Sm1 N1 2.566(14) . ?
Sm1 N2 2.527(8) 3_565 ?
Sm1 N2 2.527(8) 2_665 ?
Sm1 N2 2.527(8) . ?
Br1 C8 1.892(8) . ?
Br2 C9 1.898(8) . ?
Br3 C10 1.900(8) . ?
Br4 C11 1.890(8) . ?
O1 C7 1.333(10) . ?
O2 H2 0.8400 . ?
O2 C12 1.370(10) . ?
N1 C1 1.484(12) 2_665 ?
N1 C1 1.484(12) 3_565 ?
N1 C1 1.484(12) . ?
N2 C2 1.342(12) . ?
N2 C6 1.336(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.493(16) . ?
C2 C3 1.404(14) . ?
C3 H3 0.9500 . ?
C3 C4 1.373(18) . ?
C4 H4 0.9500 . ?
C4 C5 1.416(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.357(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.404(10) . ?
C7 C12 1.400(10) . ?
C8 C9 1.392(11) . ?
C9 C10 1.384(9) . ?
C10 C11 1.403(11) . ?
C11 C12 1.374(11) . ?

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
O1 Sm1 O1 83.4(2) 2_665 . ?
O1 Sm1 O1 83.4(2) 2_665 3_565 ?
O1 Sm1 O1 83.4(2) . 3_565 ?
O1 Sm1 N1 129.79(15) 2_665 . ?
O1 Sm1 N1 129.79(15) 3_565 . ?
O1 Sm1 N1 129.79(15) . . ?
O1 Sm1 N2 87.1(2) 2_665 . ?
O1 Sm1 N2 83.5(2) 3_565 3_565 ?
O1 Sm1 N2 83.5(2) 2_665 2_665 ?
O1 Sm1 N2 83.5(2) . . ?
O1 Sm1 N2 87.1(2) 3_565 2_665 ?
O1 Sm1 N2 87.1(2) . 3_565 ?
O1 Sm1 N2 164.7(2) 3_565 . ?
O1 Sm1 N2 164.7(2) 2_665 3_565 ?
O1 Sm1 N2 164.7(2) . 2_665 ?
N2 Sm1 N1 65.36(19) . . ?
N2 Sm1 N1 65.35(19) 2_665 . ?
N2 Sm1 N1 65.35(19) 3_565 . ?
N2 Sm1 N2 103.8(2) 3_565 . ?
N2 Sm1 N2 103.8(2) 2_665 . ?
N2 Sm1 N2 103.8(2) 2_665 3_565 ?
C7 O1 Sm1 143.0(5) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Sm1 108.2(7) 3_565 . ?
C1 N1 Sm1 108.2(7) 2_665 . ?
C1 N1 Sm1 108.2(7) . . ?
C1 N1 C1 110.7(6) 2_665 3_565 ?
C1 N1 C1 110.7(6) 3_565 . ?
C1 N1 C1 110.7(6) 2_665 . ?
C2 N2 Sm1 117.6(7) . . ?
C6 N2 Sm1 121.7(6) . . ?
C6 N2 C2 119.2(8) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
N1 C1 C2 113.2(8) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
N2 C2 C1 117.3(9) . . ?
N2 C2 C3 120.7(10) . . ?
C3 C2 C1 121.9(9) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.1(9) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.7(9) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 121.5 . . ?
C6 C5 C4 117.0(10) . . ?
C6 C5 H5 121.5 . . ?
N2 C6 C5 124.3(9) . . ?
N2 C6 H6 117.8 . . ?
C5 C6 H6 117.8 . . ?
O1 C7 C8 123.7(7) . . ?
O1 C7 C12 118.3(7) . . ?
C12 C7 C8 118.0(8) . . ?
C7 C8 Br1 116.6(6) . . ?
C9 C8 Br1 122.5(6) . . ?
C9 C8 C7 120.9(8) . . ?
C8 C9 Br2 119.1(6) . . ?
C10 C9 Br2 121.1(7) . . ?
C10 C9 C8 119.8(8) . . ?
C9 C10 Br3 120.6(7) . . ?
C9 C10 C11 119.9(8) . . ?
C11 C10 Br3 119.4(6) . . ?
C10 C11 Br4 121.5(6) . . ?
C12 C11 Br4 118.6(6) . . ?
C12 C11 C10 119.9(7) . . ?
O2 C12 C7 119.3(8) . . ?
O2 C12 C11 119.5(7) . . ?
C11 C12 C7 121.2(8) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84 2.29 2.701(8) 110.9 . yes
O2 H2 O1 0.84 2.14 2.904(8) 151.3 2_665 yes
C1 H1B Br3 0.99 2.99 3.728(12) 132.0 12_454 yes

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
Sm1 O1 C7 C8 -91.6(10) . . . . ?
Sm1 O1 C7 C12 86.4(10) . . . . ?
Sm1 N1 C1 C2 -44.7(9) . . . . ?
Sm1 N2 C2 C1 11.2(11) . . . . ?
Sm1 N2 C2 C3 -165.6(7) . . . . ?
Sm1 N2 C6 C5 164.3(7) . . . . ?
Br1 C8 C9 Br2 -2.7(10) . . . . ?
Br1 C8 C9 C10 178.3(5) . . . . ?
Br2 C9 C10 Br3 3.2(8) . . . . ?
Br2 C9 C10 C11 179.0(7) . . . . ?
Br3 C10 C11 Br4 -7.8(9) . . . . ?
Br3 C10 C11 C12 175.2(6) . . . . ?
Br4 C11 C12 O2 5.5(11) . . . . ?
Br4 C11 C12 C7 -172.5(6) . . . . ?
O1 C7 C8 Br1 3.3(10) . . . . ?
O1 C7 C8 C9 -179.0(7) . . . . ?
O1 C7 C12 O2 -1.8(10) . . . . ?
O1 C7 C12 C11 176.2(8) . . . . ?
N1 C1 C2 N2 24.0(13) . . . . ?
N1 C1 C2 C3 -159.2(9) . . . . ?
N2 C2 C3 C4 0.2(14) . . . . ?
C1 N1 C1 C2 -163.1(9) 3_565 . . . ?
C1 N1 C1 C2 73.7(15) 2_665 . . . ?
C1 C2 C3 C4 -176.6(10) . . . . ?
C2 N2 C6 C5 -1.4(13) . . . . ?
C2 C3 C4 C5 -0.4(15) . . . . ?
C3 C4 C5 C6 -0.2(14) . . . . ?
C4 C5 C6 N2 1.1(14) . . . . ?
C6 N2 C2 C1 177.5(9) . . . . ?
C6 N2 C2 C3 0.7(13) . . . . ?
C7 C8 C9 Br2 179.8(6) . . . . ?
C7 C8 C9 C10 0.7(11) . . . . ?
C8 C7 C12 O2 176.3(7) . . . . ?
C8 C7 C12 C11 -5.8(10) . . . . ?
C8 C9 C10 Br3 -177.8(7) . . . . ?
C8 C9 C10 C11 -1.9(10) . . . . ?
C9 C10 C11 Br4 176.3(5) . . . . ?
C9 C10 C11 C12 -0.7(11) . . . . ?
C10 C11 C12 O2 -177.4(7) . . . . ?
C10 C11 C12 C7 4.7(12) . . . . ?
C12 C7 C8 Br1 -174.6(5) . . . . ?
C12 C7 C8 C9 3.1(11) . . . . ?

_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 1.495
_oxdiff_exptl_absorpt_empirical_full_min 0.840
_exptl_crystal_recrystallization_method 'From reaction'
####################################################################### 
# 
# 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_sb01-05-er2-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405955'
loop_
_audit_author_name
_audit_author_address
'Robert W Gable'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2025-01-23 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 Er N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Er N4 O6'
_chemical_formula_weight         1731.75
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C36 Er Br12 O6 N4'
_chemical_oxdiff_usercomment     'Small colourless cube in oil 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -9.4367 3.9380 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.1015(2)
_cell_length_b                   13.1015(2)
_cell_length_c                   46.1778(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6864.5(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    10493
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      79.9090
_cell_measurement_theta_min      4.1460
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.089
_exptl_absorpt_correction_T_max  0.576
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4806
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -4 25 0.0219
-4 -3 -18 0.0384
-1 7 -9 0.0099
8 -6 2 0.0273
-5 2 24 0.0294
-8 6 0 0.0225
-5 5 -22 0.0240
4 -1 -26 0.0278
-3 -3 23 0.0408
-7 0 10 0.0383
-8 2 -5 0.0372
-5 4 -24 0.0238
6 1 -11 0.0119
3 4 17 0.0114
-4 -3 -17 0.0388
-1 7 -7 0.0094

_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.047
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.3064 -3.7691 24.9834 -0.0082 -0.0313 0.9995
-3.6374 -3.2394 -17.6166 0.1978 0.8250 -0.5293
-0.9615 7.4468 -9.1626 -0.1945 -0.8142 -0.5470
8.2848 -5.6856 2.4473 -0.7722 0.1855 0.6076
-5.1519 2.3917 23.8334 0.9065 -0.2165 0.3625
-8.3399 5.6041 0.1805 0.8218 -0.1973 -0.5345
-5.2296 4.5256 -22.3070 0.1384 -0.0343 -0.9898
3.9589 -1.4710 -26.4439 -0.8333 0.1988 -0.5159
-2.7001 -2.7500 23.0124 0.7265 0.3021 0.6172
-6.7072 -0.4304 10.1278 0.9235 0.3833 0.0142
-7.9936 1.7612 -4.6409 0.7876 0.3264 -0.5227
-4.9416 3.9178 -23.6586 0.0974 0.0395 -0.9945
6.4675 0.6401 -11.4203 -0.9215 -0.3825 -0.0671
3.4979 3.5653 16.6967 -0.2036 -0.8494 0.4870
-3.5467 -3.4544 -17.0171 0.2017 0.8412 -0.5016
-0.5983 7.4319 -7.2199 -0.2042 -0.8546 -0.4775

