#------------------------------------------------------------------------------
#$Date: 2020-05-04 05:24:41 +0300 (Mon, 04 May 2020) $
#$Revision: 251428 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/75/4517541.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_4517541
loop_
_publ_author_name
'Thomas, Kolle E.'
'Slebodnick, Carla'
'Ghosh, Abhik'
_publ_section_title
;
 Facile Supramolecular Engineering of Porphyrin cis Tautomers: The Case of
 β-Octabromo-meso-tetraarylporphyrins.
;
_journal_issue                   15
_journal_name_full               'ACS omega'
_journal_page_first              8893
_journal_page_last               8901
_journal_paper_doi               10.1021/acsomega.0c00517
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C48 H18 Br8 F12 N4, 2(C H4 O)'
_chemical_formula_sum            'C50 H26 Br8 F12 N4 O2'
_chemical_formula_weight         1582.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.8497(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.7959(4)
_cell_length_b                   10.19901(8)
_cell_length_c                   30.7172(3)
_cell_measurement_reflns_used    71729
_cell_measurement_temperature    99.99(11)
_cell_measurement_theta_max      77.5260
_cell_measurement_theta_min      3.8370
_cell_volume                     10623.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.16a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.16a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -60.00  28.00   0.50    4.00    --  -47.45  19.00 -30.00  176
  2  ω     24.00  90.00   0.50    4.00    --   47.45-114.00  33.00  132
  3  ω     58.00 134.00   0.50   16.00    --  107.75-178.00-102.00  152
  4  ω     35.00 104.00   0.50   16.00    --  107.75-114.00  33.00  138
  5  ω     83.00 106.50   0.50   16.00    --  107.75-125.00 150.00   47
  6  ω     33.00  69.00   0.50   16.00    --  107.75 -30.00   0.00   72
  7  ω     38.00  77.00   0.50   16.00    --  107.75 -45.00  60.00   78
  8  ω     35.00 124.00   0.50   16.00    --  107.75 -61.00  60.00  178
  9  ω     94.00 178.00   0.50   16.00    --  107.75  15.00 150.00  168
 10  ω     99.00 178.00   0.50   16.00    --  107.75 114.00 124.00  158
 11  ω     95.00 178.00   0.50   16.00    --  107.75  30.00  60.00  166
 12  ω     95.00 178.00   0.50   16.00    --  107.75  45.00 -60.00  166
 13  ω     97.00 133.00   0.50   16.00    --  107.75  45.00 -90.00   72
 14  ω    106.00 132.00   0.50   16.00    --  107.75  30.00-120.00   52
 15  ω     91.00 178.00   0.50   16.00    --  107.75  61.00   0.00  174
 16  ω     85.00 178.00   0.50   16.00    --  107.75  78.00 110.08  186
 17  ω     85.00 178.00   0.50   16.00    --  107.75  77.00  30.00  186
 18  ω     60.00 120.00   0.50    4.00    --   47.45 178.00 -99.00  120
 19  ω     55.00  85.00   0.50   16.00    --  107.75 -20.00-122.17   60
 20  ω     36.00  77.00   0.50   16.00    --  107.75 -45.00-120.00   82
 21  ω     35.00  88.50   0.50   16.00    --  107.75 -77.00-180.00  107
 22  ω     36.00  61.00   0.50   16.00    --  107.75 -45.00-180.00   50
 23  ω     35.00 124.00   0.50   16.00    --  107.75 -61.00-120.00  178
 24  ω     33.00  69.00   0.50   16.00    --  107.75 -30.00 -90.00   72
 25  ω     35.00 131.00   0.50   16.00    --  107.75 -77.00  30.00  192
 26  ω     33.00  69.00   0.50   16.00    --  107.75 -30.00 120.00   72
 27  ω     35.00 124.00   0.50   16.00    --  107.75 -61.00 120.00  178
 28  ω     35.00 110.00   0.50   16.00    --  107.75-125.00  60.00  150
 29  ω     35.00  98.50   0.50   16.00    --  107.75 -94.00  90.00  127
 30  ω     35.00 131.00   0.50   16.00    --  107.75 -77.00  60.00  192
 31  ω     35.00  91.50   0.50   16.00    --  107.75 -77.00 150.00  113
 32  ω     33.00  67.00   0.50   16.00    --  107.75 -30.00 150.00   68
 33  ω    -87.00  -2.00   0.50    4.00    --  -47.45 114.00 124.00  170
 34  ω    -86.00 -13.00   0.50   16.00    --  -86.25 114.00 124.00  146
 35  ω   -131.00 -36.00   0.50   16.00    --  -86.25 178.00 -99.00  190
 36  ω   -159.00 -77.00   0.50   16.00    --  -86.25-114.00  33.00  164
 37  ω   -120.00 -38.00   0.50    4.00    --  -47.45-178.00-102.00  164
 38  ω   -120.00 -70.00   0.50    4.00    --  -47.45-125.00-150.00  100
 39  ω   -120.00 -70.00   0.50    4.00    --  -47.45-125.00-180.00  100
;
_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      -0.0332237000
_diffrn_orient_matrix_UB_12      0.0537237000
_diffrn_orient_matrix_UB_13      -0.0447246000
_diffrn_orient_matrix_UB_21      0.0241533000
_diffrn_orient_matrix_UB_22      -0.0362089000
_diffrn_orient_matrix_UB_23      -0.0294943000
_diffrn_orient_matrix_UB_31      -0.0194397000
_diffrn_orient_matrix_UB_32      -0.1363861000
_diffrn_orient_matrix_UB_33      -0.0097048000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            177057
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.524
_diffrn_reflns_theta_min         3.823
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.997
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16a (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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       plate
_exptl_crystal_F_000             6064
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1505
_refine_ls_number_reflns         22336
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0595P)²+33.8368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20330
_reflns_number_total             22336
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao0c00517_si_003.cif
_cod_data_source_block           cs2495
_cod_depositor_comments
'Adding full bibliography for 4517540--4517541.cif.'
_cod_original_cell_volume        10623.00(19)
_cod_database_code               4517541
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C50 H26 Br8 F12 N4 O2'
_chemical_oxdiff_usercomment
'Abhik Ghosh / Thomas Kolle Ekaney (Tromso)  Br8P-CF3PP'
_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.
;
_reflns_odcompleteness_completeness 95.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1 = N4-H4
 0.88 with sigma of 0.02
 O1-H1S = O2-H2S
 0.84 with sigma of 0.02
 N5-H5 = N8-H8
 0.88 with sigma of 0.02
 O3-H3S = O4-H4S
 0.84 with sigma of 0.02
 H3S-N6
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C27B)
Uanis(C48A) = Uanis(C48B)
4. Rigid body (RIGU) restrains
 F1A, F2A, F1B, F2B, F3, C27A, C27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10A, F11A, F10B, F11B, F12, C48A, C48B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19A, F20A, F21A, F19B, F20B, F21B, C91
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4A, F5A, F6A, F4B, F5B, F6B, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F1B)=Sof(F2B)=Sof(C27B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(C27A)=FVAR(1)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(2)
 Sof(F10B)=Sof(F11B)=Sof(C48B)=1-FVAR(3)
 Sof(F10A)=Sof(F11A)=Sof(C48A)=FVAR(3)
 Sof(F19B)=Sof(F20B)=Sof(F21B)=1-FVAR(4)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32),
 C33(H33), C36(H36), C37(H37), C39(H39), C40(H40), C43(H43), C44(H44), C46(H46),
  C47(H47), C72(H72), C73(H73), C75(H75), C76(H76), C79(H79), C80(H80),
 C82(H82), C83(H83), C86(H86), C87(H87), C89(H89), C90(H90), C93(H93), C94(H94),
  C96(H96), C97(H97)
6.b Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C99(H99A,H99B,H99C), C100(H10A,H10B,
 H10C)
;
_olex2_date_sample_data_collection 2018-09-10
_olex2_date_sample_submission    2018-09-10
_olex2_submission_original_sample_id Br8P-CF3PP
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.589
_oxdiff_exptl_absorpt_empirical_full_min 0.522
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.44314(2) 1.07576(4) 0.26525(2) 0.02700(10) Uani 1 1 d . . . . .
Br2 Br 0.46297(2) 1.06712(4) 0.16309(2) 0.02778(10) Uani 1 1 d . . . . .
Br3 Br 0.60723(2) 0.68352(5) 0.16319(2) 0.03171(11) Uani 1 1 d . . . . .
Br4 Br 0.70333(2) 0.76536(5) 0.23706(2) 0.03183(11) Uani 1 1 d . . . . .
Br5 Br 0.72184(2) 1.34982(5) 0.33862(2) 0.03706(12) Uani 1 1 d . . . . .
Br6 Br 0.69894(2) 1.37175(5) 0.43867(2) 0.03424(11) Uani 1 1 d . . . . .
Br7 Br 0.64190(2) 0.83686(5) 0.51451(2) 0.03233(11) Uani 1 1 d . . . . .
Br8 Br 0.54750(2) 0.72596(5) 0.44815(2) 0.03111(11) Uani 1 1 d . . . . .
F1A F 0.41817(19) 0.8342(14) -0.0003(2) 0.103(4) Uani 0.708(15) 1 d . U P A 1
F2A F 0.4464(4) 0.6566(8) 0.0027(2) 0.091(4) Uani 0.708(15) 1 d . U P A 1
F1B F 0.4266(5) 0.730(3) 0.0014(5) 0.065(6) Uani 0.292(15) 1 d . U P A 2
F2B F 0.4789(8) 0.6417(16) 0.0027(5) 0.078(6) Uani 0.292(15) 1 d . U P A 2
F3 F 0.46645(12) 0.8271(4) -0.02180(11) 0.0592(10) Uani 1 1 d . U . . .
