#------------------------------------------------------------------------------
#$Date: 2023-09-05 22:43:50 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286121 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/71/7247119.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_7247119
loop_
_publ_author_name
'Matsumoto, Daiki'
'Tanaka, Chiaki'
'Fujibayashi, Masaru'
'Nishihara, Sadafumi'
'Takahashi, Kiyonori'
'Nakamura, Takayoshi'
'Akutagawa, Tomoyuki'
'Masuya-Suzuki, Atsuko'
'Tsunashima, Ryo'
_publ_section_title
;
 Crystallographic and dielectric studies of tetrahedral {NH4@Fe4}
 crystallized with halomethane molecules
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              4793
_journal_page_last               4797
_journal_paper_doi               10.1039/D3CE00429E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         '2(C H Br3), C72 H72 Fe4 O60, 0.5(H8 N2)'
_chemical_formula_sum            'C74 H78 Br6 Fe4 N O60'
_chemical_formula_weight         2644.23
_chemical_name_systematic        C72H72O60Fe4(CHBr3)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-13 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 133.527(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.5848(4)
_cell_length_b                   17.97775(10)
_cell_length_c                   15.1052(2)
_cell_measurement_reflns_used    20804
_cell_measurement_temperature    223
_cell_measurement_theta_max      72.4000
_cell_measurement_theta_min      3.8980
_cell_volume                     5431.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223.15
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00 -14.00   0.50    1.16    --  -43.03  95.00  95.00  108
  2  ω    -11.00  25.00   0.50    1.16    --  -43.03  95.00  95.00   72
  3  ω      9.00  67.00   0.50    1.16    --   43.03 -95.00 -14.00  116
  4  ω    -25.00   3.00   0.50    1.16    --   43.03 -95.00 -14.00   56
  5  ω    -67.00 -40.00   0.50    4.64    -- -103.00  95.00  95.00   54
  6  ω     92.00 178.00   0.50    4.64    --  113.50  95.00  95.00  172
  7  ω     21.00 115.00   0.50    1.16    --   43.03  57.00  30.00  188
  8  ω     26.00  64.00   0.50    1.16    --   43.03 -38.00 -30.00   76
  9  ω    -32.00  22.00   0.50    1.16    --   43.03 -38.00 -30.00  108
 10  ω     22.00 116.00   0.50    1.16    --   43.03  57.00  90.00  188
 11  ω     23.00 116.00   0.50    1.16    --   43.03  57.00 -90.00  186
 12  ω   -153.00-128.00   0.50    4.64    -- -103.00 -95.00 -14.00   50
 13  ω     39.00 105.00   0.50    4.64    --  113.50 -95.00  90.00  132
 14  ω     98.00 135.00   0.50    4.64    --  113.50 -45.00-180.00   74
 15  ω     85.00 178.00   0.50    4.64    --  113.50  77.00-120.00  186
 16  ω     38.00  90.00   0.50    4.64    --  113.50 -45.00-180.00  104
 17  ω     90.00 172.00   0.50    4.64    --  113.50  61.00  60.00  164
 18  ω     38.00  82.00   0.50    4.64    --  113.50 -45.00 -60.00   88
 19  ω     89.00 134.00   0.50    4.64    --  113.50 -45.00 -60.00   90
 20  ω     90.00 174.00   0.50    4.64    --  113.50  61.00 -60.00  168
 21  ω     39.00 105.00   0.50    4.64    --  113.50 -95.00 120.00  132
 22  ω     85.00 173.00   0.50    4.64    --  113.50  77.00  30.00  176
 23  ω     90.00 178.00   0.50    4.64    --  113.50  61.00-150.00  176
 24  ω     91.00 177.00   0.50    4.64    --  113.50  45.00-180.00  172
 25  ω     41.00 105.00   0.50    4.64    --  113.50 -95.00 -90.00  128
 26  ω     39.00 103.00   0.50    4.64    --  113.50 -95.00  30.00  128
 27  ω     43.00 103.00   0.50    4.64    --  113.50 -95.00 -60.00  120
 28  ω     57.00 105.00   0.50    4.64    --  113.50 -95.00 -14.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.744
_diffrn_reflns_theta_min         3.305
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    7.656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (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_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             2646
_exptl_crystal_preparation       'local laboratory'
_exptl_crystal_recrystallization_method 'vaper diffusion with hexane'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.937
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.441(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10523
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0708
_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)+(0.1438P)²+24.0166P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                10136
_reflns_number_total             10523
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce00429e2.cif
_cod_data_source_block           1-chbr3
_cod_depositor_comments
'Adding full bibliography for 7247116--7247119.cif.'