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            26953
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.198
_diffrn_reflns_theta_min         4.342
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00  76.00   0.50    0.08    --   47.51-125.00 -90.00   84
  2  ω     51.00  95.00   0.50    0.32    --  113.25-125.00-150.00   88
  3  ω     86.00 111.00   0.50    0.32    --  113.25-125.00-120.00   50
  4  ω     47.00  72.00   0.50    0.32    --  113.25-125.00-180.00   50
  5  ω     55.00  81.00   0.50    0.32    --  113.25-125.00-120.00   52
  6  ω     59.00 106.00   0.50    0.32    --  113.25-108.00-127.96   94
  7  ω     52.00  78.00   0.50    0.32    --  113.25-125.00 -30.00   52
  8  ω     82.00 107.00   0.50    0.32    --  113.25-103.00 -18.05   50
  9  ω     44.00  76.00   0.50    0.32    --  113.25-103.00 -18.05   64
 10  ω     48.00 111.00   0.50    0.32    --  113.25-125.00  90.00  126
 11  ω     47.00 107.00   0.50    0.32    --  113.25-125.00 120.00  120
 12  ω     57.00 103.00   0.50    0.32    --  113.25 -94.00 120.00   92
 13  ω     71.00 105.00   0.50    0.32    --  113.25 -94.00  90.00   68
 14  ω     46.00 100.00   0.50    0.32    --  113.25 -94.00   0.00  108
 15  ω     80.00 106.00   0.50    0.32    --  113.25 -94.00 -60.00   52
 16  ω     77.00 104.00   0.50    0.32    --  113.25 -94.00-120.00   54
 17  ω     79.00 105.00   0.50    0.32    --  113.25 -94.00 -90.00   52
 18  ω     43.00  76.00   0.50    0.32    --  113.25 -77.00   0.00   66
 19  ω     44.00  71.00   0.50    0.32    --  113.25 -61.00  60.00   54
 20  ω     45.00  70.00   0.50    0.32    --  113.25 -77.00 -60.00   50
 21  ω     42.00  70.00   0.50    0.32    --  113.25 -77.00 -90.00   56
 22  ω     44.00  78.00   0.50    0.32    --  113.25 -77.00-150.00   68
 23  ω     -6.00  30.00   0.50    0.08    --   47.51 -19.00 150.00   72
 24  ω    -18.00  29.00   0.50    0.08    --   47.51 -19.00  90.00   94
 25  ω     42.00  68.00   0.50    0.32    --  113.25 -61.00 120.00   52
 26  ω     42.00  67.00   0.50    0.32    --  113.25 -61.00  30.00   50
 27  ω     44.00  69.00   0.50    0.32    --  113.25 -77.00-120.00   50
 28  ω    103.00 178.00   0.50    0.32    --  113.25  15.00 -60.00  150
 29  ω    148.00 173.00   0.50    0.32    --  113.25  45.00-120.00   50
 30  ω    105.00 131.00   0.50    0.32    --  113.25  45.00-120.00   52
 31  ω    107.00 143.00   0.50    0.32    --  113.25  30.00-150.00   72
 32  ω    111.00 178.00   0.50    0.32    --  113.25  45.00  30.00  134
 33  ω    122.00 162.00   0.50    0.32    --  113.25  45.00  90.00   80
 34  ω    103.00 176.00   0.50    0.32    --  113.25  45.00 120.00  146
 35  ω    148.00 178.00   0.50    0.32    --  113.25  15.00 150.00   60
 36  ω    103.00 141.00   0.50    0.32    --  113.25  15.00  60.00   76
 37  ω    146.00 174.00   0.50    0.32    --  113.25  15.00  60.00   56
 38  ω    112.00 178.00   0.50    0.32    --  113.25  30.00   0.00  132
 39  ω     50.00 105.00   0.50    0.08    --   47.51  19.00  90.00  110
 40  ω    -22.00  20.00   0.50    0.08    --  -47.51  77.00  60.00   84
 41  ω    -63.00 -26.00   0.50    0.08    --  -47.51  77.00  60.00   74
 42  ω    -50.00 -25.00   0.50    0.32    --  -91.75  45.00  90.00   50
 43  ω    -30.00  26.00   0.50    0.08    --  -47.51  19.00  60.00  112
 44  ω    -55.00  22.00   0.50    0.08    --  -47.51  57.00 -30.00  154
 45  ω    -82.00 -55.00   0.50    0.32    --  -91.75 125.00-120.00   54
 46  ω    -67.00 -37.00   0.50    0.08    --  -47.51 -38.00 -90.00   60
 47  ω   -118.00 -85.00   0.50    0.08    --  -47.51 -38.00 -90.00   66
 48  ω   -109.00 -80.00   0.50    0.32    --  -91.75 -30.00 150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1123868000
_diffrn_orient_matrix_UB_12      -0.0211165000
_diffrn_orient_matrix_UB_13      0.0158599000
_diffrn_orient_matrix_UB_21      -0.0636859000
_diffrn_orient_matrix_UB_22      -0.1296700000
_diffrn_orient_matrix_UB_23      -0.0098388000
_diffrn_orient_matrix_UB_31      0.0418330000
_diffrn_orient_matrix_UB_32      -0.0340103000
_diffrn_orient_matrix_UB_33      0.0276640000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.905
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                2929
_reflns_number_total             3133
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.486
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 
;
 Flack x determined using 1251 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3133
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.125
_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)+(0.0673P)²+43.0451P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1169
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.333333 0.666667 0.47600(3) 0.0180(2) Uani 1 3 d S T P . .
Br1 Br 0.55044(11) 0.50946(11) 0.47079(2) 0.0228(3) Uani 1 1 d . . . . .
Br2 Br 0.80827(12) 0.57972(14) 0.50079(3) 0.0279(3) Uani 1 1 d . . . . .
Br3 Br 0.89857(11) 0.75647(13) 0.55830(3) 0.0279(3) Uani 1 1 d . . . . .
Br4 Br 0.71479(11) 0.83167(11) 0.58848(3) 0.0245(3) Uani 1 1 d . . . . .
O1 O 0.4218(8) 0.6072(8) 0.50599(18) 0.0206(18) Uani 1 1 d . U . . .
O2 O 0.5007(8) 0.7567(9) 0.55157(18) 0.0235(16) Uani 1 1 d . . . . .
H2 H 0.442433 0.736872 0.540674 0.035 Uiso 1 1 calc R U . . .
N1 N 0.333333 0.666667 0.4222(5) 0.030(4) Uani 1 3 d S T P . .
N2 N 0.5309(10) 0.7788(10) 0.4551(2) 0.024(2) Uani 1 1 d . . . . .
C1 C 0.4391(12) 0.6650(14) 0.4120(3) 0.034(3) Uani 1 1 d . . . . .
H1A H 0.450982 0.685331 0.391152 0.041 Uiso 1 1 calc R U . . .
H1B H 0.426898 0.584553 0.414251 0.041 Uiso 1 1 calc R U . . .
C2 C 0.5465(13) 0.7500(11) 0.4284(3) 0.027(3) Uani 1 1 d . . . . .
C3 C 0.6613(12) 0.7929(11) 0.4171(3) 0.028(3) Uani 1 1 d . . . . .
H3 H 0.671209 0.770698 0.398205 0.034 Uiso 1 1 calc R U . . .
C4 C 0.7596(13) 0.8674(13) 0.4336(4) 0.034(3) Uani 1 1 d . . . . .
H4 H 0.837344 0.895927 0.426494 0.041 Uiso 1 1 calc R U . . .
C5 C 0.7385(12) 0.8986(11) 0.4612(4) 0.030(3) Uani 1 1 d . . . . .
H5 H 0.802712 0.951303 0.473025 0.036 Uiso 1 1 calc R U . . .
C6 C 0.6254(13) 0.8530(13) 0.4710(3) 0.030(3) Uani 1 1 d . . . . .
H6 H 0.613030 0.874529 0.489753 0.036 Uiso 1 1 calc R U . . .
C7 C 0.5288(10) 0.6387(10) 0.5166(3) 0.020(2) Uani 1 1 d . . . . .
C8 C 0.6030(10) 0.6015(11) 0.5050(3) 0.022(2) Uani 1 1 d . . . . .
C9 C 0.7117(11) 0.6336(12) 0.5172(3) 0.024(2) Uani 1 1 d . . . . .
C10 C 0.7486(10) 0.7057(11) 0.5418(3) 0.020(2) Uani 1 1 d . . . . .
C11 C 0.6743(11) 0.7442(11) 0.5539(3) 0.021(2) Uani 1 1 d . . . . .
C12 C 0.5684(10) 0.7141(11) 0.5408(3) 0.018(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.184(7) 3_565 ?
Er1 O1 2.184(7) . ?
Er1 O1 2.184(7) 2_665 ?
Er1 N1 2.48(2) . ?
Er1 N2 2.447(11) . ?
Er1 N2 2.447(11) 2_665 ?
Er1 N2 2.447(11) 3_565 ?
Br1 C8 1.898(14) . ?
Br2 C9 1.888(13) . ?
Br3 C10 1.892(11) . ?
Br4 C11 1.881(13) . ?
O1 C7 1.340(15) . ?
O2 H2 0.8400 . ?
O2 C12 1.356(15) . ?
N1 C1 1.473(16) . ?
N1 C1 1.473(16) 3_565 ?
N1 C1 1.473(16) 2_665 ?
N2 C2 1.335(17) . ?
N2 C6 1.345(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.49(2) . ?
C2 C3 1.416(18) . ?
C3 H3 0.9500 . ?
C3 C4 1.39(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.41(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.368(18) . ?
C6 H6 0.9500 . ?
C7 C8 1.393(18) . ?
C7 C12 1.408(14) . ?
C8 C9 1.386(18) . ?
C9 C10 1.400(13) . ?
C10 C11 1.415(17) . ?
C11 C12 1.378(17) . ?