F4A F 0.8246(3) 1.1289(10) 0.2251(3) 0.040(2) Uani 0.62(4) 1 d . U P B 1
F5A F 0.8525(5) 1.203(2) 0.2944(5) 0.061(4) Uani 0.62(4) 1 d . U P B 1
F6A F 0.8530(5) 0.9972(18) 0.2812(10) 0.079(6) Uani 0.62(4) 1 d . U P B 1
F4B F 0.8310(7) 1.074(5) 0.2333(10) 0.094(10) Uani 0.38(4) 1 d . U P B 2
F5B F 0.8468(8) 1.2318(19) 0.2874(10) 0.065(5) Uani 0.38(4) 1 d . U P B 2
F6B F 0.8615(4) 1.041(2) 0.3058(9) 0.054(5) Uani 0.38(4) 1 d . U P B 2
F7 F 0.79409(12) 1.2991(4) 0.61502(14) 0.0687(13) Uani 1 1 d . . . . .
F8 F 0.75950(11) 1.2268(5) 0.65191(12) 0.0651(12) Uani 1 1 d . . . . .
F9 F 0.79935(8) 1.1002(3) 0.63733(10) 0.0381(6) Uani 1 1 d . . . . .
F10A F 0.37429(19) 0.8188(14) 0.4020(2) 0.070(3) Uani 0.75(2) 1 d . U P C 1
F11A F 0.3764(3) 0.6392(7) 0.3670(7) 0.102(4) Uani 0.75(2) 1 d . U P C 1
F10B F 0.3664(9) 0.895(4) 0.3891(14) 0.085(8) Uani 0.25(2) 1 d . U P C 2
F11B F 0.3813(6) 0.692(4) 0.3942(9) 0.072(9) Uani 0.25(2) 1 d . U P C 2
F12 F 0.34755(10) 0.7971(6) 0.32806(15) 0.0750(13) Uani 1 1 d . U . . .
N1 N 0.54680(10) 0.9078(3) 0.28026(12) 0.0208(7) Uani 1 1 d D . . . .
H1 H 0.5685(12) 0.863(6) 0.294(2) 0.047(18) Uiso 1 1 d D . . . .
N2 N 0.61694(10) 0.9793(4) 0.25789(12) 0.0232(7) Uani 1 1 d . . . . .
N3 N 0.66170(10) 1.0354(4) 0.36101(12) 0.0226(7) Uani 1 1 d . . . . .
N4 N 0.58990(10) 0.9989(3) 0.38388(12) 0.0214(7) Uani 1 1 d D . . . .
H4 H 0.5895(16) 1.046(5) 0.3600(13) 0.027(13) Uiso 1 1 d D . . . .
C1 C 0.51921(11) 0.9386(4) 0.29816(15) 0.0216(8) Uani 1 1 d . . . . .
C2 C 0.48645(12) 0.9927(4) 0.26011(16) 0.0244(8) Uani 1 1 d . . . . .
C3 C 0.49438(11) 0.9887(4) 0.22041(14) 0.0214(8) Uani 1 1 d . . . . .
C4 C 0.53297(12) 0.9331(4) 0.23270(15) 0.0212(8) Uani 1 1 d . . . . .
C5 C 0.55288(12) 0.9018(4) 0.20314(15) 0.0230(8) Uani 1 1 d . . . . .
C6 C 0.59477(12) 0.9006(4) 0.22109(14) 0.0224(8) Uani 1 1 d . . . . .
C7 C 0.62067(13) 0.8233(4) 0.20597(15) 0.0250(8) Uani 1 1 d . . . . .
C8 C 0.65806(12) 0.8574(4) 0.23392(16) 0.0252(8) Uani 1 1 d . . . . .
C9 C 0.65580(12) 0.9584(4) 0.26565(15) 0.0237(8) Uani 1 1 d . . . . .
C10 C 0.68613(12) 1.0356(4) 0.29797(15) 0.0238(8) Uani 1 1 d . . . . .
C11 C 0.68199(11) 1.0944(4) 0.33742(15) 0.0229(8) Uani 1 1 d . . . . .
C12 C 0.69969(13) 1.2142(4) 0.36160(16) 0.0272(9) Uani 1 1 d . . . . .
C13 C 0.69087(12) 1.2233(4) 0.39999(16) 0.0249(8) Uani 1 1 d . . . . .
C14 C 0.66753(12) 1.1083(4) 0.40028(15) 0.0240(8) Uani 1 1 d . . . . .
C15 C 0.65630(13) 1.0657(4) 0.43682(15) 0.0249(8) Uani 1 1 d . . . . .
C16 C 0.62129(12) 0.9936(4) 0.42710(15) 0.0233(8) Uani 1 1 d . . . . .
C17 C 0.60966(12) 0.9055(4) 0.45533(15) 0.0262(9) Uani 1 1 d . . . . .
C18 C 0.57244(12) 0.8610(4) 0.42950(15) 0.0249(8) Uani 1 1 d . . . . .
C19 C 0.55936(12) 0.9222(4) 0.38384(15) 0.0216(8) Uani 1 1 d . . . . .
C20 C 0.52291(12) 0.9140(4) 0.34510(14) 0.0203(8) Uani 1 1 d . . . . .
C21 C 0.52917(12) 0.8674(4) 0.15337(15) 0.0241(8) Uani 1 1 d . . . . .
C22 C 0.49581(13) 0.7867(4) 0.14242(16) 0.0260(8) Uani 1 1 d . . . . .
H22 H 0.489368 0.751712 0.167184 0.031 Uiso 1 1 calc R . . . .
C23 C 0.47243(14) 0.7580(5) 0.09628(16) 0.0297(9) Uani 1 1 d . . . . .
H23 H 0.449976 0.703253 0.089193 0.036 Uiso 1 1 calc R . . . .
C24 C 0.48176(15) 0.8093(5) 0.06010(17) 0.0348(10) Uani 1 1 d . . . . .
C25 C 0.51501(15) 0.8894(5) 0.07030(17) 0.0355(11) Uani 1 1 d . . . . .
H25 H 0.521406 0.923822 0.045418 0.043 Uiso 1 1 calc R . . . .
C26 C 0.53845(14) 0.9179(5) 0.11681(17) 0.0312(10) Uani 1 1 d . . . . .
H26 H 0.560993 0.972265 0.123860 0.037 Uiso 1 1 calc R . . . .
C27A C 0.4536(3) 0.7864(11) 0.0105(3) 0.0394(17) Uani 0.708(15) 1 d . U P A 1
C27B C 0.4633(8) 0.748(3) 0.0082(9) 0.0394(17) Uani 0.292(15) 1 d . U P A 2
C28 C 0.72325(13) 1.0564(5) 0.29129(16) 0.0280(9) Uani 1 1 d . . . . .
C29 C 0.72295(13) 1.0784(5) 0.24640(16) 0.0295(9) Uani 1 1 d . . . . .
H29 H 0.698531 1.082395 0.219948 0.035 Uiso 1 1 calc R . . . .
C30 C 0.75798(14) 1.0946(5) 0.23993(18) 0.0336(10) Uani 1 1 d . . . . .
H30 H 0.757605 1.108710 0.209187 0.040 Uiso 1 1 calc R . . . .
C31 C 0.79327(14) 1.0902(5) 0.27846(19) 0.0331(10) Uani 1 1 d . . . . .
C32 C 0.79450(13) 1.0718(5) 0.32400(18) 0.0312(10) Uani 1 1 d . . . . .
H32 H 0.818973 1.071672 0.350437 0.037 Uiso 1 1 calc R . . . .
C33 C 0.75913(13) 1.0537(4) 0.33010(16) 0.0276(9) Uani 1 1 d . . . . .
H33 H 0.759537 1.039566 0.360858 0.033 Uiso 1 1 calc R . . . .
C34 C 0.83105(15) 1.1069(6) 0.2715(2) 0.0390(11) Uani 1 1 d . U . . .
C35 C 0.68454(12) 1.0936(4) 0.48547(15) 0.0236(8) Uani 1 1 d . . . . .
C36 C 0.72482(13) 1.0760(4) 0.49501(16) 0.0267(9) Uani 1 1 d . . . . .
H36 H 0.732633 1.040996 0.471309 0.032 Uiso 1 1 calc R . . . .
C37 C 0.75304(13) 1.1091(4) 0.53851(17) 0.0282(9) Uani 1 1 d . . . . .
H37 H 0.780247 1.098108 0.544727 0.034 Uiso 1 1 calc R . . . .
C38 C 0.74142(13) 1.1585(4) 0.57306(16) 0.0275(9) Uani 1 1 d . . . . .
C39 C 0.70168(14) 1.1735(4) 0.56477(16) 0.0282(9) Uani 1 1 d . . . . .
H39 H 0.693998 1.205193 0.589020 0.034 Uiso 1 1 calc R . . . .
C40 C 0.67332(13) 1.1416(5) 0.52059(16) 0.0284(9) Uani 1 1 d . . . . .
H40 H 0.646141 1.152823 0.514475 0.034 Uiso 1 1 calc R . . . .
C41 C 0.77333(15) 1.1965(5) 0.61922(18) 0.0361(11) Uani 1 1 d . . . . .
C42 C 0.48629(12) 0.8772(4) 0.35188(16) 0.0239(8) Uani 1 1 d . . . . .
C43 C 0.47728(13) 0.9338(4) 0.38771(16) 0.0265(9) Uani 1 1 d . . . . .
H43 H 0.495149 0.993720 0.409143 0.032 Uiso 1 1 calc R . . . .
C44 C 0.44186(13) 0.9024(5) 0.39206(17) 0.0307(10) Uani 1 1 d . . . . .
H44 H 0.435425 0.941233 0.416256 0.037 Uiso 1 1 calc R . . . .
C45 C 0.41632(13) 0.8143(5) 0.36092(18) 0.0344(11) Uani 1 1 d . . . . .
C46 C 0.42492(13) 0.7569(5) 0.32509(17) 0.0318(10) Uani 1 1 d . . . . .
H46 H 0.407092 0.696348 0.303934 0.038 Uiso 1 1 calc R . . . .
C47 C 0.46011(12) 0.7893(4) 0.32058(15) 0.0256(9) Uani 1 1 d . . . . .
H47 H 0.466252 0.751189 0.296045 0.031 Uiso 1 1 calc R . . . .
C48A C 0.3788(5) 0.7673(12) 0.3649(6) 0.042(2) Uani 0.75(2) 1 d . U P C 1
C48B C 0.3777(17) 0.804(4) 0.3684(19) 0.042(2) Uani 0.25(2) 1 d . U P C 2
Br9 Br 0.71379(2) 0.75566(5) 0.96070(2) 0.02974(10) Uani 1 1 d . . . . .