_cod_original_cell_volume        5431.3(2)
_cod_database_code               7247119
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.572
_shelx_estimated_absorpt_t_min   0.443
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.559(7)
 0.441(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H1A
 1.07 with sigma of 0.02
 N1-H1B
 1.07 with sigma of 0.02
 N1-H1C
 1.07 with sigma of 0.02
 N1-H1D
 1.07 with sigma of 0.02
 H1A-H1B
 1.75 with sigma of 0.04
 H1A-H1C
 1.75 with sigma of 0.04
 H1A-H1D
 1.75 with sigma of 0.04
 H1B-H1C
 1.75 with sigma of 0.04
 H1B-H1D
 1.75 with sigma of 0.04
 H1C-H1D
 1.75 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(O8)
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
6.a Ternary CH refined with riding coordinates:
 C99(H99)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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
Br1 Br 0.54160(15) 0.45255(12) 0.3214(2) 0.1013(8) Uani 1 1 d . . . . .
Br2 Br 0.57576(15) 0.45605(18) 0.1630(3) 0.1185(10) Uani 1 1 d . . . . .
Br3 Br 0.49331(16) 0.32099(15) 0.1362(3) 0.1136(9) Uani 1 1 d . . . . .
C99 C 0.5117(9) 0.4265(10) 0.1705(16) 0.069(4) Uani 1 1 d . . . . .
H99 H 0.469579 0.453755 0.106059 0.083 Uiso 1 1 calc R U . . .
Fe1 Fe 0.66061(6) 0.45646(7) 0.72002(10) 0.0197(3) Uani 1 1 d . . . . .
Fe2 Fe 0.50967(6) 0.70521(7) 0.29995(10) 0.0192(3) Uani 1 1 d . . . . .
O1 O 0.6755(3) 0.3666(3) 0.6640(6) 0.0264(12) Uani 1 1 d . . . . .
O2 O 0.6575(4) 0.2795(4) 0.5416(8) 0.0438(18) Uani 1 1 d . . . . .
O3 O 0.5546(4) 0.1905(4) 0.4560(8) 0.053(2) Uani 1 1 d . . . . .
O4 O 0.4640(3) 0.2634(5) 0.3345(7) 0.0480(19) Uani 1 1 d . . . . .
O5 O 0.5664(3) 0.4225(3) 0.6072(6) 0.0270(12) Uani 1 1 d . . . . .
O6 O 0.7537(3) 0.5014(4) 0.8313(6) 0.0301(13) Uani 1 1 d . . . . .
O7 O 0.8205(3) 0.6004(4) 0.9212(6) 0.0343(14) Uani 1 1 d . . . . .
O8 O 0.8152(5) 0.6904(7) 0.7783(10) 0.088(4) Uani 1 1 d . . . . .
O9 O 0.7090(5) 0.7319(4) 0.6400(8) 0.053(2) Uani 1 1 d . . . . .
O10 O 0.6420(3) 0.5187(3) 0.5935(5) 0.0260(12) Uani 1 1 d . . . . .
O11 O 0.5543(3) 0.6731(4) 0.2417(6) 0.0277(12) Uani 1 1 d . . . . .
O12 O 0.6382(4) 0.6452(5) 0.2576(6) 0.0381(16) Uani 1 1 d . . . . .
O13 O 0.7628(4) 0.6362(6) 0.5128(10) 0.063(3) Uani 1 1 d . . . . .
O14 O 0.7333(5) 0.5230(6) 0.5111(13) 0.077(3) Uani 1 1 d . . . . .
O15 O 0.5758(3) 0.6430(4) 0.4423(5) 0.0257(12) Uani 1 1 d . . . . .
O16 O 0.5681(3) 0.7952(3) 0.3640(6) 0.0285(13) Uani 1 1 d . . . . .
O17 O 0.6380(4) 0.8845(4) 0.4921(7) 0.0381(16) Uani 1 1 d . . . . .
O18 O 0.6026(5) 0.8794(5) 0.6904(8) 0.052(2) Uani 1 1 d . . . . .
O19 O 0.5916(5) 0.9696(4) 0.5775(9) 0.057(2) Uani 1 1 d . . . . .
O20 O 0.4855(3) 0.7426(3) 0.3881(5) 0.0241(11) Uani 1 1 d . . . . .
O21 O 0.4352(3) 0.7533(3) 0.1371(5) 0.0257(12) Uani 1 1 d . . . . .
O22 O 0.3322(3) 0.7811(4) -0.0379(6) 0.0373(15) Uani 1 1 d . . . . .
O23 O 0.2491(4) 0.6644(5) -0.1631(7) 0.051(2) Uani 1 1 d . . . . .
O24 O 0.2398(4) 0.6283(5) -0.0331(8) 0.0474(19) Uani 1 1 d . . . . .
O25 O 0.4484(3) 0.6212(3) 0.2352(5) 0.0246(11) Uani 1 1 d . . . . .
O26 O 0.3116(3) 0.3978(3) 0.1370(6) 0.0283(13) Uani 1 1 d . . . . .
O27 O 0.3060(5) 0.3641(4) -0.0104(8) 0.0468(19) Uani 1 1 d . . . . .
O28 O 0.2716(4) 0.4866(5) -0.1561(6) 0.0452(18) Uani 1 1 d . . . . .
O29 O 0.3773(4) 0.5239(5) -0.0334(7) 0.0422(17) Uani 1 1 d . . . . .