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
O1 Er1 O1 84.1(3) 3_565 2_665 ?
O1 Er1 O1 84.1(3) 3_565 . ?
O1 Er1 O1 84.1(3) 2_665 . ?
O1 Er1 N1 129.3(2) 3_565 . ?
O1 Er1 N1 129.3(2) . . ?
O1 Er1 N1 129.3(2) 2_665 . ?
O1 Er1 N2 82.7(3) 3_565 3_565 ?
O1 Er1 N2 82.7(3) . . ?
O1 Er1 N2 85.2(4) 3_565 2_665 ?
O1 Er1 N2 163.8(3) 2_665 3_565 ?
O1 Er1 N2 163.8(3) . 2_665 ?
O1 Er1 N2 85.2(4) 2_665 . ?
O1 Er1 N2 85.2(4) . 3_565 ?
O1 Er1 N2 163.8(3) 3_565 . ?
O1 Er1 N2 82.7(3) 2_665 2_665 ?
N2 Er1 N1 66.8(3) 3_565 . ?
N2 Er1 N1 66.8(3) 2_665 . ?
N2 Er1 N1 66.8(3) . . ?
N2 Er1 N2 105.5(3) . 3_565 ?
N2 Er1 N2 105.5(3) 2_665 3_565 ?
N2 Er1 N2 105.5(3) 2_665 . ?
C7 O1 Er1 141.5(8) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Er1 108.6(10) 3_565 . ?
C1 N1 Er1 108.6(10) 2_665 . ?
C1 N1 Er1 108.6(10) . . ?
C1 N1 C1 110.3(10) 2_665 3_565 ?
C1 N1 C1 110.3(10) 3_565 . ?
C1 N1 C1 110.3(10) 2_665 . ?
C2 N2 Er1 117.4(9) . . ?
C2 N2 C6 119.5(12) . . ?
C6 N2 Er1 122.3(9) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C2 111.7(11) . . ?
H1A C1 H1B 107.9 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
N2 C2 C1 117.3(12) . . ?
N2 C2 C3 120.7(13) . . ?
C3 C2 C1 121.9(12) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(13) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.8(12) . . ?
C5 C4 H4 121.6 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0(14) . . ?
C6 C5 H5 120.0 . . ?
N2 C6 C5 122.7(13) . . ?
N2 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
O1 C7 C8 123.9(11) . . ?
O1 C7 C12 117.9(12) . . ?
C8 C7 C12 118.2(12) . . ?
C7 C8 Br1 116.5(9) . . ?
C9 C8 Br1 121.4(10) . . ?
C9 C8 C7 122.0(12) . . ?
C8 C9 Br2 120.2(10) . . ?
C8 C9 C10 119.2(13) . . ?
C10 C9 Br2 120.6(11) . . ?
C9 C10 Br3 120.7(10) . . ?
C9 C10 C11 119.6(12) . . ?
C11 C10 Br3 119.6(9) . . ?
C10 C11 Br4 121.2(9) . . ?
C12 C11 Br4 118.9(9) . . ?
C12 C11 C10 119.9(11) . . ?
O2 C12 C7 119.5(12) . . ?
O2 C12 C11 119.6(11) . . ?
C11 C12 C7 120.9(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84 2.25 2.704(12) 114.0 . yes
O2 H2 O1 0.84 2.17 2.843(12) 137.6 2_665 yes
C1 H1B Br3 0.99 3.00 3.727(15) 131.1 12_454 yes

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
Er1 O1 C7 C8 -93.6(16) . . . . ?
Er1 O1 C7 C12 86.1(14) . . . . ?
Er1 N1 C1 C2 -44.7(12) . . . . ?
Er1 N2 C2 C1 9.1(15) . . . . ?
Er1 N2 C2 C3 -166.9(9) . . . . ?
Er1 N2 C6 C5 167.2(10) . . . . ?
Br1 C8 C9 Br2 -2.9(16) . . . . ?
Br1 C8 C9 C10 177.4(8) . . . . ?
Br2 C9 C10 Br3 2.6(12) . . . . ?
Br2 C9 C10 C11 -179.4(11) . . . . ?
Br3 C10 C11 Br4 -6.6(15) . . . . ?
Br3 C10 C11 C12 175.6(9) . . . . ?
Br4 C11 C12 O2 5.8(16) . . . . ?
Br4 C11 C12 C7 -173.4(8) . . . . ?
O1 C7 C8 Br1 4.1(17) . . . . ?
O1 C7 C8 C9 -178.2(12) . . . . ?
O1 C7 C12 O2 -3.2(15) . . . . ?
O1 C7 C12 C11 176.0(12) . . . . ?
N1 C1 C2 N2 25.1(18) . . . . ?
N1 C1 C2 C3 -158.9(13) . . . . ?
N2 C2 C3 C4 -1.0(19) . . . . ?
C1 N1 C1 C2 -163.6(13) 3_565 . . . ?
C1 N1 C1 C2 74(2) 2_665 . . . ?
C1 C2 C3 C4 -176.9(13) . . . . ?
C2 N2 C6 C5 -2(2) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
C3 C4 C5 C6 2(2) . . . . ?
C4 C5 C6 N2 -1(2) . . . . ?
C6 N2 C2 C1 178.5(12) . . . . ?
C6 N2 C2 C3 2.5(18) . . . . ?
C7 C8 C9 Br2 179.5(10) . . . . ?
C7 C8 C9 C10 -0.2(18) . . . . ?
C8 C7 C12 O2 176.5(12) . . . . ?
C8 C7 C12 C11 -4.3(15) . . . . ?
C8 C9 C10 Br3 -177.6(11) . . . . ?
C8 C9 C10 C11 0.3(15) . . . . ?
C9 C10 C11 Br4 175.4(8) . . . . ?
C9 C10 C11 C12 -2.4(17) . . . . ?
C10 C11 C12 O2 -176.3(11) . . . . ?
C10 C11 C12 C7 4.4(18) . . . . ?
C12 C7 C8 Br1 -175.5(8) . . . . ?
C12 C7 C8 C9 2.1(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.789

# start Validation Reply Form
_vrf_PLAT342_sb01-05-er2-xrd-100k_abs 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02073 Ang.  
RESPONSE: Due to refining light atoms in the presence of several Br & Y atoms, 
          slight disorder of the crystal and slightly high Rint value.
;
_vrf_PLAT973_sb01-05-er2-xrd-100k_abs 
;
PROBLEM: Check Calcd Positive Resid. Density on       Er1       1.65 eA-3  
RESPONSE: Due to slight disorder of the crystal.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_sb01-05-gd2-xrd-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405956'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 Gd N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Gd N4 O6'
_chemical_formula_weight         1721.74
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Gd C36 Br12 O6 N4'
_chemical_oxdiff_usercomment     'clear cube in oil at 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.14520(10)
_cell_length_b                   13.14520(10)
_cell_length_c                   46.4914(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6957.25(15)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    24018
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.1920
_cell_measurement_theta_min      4.3240
_shelx_estimated_absorpt_T_max   0.311
_shelx_estimated_absorpt_T_min   0.151
_exptl_absorpt_coefficient_mu    21.764
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.144
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.466
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4782
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 8 -5 0.0421
-6 4 19 0.0525
0 -6 17 0.0369
5 -8 3 0.0381
6 -3 -21 0.0526
0 6 -17 0.0421
2 5 17 0.0519
-4 8 5 0.0493
-7 6 -10 0.0384
-2 -4 -18 0.0444
2 -8 -10 0.0448
7 -6 11 0.0304
-3 8 -2 0.0467
-8 4 9 0.0433
-4 -4 9 0.0279
5 -9 -1 0.0384
8 -3 -10 0.0465
4 4 -10 0.0449

_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.07
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.9116 8.3925 -5.3470 -0.0524 0.2897 0.9557
-6.4470 4.2889 19.2891 0.1448 -0.7732 0.6174
0.4114 -6.3550 16.6761 0.1381 -0.7476 -0.6497
4.5075 -8.4946 2.6969 0.0319 -0.1796 -0.9832
6.0136 -2.8422 -21.4028 -0.1631 0.8730 -0.4597
-0.2796 6.2420 -16.9958 -0.1405 0.7601 0.6345
1.7868 4.9793 17.1916 0.8418 0.1560 0.5168
-4.2055 8.4032 5.2689 0.1916 0.0345 0.9809
-7.4597 6.3024 -10.2061 -0.5891 -0.1106 0.8004
-2.4309 -4.3517 -17.8831 -0.8836 -0.1639 -0.4386
2.4644 -7.8870 -9.8206 -0.4322 -0.0794 -0.8983
7.4996 -6.0403 10.9333 0.6242 0.1171 -0.7724
-2.9093 8.3830 -2.1380 0.1155 0.3226 0.9395
-8.1254 4.3918 9.1205 -0.2535 -0.7203 0.6457
-3.9941 -4.1095 9.4566 -0.3144 -0.8884 -0.3345
4.7873 -8.5098 -0.6747 -0.0300 -0.0804 -0.9963
7.9029 -2.6814 -10.1324 0.2947 0.8361 -0.4626
4.1567 3.9354 -9.5707 0.3169 0.8955 0.3126