Br10 Br 0.74153(2) 0.77117(5) 0.86499(2) 0.03044(11) Uani 1 1 d . . . . .
Br11 Br 0.92791(2) 0.81243(5) 0.90095(2) 0.03729(12) Uani 1 1 d . . . . .
Br12 Br 0.98125(2) 0.51934(5) 0.93414(2) 0.03115(11) Uani 1 1 d . . . . .
Br13 Br 0.90019(2) 0.00772(4) 0.98969(2) 0.02994(10) Uani 1 1 d . . . . .
Br14 Br 0.88134(2) 0.03076(5) 1.09310(2) 0.03273(11) Uani 1 1 d . . . . .
Br15 Br 0.91492(2) 0.55690(6) 1.22060(2) 0.03719(12) Uani 1 1 d . . . . .
Br16 Br 0.84993(2) 0.81252(5) 1.17230(2) 0.03265(11) Uani 1 1 d . . . . .
F13 F 0.77272(15) 1.1104(4) 0.73962(14) 0.0719(12) Uani 1 1 d . . . . .
F14 F 0.77347(14) 0.9274(4) 0.70598(12) 0.0665(11) Uani 1 1 d . . . . .
F15 F 0.82498(15) 1.0468(5) 0.73223(16) 0.0803(14) Uani 1 1 d . . . . .
F16 F 0.99941(12) 0.1188(4) 0.83976(14) 0.0537(9) Uani 1 1 d . . . . .
F17 F 0.96087(9) -0.0415(3) 0.83354(11) 0.0401(7) Uani 1 1 d . . . . .
F18 F 1.01728(10) -0.0388(4) 0.89099(12) 0.0507(8) Uani 1 1 d . . . . .
F19A F 0.9601(5) -0.0878(10) 1.2750(5) 0.086(5) Uani 0.63(4) 1 d . U P D 1
F20A F 0.9537(6) 0.064(2) 1.3180(4) 0.089(5) Uani 0.63(4) 1 d . U P D 1
F21A F 1.0058(3) 0.0500(13) 1.3076(4) 0.067(3) Uani 0.63(4) 1 d . U P D 1
F19B F 0.9801(14) -0.076(3) 1.2705(8) 0.110(10) Uani 0.37(4) 1 d . U P D 2
F20B F 0.9429(6) -0.011(4) 1.3009(14) 0.107(12) Uani 0.37(4) 1 d . U P D 2
F21B F 0.9956(14) 0.081(4) 1.3160(12) 0.143(13) Uani 0.37(4) 1 d . U P D 2
F22 F 0.66258(10) 0.8812(3) 1.11415(14) 0.0502(8) Uani 1 1 d . . . . .
F23 F 0.69644(9) 1.0592(3) 1.13242(11) 0.0452(8) Uani 1 1 d . . . . .
F24 F 0.65728(9) 1.0248(3) 1.06121(11) 0.0453(8) Uani 1 1 d . . . . .
N5 N 0.83091(10) 0.7152(4) 0.99207(13) 0.0230(7) Uani 1 1 d D . . . .
H5 H 0.8558(7) 0.712(6) 1.0110(17) 0.034(15) Uiso 1 1 d D . . . .
N6 N 0.87747(11) 0.5331(4) 0.95529(13) 0.0248(7) Uani 1 1 d D . . . .
N7 N 0.90621(11) 0.3788(4) 1.04452(13) 0.0244(7) Uani 1 1 d . . . . .
N8 N 0.85225(10) 0.5361(4) 1.07838(13) 0.0231(7) Uani 1 1 d D . . . .
H8 H 0.8439(19) 0.493(6) 1.0519(14) 0.048(18) Uiso 1 1 d D . . . .
C51 C 0.80080(12) 0.7281(4) 1.00725(15) 0.0223(8) Uani 1 1 d . . . . .
C52 C 0.76602(12) 0.7553(4) 0.96556(15) 0.0234(8) Uani 1 1 d . . . . .
C53 C 0.77679(13) 0.7620(4) 0.92823(15) 0.0248(8) Uani 1 1 d . . . . .
C54 C 0.81827(13) 0.7381(4) 0.94452(15) 0.0241(8) Uani 1 1 d . . . . .
C55 C 0.84297(13) 0.7338(4) 0.91896(15) 0.0248(8) Uani 1 1 d . . . . .
C56 C 0.87610(13) 0.6504(4) 0.93270(15) 0.0245(8) Uani 1 1 d . . . . .
C57 C 0.91082(13) 0.6622(4) 0.92204(16) 0.0275(9) Uani 1 1 d . . . . .
C58 C 0.93168(13) 0.5493(4) 0.93596(16) 0.0255(8) Uani 1 1 d . . . . .
C59 C 0.91019(13) 0.4685(4) 0.95659(15) 0.0238(8) Uani 1 1 d . . . . .
C60 C 0.91934(12) 0.3374(4) 0.97406(15) 0.0247(8) Uani 1 1 d . . . . .
C61 C 0.91042(12) 0.2940(4) 1.01173(15) 0.0231(8) Uani 1 1 d . . . . .
C62 C 0.90528(12) 0.1609(4) 1.02525(16) 0.0248(8) Uani 1 1 d . . . . .
C63 C 0.89835(12) 0.1679(4) 1.06523(16) 0.0253(8) Uani 1 1 d . . . . .
C64 C 0.90006(12) 0.3064(4) 1.07757(15) 0.0223(8) Uani 1 1 d . . . . .
C65 C 0.89753(12) 0.3594(4) 1.11947(15) 0.0238(8) Uani 1 1 d . . . . .
C66 C 0.87887(12) 0.4793(4) 1.11956(15) 0.0236(8) Uani 1 1 d . . . . .
C67 C 0.88008(12) 0.5645(4) 1.15720(15) 0.0259(9) Uani 1 1 d . . . . .
C68 C 0.85422(13) 0.6642(4) 1.13898(16) 0.0260(9) Uani 1 1 d . . . . .
C69 C 0.83575(12) 0.6458(4) 1.08867(15) 0.0232(8) Uani 1 1 d . . . . .
C70 C 0.80519(12) 0.7199(4) 1.05487(15) 0.0235(8) Uani 1 1 d . . . . .
C71 C 0.83215(14) 0.8087(5) 0.87460(17) 0.0294(9) Uani 1 1 d . . . . .
C72 C 0.81961(14) 0.9393(4) 0.87098(17) 0.0298(9) Uani 1 1 d . . . . .
H72 H 0.819300 0.983423 0.898060 0.036 Uiso 1 1 calc R . . . .
C73 C 0.80767(15) 1.0043(5) 0.82822(18) 0.0335(10) Uani 1 1 d . . . . .
H73 H 0.799659 1.093411 0.825979 0.040 Uiso 1 1 calc R . . . .
C74 C 0.80745(16) 0.9383(5) 0.78847(19) 0.0365(11) Uani 1 1 d . . . . .
C75 C 0.82039(17) 0.8092(5) 0.79168(18) 0.0375(11) Uani 1 1 d . . . . .
H75 H 0.820662 0.764882 0.764611 0.045 Uiso 1 1 calc R . . . .
C76 C 0.83276(15) 0.7469(5) 0.83462(17) 0.0322(10) Uani 1 1 d . . . . .
H76 H 0.841977 0.659099 0.837043 0.039 Uiso 1 1 calc R . . . .
C77 C 0.7941(2) 1.0051(6) 0.7416(2) 0.0473(14) Uani 1 1 d . . . . .
C78 C 0.93665(13) 0.2521(4) 0.94816(16) 0.0247(8) Uani 1 1 d . . . . .
C79 C 0.91809(14) 0.2461(5) 0.89877(17) 0.0323(10) Uani 1 1 d . . . . .
H79 H 0.894165 0.292581 0.883041 0.039 Uiso 1 1 calc R . . . .
C80 C 0.93407(14) 0.1739(5) 0.87289(17) 0.0306(9) Uani 1 1 d . . . . .
H80 H 0.920826 0.168574 0.839537 0.037 Uiso 1 1 calc R . . . .
C81 C 0.96952(13) 0.1087(4) 0.89541(17) 0.0284(9) Uani 1 1 d . . . . .
C82 C 0.98844(13) 0.1125(4) 0.94440(16) 0.0273(9) Uani 1 1 d . . . . .
H82 H 1.012601 0.067062 0.959806 0.033 Uiso 1 1 calc R . . . .
C83 C 0.97170(13) 0.1836(4) 0.97073(15) 0.0262(9) Uani 1 1 d . . . . .
H83 H 0.984273 0.185275 1.004207 0.031 Uiso 1 1 calc R . . . .
C84 C 0.98725(15) 0.0371(5) 0.86537(19) 0.0343(10) Uani 1 1 d . . . . .
C85 C 0.91545(12) 0.2810(4) 1.16327(15) 0.0249(8) Uani 1 1 d . . . . .
C86 C 0.95352(14) 0.2317(5) 1.17535(17) 0.0297(9) Uani 1 1 d . . . . .
H86 H 0.967618 0.251444 1.156004 0.036 Uiso 1 1 calc R . . . .
C87 C 0.97113(14) 0.1540(5) 1.21537(17) 0.0337(10) Uani 1 1 d . . . . .
H87 H 0.997255 0.122304 1.223723 0.040 Uiso 1 1 calc R . . . .
C88 C 0.95006(15) 0.1236(5) 1.24274(17) 0.0347(10) Uani 1 1 d . . . . .
C89 C 0.91233(15) 0.1724(6) 1.23133(18) 0.0369(11) Uani 1 1 d . . . . .
H89 H 0.898247 0.151592 1.250612 0.044 Uiso 1 1 calc R . . . .
C90 C 0.89514(14) 0.2509(5) 1.19216(17) 0.0326(10) Uani 1 1 d . . . . .
H90 H 0.869371 0.284700 1.184732 0.039 Uiso 1 1 calc R . . . .
C91 C 0.96757(17) 0.0346(7) 1.2848(2) 0.0464(12) Uani 1 1 d . U . . .