O30 O 0.3660(3) 0.5358(3) 0.2322(5) 0.0246(12) Uani 1 1 d . . . . .
C1 C 0.6362(4) 0.3224(5) 0.5789(8) 0.0235(16) Uani 1 1 d . . . . .
C2 C 0.7276(7) 0.2923(11) 0.6042(18) 0.081(6) Uani 1 1 d . . . . .
H2A H 0.729175 0.314401 0.547658 0.121 Uiso 1 1 calc R U . . .
H2B H 0.751361 0.245223 0.633482 0.121 Uiso 1 1 calc R U . . .
H2C H 0.748464 0.325551 0.672754 0.121 Uiso 1 1 calc R U . . .
C3 C 0.5155(8) 0.1289(9) 0.3771(17) 0.079(5) Uani 1 1 d . . . . .
H3A H 0.494349 0.141345 0.294623 0.118 Uiso 1 1 calc R U . . .
H3B H 0.481428 0.117583 0.377892 0.118 Uiso 1 1 calc R U . . .
H3C H 0.544173 0.085889 0.405120 0.118 Uiso 1 1 calc R U . . .
C4 C 0.5236(4) 0.2536(6) 0.4261(8) 0.0300(18) Uani 1 1 d . . . . .
C5 C 0.5659(4) 0.3156(5) 0.5152(8) 0.0252(16) Uani 1 1 d . . . . .
C6 C 0.5369(4) 0.3653(4) 0.5343(7) 0.0219(15) Uani 1 1 d . . . . .
C7 C 0.7684(4) 0.5667(5) 0.8248(7) 0.0244(16) Uani 1 1 d . . . . .
C8 C 0.8616(6) 0.5597(7) 1.0345(9) 0.045(3) Uani 1 1 d . . . . .
H8A H 0.890604 0.526113 1.038685 0.068 Uiso 1 1 calc R U . . .
H8B H 0.833255 0.531394 1.038605 0.068 Uiso 1 1 calc R U . . .
H8C H 0.888509 0.594333 1.102357 0.068 Uiso 1 1 calc R U . . .
C9 C 0.8382(7) 0.7661(11) 0.7851(14) 0.088(4) Uani 1 1 d . . . . .
H9A H 0.831326 0.775321 0.713882 0.132 Uiso 1 1 calc R U . . .
H9B H 0.885317 0.770784 0.858314 0.132 Uiso 1 1 calc R U . . .
H9C H 0.812894 0.802071 0.787589 0.132 Uiso 1 1 calc R U . . .
C10 C 0.7495(5) 0.6843(6) 0.7078(9) 0.035(2) Uani 1 1 d . . . . .
C11 C 0.7291(4) 0.6085(5) 0.7115(8) 0.0250(16) Uani 1 1 d . . . . .
C12 C 0.6720(4) 0.5786(5) 0.6067(8) 0.0226(15) Uani 1 1 d . . . . .
C13 C 0.6122(4) 0.6472(5) 0.3041(8) 0.0275(17) Uani 1 1 d . . . . .
C14 C 0.5992(7) 0.6695(9) 0.1346(11) 0.053(3) Uani 1 1 d . . . . .
H14A H 0.583590 0.719836 0.125382 0.080 Uiso 1 1 calc R U . . .
H14B H 0.561084 0.636713 0.079149 0.080 Uiso 1 1 calc R U . . .
H14C H 0.626450 0.668448 0.115761 0.080 Uiso 1 1 calc R U . . .
C15 C 0.8287(7) 0.6052(15) 0.5697(18) 0.094(7) Uani 1 1 d . . . . .
H15A H 0.855446 0.643791 0.575688 0.141 Uiso 1 1 calc R U . . .
H15B H 0.822193 0.564701 0.519815 0.141 Uiso 1 1 calc R U . . .
H15C H 0.851663 0.586685 0.650630 0.141 Uiso 1 1 calc R U . . .
C16 C 0.7201(5) 0.5862(6) 0.4853(9) 0.033(2) Uani 1 1 d . . . . .
C17 C 0.6537(4) 0.6210(5) 0.4261(8) 0.0259(16) Uani 1 1 d . . . . .
C18 C 0.6323(4) 0.6178(4) 0.4836(8) 0.0230(15) Uani 1 1 d . . . . .
C19 C 0.5871(4) 0.8405(5) 0.4454(8) 0.0272(17) Uani 1 1 d . . . . .
C20 C 0.6714(6) 0.8746(7) 0.4483(13) 0.050(3) Uani 1 1 d . . . . .
H20A H 0.676752 0.821893 0.443156 0.076 Uiso 1 1 calc R U . . .
H20B H 0.714917 0.898255 0.504696 0.076 Uiso 1 1 calc R U . . .
H20C H 0.644453 0.897000 0.368226 0.076 Uiso 1 1 calc R U . . .
C21 C 0.6236(10) 0.9336(12) 0.7811(15) 0.086(6) Uani 1 1 d . . . . .
