# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tsu_1
_database_code_depnum_ccdc_archive 'CCDC 2201797'
loop_
_audit_author_name
_audit_author_address
'Eric Reinheimer'
;Rigaku Oxford Diffraction
United States of America
;
_audit_update_record             
;
2022-08-16 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_audit_creation_date             2021-12-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C53 H61 N5 O4'
_chemical_formula_sum            'C53 H61 N5 O4'
_chemical_formula_weight         832.06
_chemical_melting_point          ?
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   13.6441(2)
_cell_length_b                   13.8612(2)
_cell_length_c                   25.1810(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.1817(19)
_cell_angle_gamma                90
_cell_volume                     4636.84(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12942
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3800
_cell_measurement_theta_min      3.5680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 -4 -10 0.0324
-4 -6 12 0.0523
3 -8 4 0.0290
-6 0 14 0.0434
-1 8 -8 0.0175
2 -8 -6 0.0215
-8 2 10 0.0470
-2 -3 -14 0.0042
1 4 14 0.0238

_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.029
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27365
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.589
_diffrn_reflns_theta_max         66.589
_diffrn_reflns_theta_min         6.287
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -36.00  27.00   0.50   12.00    --   -5.92   0.00 150.00  126
  2  ω    -56.00  13.00   0.50   12.00    --    5.92 -37.00 150.00  138
  3  ω    -64.00 -13.00   0.50   50.00    --  -84.25  37.00 120.00  102
  4  ω    -52.00 -26.00   0.50   50.00    --  -84.25  19.00  90.00   52
  5  ω    -47.00   6.00   0.50   12.00    --    5.92 -77.00-120.00  106
  6  ω     35.00 115.00   0.50   50.00    --  105.75 -57.00  30.00  160
  7  ω    151.00 178.00   0.50   50.00    --  105.75  19.00 120.00   54
  8  ω    111.00 175.00   0.50   50.00    --  105.75  86.00 155.00  128
  9  ω    105.00 136.00   0.50   50.00    --  105.75  19.00 120.00   62
 10  ω     98.00 146.00   0.50   50.00    --  105.75  37.00 150.00   96
 11  ω     48.00 127.00   0.50   50.00    --  105.75 -77.00  30.00  158
 12  ω    114.00 140.00   0.50   50.00    --  105.75  19.00 -90.00   52
 13  ω    151.00 178.00   0.50   50.00    --  105.75  19.00 -90.00   54
 14  ω     36.00  62.00   0.50   50.00    --  105.75 -37.00 -60.00   52
 15  ω     35.00  65.00   0.50   50.00    --  105.75 -37.00-120.00   60
 16  ω     38.00  64.00   0.50   50.00    --  105.75 -37.00-150.00   52
 17  ω     33.00  65.00   0.50   50.00    --  105.75 -37.00-180.00   64
 18  ω     37.00  63.00   0.50   50.00    --  105.75 -99.00-180.00   52
 19  ω     33.00  61.00   0.50   50.00    --  105.75 -37.00  30.00   56
 20  ω     36.00  65.00   0.50   50.00    --  105.75 -37.00 120.00   58
 21  ω    -95.00 -15.00   0.50   50.00    --  -84.25 125.00-180.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Cu PhotonJet-S microsource'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6821
_reflns_number_total             8177
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         8177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.054
_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)+(0.0683P)²+0.9416P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1206
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.72776(7) 0.68627(7) 0.39273(4) 0.0222(2) Uani 1 1 d . . . . .
O3 O 0.55824(8) 0.79770(8) 0.51107(4) 0.0261(3) Uani 1 1 d . . . . .
O2 O 0.01904(8) 0.37006(8) 0.24968(5) 0.0281(3) Uani 1 1 d . . . . .
O1 O 0.08852(9) 0.50885(8) 0.09205(5) 0.0289(3) Uani 1 1 d . . . . .
N5 N 0.55985(9) 0.70969(9) 0.35955(5) 0.0188(3) Uani 1 1 d . . . . .
N2 N 0.07306(9) 0.52386(8) 0.25035(5) 0.0179(3) Uani 1 1 d . . . . .
N3 N 0.19909(9) 0.64914(9) 0.25877(5) 0.0178(3) Uani 1 1 d . . . . .
N4 N 0.47572(9) 0.78717(9) 0.42216(5) 0.0183(3) Uani 1 1 d . . . . .
N1 N 0.11440(9) 0.59452(8) 0.16984(5) 0.0179(3) Uani 1 1 d . . . . .
C42 C 0.64338(11) 0.69205(10) 0.40079(6) 0.0186(3) Uani 1 1 d . . . . .
C1 C 0.10575(10) 0.61039(10) 0.22543(6) 0.0173(3) Uani 1 1 d . . . . .
H1 H 0.0567(12) 0.6610(12) 0.2273(7) 0.013(4) Uiso 1 1 d . . . . .
C4 C 0.37726(11) 0.71157(10) 0.33541(6) 0.0185(3) Uani 1 1 d . . . . .
C2 C 0.29012(11) 0.60352(10) 0.26254(6) 0.0188(3) Uani 1 1 d . . . . .
H2 H 0.2877(12) 0.5446(13) 0.2383(7) 0.016(4) Uiso 1 1 d . . . . .
C31 C 0.39726(11) 0.84727(11) 0.43556(6) 0.0199(3) Uani 1 1 d . . . . .
C3 C 0.37529(11) 0.63329(10) 0.29644(6) 0.0204(3) Uani 1 1 d . . . . .
H3 H 0.4364(13) 0.5948(12) 0.2953(7) 0.018(4) Uiso 1 1 d . . . . .