C92 C 0.77603(13) 0.7863(4) 1.06947(15) 0.0247(8) Uani 1 1 d . . . . .
C93 C 0.75824(13) 0.7185(4) 1.09568(16) 0.0268(9) Uani 1 1 d . . . . .
H93 H 0.766690 0.632081 1.106432 0.032 Uiso 1 1 calc R . . . .
C94 C 0.72855(13) 0.7760(5) 1.10606(16) 0.0278(9) Uani 1 1 d . . . . .
H94 H 0.716833 0.729892 1.124167 0.033 Uiso 1 1 calc R . . . .
C95 C 0.71599(13) 0.9015(5) 1.08981(16) 0.0276(9) Uani 1 1 d . . . . .
C96 C 0.73399(14) 0.9731(5) 1.06509(16) 0.0289(9) Uani 1 1 d . . . . .
H96 H 0.725717 1.060152 1.055039 0.035 Uiso 1 1 calc R . . . .
C97 C 0.76424(14) 0.9156(4) 1.05531(17) 0.0286(9) Uani 1 1 d . . . . .
H97 H 0.777013 0.964127 1.038933 0.034 Uiso 1 1 calc R . . . .
C98 C 0.68305(14) 0.9648(5) 1.09938(17) 0.0304(9) Uani 1 1 d . . . . .
O1 O 0.61855(10) 0.7908(3) 0.33807(14) 0.0393(8) Uani 1 1 d D . . . .
H1S H 0.6313(17) 0.858(4) 0.350(2) 0.046(18) Uiso 1 1 d D . . . .
C49 C 0.63722(18) 0.6777(7) 0.3361(3) 0.0584(17) Uani 1 1 d . . . . .
H49A H 0.644575 0.679790 0.308668 0.088 Uiso 1 1 calc GR . . . .
H49B H 0.619558 0.603283 0.333175 0.088 Uiso 1 1 calc GR . . . .
H49C H 0.661004 0.668140 0.364997 0.088 Uiso 1 1 calc GR . . . .
O2 O 0.58176(10) 1.1574(3) 0.30445(12) 0.0315(7) Uani 1 1 d D . . . .
H2S H 0.594(2) 1.125(8) 0.289(3) 0.07(2) Uiso 1 1 d D . . . .
C50 C 0.59690(15) 1.2840(5) 0.3115(2) 0.0374(11) Uani 1 1 d . . . . .
H50A H 0.600535 1.313686 0.283115 0.056 Uiso 1 1 calc GR . . . .
H50B H 0.622343 1.284835 0.338459 0.056 Uiso 1 1 calc GR . . . .
H50C H 0.578484 1.342782 0.317896 0.056 Uiso 1 1 calc GR . . . .
O3 O 0.81743(10) 0.4322(3) 0.98225(13) 0.0339(7) Uani 1 1 d D . . . .
H3S H 0.8312(18) 0.457(10) 0.967(2) 0.11(4) Uiso 1 1 d D . . . .
C99 C 0.80781(16) 0.3006(5) 0.9663(2) 0.0388(11) Uani 1 1 d . . . . .
H99A H 0.813556 0.286391 0.938072 0.058 Uiso 1 1 calc GR . . . .
H99B H 0.779714 0.285019 0.958641 0.058 Uiso 1 1 calc GR . . . .
H99C H 0.823545 0.239947 0.991246 0.058 Uiso 1 1 calc GR . . . .
C100 C 0.93659(16) 0.7080(5) 1.0867(2) 0.0398(11) Uani 1 1 d . . . . .
H10A H 0.937018 0.804029 1.085853 0.060 Uiso 1 1 calc GR . . . .
H10B H 0.963080 0.674046 1.093086 0.060 Uiso 1 1 calc GR . . . .
H10C H 0.928113 0.679329 1.111767 0.060 Uiso 1 1 calc GR . . . .
O4 O 0.91068(10) 0.6611(3) 1.04387(13) 0.0338(7) Uani 1 1 d D . . . .
H4S H 0.911(3) 0.579(2) 1.045(3) 0.07(3) Uiso 1 1 d 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'
F F 0.0727 0.0534 '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
2 0 -5 0.0056
-2 0 5 0.0056
13 1 0 0.0514
-1 0 0 0.0536
-5 4 1 0.0672
5 -4 -1 0.0502
-5 -1 0 0.0333
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
C1 N1 C4 111.0(3) . . ?
C6 N2 C9 107.4(4) . . ?
C14 N3 C11 107.4(3) . . ?
C19 N4 C16 111.0(3) . . ?
N1 C1 C2 106.5(4) . . ?
N1 C1 C20 125.2(4) . . ?
C20 C1 C2 128.3(4) . . ?
C1 C2 Br1 125.8(3) . . ?
C3 C2 Br1 125.3(3) . . ?
C3 C2 C1 108.4(4) . . ?
C2 C3 Br2 124.2(3) . . ?
C2 C3 C4 108.1(4) . . ?
C4 C3 Br2 127.1(3) . . ?
N1 C4 C3 105.9(4) . . ?
N1 C4 C5 125.0(4) . . ?
C5 C4 C3 129.0(4) . . ?
C4 C5 C6 120.6(4) . . ?
C4 C5 C21 118.4(4) . . ?
C6 C5 C21 121.0(4) . . ?
N2 C6 C5 121.6(4) . . ?
N2 C6 C7 109.2(4) . . ?
C5 C6 C7 129.1(4) . . ?
C6 C7 Br3 127.9(3) . . ?
C8 C7 Br3 124.6(3) . . ?
C8 C7 C6 106.9(4) . . ?
C7 C8 Br4 124.5(3) . . ?
C7 C8 C9 107.5(4) . . ?
C9 C8 Br4 127.1(3) . . ?
N2 C9 C8 108.9(4) . . ?
N2 C9 C10 121.5(4) . . ?
C10 C9 C8 129.5(4) . . ?
C9 C10 C11 121.4(4) . . ?
C9 C10 C28 120.3(4) . . ?
C11 C10 C28 118.3(4) . . ?
N3 C11 C10 122.1(4) . . ?
N3 C11 C12 109.2(4) . . ?
C10 C11 C12 128.4(4) . . ?
C11 C12 Br5 127.2(3) . . ?
C13 C12 Br5 124.6(3) . . ?
C13 C12 C11 107.2(4) . . ?
C12 C13 Br6 125.4(3) . . ?
C12 C13 C14 107.1(4) . . ?
C14 C13 Br6 126.5(3) . . ?
N3 C14 C13 109.0(4) . . ?
N3 C14 C15 123.0(4) . . ?
C15 C14 C13 127.6(4) . . ?
C14 C15 C16 121.3(4) . . ?
C14 C15 C35 116.0(4) . . ?
C16 C15 C35 122.6(4) . . ?
N4 C16 C15 122.5(4) . . ?
N4 C16 C17 105.8(3) . . ?
C15 C16 C17 131.7(4) . . ?
C16 C17 Br7 126.7(3) . . ?
C18 C17 Br7 123.5(3) . . ?
C18 C17 C16 109.0(4) . . ?
C17 C18 Br8 124.7(3) . . ?
C17 C18 C19 107.6(4) . . ?
C19 C18 Br8 127.1(3) . . ?
N4 C19 C18 106.5(3) . . ?
N4 C19 C20 123.1(4) . . ?
C20 C19 C18 130.4(4) . . ?
C1 C20 C42 116.9(4) . . ?
C19 C20 C1 122.2(4) . . ?
C19 C20 C42 120.9(4) . . ?
C22 C21 C5 119.7(4) . . ?
C26 C21 C5 121.0(4) . . ?
C26 C21 C22 119.2(4) . . ?
C23 C22 C21 120.7(4) . . ?
C22 C23 C24 119.7(4) . . ?
C23 C24 C25 120.5(4) . . ?
C23 C24 C27A 118.0(6) . . ?
C23 C24 C27B 120.7(11) . . ?
C25 C24 C27A 121.3(6) . . ?
C25 C24 C27B 116.5(11) . . ?
C26 C25 C24 119.6(5) . . ?
C25 C26 C21 120.3(4) . . ?
F1A C27A F2A 102.2(10) . . ?
F1A C27A F3 107.8(9) . . ?
F1A C27A C24 115.4(8) . . ?
F2A C27A C24 110.1(8) . . ?
F3 C27A F2A 106.2(8) . . ?
F3 C27A C24 114.1(7) . . ?
F1B C27B C24 103.2(19) . . ?
F2B C27B F1B 111(3) . . ?
F2B C27B C24 116(2) . . ?
F3 C27B F1B 111(2) . . ?
F3 C27B F2B 106(2) . . ?
F3 C27B C24 110.8(19) . . ?
C29 C28 C10 120.6(4) . . ?
C29 C28 C33 119.4(4) . . ?
C33 C28 C10 120.0(4) . . ?
C30 C29 C28 120.7(4) . . ?
C31 C30 C29 119.4(5) . . ?
C30 C31 C32 121.3(4) . . ?
C30 C31 C34 119.5(5) . . ?
C32 C31 C34 119.2(4) . . ?
C31 C32 C33 118.9(4) . . ?
C28 C33 C32 120.3(4) . . ?
F4A C34 C31 111.9(6) . . ?
F5A C34 F4A 105.5(9) . . ?
F5A C34 F6A 109.0(10) . . ?
F5A C34 C31 114.5(8) . . ?
F6A C34 F4A 102.4(9) . . ?
F6A C34 C31 112.7(6) . . ?
F4B C34 F5B 115(2) . . ?
F4B C34 F6B 107.4(15) . . ?
F4B C34 C31 116.9(11) . . ?
F5B C34 C31 109.5(12) . . ?
F6B C34 F5B 94.3(12) . . ?
F6B C34 C31 111.1(8) . . ?
C36 C35 C15 117.1(4) . . ?
C40 C35 C15 123.4(4) . . ?
C40 C35 C36 119.4(4) . . ?
C37 C36 C35 120.5(4) . . ?
C36 C37 C38 119.4(4) . . ?
C37 C38 C39 121.0(4) . . ?
C37 C38 C41 117.2(4) . . ?
C39 C38 C41 121.7(4) . . ?
C40 C39 C38 119.3(4) . . ?