H21A H 0.584651 0.958788 0.756042 0.129 Uiso 1 1 calc R U . . .
H21B H 0.652729 0.969719 0.789682 0.129 Uiso 1 1 calc R U . . .
H21C H 0.647474 0.908944 0.858677 0.129 Uiso 1 1 calc R U . . .
C22 C 0.5860(5) 0.9058(5) 0.5909(9) 0.033(2) Uani 1 1 d . . . . .
C23 C 0.5604(4) 0.8440(5) 0.4998(8) 0.0269(17) Uani 1 1 d . . . . .
C24 C 0.5132(4) 0.7952(5) 0.4692(7) 0.0231(16) Uani 1 1 d . . . . .
C25 C 0.3746(4) 0.7339(5) 0.0530(8) 0.0245(16) Uani 1 1 d . . . . .
C26 C 0.3587(6) 0.8482(6) -0.0435(11) 0.048(3) Uani 1 1 d . . . . .
H26A H 0.395315 0.835694 -0.036711 0.072 Uiso 1 1 calc R U . . .
H26B H 0.374697 0.880918 0.023116 0.072 Uiso 1 1 calc R U . . .
H26C H 0.323759 0.873117 -0.120706 0.072 Uiso 1 1 calc R U . . .
C27 C 0.1778(6) 0.6510(8) -0.2619(11) 0.062(4) Uani 1 1 d . . . . .
H27A H 0.164287 0.612193 -0.238096 0.093 Uiso 1 1 calc R U . . .
H27B H 0.168146 0.635564 -0.334222 0.093 Uiso 1 1 calc R U . . .
H27C H 0.153502 0.696348 -0.279243 0.093 Uiso 1 1 calc R U . . .
C28 C 0.2733(4) 0.6510(5) -0.0514(8) 0.0293(18) Uani 1 1 d . . . . .
C29 C 0.3461(4) 0.6663(5) 0.0472(7) 0.0246(16) Uani 1 1 d . . . . .
C30 C 0.3866(4) 0.6142(4) 0.1397(7) 0.0200(15) Uani 1 1 d . . . . .
C31 C 0.3167(5) 0.4149(5) 0.0634(8) 0.0256(16) Uani 1 1 d . . . . .
C32 C 0.2927(9) 0.2887(6) 0.0033(16) 0.064(4) Uani 1 1 d . . . . .
H32A H 0.246084 0.284381 -0.038526 0.097 Uiso 1 1 calc R U . . .
H32B H 0.320800 0.277713 0.089300 0.097 Uiso 1 1 calc R U . . .
H32C H 0.302428 0.253848 -0.031776 0.097 Uiso 1 1 calc R U . . .
C33 C 0.2626(8) 0.4969(9) -0.2608(11) 0.064(4) Uani 1 1 d . . . . .
H33A H 0.245437 0.451453 -0.308379 0.095 Uiso 1 1 calc R U . . .
H33B H 0.305206 0.509254 -0.234248 0.095 Uiso 1 1 calc R U . . .
H33C H 0.231151 0.537092 -0.310532 0.095 Uiso 1 1 calc R U . . .
C34 C 0.3317(5) 0.5002(5) -0.0476(8) 0.0305(18) Uani 1 1 d . . . . .
C35 C 0.3353(4) 0.4861(5) 0.0547(8) 0.0229(15) Uani 1 1 d . . . . .
C36 C 0.3588(4) 0.5411(4) 0.1397(7) 0.0203(15) Uani 1 1 d . . . . .
N1 N 0.500000 0.5781(7) 0.500000 0.035(2) Uani 1 2 d DS T P . .
H1A H 0.533(7) 0.605(10) 0.497(17) 0.041 Uiso 0.5 1 d D U P A -1
H1B H 0.496(9) 0.607(10) 0.556(14) 0.041 Uiso 0.5 1 d D U P B -1
H1C H 0.514(8) 0.521(3) 0.527(14) 0.041 Uiso 0.5 1 d D U P C -1
H1D H 0.451(4) 0.576(9) 0.408(7) 0.041 Uiso 0.5 1 d D U P D -1
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'
Fe Fe -1.1336 3.1974 '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
-17 2 7 0.0643
-9 9 1 0.0598
16 3 -8 0.0524
7 -10 0 0.0301
8 8 0 0.0192
-9 -8 0 0.0612
14 1 -10 0.0503
-9 3 9 0.0411
-15 -5 8 0.0621
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
Br1 C99 Br2 110.5(9) . . ?
Br1 C99 Br3 112.7(8) . . ?
Br1 C99 H99 107.9 . . ?
Br2 C99 Br3 109.6(9) . . ?
Br2 C99 H99 107.9 . . ?
Br3 C99 H99 107.9 . . ?
O1 Fe1 O6 99.2(3) . . ?
O1 Fe1 O26 89.6(3) . 2_656 ?
O5 Fe1 O1 85.3(2) . . ?
O5 Fe1 O6 174.5(3) . . ?