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            28668
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.972
_diffrn_reflns_theta_min         4.324
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     46.00  71.00   0.50    0.19    --  113.25-125.00 150.00   50
  2  ω     84.00 110.00   0.50    0.19    --  113.25-125.00 150.00   52
  3  ω     47.00  92.00   0.50    0.19    --  113.25-125.00   0.00   90
  4  ω     76.00 111.00   0.50    0.19    --  113.25-125.00 -90.00   70
  5  ω     48.00 104.00   0.50    0.19    --  113.25 -96.00-127.11  112
  6  ω     76.00 101.00   0.50    0.19    --  113.25 -94.00 -90.00   50
  7  ω     45.00  70.00   0.50    0.19    --  113.25 -94.00 -90.00   50
  8  ω     69.00 101.00   0.50    0.19    --  113.25 -94.00-120.00   64
  9  ω     73.00 104.00   0.50    0.19    --  113.25 -94.00   0.00   62
 10  ω     78.00 106.00   0.50    0.19    --  113.25 -94.00 -30.00   56
 11  ω     44.00  75.00   0.50    0.19    --  113.25 -94.00  30.00   62
 12  ω     79.00 106.00   0.50    0.19    --  113.25 -94.00  60.00   54
 13  ω     43.00  97.00   0.50    0.19    --  113.25 -94.00  90.00  108
 14  ω     43.00  69.00   0.50    0.19    --  113.25 -94.00 120.00   52
 15  ω     74.00 100.00   0.50    0.19    --  113.25 -94.00 150.00   52
 16  ω     78.00 103.00   0.50    0.19    --  113.25 -94.00 120.00   50
 17  ω     46.00  72.00   0.50    0.19    --  113.25 -94.00 150.00   52
 18  ω     77.00 103.00   0.50    0.19    --  113.25 -94.00  30.00   52
 19  ω     76.00 103.00   0.50    0.19    --  113.25 -94.00 -60.00   54
 20  ω     45.00  98.00   0.50    0.19    --  113.25 -94.00-180.00  106
 21  ω    -23.00  30.00   0.50    0.05    --   47.26 -19.00-180.00  106
 22  ω     42.00  71.00   0.50    0.19    --  113.25 -61.00-180.00   58
 23  ω     42.00  70.00   0.50    0.19    --  113.25 -61.00 -90.00   56
 24  ω     42.00  71.00   0.50    0.19    --  113.25 -61.00-150.00   58
 25  ω     45.00  71.00   0.50    0.19    --  113.25 -61.00-120.00   52
 26  ω     44.00  83.00   0.50    0.19    --  113.25 -77.00 -30.00   78
 27  ω     46.00  71.00   0.50    0.19    --  113.25 -61.00  30.00   50
 28  ω     46.00  71.00   0.50    0.19    --  113.25 -61.00  90.00   50
 29  ω    150.00 176.00   0.50    0.19    --  113.25   0.00  30.00   52
 30  ω    145.00 171.00   0.50    0.19    --  113.25  77.00 150.00   52
 31  ω     91.00 130.00   0.50    0.19    --  113.25  77.00 150.00   78
 32  ω    101.00 151.00   0.50    0.19    --  113.25  45.00  60.00  100
 33  ω    133.00 158.00   0.50    0.19    --  113.25  45.00  30.00   50
 34  ω    107.00 169.00   0.50    0.19    --  113.25  30.00 150.00  124
 35  ω    102.00 149.00   0.50    0.19    --  113.25  45.00   0.00   94
 36  ω    101.00 155.00   0.50    0.19    --  113.25  45.00 -60.00  108
 37  ω    106.00 178.00   0.50    0.19    --  113.25  30.00-150.00  144
 38  ω    112.00 178.00   0.50    0.19    --  113.25  15.00 -90.00  132
 39  ω     84.00 109.00   0.50    0.19    --  113.25   0.00  30.00   50
 40  ω    112.00 138.00   0.50    0.19    --  113.25  15.00 120.00   52
 41  ω    141.00 166.00   0.50    0.19    --  113.25  15.00 120.00   50
 42  ω    -69.00  21.00   0.50    0.05    --  -47.26  77.00-120.00  180
 43  ω    -21.00  15.00   0.50    0.05    --  -47.26  38.00  30.00   72
 44  ω     -7.00  20.00   0.50    0.05    --  -47.26  57.00  30.00   54
 45  ω    -61.00 -26.00   0.50    0.05    --  -47.26  57.00  30.00   70
 46  ω    -29.00  27.00   0.50    0.05    --  -47.26  19.00 150.00  112
 47  ω    -67.00 -20.00   0.50    0.19    --  -91.75  61.00 150.00   94
 48  ω    -48.00 -22.00   0.50    0.19    --  -91.75  45.00  90.00   52
 49  ω    -51.00 -22.00   0.50    0.19    --  -91.75  45.00  60.00   58
 50  ω    -53.00 -19.00   0.50    0.19    --  -91.75  61.00-150.00   68
 51  ω   -162.00-124.00   0.50    0.19    --  -91.75 -61.00-180.00   76
 52  ω   -120.00 -49.00   0.50    0.05    --  -47.26 -77.00-180.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0868745000
_diffrn_orient_matrix_UB_12      0.0503864000
_diffrn_orient_matrix_UB_13      0.0253402000
_diffrn_orient_matrix_UB_21      0.1016955000
_diffrn_orient_matrix_UB_22      0.0683491000
_diffrn_orient_matrix_UB_23      -0.0212906000
_diffrn_orient_matrix_UB_31      -0.0206219000
_diffrn_orient_matrix_UB_32      0.1053422000
_diffrn_orient_matrix_UB_33      0.0016949000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.974
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                3308
_reflns_number_total             3342
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.612
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 
;
 Flack x determined using 1595 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3342
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.166
_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)+(0.0627P)²+38.0844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.0998
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.333333 0.666667 0.47562(2) 0.02464(19) Uani 1 3 d S T P . .
Br1 Br 0.55291(9) 0.51153(9) 0.47103(2) 0.0298(2) Uani 1 1 d . . . . .
Br2 Br 0.81041(9) 0.58223(10) 0.50078(2) 0.0360(3) Uani 1 1 d . . . . .
Br3 Br 0.89897(9) 0.75614(10) 0.55842(2) 0.0360(3) Uani 1 1 d . . . . .
Br4 Br 0.71560(9) 0.83127(8) 0.58825(2) 0.0313(2) Uani 1 1 d . . . . .
O1 O 0.4252(5) 0.6090(6) 0.50616(14) 0.0279(13) Uani 1 1 d . . . . .
O2 O 0.5032(6) 0.7577(6) 0.55148(15) 0.0329(13) Uani 1 1 d . . . . .
H2 H 0.458517 0.757584 0.538555 0.049 Uiso 1 1 calc R U . . .
N1 N 0.333333 0.666667 0.4212(4) 0.040(3) Uani 1 3 d S T P . .
N2 N 0.5325(8) 0.7808(8) 0.45361(18) 0.0343(16) Uani 1 1 d . . . . .
C1 C 0.4400(10) 0.6673(11) 0.4107(2) 0.043(2) Uani 1 1 d . . . . .
H1A H 0.451413 0.689123 0.390118 0.052 Uiso 1 1 calc R U . . .
H1B H 0.428320 0.587089 0.412420 0.052 Uiso 1 1 calc R U . . .
C2 C 0.5478(10) 0.7504(9) 0.4269(2) 0.037(2) Uani 1 1 d . . . . .
C3 C 0.6619(10) 0.7930(9) 0.4159(2) 0.039(2) Uani 1 1 d . . . . .
H3 H 0.672192 0.771015 0.397150 0.047 Uiso 1 1 calc R U . . .
C4 C 0.7577(10) 0.8655(9) 0.4321(3) 0.044(3) Uani 1 1 d . . . . .
H4 H 0.834794 0.893842 0.424827 0.053 Uiso 1 1 calc R U . . .
C5 C 0.7402(10) 0.8976(9) 0.4598(3) 0.038(2) Uani 1 1 d . . . . .
H5 H 0.805045 0.947917 0.471605 0.045 Uiso 1 1 calc R U . . .
C6 C 0.6279(10) 0.8546(10) 0.4691(2) 0.036(2) Uani 1 1 d . . . . .
H6 H 0.616166 0.877867 0.487606 0.044 Uiso 1 1 calc R U . . .
C7 C 0.5309(8) 0.6397(8) 0.51694(18) 0.0258(16) Uani 1 1 d . . . . .
C8 C 0.6053(8) 0.6029(8) 0.5052(2) 0.0269(17) Uani 1 1 d . . . . .
C9 C 0.7129(8) 0.6345(9) 0.51761(19) 0.0281(17) Uani 1 1 d . . . . .
C10 C 0.7495(8) 0.7055(8) 0.5421(2) 0.0277(17) Uani 1 1 d . . . . .
C11 C 0.6762(8) 0.7439(8) 0.55374(19) 0.0259(17) Uani 1 1 d . . . . .
C12 C 0.5703(8) 0.7152(8) 0.5407(2) 0.0275(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.228(6) 3_565 ?
Gd1 O1 2.228(6) . ?
Gd1 O1 2.228(6) 2_665 ?
Gd1 N1 2.530(17) . ?
Gd1 N2 2.495(9) 3_565 ?
Gd1 N2 2.494(9) 2_665 ?
Gd1 N2 2.495(9) . ?
Br1 C8 1.899(9) . ?
Br2 C9 1.899(9) . ?
Br3 C10 1.890(9) . ?
Br4 C11 1.889(9) . ?
O1 C7 1.335(11) . ?
O2 H2 0.8400 . ?
O2 C12 1.355(12) . ?
N1 C1 1.480(13) 2_665 ?
N1 C1 1.480(13) 3_565 ?
N1 C1 1.480(13) . ?
N2 C2 1.350(13) . ?
N2 C6 1.349(15) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.489(17) . ?
C2 C3 1.409(15) . ?
C3 H3 0.9500 . ?
C3 C4 1.363(19) . ?
C4 H4 0.9500 . ?
C4 C5 1.409(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.361(14) . ?
C6 H6 0.9500 . ?
C7 C8 1.402(12) . ?
C7 C12 1.399(11) . ?
C8 C9 1.386(13) . ?
C9 C10 1.395(10) . ?
C10 C11 1.401(13) . ?
C11 C12 1.387(13) . ?

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
O1 Gd1 O1 83.7(3) 3_565 2_665 ?
O1 Gd1 O1 83.7(3) 3_565 . ?
O1 Gd1 O1 83.7(3) 2_665 . ?
O1 Gd1 N1 129.58(17) 3_565 . ?
O1 Gd1 N1 129.58(17) . . ?
O1 Gd1 N1 129.58(17) 2_665 . ?
O1 Gd1 N2 164.5(3) 3_565 . ?
O1 Gd1 N2 86.5(3) . 3_565 ?
O1 Gd1 N2 86.5(3) 3_565 2_665 ?
O1 Gd1 N2 86.5(3) 2_665 . ?
O1 Gd1 N2 164.5(3) . 2_665 ?
O1 Gd1 N2 164.5(3) 2_665 3_565 ?
O1 Gd1 N2 83.2(3) . . ?
O1 Gd1 N2 83.2(3) 3_565 3_565 ?
O1 Gd1 N2 83.2(3) 2_665 2_665 ?
N2 Gd1 N1 65.8(2) . . ?
N2 Gd1 N1 65.8(2) 2_665 . ?
N2 Gd1 N1 65.8(2) 3_565 . ?
N2 Gd1 N2 104.3(2) 3_565 . ?
N2 Gd1 N2 104.3(2) 2_665 . ?
N2 Gd1 N2 104.3(2) 2_665 3_565 ?
C7 O1 Gd1 142.7(6) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Gd1 109.2(7) 3_565 . ?
C1 N1 Gd1 109.2(7) 2_665 . ?
C1 N1 Gd1 109.2(7) . . ?
C1 N1 C1 109.8(7) 2_665 3_565 ?
C1 N1 C1 109.8(7) 3_565 . ?
C1 N1 C1 109.8(7) 2_665 . ?
C2 N2 Gd1 117.8(8) . . ?
C6 N2 Gd1 122.2(6) . . ?
C6 N2 C2 118.8(9) . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
N1 C1 C2 112.9(9) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
N2 C2 C1 116.9(10) . . ?
N2 C2 C3 120.2(11) . . ?
C3 C2 C1 122.8(10) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(10) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.8(10) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 120.9 . . ?
C6 C5 C4 118.2(11) . . ?
C6 C5 H5 120.9 . . ?
N2 C6 C5 123.6(10) . . ?
N2 C6 H6 118.2 . . ?
C5 C6 H6 118.2 . . ?
O1 C7 C8 123.3(8) . . ?
O1 C7 C12 118.1(8) . . ?
C12 C7 C8 118.5(9) . . ?
C7 C8 Br1 116.7(7) . . ?
C9 C8 Br1 122.1(7) . . ?
C9 C8 C7 121.1(9) . . ?
C8 C9 Br2 119.4(7) . . ?
C8 C9 C10 120.0(9) . . ?
C10 C9 Br2 120.6(7) . . ?
C9 C10 Br3 120.9(8) . . ?
C9 C10 C11 119.2(9) . . ?
C11 C10 Br3 119.9(7) . . ?
C10 C11 Br4 121.3(7) . . ?
C12 C11 Br4 118.0(7) . . ?
C12 C11 C10 120.6(8) . . ?
O2 C12 C7 119.9(9) . . ?
O2 C12 C11 119.8(8) . . ?
C11 C12 C7 120.3(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84 2.08 2.889(9) 160.8 2_665 yes
C1 H1B Br3 0.99 2.99 3.738(12) 133.2 12_454 yes