C40 C 0.55063(11) 0.76095(10) 0.46629(6) 0.0201(3) Uani 1 1 d . . . . .
C8 C 0.04832(11) 0.54199(10) 0.30244(6) 0.0190(3) Uani 1 1 d . . . . .
C7 C 0.46545(11) 0.73614(10) 0.37132(6) 0.0185(3) Uani 1 1 d . . . . .
C12 C -0.06338(12) 0.61233(11) 0.35245(7) 0.0226(3) Uani 1 1 d . . . . .
H12 H -0.1263(14) 0.6424(13) 0.3539(7) 0.024(4) Uiso 1 1 d . . . . .
C6 C 0.19723(11) 0.72787(10) 0.29282(6) 0.0197(3) Uani 1 1 d . . . . .
H6 H 0.1307(14) 0.7623(13) 0.2882(7) 0.022(4) Uiso 1 1 d . . . . .
C23 C 0.06069(11) 0.75164(11) 0.12791(6) 0.0205(3) Uani 1 1 d . . . . .
C45 C 0.57415(10) 0.71986(11) 0.30443(6) 0.0196(3) Uani 1 1 d . . . . .
C22 C 0.13522(11) 0.68051(10) 0.14120(6) 0.0188(3) Uani 1 1 d . . . . .
C46 C 0.60402(10) 0.63962(11) 0.27778(6) 0.0217(3) Uani 1 1 d . . . . .
C32 C 0.40381(11) 0.94773(11) 0.43295(6) 0.0201(3) Uani 1 1 d . . . . .
C17 C 0.05249(10) 0.43539(10) 0.22626(7) 0.0207(3) Uani 1 1 d . . . . .
C27 C 0.22857(11) 0.69058(11) 0.12781(6) 0.0222(3) Uani 1 1 d . . . . .
C5 C 0.27930(11) 0.75803(11) 0.32941(6) 0.0201(3) Uani 1 1 d . . . . .
H5 H 0.2723(14) 0.8154(15) 0.3508(8) 0.031(5) Uiso 1 1 d . . . . .
C50 C 0.55751(11) 0.80959(11) 0.27829(7) 0.0216(3) Uani 1 1 d . . . . .
C26 C 0.24839(12) 0.77725(12) 0.10429(7) 0.0247(3) Uani 1 1 d . . . . .
H26 H 0.3128(14) 0.7861(13) 0.0951(7) 0.019(4) Uiso 1 1 d . . . . .
C37 C 0.49331(12) 0.99947(11) 0.42084(7) 0.0221(3) Uani 1 1 d . . . . .
H37A H 0.5547(15) 0.9578(15) 0.4265(8) 0.029(5) Uiso 1 1 d . . . . .
H37B H 0.5086(14) 1.0555(15) 0.4458(8) 0.029(5) Uiso 1 1 d . . . . .
H37C H 0.4817(13) 1.0188(13) 0.3837(8) 0.023(4) Uiso 1 1 d . . . . .
C9 C 0.11733(11) 0.51940(10) 0.35102(7) 0.0209(3) Uani 1 1 d . . . . .
C24 C 0.08499(12) 0.83734(11) 0.10488(7) 0.0238(3) Uani 1 1 d . . . . .
H24 H 0.0331(15) 0.8858(15) 0.0970(8) 0.029(5) Uiso 1 1 d . . . . .
C19 C 0.09105(11) 0.51066(11) 0.14051(7) 0.0208(3) Uani 1 1 d . . . . .
C18 C 0.07467(11) 0.41917(10) 0.17076(7) 0.0213(3) Uani 1 1 d . . . . .
C41 C 0.62097(11) 0.68054(11) 0.45686(6) 0.0219(3) Uani 1 1 d . . . . .
C36 C 0.32147(11) 0.80289(11) 0.45628(6) 0.0231(3) Uani 1 1 d . . . . .
C13 C -0.04451(11) 0.58437(11) 0.30265(7) 0.0216(3) Uani 1 1 d . . . . .
C28 C -0.04485(12) 0.73787(12) 0.13517(7) 0.0241(3) Uani 1 1 d . . . . .
H28A H -0.0615(14) 0.6683(15) 0.1378(8) 0.029(5) Uiso 1 1 d . . . . .
H28B H -0.0935(17) 0.7670(17) 0.1038(10) 0.046(6) Uiso 1 1 d . . . . .
H28C H -0.0542(14) 0.7676(14) 0.1692(8) 0.027(5) Uiso 1 1 d . . . . .
C10 C 0.09497(11) 0.54891(11) 0.39972(7) 0.0228(3) Uani 1 1 d . . . . .
H10 H 0.1425(14) 0.5328(14) 0.4347(8) 0.029(5) Uiso 1 1 d . . . . .
C11 C 0.00685(12) 0.59828(10) 0.40124(7) 0.0230(3) Uani 1 1 d . . . . .
C33 C 0.32648(11) 1.00239(11) 0.44586(7) 0.0235(3) Uani 1 1 d . . . . .
H33 H 0.3319(13) 1.0759(14) 0.4437(8) 0.026(5) Uiso 1 1 d . . . . .
C25 C 0.17894(12) 0.85178(11) 0.09387(7) 0.0246(3) Uani 1 1 d . . . . .
C49 C 0.56721(12) 0.81700(12) 0.22468(7) 0.0255(3) Uani 1 1 d . . . . .
H49 H 0.5561(14) 0.8816(15) 0.2060(8) 0.027(5) Uiso 1 1 d . . . . .