O5 Fe1 O26 93.8(3) . 2_656 ?
O10 Fe1 O1 92.4(3) . . ?
O10 Fe1 O5 91.7(3) . . ?
O10 Fe1 O6 85.0(3) . . ?
O10 Fe1 O26 174.3(3) . 2_656 ?
O10 Fe1 O30 91.8(3) . 2_656 ?
O26 Fe1 O6 89.4(3) 2_656 . ?
O30 Fe1 O1 170.9(3) 2_656 . ?
O30 Fe1 O5 86.5(3) 2_656 . ?
O30 Fe1 O6 89.2(3) 2_656 . ?
O30 Fe1 O26 87.0(2) 2_656 2_656 ?
O15 Fe2 O11 86.0(2) . . ?
O15 Fe2 O16 95.8(3) . . ?
O15 Fe2 O20 86.9(2) . . ?
O15 Fe2 O21 170.4(3) . . ?
O15 Fe2 O25 86.4(3) . . ?
O16 Fe2 O11 84.9(3) . . ?
O16 Fe2 O21 92.7(3) . . ?
O20 Fe2 O11 167.9(3) . . ?
O20 Fe2 O16 86.2(2) . . ?
O20 Fe2 O21 98.3(3) . . ?
O21 Fe2 O11 90.3(3) . . ?
O25 Fe2 O11 97.9(3) . . ?
O25 Fe2 O16 176.6(3) . . ?
O25 Fe2 O20 91.3(3) . . ?
O25 Fe2 O21 85.3(2) . . ?
C1 O1 Fe1 132.1(5) . . ?
C1 O2 C2 114.3(8) . . ?
C4 O3 C3 116.6(9) . . ?
C6 O5 Fe1 130.9(5) . . ?
C7 O6 Fe1 126.4(5) . . ?
C7 O7 C8 117.0(8) . . ?
C10 O8 C9 114.5(12) . . ?
C12 O10 Fe1 128.3(5) . . ?
C13 O11 Fe2 128.1(6) . . ?
C13 O12 C14 119.4(8) . . ?
C16 O13 C15 113.8(12) . . ?
C18 O15 Fe2 129.2(5) . . ?
C19 O16 Fe2 130.9(5) . . ?
C19 O17 C20 117.0(8) . . ?
C22 O18 C21 115.9(11) . . ?
C24 O20 Fe2 129.1(5) . . ?
C25 O21 Fe2 129.6(5) . . ?
C25 O22 C26 118.3(8) . . ?
C28 O23 C27 114.3(10) . . ?
C30 O25 Fe2 131.7(5) . . ?
C31 O26 Fe1 129.1(5) . 2_656 ?
C31 O27 C32 117.5(8) . . ?
C34 O28 C33 117.4(9) . . ?
C36 O30 Fe1 130.2(5) . 2_656 ?
O1 C1 O2 119.5(8) . . ?
O1 C1 C5 123.5(7) . . ?
O2 C1 C5 117.0(8) . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O3 C4 C5 114.7(7) . . ?
O4 C4 O3 124.4(9) . . ?
O4 C4 C5 120.9(8) . . ?
C1 C5 C4 120.8(7) . . ?
C6 C5 C1 121.0(8) . . ?
C6 C5 C4 118.2(7) . . ?
O5 C6 C5 125.8(7) . . ?
O5 C6 C6 109.8(6) . 2_656 ?
C5 C6 C6 124.3(7) . 2_656 ?
O6 C7 O7 120.9(8) . . ?
O6 C7 C11 123.4(7) . . ?
O7 C7 C11 115.7(8) . . ?
O7 C8 H8A 109.5 . . ?
O7 C8 H8B 109.5 . . ?
O7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O8 C9 H9A 109.5 . . ?
O8 C9 H9B 109.5 . . ?
O8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O8 C10 C11 112.8(9) . . ?
O9 C10 O8 125.2(10) . . ?
O9 C10 C11 121.8(9) . . ?
C7 C11 C10 121.5(8) . . ?
C12 C11 C7 119.6(8) . . ?
C12 C11 C10 118.9(8) . . ?
O10 C12 C11 128.2(8) . . ?
O10 C12 C18 110.5(7) . . ?
C11 C12 C18 121.3(7) . . ?
O11 C13 O12 119.5(8) . . ?
O11 C13 C17 124.5(8) . . ?
O12 C13 C17 116.0(8) . . ?
O12 C14 H14A 109.5 . . ?
O12 C14 H14B 109.5 . . ?
O12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O13 C15 H15A 109.5 . . ?
O13 C15 H15B 109.5 . . ?
O13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O13 C16 C17 111.3(8) . . ?
O14 C16 O13 123.8(10) . . ?
O14 C16 C17 124.7(10) . . ?
C13 C17 C16 118.0(8) . . ?
C18 C17 C13 122.1(8) . . ?
C18 C17 C16 119.4(8) . . ?
O15 C18 C12 111.3(7) . . ?
O15 C18 C17 126.2(8) . . ?
C17 C18 C12 122.5(7) . . ?