C35 C40 C39 120.3(4) . . ?
F7 C41 F9 105.9(4) . . ?
F7 C41 C38 112.3(4) . . ?
F8 C41 F7 107.0(5) . . ?
F8 C41 F9 106.3(4) . . ?
F8 C41 C38 112.7(4) . . ?
F9 C41 C38 112.1(4) . . ?
C43 C42 C20 120.8(4) . . ?
C47 C42 C20 119.1(4) . . ?
C47 C42 C43 120.0(4) . . ?
C42 C43 C44 119.8(4) . . ?
C45 C44 C43 119.5(5) . . ?
C44 C45 C46 121.4(4) . . ?
C44 C45 C48A 123.2(7) . . ?
C44 C45 C48B 111.2(19) . . ?
C46 C45 C48A 115.3(7) . . ?
C46 C45 C48B 127.1(19) . . ?
C45 C46 C47 119.0(4) . . ?
C42 C47 C46 120.3(4) . . ?
F10A C48A C45 111.6(11) . . ?
F11A C48A F10A 108.6(12) . . ?
F11A C48A C45 113.7(10) . . ?
F12 C48A F10A 107.0(10) . . ?
F12 C48A F11A 102.8(12) . . ?
F12 C48A C45 112.5(10) . . ?
F10B C48B F11B 107(4) . . ?
F10B C48B F12 101(4) . . ?
F10B C48B C45 122(4) . . ?
F11B C48B C45 105(3) . . ?
F12 C48B F11B 111(4) . . ?
F12 C48B C45 111(3) . . ?
C51 N5 C54 111.3(4) . . ?
C59 N6 C56 107.2(4) . . ?
C64 N7 C61 107.8(4) . . ?
C69 N8 C66 110.5(4) . . ?
N5 C51 C52 105.9(4) . . ?
N5 C51 C70 124.6(4) . . ?
C70 C51 C52 129.5(4) . . ?
C51 C52 Br9 127.0(3) . . ?
C53 C52 Br9 124.3(3) . . ?
C53 C52 C51 108.1(4) . . ?
C52 C53 Br10 124.7(3) . . ?
C52 C53 C54 108.6(4) . . ?
C54 C53 Br10 125.9(3) . . ?
N5 C54 C53 106.0(4) . . ?
N5 C54 C55 124.2(4) . . ?
C55 C54 C53 129.8(4) . . ?
C54 C55 C71 119.7(4) . . ?
C56 C55 C54 121.3(4) . . ?
C56 C55 C71 118.7(4) . . ?
N6 C56 C55 122.3(4) . . ?
N6 C56 C57 109.0(4) . . ?
C55 C56 C57 128.4(4) . . ?
C56 C57 Br11 126.5(3) . . ?
C58 C57 Br11 125.5(3) . . ?
C58 C57 C56 107.5(4) . . ?
C57 C58 Br12 124.6(3) . . ?
C57 C58 C59 106.4(4) . . ?
C59 C58 Br12 128.6(3) . . ?
N6 C59 C58 109.8(4) . . ?
N6 C59 C60 122.7(4) . . ?
C60 C59 C58 127.4(4) . . ?
C59 C60 C78 115.8(4) . . ?
C61 C60 C59 120.8(4) . . ?
C61 C60 C78 123.4(4) . . ?
N7 C61 C60 122.5(4) . . ?
N7 C61 C62 108.2(4) . . ?
C60 C61 C62 129.3(4) . . ?
C61 C62 Br13 127.4(3) . . ?
C63 C62 Br13 124.3(3) . . ?
C63 C62 C61 107.6(4) . . ?
C62 C63 Br14 126.3(3) . . ?
C62 C63 C64 106.5(4) . . ?
C64 C63 Br14 126.4(3) . . ?
N7 C64 C63 109.8(4) . . ?
N7 C64 C65 124.1(4) . . ?
C65 C64 C63 126.0(4) . . ?
C64 C65 C85 116.8(4) . . ?
C66 C65 C64 122.2(4) . . ?
C66 C65 C85 120.9(4) . . ?
N8 C66 C65 122.3(4) . . ?
N8 C66 C67 105.7(4) . . ?
C65 C66 C67 131.9(4) . . ?
C66 C67 Br15 127.5(3) . . ?
C68 C67 Br15 123.2(3) . . ?
C68 C67 C66 108.9(4) . . ?
C67 C68 Br16 125.2(3) . . ?
C67 C68 C69 108.0(4) . . ?
C69 C68 Br16 126.1(3) . . ?
N8 C69 C68 106.8(4) . . ?
N8 C69 C70 124.4(4) . . ?
C70 C69 C68 128.8(4) . . ?
C51 C70 C69 122.0(4) . . ?
C51 C70 C92 118.9(4) . . ?
C69 C70 C92 119.0(4) . . ?
C72 C71 C55 121.9(4) . . ?
C76 C71 C55 119.4(4) . . ?
C76 C71 C72 118.7(4) . . ?
C73 C72 C71 120.4(5) . . ?
C72 C73 C74 119.6(4) . . ?
C73 C74 C77 121.0(5) . . ?
C75 C74 C73 120.7(5) . . ?
C75 C74 C77 118.4(5) . . ?
C76 C75 C74 118.9(5) . . ?
C75 C76 C71 121.7(5) . . ?
F13 C77 F14 108.0(5) . . ?
F13 C77 F15 105.8(5) . . ?
F13 C77 C74 112.4(5) . . ?
F14 C77 F15 106.0(5) . . ?
F14 C77 C74 113.0(5) . . ?
F15 C77 C74 111.2(5) . . ?
C79 C78 C60 118.5(4) . . ?
C83 C78 C60 122.4(4) . . ?
C83 C78 C79 119.0(4) . . ?
C80 C79 C78 120.8(4) . . ?
C79 C80 C81 120.0(4) . . ?
C80 C81 C82 120.3(4) . . ?
C80 C81 C84 118.3(4) . . ?
C82 C81 C84 121.4(4) . . ?
C81 C82 C83 119.5(4) . . ?
C78 C83 C82 120.3(4) . . ?
F16 C84 F17 104.8(4) . . ?
F16 C84 C81 112.4(4) . . ?
F17 C84 C81 111.8(4) . . ?
F18 C84 F16 108.7(4) . . ?
F18 C84 F17 106.4(4) . . ?
F18 C84 C81 112.2(4) . . ?
C86 C85 C65 118.9(4) . . ?
C86 C85 C90 118.7(4) . . ?
C90 C85 C65 122.4(4) . . ?
C87 C86 C85 121.0(4) . . ?
C88 C87 C86 119.1(4) . . ?
C87 C88 C89 120.6(4) . . ?
C87 C88 C91 120.3(4) . . ?
C89 C88 C91 119.1(5) . . ?
C90 C89 C88 120.3(5) . . ?
C89 C90 C85 120.3(4) . . ?
F19A C91 F20A 106.4(9) . . ?
F19A C91 F21A 109.1(9) . . ?
F19A C91 C88 113.7(7) . . ?
F20A C91 C88 111.0(7) . . ?
F21A C91 F20A 102.2(10) . . ?
F21A C91 C88 113.5(7) . . ?
F19B C91 C88 108.0(9) . . ?
F20B C91 F19B 101.8(16) . . ?
F20B C91 C88 114.8(10) . . ?
F21B C91 F19B 107(2) . . ?
F21B C91 F20B 111(2) . . ?
F21B C91 C88 113.5(16) . . ?
C93 C92 C70 120.3(4) . . ?
C93 C92 C97 119.0(4) . . ?
C97 C92 C70 120.6(4) . . ?
C94 C93 C92 120.7(4) . . ?
C93 C94 C95 119.5(4) . . ?
C94 C95 C96 121.2(4) . . ?
C94 C95 C98 120.6(4) . . ?
C96 C95 C98 118.2(4) . . ?
C97 C96 C95 119.1(4) . . ?
C96 C97 C92 120.4(4) . . ?
F22 C98 F23 107.0(4) . . ?
F22 C98 F24 106.9(4) . . ?
F22 C98 C95 113.5(4) . . ?
F23 C98 C95 111.6(4) . . ?
F24 C98 F23 105.2(4) . . ?
F24 C98 C95 112.2(4) . . ?
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 C2 1.865(4) . ?
Br2 C3 1.869(4) . ?
Br3 C7 1.871(4) . ?
Br4 C8 1.882(4) . ?
Br5 C12 1.877(5) . ?
Br6 C13 1.876(4) . ?
Br7 C17 1.878(4) . ?
Br8 C18 1.864(4) . ?
F1A C27A 1.308(12) . ?
F2A C27A 1.354(13) . ?
F1B C27B 1.30(3) . ?
F2B C27B 1.27(3) . ?
F3 C27A 1.320(11) . ?
F3 C27B 1.26(3) . ?
F4A C34 1.370(9) . ?
F5A C34 1.285(15) . ?
F6A C34 1.344(11) . ?
F4B C34 1.22(2) . ?
F5B C34 1.41(2) . ?
F6B C34 1.380(15) . ?
F7 C41 1.331(7) . ?
F8 C41 1.326(7) . ?
F9 C41 1.333(6) . ?
F10A C48A 1.323(15) . ?
F11A C48A 1.312(12) . ?
F10B C48B 1.28(5) . ?
F11B C48B 1.37(5) . ?
F12 C48A 1.299(17) . ?
F12 C48B 1.31(6) . ?
N1 C1 1.366(6) . ?
N1 C4 1.372(5) . ?
N2 C6 1.368(5) . ?
N2 C9 1.372(6) . ?
N3 C11 1.365(6) . ?
N3 C14 1.361(6) . ?
N4 C16 1.382(5) . ?
N4 C19 1.369(5) . ?
C1 C2 1.425(6) . ?
C1 C20 1.417(6) . ?
C2 C3 1.360(6) . ?
C3 C4 1.437(6) . ?
C4 C5 1.407(6) . ?
C5 C6 1.421(6) . ?
C5 C21 1.478(6) . ?
C6 C7 1.445(6) . ?
C7 C8 1.354(6) . ?
C8 C9 1.443(6) . ?
C9 C10 1.411(6) . ?
C10 C11 1.412(6) . ?