C35 C 0.24743(12) 0.86033(12) 0.46966(7) 0.0254(3) Uani 1 1 d . . . . .
H35 H 0.1958(13) 0.8311(12) 0.4843(7) 0.014(4) Uiso 1 1 d . . . . .
C34 C 0.24757(11) 0.96078(12) 0.46385(7) 0.0259(3) Uani 1 1 d . . . . .
C14 C 0.21252(12) 0.46369(13) 0.35202(8) 0.0265(4) Uani 1 1 d . . . . .
H14A H 0.214(2) 0.428(2) 0.3170(13) 0.073(8) Uiso 1 1 d . . . . .
H14B H 0.231(2) 0.423(2) 0.3847(12) 0.063(7) Uiso 1 1 d . . . . .
H14C H 0.267(2) 0.503(2) 0.3545(13) 0.080(9) Uiso 1 1 d . . . . .
C47 C 0.61196(11) 0.65080(12) 0.22406(7) 0.0251(3) Uani 1 1 d . . . . .
H47 H 0.6335(15) 0.5959(15) 0.2038(9) 0.033(5) Uiso 1 1 d . . . . .
C53 C 0.53407(13) 0.89744(11) 0.30783(7) 0.0255(3) Uani 1 1 d . . . . .
H53A H 0.4631(14) 0.8972(13) 0.3127(7) 0.023(4) Uiso 1 1 d . . . . .
H53B H 0.5447(14) 0.9568(15) 0.2873(8) 0.029(5) Uiso 1 1 d . . . . .
H53C H 0.5785(15) 0.9014(15) 0.3438(9) 0.035(5) Uiso 1 1 d . . . . .
C51 C 0.62962(12) 0.54378(12) 0.30563(7) 0.0252(3) Uani 1 1 d . . . . .
H51A H 0.7028(17) 0.5418(17) 0.3265(9) 0.045(6) Uiso 1 1 d . . . . .
H51B H 0.6235(15) 0.4912(16) 0.2792(9) 0.036(5) Uiso 1 1 d . . . . .
H51C H 0.5848(15) 0.5301(15) 0.3322(9) 0.034(5) Uiso 1 1 d . . . . .
C48 C 0.59330(12) 0.73853(12) 0.19633(7) 0.0271(4) Uani 1 1 d . . . . .
C21 C -0.01317(13) 0.36279(12) 0.13517(7) 0.0267(4) Uani 1 1 d . . . . .
H21A H -0.0187(16) 0.3001(17) 0.1523(9) 0.041(6) Uiso 1 1 d . . . . .
H21B H 0.0002(15) 0.3548(15) 0.0991(9) 0.033(5) Uiso 1 1 d . . . . .
H21C H -0.0786(15) 0.3986(15) 0.1306(8) 0.031(5) Uiso 1 1 d . . . . .
C30 C 0.30678(12) 0.61190(13) 0.13466(8) 0.0279(4) Uani 1 1 d . . . . .
H30A H 0.3676(19) 0.6297(18) 0.1632(11) 0.053(7) Uiso 1 1 d . . . . .
H30B H 0.3253(17) 0.6019(17) 0.1004(10) 0.045(6) Uiso 1 1 d . . . . .
H30C H 0.2817(15) 0.5484(16) 0.1432(8) 0.032(5) Uiso 1 1 d . . . . .
C20 C 0.17277(12) 0.35969(12) 0.17922(8) 0.0277(4) Uani 1 1 d . . . . .
H20A H 0.2329(16) 0.3959(15) 0.2015(8) 0.033(5) Uiso 1 1 d . . . . .
H20B H 0.1865(16) 0.3421(16) 0.1436(10) 0.039(5) Uiso 1 1 d . . . . .
H20C H 0.1654(15) 0.2995(16) 0.1995(9) 0.037(5) Uiso 1 1 d . . . . .
C39 C 0.32014(14) 0.69507(12) 0.46448(8) 0.0293(4) Uani 1 1 d . . . . .
H39A H 0.3202(16) 0.6594(17) 0.4292(10) 0.043(6) Uiso 1 1 d . . . . .
H39B H 0.2620(16) 0.6762(15) 0.4782(9) 0.036(5) Uiso 1 1 d . . . . .
H39C H 0.3797(17) 0.6732(16) 0.4927(9) 0.041(6) Uiso 1 1 d . . . . .
C15 C -0.01235(14) 0.63642(13) 0.45408(8) 0.0304(4) Uani 1 1 d . . . . .
H15A H 0.0386(18) 0.6853(17) 0.4686(10) 0.046(6) Uiso 1 1 d . . . . .
H15B H -0.0062(18) 0.5859(19) 0.4819(11) 0.056(7) Uiso 1 1 d . . . . .
H15C H -0.0791(18) 0.6664(17) 0.4489(9) 0.045(6) Uiso 1 1 d . . . . .
C44 C 0.71891(13) 0.68384(14) 0.50069(7) 0.0297(4) Uani 1 1 d . . . . .
H44A H 0.7658(15) 0.6298(15) 0.4968(8) 0.033(5) Uiso 1 1 d . . . . .
H44B H 0.7042(16) 0.6793(16) 0.5356(10) 0.040(6) Uiso 1 1 d . . . . .
H44C H 0.7589(16) 0.7456(16) 0.4994(9) 0.038(5) Uiso 1 1 d . . . . .
C43 C 0.56529(14) 0.58397(12) 0.45974(8) 0.0297(4) Uani 1 1 d . . . . .
H43A H 0.4994(16) 0.5816(15) 0.4304(9) 0.038(5) Uiso 1 1 d . . . . .