O16 C19 O17 119.3(8) . . ?
O16 C19 C23 124.0(8) . . ?
O17 C19 C23 116.5(8) . . ?
O17 C20 H20A 109.5 . . ?
O17 C20 H20B 109.5 . . ?
O17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O18 C21 H21A 109.5 . . ?
O18 C21 H21B 109.5 . . ?
O18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O18 C22 C23 110.5(8) . . ?
O19 C22 O18 123.7(9) . . ?
O19 C22 C23 125.8(9) . . ?
C19 C23 C22 116.9(8) . . ?
C24 C23 C19 121.8(8) . . ?
C24 C23 C22 121.3(8) . . ?
O20 C24 C23 126.4(7) . . ?
O20 C24 C24 110.8(7) . 2_656 ?
C23 C24 C24 122.7(7) . 2_656 ?
O21 C25 O22 118.4(8) . . ?
O21 C25 C29 126.2(8) . . ?
O22 C25 C29 115.3(7) . . ?
O22 C26 H26A 109.5 . . ?
O22 C26 H26B 109.5 . . ?
O22 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O23 C27 H27A 109.5 . . ?
O23 C27 H27B 109.5 . . ?
O23 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O23 C28 C29 112.6(8) . . ?
O24 C28 O23 123.7(8) . . ?
O24 C28 C29 123.7(9) . . ?
C25 C29 C28 122.0(7) . . ?
C30 C29 C25 119.3(7) . . ?
C30 C29 C28 118.6(8) . . ?
O25 C30 C29 126.5(8) . . ?
O25 C30 C36 111.6(7) . . ?
C29 C30 C36 121.8(7) . . ?
O26 C31 O27 119.2(8) . . ?
O26 C31 C35 125.0(8) . . ?
O27 C31 C35 115.8(7) . . ?
O27 C32 H32A 109.5 . . ?
O27 C32 H32B 109.5 . . ?
O27 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O28 C33 H33A 109.5 . . ?
O28 C33 H33B 109.5 . . ?
O28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O28 C34 C35 112.5(7) . . ?
O29 C34 O28 123.5(8) . . ?
O29 C34 C35 123.9(8) . . ?
C31 C35 C34 118.5(7) . . ?
C36 C35 C31 121.8(7) . . ?
C36 C35 C34 119.6(7) . . ?
O30 C36 C30 111.5(7) . . ?
O30 C36 C35 126.1(7) . . ?
C35 C36 C30 122.2(7) . . ?
H1A N1 H1B 113(5) . . ?
H1A N1 H1C 111(5) . . ?
H1A N1 H1D 108(5) . . ?
H1B N1 H1C 112(5) . . ?
H1B N1 H1D 108(5) . . ?
H1C N1 H1D 105(5) . . ?
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
Br1 C99 1.872(17) . ?
Br2 C99 1.923(15) . ?
Br3 C99 1.939(18) . ?
C99 H99 0.9900 . ?
Fe1 O1 1.993(6) . ?
Fe1 O5 1.983(6) . ?
Fe1 O6 2.031(6) . ?
Fe1 O10 1.954(6) . ?
Fe1 O26 2.021(6) 2_656 ?
Fe1 O30 1.956(6) 2_656 ?
Fe2 O11 2.027(6) . ?
Fe2 O15 1.949(6) . ?
Fe2 O16 2.002(6) . ?
Fe2 O20 1.974(5) . ?
Fe2 O21 2.014(6) . ?
Fe2 O25 1.954(6) . ?
O1 C1 1.242(11) . ?
O2 C1 1.309(10) . ?
O2 C2 1.471(14) . ?
O3 C3 1.428(15) . ?
O3 C4 1.301(12) . ?
O4 C4 1.231(12) . ?
O5 C6 1.303(10) . ?
O6 C7 1.268(11) . ?
O7 C7 1.293(11) . ?
O7 C8 1.440(12) . ?
O8 C9 1.474(17) . ?
O8 C10 1.332(14) . ?
O9 C10 1.206(14) . ?
O10 C12 1.287(11) . ?
O11 C13 1.260(11) . ?
O12 C13 1.304(11) . ?
O12 C14 1.432(13) . ?
O13 C15 1.484(18) . ?
O13 C16 1.303(14) . ?
O14 C16 1.174(15) . ?
O15 C18 1.298(10) . ?
O16 C19 1.250(11) . ?
O17 C19 1.314(11) . ?
O17 C20 1.467(11) . ?
O18 C21 1.439(15) . ?
O18 C22 1.321(13) . ?
O19 C22 1.193(14) . ?
O20 C24 1.301(10) . ?
O21 C25 1.267(10) . ?
O22 C25 1.328(10) . ?
O22 C26 1.442(12) . ?
O23 C27 1.452(13) . ?
O23 C28 1.342(13) . ?
O24 C28 1.203(13) . ?
O25 C30 1.272(10) . ?
O26 C31 1.251(10) . ?
O27 C31 1.308(11) . ?
O27 C32 1.454(13) . ?