C10 C28 1.473(6) . ?
C11 C12 1.447(6) . ?
C12 C13 1.342(7) . ?
C13 C14 1.456(6) . ?
C14 C15 1.407(6) . ?
C15 C16 1.411(6) . ?
C15 C35 1.479(6) . ?
C16 C17 1.426(6) . ?
C17 C18 1.366(6) . ?
C18 C19 1.437(6) . ?
C19 C20 1.408(6) . ?
C20 C42 1.489(6) . ?
C21 C22 1.406(6) . ?
C21 C26 1.393(6) . ?
C22 C23 1.374(6) . ?
C23 C24 1.387(7) . ?
C24 C25 1.401(7) . ?
C24 C27A 1.492(10) . ?
C24 C27B 1.60(3) . ?
C25 C26 1.383(7) . ?
C28 C29 1.393(7) . ?
C28 C33 1.394(6) . ?
C29 C30 1.388(6) . ?
C30 C31 1.377(7) . ?
C31 C32 1.395(7) . ?
C31 C34 1.496(7) . ?
C32 C33 1.397(6) . ?
C35 C36 1.406(6) . ?
C35 C40 1.385(6) . ?
C36 C37 1.379(6) . ?
C37 C38 1.384(7) . ?
C38 C39 1.392(7) . ?
C38 C41 1.499(6) . ?
C39 C40 1.392(6) . ?
C42 C43 1.392(6) . ?
C42 C47 1.392(6) . ?
C43 C44 1.398(6) . ?
C44 C45 1.381(7) . ?
C45 C46 1.387(8) . ?
C45 C48A 1.509(16) . ?
C45 C48B 1.53(6) . ?
C46 C47 1.395(6) . ?
Br9 C52 1.869(4) . ?
Br10 C53 1.873(4) . ?
Br11 C57 1.866(5) . ?
Br12 C58 1.872(4) . ?
Br13 C62 1.874(4) . ?
Br14 C63 1.870(4) . ?
Br15 C67 1.872(4) . ?
Br16 C68 1.867(4) . ?
F13 C77 1.320(7) . ?
F14 C77 1.325(8) . ?
F15 C77 1.343(8) . ?
F16 C84 1.336(6) . ?
F17 C84 1.343(6) . ?
F18 C84 1.329(6) . ?
F19A C91 1.289(12) . ?
F20A C91 1.337(11) . ?
F21A C91 1.314(11) . ?
F19B C91 1.357(19) . ?
F20B C91 1.279(18) . ?
F21B C91 1.20(3) . ?
F22 C98 1.329(6) . ?
F23 C98 1.346(6) . ?
F24 C98 1.336(6) . ?
N5 C51 1.365(5) . ?
N5 C54 1.370(6) . ?
N6 C56 1.374(6) . ?
N6 C59 1.360(6) . ?
N7 C61 1.381(6) . ?
N7 C64 1.344(6) . ?
N8 C66 1.391(5) . ?
N8 C69 1.367(6) . ?
C51 C52 1.443(6) . ?
C51 C70 1.411(6) . ?
C52 C53 1.353(6) . ?
C53 C54 1.430(6) . ?
C54 C55 1.414(6) . ?
C55 C56 1.410(6) . ?
C55 C71 1.476(6) . ?
C56 C57 1.442(6) . ?
C57 C58 1.357(6) . ?
C58 C59 1.448(6) . ?
C59 C60 1.431(6) . ?
C60 C61 1.392(6) . ?
C60 C78 1.479(6) . ?
C61 C62 1.454(6) . ?
C62 C63 1.349(7) . ?
C63 C64 1.458(6) . ?
C64 C65 1.432(6) . ?
C65 C66 1.403(6) . ?
C65 C85 1.482(6) . ?
C66 C67 1.433(6) . ?
C67 C68 1.356(6) . ?
C68 C69 1.439(6) . ?
C69 C70 1.417(6) . ?
C70 C92 1.478(6) . ?
C71 C72 1.399(6) . ?
C71 C76 1.389(7) . ?
C72 C73 1.382(7) . ?
C73 C74 1.391(8) . ?
C74 C75 1.391(7) . ?
C74 C77 1.494(7) . ?
C75 C76 1.373(7) . ?
C78 C79 1.403(6) . ?
C78 C83 1.392(6) . ?
C79 C80 1.372(7) . ?
C80 C81 1.386(7) . ?
C81 C82 1.392(7) . ?
C81 C84 1.509(6) . ?
C82 C83 1.395(6) . ?
C85 C86 1.396(6) . ?
C85 C90 1.398(6) . ?
C86 C87 1.393(7) . ?
C87 C88 1.382(7) . ?
C88 C89 1.386(7) . ?
C88 C91 1.504(7) . ?
C89 C90 1.378(7) . ?
C92 C93 1.401(6) . ?
C92 C97 1.404(6) . ?
C93 C94 1.382(6) . ?
C94 C95 1.387(7) . ?
C95 C96 1.393(7) . ?
C95 C98 1.500(6) . ?
C96 C97 1.390(6) . ?
O1 C49 1.356(8) . ?
O2 C50 1.390(6) . ?
O3 C99 1.426(6) . ?
C100 O4 1.377(7) . ?
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
N1 H1 O1 0.88(2) 1.95(3) 2.812(5) 166(6) . yes
N4 H4 O2 0.87(2) 1.98(2) 2.844(5) 173(5) . yes
N5 H5 O4 0.87(2) 1.95(3) 2.797(5) 165(6) . yes
N8 H8 O3 0.87(2) 2.07(3) 2.923(5) 166(6) . yes
O1 H1S N3 0.83(2) 2.09(3) 2.894(5) 164(6) . yes
O2 H2S N2 0.84(2) 2.11(4) 2.908(5) 159(8) . yes
O3 H3S N6 0.859(19) 2.022(19) 2.837(5) 158(6) . yes
O4 H4S N7 0.84(2) 2.05(2) 2.884(5) 174(9) . 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
Br1 C2 C3 Br2 0.2(5) . . . . ?
Br1 C2 C3 C4 171.6(3) . . . . ?
Br2 C3 C4 N1 170.2(3) . . . . ?
Br2 C3 C4 C5 -13.3(6) . . . . ?
Br3 C7 C8 Br4 -3.2(6) . . . . ?
Br3 C7 C8 C9 -172.9(3) . . . . ?
Br4 C8 C9 N2 -166.5(3) . . . . ?
Br4 C8 C9 C10 18.0(7) . . . . ?
Br5 C12 C13 Br6 -0.3(6) . . . . ?
Br5 C12 C13 C14 169.1(3) . . . . ?
Br6 C13 C14 N3 167.0(3) . . . . ?
Br6 C13 C14 C15 -20.5(6) . . . . ?
Br7 C17 C18 Br8 -0.1(6) . . . . ?
Br7 C17 C18 C19 -171.5(3) . . . . ?
Br8 C18 C19 N4 -169.7(3) . . . . ?
Br8 C18 C19 C20 11.8(7) . . . . ?
N1 C1 C2 Br1 -170.1(3) . . . . ?
N1 C1 C2 C3 2.2(5) . . . . ?
N1 C1 C20 C19 35.0(6) . . . . ?
N1 C1 C20 C42 -144.3(4) . . . . ?
N1 C4 C5 C6 -30.9(6) . . . . ?
N1 C4 C5 C21 147.8(4) . . . . ?
N2 C6 C7 Br3 170.7(3) . . . . ?
N2 C6 C7 C8 -0.2(5) . . . . ?
N2 C9 C10 C11 28.3(6) . . . . ?
N2 C9 C10 C28 -152.0(4) . . . . ?
N3 C11 C12 Br5 -166.6(3) . . . . ?
N3 C11 C12 C13 1.9(5) . . . . ?
N3 C14 C15 C16 -37.2(6) . . . . ?
N3 C14 C15 C35 139.0(4) . . . . ?
N4 C16 C17 Br7 170.2(3) . . . . ?
N4 C16 C17 C18 -0.3(5) . . . . ?
N4 C19 C20 C1 25.9(6) . . . . ?
N4 C19 C20 C42 -154.8(4) . . . . ?
C1 N1 C4 C3 2.4(4) . . . . ?
C1 N1 C4 C5 -174.3(4) . . . . ?
C1 C2 C3 Br2 -172.2(3) . . . . ?
C1 C2 C3 C4 -0.8(5) . . . . ?
C1 C20 C42 C43 -135.0(4) . . . . ?
C1 C20 C42 C47 42.3(6) . . . . ?
C2 C1 C20 C19 -148.3(4) . . . . ?
C2 C1 C20 C42 32.4(6) . . . . ?
C2 C3 C4 N1 -0.9(5) . . . . ?
C2 C3 C4 C5 175.6(4) . . . . ?
C3 C4 C5 C6 153.2(4) . . . . ?
C3 C4 C5 C21 -28.1(6) . . . . ?
C4 N1 C1 C2 -2.8(5) . . . . ?
C4 N1 C1 C20 174.5(4) . . . . ?
C4 C5 C6 N2 -29.0(6) . . . . ?
C4 C5 C6 C7 150.9(4) . . . . ?
C4 C5 C21 C22 -41.4(6) . . . . ?
C4 C5 C21 C26 136.1(5) . . . . ?
C5 C6 C7 Br3 -9.1(7) . . . . ?
C5 C6 C7 C8 179.9(4) . . . . ?
C5 C21 C22 C23 177.3(4) . . . . ?
C5 C21 C26 C25 -177.2(5) . . . . ?
C6 N2 C9 C8 -3.0(5) . . . . ?
C6 N2 C9 C10 172.9(4) . . . . ?
C6 C5 C21 C22 137.3(4) . . . . ?
C6 C5 C21 C26 -45.2(6) . . . . ?
C6 C7 C8 Br4 168.2(3) . . . . ?
C6 C7 C8 C9 -1.6(5) . . . . ?
C7 C8 C9 N2 2.9(5) . . . . ?
C7 C8 C9 C10 -172.5(4) . . . . ?
C8 C9 C10 C11 -156.8(4) . . . . ?
C8 C9 C10 C28 22.9(7) . . . . ?
C9 N2 C6 C5 -178.1(4) . . . . ?