H43B H 0.5498(16) 0.5784(16) 0.4961(10) 0.041(6) Uiso 1 1 d . . . . .
H43C H 0.6099(14) 0.5331(14) 0.4544(8) 0.025(5) Uiso 1 1 d . . . . .
C29 C 0.20378(15) 0.94490(12) 0.06899(9) 0.0320(4) Uani 1 1 d . . . . .
H29A H 0.279(2) 0.947(2) 0.0722(12) 0.072(8) Uiso 1 1 d . . . . .
H29B H 0.1901(18) 1.001(2) 0.0889(11) 0.056(7) Uiso 1 1 d . . . . .
H29C H 0.172(2) 0.951(2) 0.0332(14) 0.074(9) Uiso 1 1 d . . . . .
C16 C -0.12360(13) 0.59979(15) 0.25074(8) 0.0322(4) Uani 1 1 d . . . . .
H16A H -0.107(2) 0.657(2) 0.2305(13) 0.074(8) Uiso 1 1 d . . . . .
H16B H -0.1895(17) 0.6137(16) 0.2588(9) 0.042(6) Uiso 1 1 d . . . . .
H16C H -0.126(2) 0.551(2) 0.2250(13) 0.070(8) Uiso 1 1 d . . . . .
C38 C 0.16716(14) 1.02211(15) 0.47908(9) 0.0344(4) Uani 1 1 d . . . . .
H38A H 0.178(2) 1.021(2) 0.5162(15) 0.085(10) Uiso 1 1 d . . . . .
H38B H 0.098(3) 0.995(3) 0.4692(15) 0.098(11) Uiso 1 1 d . . . . .
H38C H 0.167(3) 1.087(3) 0.4629(16) 0.111(12) Uiso 1 1 d . . . . .
C52 C 0.60138(18) 0.74813(16) 0.13812(8) 0.0392(4) Uani 1 1 d . . . . .
H52A H 0.542(2) 0.722(2) 0.1132(13) 0.076(9) Uiso 1 1 d . . . . .
H52B H 0.662(2) 0.716(2) 0.1339(12) 0.072(8) Uiso 1 1 d . . . . .
H52C H 0.606(2) 0.815(2) 0.1277(11) 0.065(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C42 1.2164(18) . ?
O3 C40 1.2200(19) . ?
O2 C17 1.2243(19) . ?
O1 C19 1.213(2) . ?
N5 C42 1.3774(19) . ?
N5 C7 1.4335(19) . ?
N5 C45 1.452(2) . ?
N2 C1 1.4693(19) . ?
N2 C8 1.449(2) . ?
N2 C17 1.3684(19) . ?
N3 C1 1.4587(18) . ?
N3 C2 1.3776(19) . ?
N3 C6 1.3917(19) . ?
N4 C31 1.4555(19) . ?
N4 C40 1.376(2) . ?
N4 C7 1.441(2) . ?
N1 C1 1.448(2) . ?
N1 C22 1.4543(19) . ?
N1 C19 1.3751(19) . ?
C42 C41 1.520(2) . ?
C1 H1 0.978(17) . ?
C4 C3 1.459(2) . ?
C4 C7 1.373(2) . ?
C4 C5 1.460(2) . ?
C2 H2 1.015(18) . ?
C2 C3 1.340(2) . ?
C31 C32 1.398(2) . ?
C31 C36 1.402(2) . ?
C3 H3 0.996(18) . ?
C40 C41 1.524(2) . ?
C8 C9 1.399(2) . ?
C8 C13 1.397(2) . ?
C12 H12 0.962(19) . ?
C12 C13 1.391(2) . ?
C12 C11 1.389(2) . ?
C6 H6 1.008(18) . ?
C6 C5 1.344(2) . ?
C23 C22 1.401(2) . ?
C23 C24 1.395(2) . ?
C23 C28 1.504(2) . ?
C45 C46 1.406(2) . ?
C45 C50 1.401(2) . ?
C22 C27 1.397(2) . ?
C46 C47 1.390(2) . ?
C46 C51 1.506(2) . ?
C32 C37 1.506(2) . ?
C32 C33 1.396(2) . ?
C17 C18 1.513(2) . ?
C27 C26 1.393(2) . ?
C27 C30 1.508(2) . ?
C5 H5 0.98(2) . ?
C50 C49 1.390(2) . ?
C50 C53 1.499(2) . ?
C26 H26 0.967(18) . ?
C26 C25 1.386(2) . ?
C37 H37A 1.00(2) . ?
C37 H37B 0.99(2) . ?
C37 H37C 0.95(2) . ?
C9 C10 1.391(2) . ?
C9 C14 1.506(2) . ?
C24 H24 0.96(2) . ?
C24 C25 1.386(2) . ?
C19 C18 1.522(2) . ?
C18 C21 1.536(2) . ?
C18 C20 1.545(2) . ?
C41 C44 1.527(2) . ?
C41 C43 1.549(2) . ?
C36 C35 1.387(2) . ?
C36 C39 1.509(2) . ?
C13 C16 1.509(2) . ?
C28 H28A 1.00(2) . ?
C28 H28B 0.99(2) . ?
C28 H28C 0.99(2) . ?
C10 H10 0.99(2) . ?
C10 C11 1.391(2) . ?
C11 C15 1.509(2) . ?
C33 H33 1.02(2) . ?
C33 C34 1.386(2) . ?
C25 C29 1.507(2) . ?
C49 H49 1.01(2) . ?
C49 C48 1.391(2) . ?
C35 H35 0.956(18) . ?
C35 C34 1.400(2) . ?