O28 C33 1.433(13) . ?
O28 C34 1.324(12) . ?
O29 C34 1.199(12) . ?
O30 C36 1.271(10) . ?
C1 C5 1.461(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 C5 1.502(13) . ?
C5 C6 1.355(12) . ?
C6 C6 1.522(15) 2_656 ?
C7 C11 1.453(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 C11 1.491(13) . ?
C11 C12 1.356(12) . ?
C12 C18 1.533(11) . ?
C13 C17 1.422(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 C17 1.513(12) . ?
C17 C18 1.347(12) . ?
C19 C23 1.434(12) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 C23 1.512(12) . ?
C23 C24 1.360(12) . ?
C24 C24 1.526(15) 2_656 ?
C25 C29 1.418(12) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C28 C29 1.486(11) . ?
C29 C30 1.388(12) . ?
C30 C36 1.521(11) . ?
C31 C35 1.420(11) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C34 C35 1.499(11) . ?
C35 C36 1.379(11) . ?
N1 H1A 1.07(3) . ?
N1 H1B 1.07(3) . ?
N1 H1C 1.08(3) . ?
N1 H1D 1.09(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O1 C1 O2 162.2(7) . . . . ?
Fe1 O1 C1 C5 -17.0(13) . . . . ?
Fe1 O5 C6 C5 -3.2(12) . . . . ?
Fe1 O5 C6 C6 -179.2(6) . . . 2_656 ?
Fe1 O6 C7 O7 151.1(7) . . . . ?
Fe1 O6 C7 C11 -28.7(12) . . . . ?
Fe1 O10 C12 C11 8.9(13) . . . . ?
Fe1 O10 C12 C18 -168.3(5) . . . . ?
Fe1 O26 C31 O27 168.6(7) 2_656 . . . ?
Fe1 O26 C31 C35 -9.6(14) 2_656 . . . ?
Fe1 O30 C36 C30 179.0(5) 2_656 . . . ?
Fe1 O30 C36 C35 -7.1(12) 2_656 . . . ?
Fe2 O11 C13 O12 -164.6(7) . . . . ?
Fe2 O11 C13 C17 13.6(13) . . . . ?
Fe2 O15 C18 C12 173.4(5) . . . . ?
Fe2 O15 C18 C17 -10.0(13) . . . . ?
Fe2 O16 C19 O17 163.5(7) . . . . ?
Fe2 O16 C19 C23 -11.1(14) . . . . ?
Fe2 O20 C24 C23 9.9(13) . . . . ?
Fe2 O20 C24 C24 -169.0(6) . . . 2_656 ?
Fe2 O21 C25 O22 169.0(6) . . . . ?
Fe2 O21 C25 C29 -8.9(13) . . . . ?
Fe2 O25 C30 C29 6.0(12) . . . . ?
Fe2 O25 C30 C36 -171.0(5) . . . . ?
O1 C1 C5 C4 -170.8(8) . . . . ?
O1 C1 C5 C6 9.6(13) . . . . ?
O2 C1 C5 C4 10.0(12) . . . . ?
O2 C1 C5 C6 -169.6(8) . . . . ?
O3 C4 C5 C1 36.5(12) . . . . ?
O3 C4 C5 C6 -143.9(9) . . . . ?
O4 C4 C5 C1 -145.2(9) . . . . ?
O4 C4 C5 C6 34.3(13) . . . . ?
O6 C7 C11 C10 -178.1(8) . . . . ?
O6 C7 C11 C12 2.6(13) . . . . ?
O7 C7 C11 C10 2.0(12) . . . . ?
O7 C7 C11 C12 -177.2(8) . . . . ?
O8 C10 C11 C7 40.0(13) . . . . ?
O8 C10 C11 C12 -140.7(10) . . . . ?
O9 C10 C11 C7 -145.2(10) . . . . ?
O9 C10 C11 C12 34.0(14) . . . . ?
O10 C12 C18 O15 66.9(9) . . . . ?
O10 C12 C18 C17 -109.9(9) . . . . ?
O11 C13 C17 C16 175.5(9) . . . . ?
O11 C13 C17 C18 4.0(14) . . . . ?
O12 C13 C17 C16 -6.3(13) . . . . ?
O12 C13 C17 C18 -177.8(9) . . . . ?
O13 C16 C17 C13 72.8(11) . . . . ?
O13 C16 C17 C18 -115.4(10) . . . . ?
O14 C16 C17 C13 -112.1(14) . . . . ?
O14 C16 C17 C18 59.7(16) . . . . ?
O16 C19 C23 C22 -175.9(9) . . . . ?
O16 C19 C23 C24 2.7(14) . . . . ?
O17 C19 C23 C22 9.3(13) . . . . ?
O17 C19 C23 C24 -172.1(9) . . . . ?
O18 C22 C23 C19 -132.6(9) . . . . ?
O18 C22 C23 C24 48.8(13) . . . . ?
O19 C22 C23 C19 46.6(15) . . . . ?
