#------------------------------------------------------------------------------
#$Date: 2025-07-06 20:11:11 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300981 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/80/7718072.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7718072
loop_
_publ_author_name
'Bagio, Stanley'
'González, Jonay'
'Gable, Robert W.'
'Hall, Christopher R.'
'Boskovic, Colette'
'Giansiracusa, Marcus J.'
_publ_section_title
;
 Redox, spectroscopic and magnetic properties of
 C₃-symmetric rare earth complexes featuring atypical
 ortho-dioxolene binding.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5061
_journal_page_last               5074
_journal_paper_doi               10.1039/d4dt03474k
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H21 Br12 Ho N4 O6'
_chemical_formula_sum            'C36 H21 Br12 Ho N4 O6'
_chemical_formula_weight         1729.42
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-28 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.12110(10)
_cell_length_b                   13.12110(10)
_cell_length_c                   46.2179(6)
_cell_measurement_reflns_used    23073
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.7810
_cell_measurement_theta_min      4.1370
_cell_volume                     6890.99(12)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_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_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_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_recrystallization_method 'From reaction'
_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.046
_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_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_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0306
_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
_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_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03474k2.cif
_cod_data_source_block           sb01-05-ho1-xrd-100k_abs
_cod_depositor_comments
'Adding full bibliography for 7718068--7718078.cif.'
_cod_original_cell_volume        6890.98(14)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7718072
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Ho Br12 O6 N4 C36'
_chemical_oxdiff_usercomment     'colourless cube in oil 100K'
_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.
;
_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)
;
_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
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'
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 . . . . .
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'
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
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_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_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) . . . . ?
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