C34 C38 1.505(2) . ?
C14 H14A 1.01(3) . ?
C14 H14B 0.98(3) . ?
C14 H14C 0.92(3) . ?
C47 H47 1.00(2) . ?
C47 C48 1.396(2) . ?
C53 H53A 1.003(19) . ?
C53 H53B 1.00(2) . ?
C53 H53C 0.97(2) . ?
C51 H51A 1.02(2) . ?
C51 H51B 0.98(2) . ?
C51 H51C 1.02(2) . ?
C48 C52 1.501(3) . ?
C21 H21A 0.98(2) . ?
C21 H21B 0.97(2) . ?
C21 H21C 1.00(2) . ?
C30 H30A 1.00(3) . ?
C30 H30B 0.96(3) . ?
C30 H30C 0.99(2) . ?
C20 H20A 1.01(2) . ?
C20 H20B 0.99(2) . ?
C20 H20C 1.00(2) . ?
C39 H39A 1.02(2) . ?
C39 H39B 0.97(2) . ?
C39 H39C 1.00(2) . ?
C15 H15A 0.98(2) . ?
C15 H15B 0.98(3) . ?
C15 H15C 0.98(2) . ?
C44 H44A 1.00(2) . ?
C44 H44B 0.95(2) . ?
C44 H44C 1.02(2) . ?
C43 H43A 1.03(2) . ?
C43 H43B 0.99(2) . ?
C43 H43C 0.96(2) . ?
C29 H29A 1.02(3) . ?
C29 H29B 0.97(3) . ?
C29 H29C 0.91(3) . ?
C16 H16A 0.99(3) . ?
C16 H16B 0.98(2) . ?
C16 H16C 0.93(3) . ?
C38 H38A 0.91(4) . ?
C38 H38B 0.99(4) . ?
C38 H38C 0.99(4) . ?
C52 H52A 0.98(3) . ?
C52 H52B 0.96(3) . ?
C52 H52C 0.97(3) . ?

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
C42 N5 C7 121.17(13) . . ?
C42 N5 C45 118.00(12) . . ?
C7 N5 C45 119.71(12) . . ?
C8 N2 C1 113.64(11) . . ?
C17 N2 C1 126.42(13) . . ?
C17 N2 C8 119.35(12) . . ?
C2 N3 C1 121.72(12) . . ?
C2 N3 C6 117.41(12) . . ?
C6 N3 C1 120.47(12) . . ?
C40 N4 C31 114.46(12) . . ?
C40 N4 C7 119.44(12) . . ?
C7 N4 C31 124.00(12) . . ?
C1 N1 C22 115.03(11) . . ?
C19 N1 C1 126.00(12) . . ?
C19 N1 C22 118.29(12) . . ?
O4 C42 N5 122.54(14) . . ?
O4 C42 C41 123.14(13) . . ?
N5 C42 C41 114.32(12) . . ?
N2 C1 H1 106.7(10) . . ?
N3 C1 N2 111.41(12) . . ?
N3 C1 H1 103.0(9) . . ?
N1 C1 N2 112.85(12) . . ?
N1 C1 N3 111.06(11) . . ?
N1 C1 H1 111.3(10) . . ?
C3 C4 C5 112.48(13) . . ?
C7 C4 C3 120.42(13) . . ?
C7 C4 C5 127.07(14) . . ?
N3 C2 H2 115.0(9) . . ?
C3 C2 N3 122.66(13) . . ?
C3 C2 H2 122.3(9) . . ?
C32 C31 N4 120.06(13) . . ?
C32 C31 C36 121.00(14) . . ?
C36 C31 N4 118.62(13) . . ?
C4 C3 H3 122.0(10) . . ?
C2 C3 C4 122.52(13) . . ?
C2 C3 H3 115.3(10) . . ?
O3 C40 N4 121.81(14) . . ?
O3 C40 C41 121.69(14) . . ?
N4 C40 C41 116.45(13) . . ?
C9 C8 N2 120.24(13) . . ?
C13 C8 N2 118.36(13) . . ?
C13 C8 C9 121.39(15) . . ?
N5 C7 N4 113.52(12) . . ?
C4 C7 N5 119.62(13) . . ?
C4 C7 N4 126.86(13) . . ?
C13 C12 H12 120.2(11) . . ?
C11 C12 H12 118.0(11) . . ?
C11 C12 C13 121.74(14) . . ?
N3 C6 H6 116.3(10) . . ?
C5 C6 N3 122.47(13) . . ?
C5 C6 H6 121.2(10) . . ?
C22 C23 C28 122.98(13) . . ?
C24 C23 C22 118.06(14) . . ?
C24 C23 C28 118.91(14) . . ?
C46 C45 N5 119.73(14) . . ?
C50 C45 N5 119.51(13) . . ?
C50 C45 C46 120.75(14) . . ?
C23 C22 N1 118.82(13) . . ?
C27 C22 N1 119.58(13) . . ?
C27 C22 C23 121.60(14) . . ?
C45 C46 C51 122.50(14) . . ?
C47 C46 C45 118.12(15) . . ?
C47 C46 C51 119.36(14) . . ?
C31 C32 C37 123.18(14) . . ?
C33 C32 C31 118.03(14) . . ?
C33 C32 C37 118.64(14) . . ?
O2 C17 N2 120.71(15) . . ?
O2 C17 C18 120.67(13) . . ?
N2 C17 C18 118.60(13) . . ?
C22 C27 C30 124.08(14) . . ?
C26 C27 C22 117.71(14) . . ?
C26 C27 C30 118.14(14) . . ?