C9 N2 C6 C7 2.1(5) . . . . ?
C9 C10 C11 N3 34.5(6) . . . . ?
C9 C10 C11 C12 -150.9(4) . . . . ?
C9 C10 C28 C29 40.6(6) . . . . ?
C9 C10 C28 C33 -139.3(5) . . . . ?
C10 C11 C12 Br5 18.2(7) . . . . ?
C10 C11 C12 C13 -173.3(4) . . . . ?
C10 C28 C29 C30 -178.4(5) . . . . ?
C10 C28 C33 C32 179.3(4) . . . . ?
C11 N3 C14 C13 3.4(5) . . . . ?
C11 N3 C14 C15 -169.5(4) . . . . ?
C11 C10 C28 C29 -139.6(5) . . . . ?
C11 C10 C28 C33 40.5(6) . . . . ?
C11 C12 C13 Br6 -169.2(3) . . . . ?
C11 C12 C13 C14 0.2(5) . . . . ?
C12 C13 C14 N3 -2.3(5) . . . . ?
C12 C13 C14 C15 170.2(4) . . . . ?
C13 C14 C15 C16 151.3(4) . . . . ?
C13 C14 C15 C35 -32.5(6) . . . . ?
C14 N3 C11 C10 172.3(4) . . . . ?
C14 N3 C11 C12 -3.3(5) . . . . ?
C14 C15 C16 N4 -23.3(7) . . . . ?
C14 C15 C16 C17 156.5(5) . . . . ?
C14 C15 C35 C36 -40.7(6) . . . . ?
C14 C15 C35 C40 136.0(5) . . . . ?
C15 C16 C17 Br7 -9.7(7) . . . . ?
C15 C16 C17 C18 179.8(5) . . . . ?
C15 C35 C36 C37 175.2(4) . . . . ?
C15 C35 C40 C39 -175.9(4) . . . . ?
C16 N4 C19 C18 -1.7(5) . . . . ?
C16 N4 C19 C20 176.9(4) . . . . ?
C16 C15 C35 C36 135.4(5) . . . . ?
C16 C15 C35 C40 -47.9(7) . . . . ?
C16 C17 C18 Br8 170.7(3) . . . . ?
C16 C17 C18 C19 -0.7(5) . . . . ?
C17 C18 C19 N4 1.4(5) . . . . ?
C17 C18 C19 C20 -177.0(4) . . . . ?
C18 C19 C20 C1 -155.8(4) . . . . ?
C18 C19 C20 C42 23.4(7) . . . . ?
C19 N4 C16 C15 -178.9(4) . . . . ?
C19 N4 C16 C17 1.3(5) . . . . ?
C19 C20 C42 C43 45.7(6) . . . . ?
C19 C20 C42 C47 -137.0(4) . . . . ?
C20 C1 C2 Br1 12.7(6) . . . . ?
C20 C1 C2 C3 -175.0(4) . . . . ?
C20 C42 C43 C44 177.1(4) . . . . ?
C20 C42 C47 C46 -177.6(4) . . . . ?
C21 C5 C6 N2 152.4(4) . . . . ?
C21 C5 C6 C7 -27.8(7) . . . . ?
C21 C22 C23 C24 -0.1(7) . . . . ?
C22 C21 C26 C25 0.2(7) . . . . ?
C22 C23 C24 C25 0.5(8) . . . . ?
C22 C23 C24 C27A -174.3(6) . . . . ?
C22 C23 C24 C27B 162.6(13) . . . . ?
C23 C24 C25 C26 -0.5(8) . . . . ?
C23 C24 C27A F1A 60.6(11) . . . . ?
C23 C24 C27A F2A -54.4(11) . . . . ?
C23 C24 C27A F3 -173.7(7) . . . . ?
C23 C24 C27B F1B 43(2) . . . . ?
C23 C24 C27B F2B -77(2) . . . . ?
C23 C24 C27B F3 162.2(13) . . . . ?
C24 C25 C26 C21 0.1(8) . . . . ?
C25 C24 C27A F1A -114.1(11) . . . . ?
C25 C24 C27A F2A 130.9(9) . . . . ?
C25 C24 C27A F3 11.6(12) . . . . ?
C25 C24 C27B F1B -153.7(17) . . . . ?
C25 C24 C27B F2B 85(2) . . . . ?
C25 C24 C27B F3 -35(2) . . . . ?
C26 C21 C22 C23 -0.2(7) . . . . ?
C27A C24 C25 C26 174.1(7) . . . . ?
C27B C24 C25 C26 -163.3(13) . . . . ?
C28 C10 C11 N3 -145.2(4) . . . . ?
C28 C10 C11 C12 29.4(6) . . . . ?
C28 C29 C30 C31 -0.7(8) . . . . ?
C29 C28 C33 C32 -0.6(7) . . . . ?
C29 C30 C31 C32 -1.1(8) . . . . ?
C29 C30 C31 C34 179.7(5) . . . . ?
C30 C31 C32 C33 2.0(8) . . . . ?
C30 C31 C34 F4A 1.7(8) . . . . ?
C30 C31 C34 F5A 121.6(12) . . . . ?
C30 C31 C34 F6A -113.0(15) . . . . ?
C30 C31 C34 F4B -27(3) . . . . ?
C30 C31 C34 F5B 106.1(13) . . . . ?
C30 C31 C34 F6B -151.1(14) . . . . ?
C31 C32 C33 C28 -1.1(7) . . . . ?
C32 C31 C34 F4A -177.6(6) . . . . ?
C32 C31 C34 F5A -57.6(12) . . . . ?
C32 C31 C34 F6A 67.7(16) . . . . ?
C32 C31 C34 F4B 153(3) . . . . ?
C32 C31 C34 F5B -73.2(13) . . . . ?
C32 C31 C34 F6B 29.7(14) . . . . ?
C33 C28 C29 C30 1.5(7) . . . . ?
C34 C31 C32 C33 -178.8(5) . . . . ?
C35 C15 C16 N4 160.8(4) . . . . ?
C35 C15 C16 C17 -19.4(7) . . . . ?
C35 C36 C37 C38 0.8(7) . . . . ?
C36 C35 C40 C39 0.7(7) . . . . ?
C36 C37 C38 C39 0.9(7) . . . . ?
C36 C37 C38 C41 -178.3(4) . . . . ?
C37 C38 C39 C40 -1.8(7) . . . . ?
C37 C38 C41 F7 67.0(6) . . . . ?
C37 C38 C41 F8 -172.0(4) . . . . ?
C37 C38 C41 F9 -52.1(6) . . . . ?
C38 C39 C40 C35 1.0(7) . . . . ?
C39 C38 C41 F7 -112.2(6) . . . . ?
C39 C38 C41 F8 8.8(7) . . . . ?
C39 C38 C41 F9 128.7(5) . . . . ?
C40 C35 C36 C37 -1.6(7) . . . . ?
C41 C38 C39 C40 177.4(4) . . . . ?
C42 C43 C44 C45 0.6(7) . . . . ?
C43 C42 C47 C46 -0.4(7) . . . . ?
C43 C44 C45 C46 -0.4(7) . . . . ?
C43 C44 C45 C48A 175.6(7) . . . . ?
C43 C44 C45 C48B -174(2) . . . . ?
C44 C45 C46 C47 -0.1(7) . . . . ?
C44 C45 C48A F10A -1.2(13) . . . . ?
C44 C45 C48A F11A -124.5(11) . . . . ?
C44 C45 C48A F12 119.1(10) . . . . ?
C44 C45 C48B F10B 21(5) . . . . ?
C44 C45 C48B F11B -101(3) . . . . ?
C44 C45 C48B F12 140(2) . . . . ?
C45 C46 C47 C42 0.5(7) . . . . ?
C46 C45 C48A F10A 175.1(8) . . . . ?
C46 C45 C48A F11A 51.8(15) . . . . ?
C46 C45 C48A F12 -64.6(10) . . . . ?
C46 C45 C48B F10B -152(4) . . . . ?
C46 C45 C48B F11B 86(4) . . . . ?
C46 C45 C48B F12 -33(4) . . . . ?
C47 C42 C43 C44 -0.2(6) . . . . ?
C48A C45 C46 C47 -176.5(7) . . . . ?
C48B C45 C46 C47 172(2) . . . . ?
Br9 C52 C53 Br10 -0.6(6) . . . . ?
Br9 C52 C53 C54 -170.8(3) . . . . ?
Br10 C53 C54 N5 -168.9(3) . . . . ?
Br10 C53 C54 C55 9.5(7) . . . . ?
Br11 C57 C58 Br12 -2.9(6) . . . . ?
Br11 C57 C58 C59 170.7(3) . . . . ?
Br12 C58 C59 N6 172.7(3) . . . . ?
Br12 C58 C59 C60 -10.3(7) . . . . ?
Br13 C62 C63 Br14 -1.5(6) . . . . ?
Br13 C62 C63 C64 -171.9(3) . . . . ?
Br14 C63 C64 N7 -167.9(3) . . . . ?
Br14 C63 C64 C65 14.8(6) . . . . ?
Br15 C67 C68 Br16 2.5(6) . . . . ?
Br15 C67 C68 C69 173.3(3) . . . . ?
Br16 C68 C69 N8 169.0(3) . . . . ?
Br16 C68 C69 C70 -13.4(7) . . . . ?
N5 C51 C52 Br9 169.0(3) . . . . ?
N5 C51 C52 C53 -2.0(5) . . . . ?
N5 C51 C70 C69 -27.4(7) . . . . ?
N5 C51 C70 C92 155.2(4) . . . . ?
N5 C54 C55 C56 30.3(7) . . . . ?
N5 C54 C55 C71 -155.3(4) . . . . ?
N6 C56 C57 Br11 -169.0(3) . . . . ?
N6 C56 C57 C58 3.2(5) . . . . ?
N6 C59 C60 C61 -35.3(6) . . . . ?
N6 C59 C60 C78 141.8(4) . . . . ?
N7 C61 C62 Br13 170.0(3) . . . . ?
N7 C61 C62 C63 -0.2(5) . . . . ?
N7 C64 C65 C66 38.2(6) . . . . ?
N7 C64 C65 C85 -142.2(4) . . . . ?