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
Gd1 O1 C7 C8 -92.5(11) . . . . ?
Gd1 O1 C7 C12 85.5(11) . . . . ?
Gd1 N1 C1 C2 -43.3(10) . . . . ?
Gd1 N2 C2 C1 11.5(12) . . . . ?
Gd1 N2 C2 C3 -165.9(7) . . . . ?
Gd1 N2 C6 C5 164.7(8) . . . . ?
Br1 C8 C9 Br2 -1.6(11) . . . . ?
Br1 C8 C9 C10 177.6(6) . . . . ?
Br2 C9 C10 Br3 2.2(9) . . . . ?
Br2 C9 C10 C11 179.2(8) . . . . ?
Br3 C10 C11 Br4 -7.3(11) . . . . ?
Br3 C10 C11 C12 174.9(7) . . . . ?
Br4 C11 C12 O2 5.2(12) . . . . ?
Br4 C11 C12 C7 -172.8(6) . . . . ?
O1 C7 C8 Br1 3.3(12) . . . . ?
O1 C7 C8 C9 -178.2(8) . . . . ?
O1 C7 C12 O2 -2.0(12) . . . . ?
O1 C7 C12 C11 176.1(8) . . . . ?
N1 C1 C2 N2 22.5(14) . . . . ?
N1 C1 C2 C3 -160.1(10) . . . . ?
N2 C2 C3 C4 -0.3(16) . . . . ?
C1 N1 C1 C2 -163.0(10) 3_565 . . . ?
C1 N1 C1 C2 76.3(16) 2_665 . . . ?
C1 C2 C3 C4 -177.5(11) . . . . ?
C2 N2 C6 C5 -2.3(15) . . . . ?
C2 C3 C4 C5 -0.5(16) . . . . ?
C3 C4 C5 C6 -0.1(16) . . . . ?
C4 C5 C6 N2 1.5(16) . . . . ?
C6 N2 C2 C1 179.1(9) . . . . ?
C6 N2 C2 C3 1.7(14) . . . . ?
C7 C8 C9 Br2 180.0(7) . . . . ?
C7 C8 C9 C10 -0.8(13) . . . . ?
C8 C7 C12 O2 176.2(9) . . . . ?
C8 C7 C12 C11 -5.8(12) . . . . ?
C8 C9 C10 Br3 -177.0(8) . . . . ?
C8 C9 C10 C11 0.0(11) . . . . ?
C9 C10 C11 Br4 175.7(6) . . . . ?
C9 C10 C11 C12 -2.1(13) . . . . ?
C10 C11 C12 O2 -176.9(8) . . . . ?
C10 C11 C12 C7 5.1(13) . . . . ?
C12 C7 C8 Br1 -174.8(6) . . . . ?
C12 C7 C8 C9 3.7(13) . . . . ?

_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.822
_exptl_crystal_recrystallization_method 'From reaction'
####################################################################### 
# 
# 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_sb01-05-y6-xrd-2-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405954'
loop_
_audit_author_name
_audit_author_address
'Robert W Gable'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2025-01-23 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 N4 O6 Y'
_chemical_formula_sum            'C36 H21 Br12 N4 O6 Y'
_chemical_formula_weight         1653.40
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Y1 C30 O6 N4 Br12'
_chemical_oxdiff_usercomment     'Transparent crystal in oil at 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 '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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.1340(2)
_cell_length_b                   13.1340(2)
_cell_length_c                   46.2582(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6910.6(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    11372
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      78.6240
_cell_measurement_theta_min      3.9820
_shelx_estimated_absorpt_T_max   0.479
_shelx_estimated_absorpt_T_min   0.358
_exptl_absorpt_coefficient_mu    14.384
_exptl_absorpt_correction_T_max  0.580
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.384
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4632
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -6 -16 0.0351
6 -8 7 0.0421
5 1 -18 0.0421
6 3 0 0.0290
-6 -2 5 0.0336
-5 0 23 0.0315
0 3 27 0.0234
3 -4 -25 0.0361
7 0 0 0.0235
-1 7 15 0.0225
-2 8 -4 0.0310
2 -2 28 0.0297
-3 -6 -3 0.0317
-8 6 4 0.0292
-6 -1 -17 0.0277
-7 7 -9 0.0284
-4 6 -21 0.0380

_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.3302 -6.4477 -15.7591 0.0317 -0.4062 0.9132
5.9476 -8.0189 6.5503 0.0787 -0.9923 0.0957
5.4939 0.7872 -17.8661 -0.9939 -0.0790 -0.0771
5.5361 2.8449 0.1770 -0.7269 -0.0584 -0.6842
-5.7916 -2.3613 5.2637 0.8428 0.0675 0.5340
-4.7904 0.1606 23.0839 0.9800 0.0776 -0.1832
0.4502 3.2212 26.5094 0.3411 0.0261 -0.9397
3.4506 -4.4500 -25.1159 -0.6155 -0.3341 0.7138
7.4365 -0.1131 0.3362 -0.7195 -0.3919 -0.5734
-1.4303 7.0433 14.6599 0.0137 0.5183 -0.8551
-1.9264 8.0990 -3.7953 -0.4193 0.7716 -0.4785
2.3404 -2.3744 28.4483 0.5602 -0.5302 -0.6364
-2.8183 -5.5163 -3.1949 0.5639 -0.2692 0.7807
-8.2405 5.7851 3.6766 0.5215 0.8523 0.0402
-5.8378 -0.5513 -16.7301 0.2372 0.3852 0.8918
-6.9464 7.1876 -8.7022 0.0255 0.9941 0.1054
-4.0649 5.8512 -21.3480 -0.4559 0.8392 0.2963