C4 C5 H5 120.3(11) . . ?
C6 C5 C4 122.24(14) . . ?
C6 C5 H5 117.4(11) . . ?
C45 C50 C53 121.19(14) . . ?
C49 C50 C45 118.73(14) . . ?
C49 C50 C53 120.02(14) . . ?
C27 C26 H26 119.1(10) . . ?
C25 C26 C27 122.19(15) . . ?
C25 C26 H26 118.7(10) . . ?
C32 C37 H37A 112.8(11) . . ?
C32 C37 H37B 107.9(11) . . ?
C32 C37 H37C 111.9(11) . . ?
H37A C37 H37B 108.3(15) . . ?
H37A C37 H37C 104.5(16) . . ?
H37B C37 H37C 111.5(16) . . ?
C8 C9 C14 122.37(15) . . ?
C10 C9 C8 117.78(14) . . ?
C10 C9 C14 119.85(14) . . ?
C23 C24 H24 116.5(12) . . ?
C25 C24 C23 121.63(14) . . ?
C25 C24 H24 121.8(12) . . ?
O1 C19 N1 120.53(14) . . ?
O1 C19 C18 120.83(14) . . ?
N1 C19 C18 118.55(13) . . ?
C17 C18 C19 114.95(12) . . ?
C17 C18 C21 108.71(13) . . ?
C17 C18 C20 107.55(13) . . ?
C19 C18 C21 108.42(13) . . ?
C19 C18 C20 106.99(12) . . ?
C21 C18 C20 110.19(13) . . ?
C42 C41 C40 109.58(12) . . ?
C42 C41 C44 109.87(13) . . ?
C42 C41 C43 109.81(13) . . ?
C40 C41 C44 110.10(13) . . ?
C40 C41 C43 106.96(12) . . ?
C44 C41 C43 110.47(14) . . ?
C31 C36 C39 121.22(14) . . ?
C35 C36 C31 118.58(14) . . ?
C35 C36 C39 120.20(14) . . ?
C8 C13 C16 121.74(15) . . ?
C12 C13 C8 118.34(14) . . ?
C12 C13 C16 119.91(14) . . ?
C23 C28 H28A 111.7(11) . . ?
C23 C28 H28B 109.6(13) . . ?
C23 C28 H28C 111.7(11) . . ?
H28A C28 H28B 109.0(17) . . ?
H28A C28 H28C 105.8(16) . . ?
H28B C28 H28C 108.9(17) . . ?
C9 C10 H10 119.0(11) . . ?
C9 C10 C11 122.25(14) . . ?
C11 C10 H10 118.7(11) . . ?
C12 C11 C10 118.08(15) . . ?
C12 C11 C15 120.49(14) . . ?
C10 C11 C15 121.43(15) . . ?
C32 C33 H33 117.4(10) . . ?
C34 C33 C32 122.35(15) . . ?
C34 C33 H33 120.2(10) . . ?
C26 C25 C24 118.56(14) . . ?
C26 C25 C29 120.55(15) . . ?
C24 C25 C29 120.84(15) . . ?
C50 C49 H49 118.8(11) . . ?
C50 C49 C48 122.19(15) . . ?
C48 C49 H49 119.0(11) . . ?
C36 C35 H35 119.5(10) . . ?
C36 C35 C34 121.81(15) . . ?
C34 C35 H35 118.7(10) . . ?
C33 C34 C35 117.89(15) . . ?
C33 C34 C38 120.94(16) . . ?
C35 C34 C38 121.11(16) . . ?
C9 C14 H14A 115.1(16) . . ?
C9 C14 H14B 111.3(16) . . ?
C9 C14 H14C 113(2) . . ?
H14A C14 H14B 114(2) . . ?
H14A C14 H14C 100(3) . . ?
H14B C14 H14C 104(2) . . ?
C46 C47 H47 120.6(12) . . ?
C46 C47 C48 122.54(15) . . ?
C48 C47 H47 116.8(12) . . ?
C50 C53 H53A 112.3(10) . . ?
C50 C53 H53B 109.8(11) . . ?
C50 C53 H53C 110.5(12) . . ?
H53A C53 H53B 108.9(15) . . ?
H53A C53 H53C 107.5(16) . . ?
H53B C53 H53C 107.6(17) . . ?
C46 C51 H51A 111.1(13) . . ?
C46 C51 H51B 111.4(12) . . ?
C46 C51 H51C 111.0(11) . . ?
H51A C51 H51B 104.6(18) . . ?
H51A C51 H51C 108.7(17) . . ?
H51B C51 H51C 109.7(17) . . ?
C49 C48 C47 117.59(15) . . ?
C49 C48 C52 121.09(16) . . ?
C47 C48 C52 121.33(16) . . ?
C18 C21 H21A 108.8(13) . . ?
C18 C21 H21B 108.4(12) . . ?
C18 C21 H21C 111.7(11) . . ?
H21A C21 H21B 111.1(18) . . ?
H21A C21 H21C 109.4(17) . . ?
H21B C21 H21C 107.5(16) . . ?
C27 C30 H30A 110.8(14) . . ?
C27 C30 H30B 109.0(14) . . ?
C27 C30 H30C 113.5(11) . . ?
H30A C30 H30B 109.6(19) . . ?
H30A C30 H30C 109.7(19) . . ?
H30B C30 H30C 104.1(18) . . ?
C18 C20 H20A 112.2(11) . . ?
C18 C20 H20B 110.1(12) . . ?
C18 C20 H20C 109.4(12) . . ?
H20A C20 H20B 109.2(17) . . ?
H20A C20 H20C 107.0(17) . . ?