N8 C66 C67 Br15 -171.1(3) . . . . ?
N8 C66 C67 C68 2.1(5) . . . . ?
N8 C69 C70 C51 -29.6(7) . . . . ?
N8 C69 C70 C92 147.8(4) . . . . ?
C51 N5 C54 C53 -2.4(5) . . . . ?
C51 N5 C54 C55 179.0(4) . . . . ?
C51 C52 C53 Br10 170.7(3) . . . . ?
C51 C52 C53 C54 0.6(5) . . . . ?
C51 C70 C92 C93 130.4(5) . . . . ?
C51 C70 C92 C97 -46.3(6) . . . . ?
C52 C51 C70 C69 155.2(4) . . . . ?
C52 C51 C70 C92 -22.2(7) . . . . ?
C52 C53 C54 N5 1.1(5) . . . . ?
C52 C53 C54 C55 179.5(4) . . . . ?
C53 C54 C55 C56 -147.8(5) . . . . ?
C53 C54 C55 C71 26.6(7) . . . . ?
C54 N5 C51 C52 2.8(5) . . . . ?
C54 N5 C51 C70 -175.1(4) . . . . ?
C54 C55 C56 N6 29.9(7) . . . . ?
C54 C55 C56 C57 -157.4(5) . . . . ?
C54 C55 C71 C72 46.2(7) . . . . ?
C54 C55 C71 C76 -131.0(5) . . . . ?
C55 C56 C57 Br11 17.6(7) . . . . ?
C55 C56 C57 C58 -170.3(4) . . . . ?
C55 C71 C72 C73 -176.5(5) . . . . ?
C55 C71 C76 C75 175.5(5) . . . . ?
C56 N6 C59 C58 2.6(5) . . . . ?
C56 N6 C59 C60 -174.6(4) . . . . ?
C56 C55 C71 C72 -139.3(5) . . . . ?
C56 C55 C71 C76 43.5(7) . . . . ?
C56 C57 C58 Br12 -175.2(3) . . . . ?
C56 C57 C58 C59 -1.5(5) . . . . ?
C57 C58 C59 N6 -0.6(5) . . . . ?
C57 C58 C59 C60 176.4(4) . . . . ?
C58 C59 C60 C61 148.1(5) . . . . ?
C58 C59 C60 C78 -34.8(6) . . . . ?
C59 N6 C56 C55 170.4(4) . . . . ?
C59 N6 C56 C57 -3.5(5) . . . . ?
C59 C60 C61 N7 -24.0(6) . . . . ?
C59 C60 C61 C62 158.3(4) . . . . ?
C59 C60 C78 C79 -49.2(6) . . . . ?
C59 C60 C78 C83 127.2(5) . . . . ?
C60 C61 C62 Br13 -12.0(7) . . . . ?
C60 C61 C62 C63 177.8(4) . . . . ?
C60 C78 C79 C80 176.6(5) . . . . ?
C60 C78 C83 C82 -175.0(4) . . . . ?
C61 N7 C64 C63 -2.6(5) . . . . ?
C61 N7 C64 C65 174.7(4) . . . . ?
C61 C60 C78 C79 127.8(5) . . . . ?
C61 C60 C78 C83 -55.8(6) . . . . ?
C61 C62 C63 Br14 169.1(3) . . . . ?
C61 C62 C63 C64 -1.3(5) . . . . ?
C62 C63 C64 N7 2.5(5) . . . . ?
C62 C63 C64 C65 -174.8(4) . . . . ?
C63 C64 C65 C66 -144.9(4) . . . . ?
C63 C64 C65 C85 34.7(6) . . . . ?
C64 N7 C61 C60 -176.4(4) . . . . ?
C64 N7 C61 C62 1.8(5) . . . . ?
C64 C65 C66 N8 18.9(6) . . . . ?
C64 C65 C66 C67 -164.0(5) . . . . ?
C64 C65 C85 C86 48.0(6) . . . . ?
C64 C65 C85 C90 -129.9(5) . . . . ?
C65 C66 C67 Br15 11.5(7) . . . . ?
C65 C66 C67 C68 -175.3(5) . . . . ?
C65 C85 C86 C87 -177.9(5) . . . . ?
C65 C85 C90 C89 176.9(5) . . . . ?
C66 N8 C69 C68 3.0(5) . . . . ?
C66 N8 C69 C70 -174.7(4) . . . . ?
C66 C65 C85 C86 -132.4(5) . . . . ?
C66 C65 C85 C90 49.8(6) . . . . ?
C66 C67 C68 Br16 -171.1(3) . . . . ?
C66 C67 C68 C69 -0.4(5) . . . . ?
C67 C68 C69 N8 -1.6(5) . . . . ?
C67 C68 C69 C70 175.9(4) . . . . ?
C68 C69 C70 C51 153.3(5) . . . . ?
C68 C69 C70 C92 -29.3(7) . . . . ?
C69 N8 C66 C65 174.5(4) . . . . ?
C69 N8 C66 C67 -3.2(5) . . . . ?
C69 C70 C92 C93 -47.1(6) . . . . ?
C69 C70 C92 C97 136.2(5) . . . . ?
C70 C51 C52 Br9 -13.2(7) . . . . ?
C70 C51 C52 C53 175.7(4) . . . . ?
C70 C92 C93 C94 -174.5(4) . . . . ?
C70 C92 C97 C96 173.6(4) . . . . ?
C71 C55 C56 N6 -144.6(4) . . . . ?
C71 C55 C56 C57 28.1(7) . . . . ?
C71 C72 C73 C74 1.2(8) . . . . ?
C72 C71 C76 C75 -1.8(8) . . . . ?
C72 C73 C74 C75 -2.2(8) . . . . ?
C72 C73 C74 C77 179.1(5) . . . . ?
C73 C74 C75 C76 1.1(8) . . . . ?
C73 C74 C77 F13 -19.0(8) . . . . ?
C73 C74 C77 F14 -141.5(6) . . . . ?
C73 C74 C77 F15 99.4(7) . . . . ?
C74 C75 C76 C71 0.9(8) . . . . ?
C75 C74 C77 F13 162.3(6) . . . . ?
C75 C74 C77 F14 39.7(8) . . . . ?
C75 C74 C77 F15 -79.4(7) . . . . ?
C76 C71 C72 C73 0.7(7) . . . . ?
C77 C74 C75 C76 179.9(5) . . . . ?
C78 C60 C61 N7 159.2(4) . . . . ?
C78 C60 C61 C62 -18.5(7) . . . . ?
C78 C79 C80 C81 -1.8(8) . . . . ?
C79 C78 C83 C82 1.4(7) . . . . ?
C79 C80 C81 C82 2.1(7) . . . . ?
C79 C80 C81 C84 -176.4(5) . . . . ?
C80 C81 C82 C83 -0.7(7) . . . . ?
C80 C81 C84 F16 67.8(6) . . . . ?
C80 C81 C84 F17 -49.9(6) . . . . ?
C80 C81 C84 F18 -169.3(4) . . . . ?
C81 C82 C83 C78 -1.1(7) . . . . ?
C82 C81 C84 F16 -110.7(5) . . . . ?
C82 C81 C84 F17 131.7(5) . . . . ?
C82 C81 C84 F18 12.2(7) . . . . ?
C83 C78 C79 C80 0.0(7) . . . . ?
C84 C81 C82 C83 177.8(4) . . . . ?
C85 C65 C66 N8 -160.7(4) . . . . ?
C85 C65 C66 C67 16.3(7) . . . . ?
C85 C86 C87 C88 1.3(8) . . . . ?
C86 C85 C90 C89 -1.0(8) . . . . ?
C86 C87 C88 C89 -1.7(8) . . . . ?
C86 C87 C88 C91 177.1(5) . . . . ?
C87 C88 C89 C90 0.7(9) . . . . ?
C87 C88 C91 F19A -89.4(13) . . . . ?
C87 C88 C91 F20A 150.6(14) . . . . ?
C87 C88 C91 F21A 36.1(10) . . . . ?
C87 C88 C91 F19B -52(2) . . . . ?
C87 C88 C91 F20B -165(3) . . . . ?
C87 C88 C91 F21B 67(4) . . . . ?
C88 C89 C90 C85 0.6(9) . . . . ?
C89 C88 C91 F19A 89.4(13) . . . . ?
C89 C88 C91 F20A -30.6(15) . . . . ?
C89 C88 C91 F21A -145.1(9) . . . . ?
C89 C88 C91 F19B 127(2) . . . . ?
C89 C88 C91 F20B 14(3) . . . . ?
C89 C88 C91 F21B -115(4) . . . . ?
C90 C85 C86 C87 0.0(7) . . . . ?
C91 C88 C89 C90 -178.1(6) . . . . ?
C92 C93 C94 C95 0.8(7) . . . . ?
C93 C92 C97 C96 -3.2(7) . . . . ?
C93 C94 C95 C96 -3.0(7) . . . . ?
C93 C94 C95 C98 178.3(4) . . . . ?
C94 C95 C96 C97 2.1(7) . . . . ?
C94 C95 C98 F22 -14.4(6) . . . . ?
C94 C95 C98 F23 106.6(5) . . . . ?
C94 C95 C98 F24 -135.7(5) . . . . ?
C95 C96 C97 C92 1.1(7) . . . . ?
C96 C95 C98 F22 166.8(4) . . . . ?
C96 C95 C98 F23 -72.2(6) . . . . ?
C96 C95 C98 F24 45.6(6) . . . . ?
C97 C92 C93 C94 2.3(7) . . . . ?
C98 C95 C96 C97 -179.2(4) . . . . ?
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
2.0023 -0.0001 -4.9976 0.1570 0.1958 0.0096
-2.0023 0.0001 4.9976 -0.1570 -0.1958 -0.0096
12.9889 0.9986 0.0047 -0.3781 0.2774 -0.3887
-0.9990 0.0002 -0.0004 0.0332 -0.0241 0.0194
-4.9890 4.0056 0.9941 0.3365 -0.2949 -0.4590
4.9890 -4.0056 -0.9941 -0.3365 0.2949 0.4590
-4.9968 -1.0002 -0.0013 0.1123 -0.0844 0.2336