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            27677
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.275
_diffrn_reflns_theta_min         4.332
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     53.00  92.00   0.50    0.05    --   47.51-125.00   0.00   78
  2  ω     86.00 111.00   0.50    0.05    --  113.25-125.00   0.00   50
  3  ω     44.00  81.00   0.50    0.05    --  113.25-125.00   0.00   74
  4  ω     48.00  74.00   0.50    0.05    --  113.25 -94.00  60.00   52
  5  ω     78.00 104.00   0.50    0.05    --  113.25 -94.00  30.00   52
  6  ω     78.00 104.00   0.50    0.05    --  113.25 -94.00  60.00   52
  7  ω     44.00 106.00   0.50    0.05    --  113.25 -94.00  90.00  124
  8  ω     45.00 104.00   0.50    0.05    --  113.25 -94.00 120.00  118
  9  ω     74.00 105.00   0.50    0.05    --  113.25 -94.00 -90.00   62
 10  ω     69.00 102.00   0.50    0.05    --  113.25 -94.00-120.00   66
 11  ω     54.00 108.00   0.50    0.05    --  113.25-106.00-142.15  108
 12  ω     67.00 106.00   0.50    0.05    --  113.25 -94.00 -30.00   78
 13  ω     74.00 106.00   0.50    0.05    --  113.25 -94.00 150.00   64
 14  ω     20.00  78.00   0.50    0.05    --   47.51 -99.00-120.00  116
 15  ω     89.00 118.00   0.50    0.05    --  113.25 -88.00-161.30   58
 16  ω     64.00 100.00   0.50    0.05    --  113.25 -77.00-150.00   72
 17  ω     44.00  71.00   0.50    0.05    --  113.25 -61.00-120.00   54
 18  ω     64.00  90.00   0.50    0.05    --  113.25 -77.00 -90.00   52
 19  ω     42.00  71.00   0.50    0.05    --  113.25 -61.00-180.00   58
 20  ω     44.00  87.00   0.50    0.05    --  113.25 -77.00 -30.00   86
 21  ω     43.00  69.00   0.50    0.05    --  113.25 -61.00   0.00   52
 22  ω     43.00  92.00   0.50    0.05    --  113.25 -77.00   0.00   98
 23  ω    -22.00  60.00   0.50    0.05    --   47.51 -57.00 -90.00  164
 24  ω     -1.00  26.00   0.50    0.05    --   47.51 -19.00 120.00   54
 25  ω     42.00  69.00   0.50    0.05    --  113.25 -61.00 120.00   54
 26  ω     42.00  71.00   0.50    0.05    --  113.25 -61.00 150.00   58
 27  ω    102.00 135.00   0.50    0.05    --  113.25  15.00  90.00   66
 28  ω    122.00 147.00   0.50    0.05    --  113.25  61.00  90.00   50
 29  ω    139.00 176.00   0.50    0.05    --  113.25  61.00   0.00   74
 30  ω    102.00 167.00   0.50    0.05    --  113.25  45.00 -30.00  130
 31  ω    103.00 176.00   0.50    0.05    --  113.25  61.00-120.00  146
 32  ω    136.00 178.00   0.50    0.05    --  113.25  77.00-150.00   84
 33  ω     94.00 126.00   0.50    0.05    --  113.25  77.00-150.00   64
 34  ω    104.00 146.00   0.50    0.05    --  113.25  45.00-180.00   84
 35  ω    105.00 163.00   0.50    0.05    --  113.25  45.00 -60.00  116
 36  ω    120.00 157.00   0.50    0.05    --  113.25  15.00 -60.00   74
 37  ω    107.00 177.00   0.50    0.05    --  113.25  15.00  30.00  140
 38  ω    102.00 162.00   0.50    0.05    --  113.25  30.00 150.00  120
 39  ω   -107.00  22.00   0.50    0.05    --  -47.51   0.00  60.00  258
 40  ω    -28.00  24.00   0.50    0.05    --  -47.51  19.00  90.00  104
 41  ω    -33.00  13.00   0.50    0.05    --  -47.51  38.00 120.00   92
 42  ω    -49.00 -23.00   0.50    0.05    --  -91.75  45.00  90.00   52
 43  ω    -51.00 -20.00   0.50    0.05    --  -91.75  45.00 120.00   62
 44  ω    -66.00 -26.00   0.50    0.05    --  -91.75 125.00  90.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0987452000
_diffrn_orient_matrix_UB_12      -0.0647506000
_diffrn_orient_matrix_UB_13      0.0224126000
_diffrn_orient_matrix_UB_21      -0.0511324000
_diffrn_orient_matrix_UB_22      0.0794469000
_diffrn_orient_matrix_UB_23      -0.0078004000
_diffrn_orient_matrix_UB_31      -0.0773997000
_diffrn_orient_matrix_UB_32      -0.0884460000
_diffrn_orient_matrix_UB_33      -0.0233846000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                3123
_reflns_number_total             3267
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 
;
 Flack x determined using 1372 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3267
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      1.142
_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)+(0.0409P)²+66.1172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0951
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.666667 0.333333 0.52407(3) 0.0212(3) Uani 1 3 d S T P . .
Br1 Br 0.51031(11) 0.55134(10) 0.52915(2) 0.0268(3) Uani 1 1 d . . . . .
Br2 Br 0.58055(12) 0.80853(11) 0.49917(2) 0.0327(3) Uani 1 1 d . . . . .
Br3 Br 0.75616(12) 0.89807(10) 0.44155(2) 0.0327(3) Uani 1 1 d . . . . .
Br4 Br 0.83199(10) 0.71483(11) 0.41170(2) 0.0287(3) Uani 1 1 d . . . . .
O1 O 0.6092(6) 0.4240(6) 0.49420(15) 0.0239(16) Uani 1 1 d . . . . .
O2 O 0.7584(7) 0.5027(7) 0.44871(16) 0.0293(16) Uani 1 1 d . . . . .
H2 H 0.748683 0.451430 0.460965 0.044 Uiso 1 1 calc R U . . .
N1 N 0.666667 0.333333 0.5786(3) 0.034(3) Uani 1 3 d S T P . .
N2 N 0.7798(8) 0.5305(9) 0.5455(2) 0.0286(19) Uani 1 1 d . . . . .
C1 C 0.6660(12) 0.4402(11) 0.5885(2) 0.039(3) Uani 1 1 d . . . . .
H1A H 0.686331 0.452512 0.609323 0.046 Uiso 1 1 calc R U . . .
H1B H 0.585694 0.428204 0.586305 0.046 Uiso 1 1 calc R U . . .
C2 C 0.7501(10) 0.5473(11) 0.5722(3) 0.031(2) Uani 1 1 d . . . . .
C3 C 0.7928(10) 0.6614(10) 0.5834(2) 0.032(2) Uani 1 1 d . . . . .
H3 H 0.770950 0.671820 0.602292 0.039 Uiso 1 1 calc R U . . .
C4 C 0.8666(10) 0.7578(11) 0.5668(3) 0.039(3) Uani 1 1 d . . . . .
H4 H 0.895447 0.835331 0.573910 0.047 Uiso 1 1 calc R U . . .
C5 C 0.8980(10) 0.7388(10) 0.5393(3) 0.035(3) Uani 1 1 d . . . . .
H5 H 0.949646 0.803038 0.527363 0.042 Uiso 1 1 calc R U . . .
C6 C 0.8524(11) 0.6255(11) 0.5299(3) 0.031(2) Uani 1 1 d . . . . .
H6 H 0.873723 0.613332 0.511146 0.037 Uiso 1 1 calc R U . . .
C7 C 0.6393(9) 0.5290(9) 0.4834(2) 0.023(2) Uani 1 1 d . . . . .
C8 C 0.6027(9) 0.6035(9) 0.4950(2) 0.021(2) Uani 1 1 d . . . . .
C9 C 0.6348(10) 0.7123(9) 0.4826(2) 0.025(2) Uani 1 1 d . . . . .
C10 C 0.7053(10) 0.7476(10) 0.4581(2) 0.024(2) Uani 1 1 d . . . . .
C11 C 0.7445(10) 0.6747(10) 0.4465(2) 0.025(2) Uani 1 1 d . . . . .
C12 C 0.7149(10) 0.5701(9) 0.4593(3) 0.025(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O1 2.190(6) 3_665 ?
Y1 O1 2.190(6) . ?
Y1 O1 2.190(6) 2_655 ?
Y1 N1 2.521(16) . ?
Y1 N2 2.459(9) . ?
Y1 N2 2.459(9) 3_665 ?
Y1 N2 2.459(9) 2_655 ?
Br1 C8 1.897(11) . ?
Br2 C9 1.895(11) . ?
Br3 C10 1.902(11) . ?
Br4 C11 1.892(12) . ?
O1 C7 1.326(13) . ?
O2 H2 0.8400 . ?
O2 C12 1.363(14) . ?
N1 C1 1.482(12) 3_665 ?
N1 C1 1.482(13) 2_655 ?
N1 C1 1.482(12) . ?
N2 C2 1.347(14) . ?
N2 C6 1.339(16) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.488(17) . ?
C2 C3 1.411(15) . ?
C3 H3 0.9500 . ?
C3 C4 1.38(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.40(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.368(16) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(15) . ?
C7 C12 1.409(12) . ?
C8 C9 1.395(15) . ?
C9 C10 1.390(11) . ?
C10 C11 1.402(16) . ?
C11 C12 1.362(16) . ?

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
O1 Y1 O1 84.4(3) 3_665 2_655 ?
O1 Y1 O1 84.4(3) 3_665 . ?
O1 Y1 O1 84.4(3) 2_655 . ?
O1 Y1 N1 129.12(19) 3_665 . ?
O1 Y1 N1 129.12(19) . . ?
O1 Y1 N1 129.12(19) 2_655 . ?
O1 Y1 N2 164.5(3) 3_665 2_655 ?
O1 Y1 N2 82.7(3) . . ?
O1 Y1 N2 82.7(3) 3_665 3_665 ?
O1 Y1 N2 82.7(3) 2_655 2_655 ?
O1 Y1 N2 164.5(3) . 3_665 ?
O1 Y1 N2 164.5(3) 2_655 . ?
O1 Y1 N2 85.8(3) . 2_655 ?
O1 Y1 N2 85.8(3) 3_665 . ?
O1 Y1 N2 85.8(3) 2_655 3_665 ?
N2 Y1 N1 66.3(2) 2_655 . ?
N2 Y1 N1 66.3(2) 3_665 . ?
N2 Y1 N1 66.3(2) . . ?
N2 Y1 N2 104.9(3) . 2_655 ?
N2 Y1 N2 104.9(3) 3_665 2_655 ?
N2 Y1 N2 104.9(3) 3_665 . ?
C7 O1 Y1 142.9(7) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Y1 108.1(8) 2_655 . ?
C1 N1 Y1 108.1(8) 3_665 . ?
C1 N1 Y1 108.1(8) . . ?
C1 N1 C1 110.8(7) 3_665 2_655 ?
C1 N1 C1 110.8(7) 2_655 . ?
C1 N1 C1 110.8(7) 3_665 . ?
C2 N2 Y1 118.0(8) . . ?
C6 N2 Y1 122.6(7) . . ?
C6 N2 C2 118.0(10) . . ?
N1 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
N1 C1 C2 112.5(10) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
N2 C2 C1 116.8(10) . . ?
N2 C2 C3 121.2(11) . . ?
C3 C2 C1 121.9(10) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.5(11) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.5(11) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.3(12) . . ?
C6 C5 H5 120.8 . . ?
N2 C6 C5 124.4(11) . . ?
N2 C6 H6 117.8 . . ?
C5 C6 H6 117.8 . . ?
O1 C7 C8 123.8(10) . . ?
O1 C7 C12 118.8(10) . . ?
C8 C7 C12 117.3(11) . . ?
C7 C8 Br1 116.7(8) . . ?
C9 C8 Br1 121.6(8) . . ?
C9 C8 C7 121.7(10) . . ?
C8 C9 Br2 119.7(8) . . ?
C10 C9 Br2 121.2(9) . . ?
C10 C9 C8 119.2(11) . . ?
C9 C10 Br3 120.3(10) . . ?
C9 C10 C11 119.8(11) . . ?
C11 C10 Br3 119.9(9) . . ?
C10 C11 Br4 121.0(8) . . ?
C12 C11 Br4 118.7(9) . . ?
C12 C11 C10 120.3(11) . . ?
O2 C12 C7 118.7(11) . . ?
C11 C12 O2 119.8(10) . . ?
C11 C12 C7 121.6(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84 2.28 2.704(9) 111.7 . yes