H20B C20 H20C 108.7(18) . . ?
C36 C39 H39A 111.1(13) . . ?
C36 C39 H39B 110.6(12) . . ?
C36 C39 H39C 111.4(13) . . ?
H39A C39 H39B 110.1(18) . . ?
H39A C39 H39C 108.2(18) . . ?
H39B C39 H39C 105.3(18) . . ?
C11 C15 H15A 108.7(14) . . ?
C11 C15 H15B 112.1(15) . . ?
C11 C15 H15C 112.0(14) . . ?
H15A C15 H15B 107(2) . . ?
H15A C15 H15C 108.3(19) . . ?
H15B C15 H15C 109(2) . . ?
C41 C44 H44A 112.3(12) . . ?
C41 C44 H44B 109.4(13) . . ?
C41 C44 H44C 112.8(12) . . ?
H44A C44 H44B 108.4(18) . . ?
H44A C44 H44C 105.4(17) . . ?
H44B C44 H44C 108.3(18) . . ?
C41 C43 H43A 110.6(12) . . ?
C41 C43 H43B 108.8(13) . . ?
C41 C43 H43C 107.2(11) . . ?
H43A C43 H43B 109.1(17) . . ?
H43A C43 H43C 110.8(16) . . ?
H43B C43 H43C 110.4(17) . . ?
C25 C29 H29A 108.4(17) . . ?
C25 C29 H29B 112.8(15) . . ?
C25 C29 H29C 113(2) . . ?
H29A C29 H29B 104(2) . . ?
H29A C29 H29C 109(3) . . ?
H29B C29 H29C 109(3) . . ?
C13 C16 H16A 111.0(17) . . ?
C13 C16 H16B 110.8(13) . . ?
C13 C16 H16C 113.6(18) . . ?
H16A C16 H16B 106(2) . . ?
H16A C16 H16C 102(2) . . ?
H16B C16 H16C 114(2) . . ?
C34 C38 H38A 107(2) . . ?
C34 C38 H38B 115(2) . . ?
C34 C38 H38C 110(2) . . ?
H38A C38 H38B 100(3) . . ?
H38A C38 H38C 115(3) . . ?
H38B C38 H38C 109(3) . . ?
C48 C52 H52A 111.1(18) . . ?
C48 C52 H52B 108.6(18) . . ?
C48 C52 H52C 111.9(17) . . ?
H52A C52 H52B 111(3) . . ?
H52A C52 H52C 106(2) . . ?
H52B C52 H52C 108(2) . . ?

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
O4 C42 C41 C40 133.64(14) . . . . ?
O4 C42 C41 C44 12.5(2) . . . . ?
O4 C42 C41 C43 -109.16(16) . . . . ?
O3 C40 C41 C42 -143.71(14) . . . . ?
O3 C40 C41 C44 -22.8(2) . . . . ?
O3 C40 C41 C43 97.31(17) . . . . ?
O2 C17 C18 C19 165.71(13) . . . . ?
O2 C17 C18 C21 44.02(18) . . . . ?
O2 C17 C18 C20 -75.27(17) . . . . ?
O1 C19 C18 C17 -164.55(13) . . . . ?
O1 C19 C18 C21 -42.70(19) . . . . ?
O1 C19 C18 C20 76.11(18) . . . . ?
N5 C42 C41 C40 -46.36(16) . . . . ?
N5 C42 C41 C44 -167.45(13) . . . . ?
N5 C42 C41 C43 70.84(16) . . . . ?
N5 C45 C46 C47 176.75(12) . . . . ?
N5 C45 C46 C51 -4.6(2) . . . . ?
N5 C45 C50 C49 -177.18(12) . . . . ?
N5 C45 C50 C53 5.5(2) . . . . ?
N2 C8 C9 C10 172.35(13) . . . . ?
N2 C8 C9 C14 -8.6(2) . . . . ?
N2 C8 C13 C12 -172.45(13) . . . . ?
N2 C8 C13 C16 7.8(2) . . . . ?
N2 C17 C18 C19 -15.97(18) . . . . ?
N2 C17 C18 C21 -137.66(13) . . . . ?
N2 C17 C18 C20 103.05(15) . . . . ?
N3 C2 C3 C4 5.2(2) . . . . ?
N3 C6 C5 C4 1.3(2) . . . . ?
N4 C31 C32 C37 -4.8(2) . . . . ?
N4 C31 C32 C33 179.63(13) . . . . ?
N4 C31 C36 C35 179.22(13) . . . . ?
N4 C31 C36 C39 -0.3(2) . . . . ?
N4 C40 C41 C42 38.79(17) . . . . ?
N4 C40 C41 C44 159.74(13) . . . . ?
N4 C40 C41 C43 -80.19(16) . . . . ?
N1 C22 C27 C26 -175.02(13) . . . . ?
N1 C22 C27 C30 8.1(2) . . . . ?
N1 C19 C18 C17 19.04(18) . . . . ?
N1 C19 C18 C21 140.89(14) . . . . ?
N1 C19 C18 C20 -100.29(15) . . . . ?
C42 N5 C7 N4 29.14(18) . . . . ?
C42 N5 C7 C4 -150.42(14) . . . . ?
C42 N5 C45 C46 67.49(17) . . . . ?
C42 N5 C45 C50 -112.82(15) . . . . ?
C1 N2 C8 C9 -100.56(15) . . . . ?
C1 N2 C8 C13 77.95(16) . . . . ?
C1 N2 C17 O2 -174.92(13) . . . . ?
C1 N2 C17 C18 6.8(2) . . . . ?