O19 C22 C23 C24 -132.0(12) . . . . ?
O21 C25 C29 C28 175.6(9) . . . . ?
O21 C25 C29 C30 -0.6(13) . . . . ?
O22 C25 C29 C28 -2.4(12) . . . . ?
O22 C25 C29 C30 -178.7(8) . . . . ?
O23 C28 C29 C25 49.7(12) . . . . ?
O23 C28 C29 C30 -134.0(9) . . . . ?
O24 C28 C29 C25 -131.1(10) . . . . ?
O24 C28 C29 C30 45.2(13) . . . . ?
O25 C30 C36 O30 59.0(9) . . . . ?
O25 C30 C36 C35 -115.1(8) . . . . ?
O26 C31 C35 C34 -173.2(9) . . . . ?
O26 C31 C35 C36 9.2(14) . . . . ?
O27 C31 C35 C34 8.6(13) . . . . ?
O27 C31 C35 C36 -169.0(9) . . . . ?
O28 C34 C35 C31 55.6(12) . . . . ?
O28 C34 C35 C36 -126.8(9) . . . . ?
O29 C34 C35 C31 -127.1(10) . . . . ?
O29 C34 C35 C36 50.5(14) . . . . ?
C1 C5 C6 O5 0.4(13) . . . . ?
C1 C5 C6 C6 175.8(8) . . . 2_656 ?
C2 O2 C1 O1 -2.9(16) . . . . ?
C2 O2 C1 C5 176.4(12) . . . . ?
C3 O3 C4 O4 -1.3(18) . . . . ?
C3 O3 C4 C5 176.9(13) . . . . ?
C4 C5 C6 O5 -179.2(8) . . . . ?
C4 C5 C6 C6 -3.8(13) . . . 2_656 ?
C7 C11 C12 O10 8.3(13) . . . . ?
C7 C11 C12 C18 -174.8(7) . . . . ?
C8 O7 C7 O6 1.8(13) . . . . ?
C8 O7 C7 C11 -178.3(8) . . . . ?
C9 O8 C10 O9 10(2) . . . . ?
C9 O8 C10 C11 -175.2(13) . . . . ?
C10 C11 C12 O10 -171.0(8) . . . . ?
C10 C11 C12 C18 5.9(12) . . . . ?
C11 C12 C18 O15 -110.5(9) . . . . ?
C11 C12 C18 C17 72.7(11) . . . . ?
C13 C17 C18 O15 -6.2(14) . . . . ?
C13 C17 C18 C12 170.1(8) . . . . ?
C14 O12 C13 O11 -2.6(15) . . . . ?
C14 O12 C13 C17 179.0(10) . . . . ?
C15 O13 C16 O14 5.7(19) . . . . ?
C15 O13 C16 C17 -179.2(12) . . . . ?
C16 C17 C18 O15 -177.6(8) . . . . ?
C16 C17 C18 C12 -1.3(13) . . . . ?
C19 C23 C24 O20 -2.1(14) . . . . ?
C19 C23 C24 C24 176.6(8) . . . 2_656 ?
C20 O17 C19 O16 -2.8(14) . . . . ?
C20 O17 C19 C23 172.2(10) . . . . ?
C21 O18 C22 O19 4.8(18) . . . . ?
C21 O18 C22 C23 -176.0(11) . . . . ?
C22 C23 C24 O20 176.4(8) . . . . ?
C22 C23 C24 C24 -4.9(14) . . . 2_656 ?
C25 C29 C30 O25 2.4(13) . . . . ?
C25 C29 C30 C36 179.1(7) . . . . ?
C26 O22 C25 O21 7.1(13) . . . . ?
C26 O22 C25 C29 -174.7(9) . . . . ?
C27 O23 C28 O24 1.5(16) . . . . ?
C27 O23 C28 C29 -179.3(10) . . . . ?
C28 C29 C30 O25 -174.0(8) . . . . ?
C28 C29 C30 C36 2.7(12) . . . . ?
C29 C30 C36 O30 -118.1(8) . . . . ?
C29 C30 C36 C35 67.8(11) . . . . ?
C31 C35 C36 O30 -0.6(14) . . . . ?
C31 C35 C36 C30 172.6(8) . . . . ?
C32 O27 C31 O26 -3.8(16) . . . . ?
C32 O27 C31 C35 174.6(11) . . . . ?
C33 O28 C34 O29 3.8(17) . . . . ?
C33 O28 C34 C35 -178.9(11) . . . . ?
C34 C35 C36 O30 -178.1(8) . . . . ?
C34 C35 C36 C30 -4.9(13) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.559(7)
2 0.441(7)
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.496 0.000 286.1 172.9 '1.5 CHBr3'
2 0.152 0.208 0.742 16.8 0.0 ?
3 0.500 0.996 1.000 286.1 172.3 '1.5 CHBr3'
4 0.348 0.708 0.258 16.8 0.0 ?
5 0.652 0.708 0.742 16.8 0.0 ?
6 0.848 0.208 0.258 16.8 0.0 ?