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
Y1 O1 C7 C8 -93.3(13) . . . . ?
Y1 O1 C7 C12 85.2(12) . . . . ?
Y1 N1 C1 C2 -44.4(10) . . . . ?
Y1 N2 C2 C1 10.8(13) . . . . ?
Y1 N2 C2 C3 -166.3(8) . . . . ?
Y1 N2 C6 C5 166.0(9) . . . . ?
Br1 C8 C9 Br2 -2.5(13) . . . . ?
Br1 C8 C9 C10 178.3(7) . . . . ?
Br2 C9 C10 Br3 3.4(10) . . . . ?
Br2 C9 C10 C11 179.7(10) . . . . ?
Br3 C10 C11 Br4 -7.8(13) . . . . ?
Br3 C10 C11 C12 175.6(9) . . . . ?
Br4 C11 C12 O2 6.7(15) . . . . ?
Br4 C11 C12 C7 -173.0(7) . . . . ?
O1 C7 C8 Br1 2.8(14) . . . . ?
O1 C7 C8 C9 -178.8(10) . . . . ?
O1 C7 C12 O2 -2.9(13) . . . . ?
O1 C7 C12 C11 176.9(11) . . . . ?
N1 C1 C2 N2 24.2(15) . . . . ?
N1 C1 C2 C3 -158.8(11) . . . . ?
N2 C2 C3 C4 -0.1(17) . . . . ?
C1 N1 C1 C2 -162.7(10) 2_655 . . . ?
C1 N1 C1 C2 73.9(17) 3_665 . . . ?
C1 C2 C3 C4 -177.1(11) . . . . ?
C2 N2 C6 C5 -0.5(16) . . . . ?
C2 C3 C4 C5 -0.8(17) . . . . ?
C3 C4 C5 C6 1.1(17) . . . . ?
C4 C5 C6 N2 -0.4(17) . . . . ?
C6 N2 C2 C1 177.9(10) . . . . ?
C6 N2 C2 C3 0.8(15) . . . . ?
C7 C8 C9 Br2 179.2(8) . . . . ?
C7 C8 C9 C10 -0.1(15) . . . . ?
C8 C7 C12 O2 175.7(10) . . . . ?
C8 C7 C12 C11 -4.6(14) . . . . ?
C8 C9 C10 Br3 -177.4(10) . . . . ?
C8 C9 C10 C11 -1.1(12) . . . . ?
C9 C10 C11 Br4 175.9(7) . . . . ?
C9 C10 C11 C12 -0.7(15) . . . . ?
C10 C11 C12 O2 -176.7(10) . . . . ?
C10 C11 C12 C7 3.6(16) . . . . ?
C12 C7 C8 Br1 -175.6(7) . . . . ?
C12 C7 C8 C9 2.8(15) . . . . ?

_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 1.292
_oxdiff_exptl_absorpt_empirical_full_min 0.824

# start Validation Reply Form
_vrf_PLAT341_sb01-05-y6-xrd-2-100k_abs 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01691 Ang.
RESPONSE: Due to refining light atoms in the presence of several Br & Y atoms, 
          slight disorder of the crystal and slightly high Rint value.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_sb01-05-lu3-xrd5-100k_abs
_database_code_depnum_ccdc_archive 'CCDC 2405952'
loop_
_audit_author_name
_audit_author_address
'Stanley Bagio'
;The University of Melbourne
Australia
;
_audit_update_record             
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/3
_audit_contact_author_emial      sbagio@student.unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H21 Br12 Lu N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Lu N4 O6'
_chemical_formula_weight         1739.46
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Lu Br8 C36 H21 O6 N4'
_chemical_oxdiff_usercomment     'colourless block in oil 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -6.6179 4.6937 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   13.09510(10)
_cell_length_b                   13.09510(10)
_cell_length_c                   45.9594(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6825.31(14)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    23109
_cell_measurement_temperature    99.97(12)
_cell_measurement_theta_max      79.3430
_cell_measurement_theta_min      4.3340
_shelx_estimated_absorpt_T_max   0.614
_shelx_estimated_absorpt_T_min   0.425
_exptl_absorpt_coefficient_mu    16.911
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.539
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4824
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -5 18 0.0247
5 -4 -22 0.0073
-8 6 -10 0.0245
7 -5 17 0.0246
3 5 1 0.0266
-5 7 -14 0.0258
-1 -7 4 0.0075
6 0 -14 0.0122
-7 0 14 0.0245
-1 6 20 0.0219
-5 3 23 0.0219

_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.032
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.4027 -4.8167 18.4976 0.0187 0.0810 0.9965
5.3544 -4.1030 -22.4297 -0.2308 -0.9638 0.1332
-7.7082 5.8236 -9.7244 0.0590 0.2440 -0.9680
6.7266 -5.2719 16.5186 -0.0264 0.0075 0.9996
3.0438 5.3457 1.3102 0.9683 -0.2316 0.0934
-4.5341 7.4141 -14.2124 0.5073 -0.1224 -0.8530
-0.6306 -6.9479 4.3852 -0.9411 0.2255 0.2518
6.4065 0.1149 -14.2574 0.4644 -0.8543 0.2336
-6.5998 0.0768 13.5109 -0.4601 0.8463 -0.2686
-1.0841 5.9814 19.7445 0.8203 0.5645 0.0918
-5.2072 3.1913 23.4486 0.1294 0.9888 -0.0740

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            27160
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.223
_diffrn_reflns_theta_min         4.348
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -59.00  22.00   0.50    0.33    --  -47.26  57.00 -30.00  162
  2  ω    -23.00   6.00   0.50    0.33    --  -47.26  19.00  90.00   58
  3  ω    -56.00  25.00   0.50    0.33    --  -47.26  57.00-150.00  162
  4  ω    -30.00  27.00   0.50    0.33    --  -47.26  19.00 120.00  114
  5  ω    -70.00  16.00   0.50    0.33    --  -47.26  77.00  90.00  172
  6  ω    -22.00   8.00   0.50    0.33    --   47.26 -19.00 -90.00   60
  7  ω    -13.00  13.00   0.50    0.33    --   47.26 -19.00 150.00   52
  8  ω   -152.00-126.00   0.50    1.31    --  -91.75 -15.00-120.00   52
  9  ω    -60.00 -31.00   0.50    1.31    --  -91.75 125.00-180.00   58
 10  ω   -111.00 -79.00   0.50    1.31    --  -91.75 -30.00 -30.00   64
 11  ω    -46.00 -20.00   0.50    1.31    --  -91.75  45.00  60.00   52
 12  ω   -146.00-120.00   0.50    1.31    --  -91.75 -30.00 -30.00   52
 13  ω     42.00  67.00   0.50    1.31    --  113.25 -61.00  90.00   50
 14  ω     42.00  71.00   0.50    1.31    --  113.25 -61.00  60.00   58
 15  ω    102.00 148.00   0.50    1.31    --  113.25  30.00   0.00   92
 16  ω     44.00  92.00   0.50    1.31    --  113.25-125.00 -90.00   96
 17  ω     60.00 101.00   0.50    1.31    --  113.25-125.00 -60.00   82
 18  ω     42.00  67.00   0.50    1.31    --  113.25 -61.00 120.00   50
 19  ω     74.00 105.00   0.50    1.31    --  113.25 -94.00 150.00   62
 20  ω    137.00 163.00   0.50    1.31    --  113.25  30.00-150.00   52
 21  ω    105.00 132.00   0.50    1.31    --  113.25  30.00-150.00   54
 22  ω    108.00 176.00   0.50    1.31    --  113.25  61.00 -60.00  136
 23  ω     48.00 105.00   0.50    1.31    --  113.25 -94.00   0.00  114
 24  ω     72.00 106.00   0.50    1.31    --  113.25 -94.00  30.00   68
 25  ω     53.00 107.00   0.50    1.31    --  113.25-125.00-180.00  108
 26  ω    102.00 149.00   0.50    1.31    --  113.25  45.00  60.00   94
 27  ω     47.00 103.00   0.50    1.31    --  113.25 -94.00 -60.00  112
 28  ω     42.00  68.00   0.50    1.31    --  113.25 -61.00   0.00   52
 29  ω     44.00  92.00   0.50    1.31    --  113.25 -77.00-120.00   96
 30  ω    106.00 161.00   0.50    1.31    --  113.25  77.00-180.00  110
 31  ω     45.00 106.00   0.50    1.31    --  113.25 -94.00  90.00  122
 32  ω     42.00  68.00   0.50    1.31    --  113.25 -94.00  30.00   52
 33  ω     51.00  98.00   0.50    1.31    --  113.25 -94.00  60.00   94
 34  ω     44.00 106.00   0.50    1.31    --  113.25 -94.00 -30.00  124
 35  ω    113.00 149.00   0.50    1.31    --  113.25  45.00   0.00   72
 36  ω    105.00 154.00   0.50    1.31    --  113.25  30.00 -90.00   98
 37  ω     71.00 103.00   0.50    1.31    --  113.25 -94.00-180.00   64
 38  ω    105.00 155.00   0.50    1.31    --  113.25  30.00 -60.00  100
 39  ω    103.00 162.00   0.50    1.31    --  113.25  45.00 120.00  118
 40  ω     79.00 104.00   0.50    1.31    --  113.25 -94.00 -90.00   50
 41  ω     47.00  73.00   0.50    1.31    --  113.25 -94.00-150.00   52
 42  ω     81.00 106.00   0.50    1.31    --  113.25 -94.00-150.00   50
 43  ω    111.00 170.00   0.50    1.31    --  113.25  30.00  90.00  118
 44  ω     47.00  83.00   0.50    1.31    --  113.25-125.00-150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0840202000
_diffrn_orient_matrix_UB_12      0.1317682000
_diffrn_orient_matrix_UB_13      0.0062417000
_diffrn_orient_matrix_UB_21      -0.0725724000
_diffrn_orient_matrix_UB_22      -0.0086844000
_diffrn_orient_matrix_UB_23      0.0272362000
_diffrn_orient_matrix_UB_31      0.0782795000
_diffrn_orient_matrix_UB_32      -0.0316516000
_diffrn_orient_matrix_UB_33      0.0185368000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                3181
_reflns_number_total             3234
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.981
_refine_diff_density_min         -1.949
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 
;
 Flack x determined using 1493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.176
_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)+(0.0536P)²+55.3523P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0927
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.333333 0.666667 0.47619(2) 0.01923(17) Uani 1 3 d S T P . .
Br1 Br 0.54874(9) 0.50790(9) 0.47066(2) 0.0231(2) Uani 1 1 d . . . . .
Br2 Br 0.80634(9) 0.57802(11) 0.50081(2) 0.0281(3) Uani 1 1 d . . . . .
Br3 Br 0.89782(9) 0.75657(10) 0.55826(2) 0.0280(3) Uani 1 1 d . . . . .
Br4 Br 0.71425(9) 0.83213(9) 0.58859(2) 0.0247(2) Uani 1 1 d . . . . .
O1 O 0.4203(6) 0.6072(6) 0.50588(14) 0.0200(13) Uani 1 1 d . . . . .
O2 O 0.5000(7) 0.7565(7) 0.55173(15) 0.0260(14) Uani 1 1 d . . . . .
H2 H 0.456386 0.758426 0.538601 0.039 Uiso 1 1 calc R U . . .
N1 N 0.333333 0.666667 0.4231(4) 0.030(3) Uani 1 3 d S T P . .
N2 N 0.5299(8) 0.7786(8) 0.45577(19) 0.0251(16) Uani 1 1 d . . . . .
C1 C 0.4395(10) 0.6643(11) 0.4123(2) 0.034(2) Uani 1 1 d . . . . .
H1A H 0.451089 0.685257 0.391357 0.041 Uiso 1 1 calc R U . . .
H1B H 0.427103 0.583590 0.414329 0.041 Uiso 1 1 calc R U . . .
C2 C 0.5471(10) 0.7490(9) 0.4289(2) 0.028(2) Uani 1 1 d . . . . .
C3 C 0.6609(10) 0.7931(9) 0.4176(2) 0.030(2) Uani 1 1 d . . . . .
H3 H 0.671647 0.772509 0.398507 0.036 Uiso 1 1 calc R U . . .
C4 C 0.7571(11) 0.8666(10) 0.4345(3) 0.034(2) Uani 1 1 d . . . . .
H4 H 0.834906 0.895242 0.427339 0.041 Uiso 1 1 calc R U . . .
C5 C 0.7384(9) 0.8984(9) 0.4623(3) 0.029(2) Uani 1 1 d . . . . .
H5 H 0.802970 0.949930 0.474274 0.034 Uiso 1 1 calc R U . . .
C6 C 0.6250(10) 0.8535(10) 0.4718(2) 0.030(2) Uani 1 1 d . . . . .
H6 H 0.612279 0.875969 0.490470 0.036 Uiso 1 1 calc R U . . .
C7 C 0.5274(8) 0.6384(8) 0.5166(2) 0.0200(17) Uani 1 1 d . . . . .
C8 C 0.6013(9) 0.6007(9) 0.5049(2) 0.0207(18) Uani 1 1 d . . . . .
C9 C 0.7093(9) 0.6321(9) 0.5173(2) 0.0216(18) Uani 1 1 d . . . . .
C10 C 0.7479(8) 0.7043(9) 0.5419(2) 0.0221(19) Uani 1 1 d . . . . .
C11 C 0.6730(8) 0.7431(8) 0.5538(2) 0.0197(17) Uani 1 1 d . . . . .
C12 C 0.5667(8) 0.7142(8) 0.5407(2) 0.0195(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O1 2.157(6) 2_665 ?
Lu1 O1 2.157(6) . ?
Lu1 O1 2.157(6) 3_565 ?
Lu1 N1 2.440(18) . ?
Lu1 N2 2.426(9) 3_565 ?
Lu1 N2 2.426(9) 2_665 ?
Lu1 N2 2.426(9) . ?
Br1 C8 1.896(10) . ?
Br2 C9 1.894(10) . ?
Br3 C10 1.883(9) . ?
Br4 C11 1.892(10) . ?
O1 C7 1.343(12) . ?
O2 H2 0.8400 . ?
O2 C12 1.346(12) . ?
N1 C1 1.492(12) . ?
N1 C1 1.492(12) 3_565 ?
N1 C1 1.492(12) 2_665 ?
N2 C2 1.346(13) . ?
N2 C6 1.354(16) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.497(16) . ?
C2 C3 1.400(14) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(18) . ?
C4 H4 0.9500 . ?
C4 C5 1.406(18) . ?
C5 H5 0.9500 . ?
C5 C6 1.366(15) . ?
C6 H6 0.9500 . ?
C7 C8 1.393(14) . ?
C7 C12 1.403(11) . ?
C8 C9 1.382(14) . ?
C9 C10 1.398(11) . ?
C10 C11 1.420(14) . ?
C11 C12 1.384(14) . ?

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
O1 Lu1 O1 84.2(3) 2_665 3_565 ?
O1 Lu1 O1 84.2(3) 2_665 . ?
O1 Lu1 O1 84.2(3) 3_565 . ?
O1 Lu1 N1 129.25(18) 2_665 . ?
O1 Lu1 N1 129.25(18) . . ?
O1 Lu1 N1 129.25(18) 3_565 . ?
O1 Lu1 N2 84.6(3) 2_665 . ?
O1 Lu1 N2 84.6(3) . 3_565 ?
O1 Lu1 N2 82.6(3) 2_665 2_665 ?
O1 Lu1 N2 163.5(3) 3_565 . ?
O1 Lu1 N2 163.5(3) . 2_665 ?
O1 Lu1 N2 82.6(3) 3_565 3_565 ?
O1 Lu1 N2 82.6(3) . . ?
O1 Lu1 N2 163.5(3) 2_665 3_565 ?
O1 Lu1 N2 84.6(3) 3_565 2_665 ?
N2 Lu1 N1 67.2(2) . . ?
N2 Lu1 N1 67.2(2) 2_665 . ?
N2 Lu1 N1 67.2(2) 3_565 . ?
N2 Lu1 N2 106.0(2) 3_565 . ?
N2 Lu1 N2 106.0(2) 2_665 . ?
N2 Lu1 N2 106.0(2) 2_665 3_565 ?
C7 O1 Lu1 141.4(6) . . ?
C12 O2 H2 109.5 . . ?
C1 N1 Lu1 109.5(8) 3_565 . ?
C1 N1 Lu1 109.5(8) 2_665 . ?
C1 N1 Lu1 109.5(8) . . ?
C1 N1 C1 109.4(8) 2_665 3_565 ?
C1 N1 C1 109.4(8) 3_565 . ?
C1 N1 C1 109.4(8) 2_665 . ?
C2 N2 Lu1 117.5(8) . . ?
C2 N2 C6 118.7(9) . . ?
C6 N2 Lu1 122.8(7) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 C2 110.9(9) . . ?
H1A C1 H1B 108.1 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
N2 C2 C1 116.8(10) . . ?
N2 C2 C3 121.2(10) . . ?
C3 C2 C1 122.0(9) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.5(10) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 118.9(10) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.4(11) . . ?
C6 C5 H5 120.8 . . ?
N2 C6 C5 123.2(10) . . ?
N2 C6 H6 118.4 . . ?
C5 C6 H6 118.4 . . ?
O1 C7 C8 123.8(9) . . ?
O1 C7 C12 117.5(9) . . ?
C8 C7 C12 118.7(10) . . ?
C7 C8 Br1 116.9(7) . . ?
C9 C8 Br1 121.4(7) . . ?
C9 C8 C7 121.7(9) . . ?
C8 C9 Br2 120.3(7) . . ?
C8 C9 C10 120.2(10) . . ?
C10 C9 Br2 119.5(8) . . ?
C9 C10 Br3 121.9(8) . . ?
C9 C10 C11 118.2(9) . . ?
C11 C10 Br3 119.8(7) . . ?
C10 C11 Br4 120.7(7) . . ?
C12 C11 Br4 118.3(7) . . ?
C12 C11 C10 121.0(9) . . ?
O2 C12 C7 120.3(9) . . ?
O2 C12 C11 119.6(9) . . ?
C11 C12 C7 120.0(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84 2.02 2.829(10) 162.6 2_665 yes
C1 H1B Br3 0.99 2.99 3.717(11) 131.3 12_454 yes
C6 H6 O1 0.95 2.66 3.221(13) 118.4 2_665 yes

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
Lu1 O1 C7 C8 -93.9(12) . . . . ?
Lu1 O1 C7 C12 85.5(11) . . . . ?
Lu1 N1 C1 C2 -44.3(9) . . . . ?
Lu1 N2 C2 C1 10.1(12) . . . . ?
Lu1 N2 C2 C3 -168.0(8) . . . . ?
Lu1 N2 C6 C5 166.3(8) . . . . ?
Br1 C8 C9 Br2 -2.2(12) . . . . ?
Br1 C8 C9 C10 177.6(6) . . . . ?
Br2 C9 C10 Br3 3.3(9) . . . . ?
Br2 C9 C10 C11 -179.8(8) . . . . ?
Br3 C10 C11 Br4 -7.3(11) . . . . ?
Br3 C10 C11 C12 174.5(7) . . . . ?
Br4 C11 C12 O2 4.6(13) . . . . ?
Br4 C11 C12 C7 -173.5(6) . . . . ?
O1 C7 C8 Br1 3.9(13) . . . . ?
O1 C7 C8 C9 -177.8(9) . . . . ?
O1 C7 C12 O2 -2.4(12) . . . . ?
O1 C7 C12 C11 175.8(9) . . . . ?
N1 C1 C2 N2 23.6(14) . . . . ?
N1 C1 C2 C3 -158.4(10) . . . . ?
N2 C2 C3 C4 1.0(16) . . . . ?
C1 N1 C1 C2 -164.4(10) 3_565 . . . ?
C1 N1 C1 C2 75.7(16) 2_665 . . . ?
C1 C2 C3 C4 -176.9(10) . . . . ?
C2 N2 C6 C5 -1.9(15) . . . . ?
C2 C3 C4 C5 -2.0(16) . . . . ?
C3 C4 C5 C6 1.0(16) . . . . ?
C4 C5 C6 N2 0.9(16) . . . . ?
C6 N2 C2 C1 179.0(10) . . . . ?
C6 N2 C2 C3 0.9(15) . . . . ?
C7 C8 C9 Br2 179.6(7) . . . . ?
C7 C8 C9 C10 -0.7(14) . . . . ?
C8 C7 C12 O2 177.0(9) . . . . ?
C8 C7 C12 C11 -4.8(12) . . . . ?
C8 C9 C10 Br3 -176.5(8) . . . . ?
C8 C9 C10 C11 0.5(11) . . . . ?
C9 C10 C11 Br4 175.7(6) . . . . ?
C9 C10 C11 C12 -2.5(13) . . . . ?
C10 C11 C12 O2 -177.1(9) . . . . ?
C10 C11 C12 C7 4.7(14) . . . . ?
C12 C7 C8 Br1 -175.5(6) . . . . ?
C12 C7 C8 C9 2.8(14) . . . . ?

_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 0.582
_exptl_crystal_recrystallization_method 'From reaction'