C1 N3 C2 C3 -174.19(14) . . . . ?
C1 N3 C6 C5 171.04(14) . . . . ?
C1 N1 C22 C23 -68.22(17) . . . . ?
C1 N1 C22 C27 111.53(15) . . . . ?
C1 N1 C19 O1 170.34(13) . . . . ?
C1 N1 C19 C18 -13.2(2) . . . . ?
C2 N3 C1 N2 72.40(17) . . . . ?
C2 N3 C1 N1 -54.32(17) . . . . ?
C2 N3 C6 C5 -1.9(2) . . . . ?
C31 N4 C40 O3 -11.0(2) . . . . ?
C31 N4 C40 C41 166.54(12) . . . . ?
C31 N4 C7 N5 159.94(13) . . . . ?
C31 N4 C7 C4 -20.5(2) . . . . ?
C31 C32 C33 C34 3.7(2) . . . . ?
C31 C36 C35 C34 -1.1(2) . . . . ?
C3 C4 C7 N5 21.0(2) . . . . ?
C3 C4 C7 N4 -158.47(14) . . . . ?
C3 C4 C5 C6 2.1(2) . . . . ?
C40 N4 C31 C32 93.64(16) . . . . ?
C40 N4 C31 C36 -79.93(16) . . . . ?
C40 N4 C7 N5 -37.47(18) . . . . ?
C40 N4 C7 C4 142.05(15) . . . . ?
C8 N2 C1 N3 63.68(15) . . . . ?
C8 N2 C1 N1 -170.58(11) . . . . ?
C8 N2 C17 O2 -4.3(2) . . . . ?
C8 N2 C17 C18 177.38(12) . . . . ?
C8 C9 C10 C11 0.8(2) . . . . ?
C7 N5 C42 O4 -166.74(13) . . . . ?
C7 N5 C42 C41 13.26(18) . . . . ?
C7 N5 C45 C46 -124.46(14) . . . . ?
C7 N5 C45 C50 55.24(18) . . . . ?
C7 N4 C31 C32 -103.00(16) . . . . ?
C7 N4 C31 C36 83.43(18) . . . . ?
C7 N4 C40 O3 -175.14(13) . . . . ?
C7 N4 C40 C41 2.36(19) . . . . ?
C7 C4 C3 C2 176.50(15) . . . . ?
C7 C4 C5 C6 -179.82(15) . . . . ?
C6 N3 C1 N2 -100.19(15) . . . . ?
C6 N3 C1 N1 133.09(13) . . . . ?
C6 N3 C2 C3 -1.4(2) . . . . ?
C23 C22 C27 C26 4.7(2) . . . . ?
C23 C22 C27 C30 -172.13(15) . . . . ?
C23 C24 C25 C26 2.5(2) . . . . ?
C23 C24 C25 C29 -179.98(15) . . . . ?
C45 N5 C42 O4 1.1(2) . . . . ?
C45 N5 C42 C41 -178.87(12) . . . . ?
C45 N5 C7 N4 -138.52(13) . . . . ?
C45 N5 C7 C4 41.91(19) . . . . ?
C45 C46 C47 C48 1.2(2) . . . . ?
C45 C50 C49 C48 -0.3(2) . . . . ?
C22 N1 C1 N2 173.24(11) . . . . ?
C22 N1 C1 N3 -60.83(15) . . . . ?
C22 N1 C19 O1 0.4(2) . . . . ?
C22 N1 C19 C18 176.78(12) . . . . ?
C22 C23 C24 C25 1.7(2) . . . . ?
C22 C27 C26 C25 -0.3(2) . . . . ?
C46 C45 C50 C49 2.5(2) . . . . ?
C46 C45 C50 C53 -174.85(14) . . . . ?
C46 C47 C48 C49 0.9(2) . . . . ?
C46 C47 C48 C52 -179.32(16) . . . . ?
C32 C31 C36 C35 5.7(2) . . . . ?
C32 C31 C36 C39 -173.77(15) . . . . ?
C32 C33 C34 C35 0.8(2) . . . . ?
C32 C33 C34 C38 178.07(16) . . . . ?
C17 N2 C1 N3 -125.24(14) . . . . ?
C17 N2 C1 N1 0.50(19) . . . . ?
C17 N2 C8 C9 87.67(16) . . . . ?
C17 N2 C8 C13 -93.82(16) . . . . ?
C27 C26 C25 C24 -3.2(2) . . . . ?
C27 C26 C25 C29 179.26(16) . . . . ?
C5 C4 C3 C2 -5.3(2) . . . . ?
C5 C4 C7 N5 -156.87(14) . . . . ?
C5 C4 C7 N4 23.6(2) . . . . ?
C50 C45 C46 C47 -2.9(2) . . . . ?
C50 C45 C46 C51 175.67(13) . . . . ?
C50 C49 C48 C47 -1.3(2) . . . . ?
C50 C49 C48 C52 178.85(16) . . . . ?
C37 C32 C33 C34 -172.08(15) . . . . ?
C9 C8 C13 C12 6.0(2) . . . . ?
C9 C8 C13 C16 -173.72(15) . . . . ?
C9 C10 C11 C12 4.3(2) . . . . ?
C9 C10 C11 C15 -175.21(14) . . . . ?
C24 C23 C22 N1 174.35(13) . . . . ?
C24 C23 C22 C27 -5.4(2) . . . . ?
C19 N1 C1 N2 2.98(19) . . . . ?
C19 N1 C1 N3 128.90(14) . . . . ?
C19 N1 C22 C23 102.84(16) . . . . ?
C19 N1 C22 C27 -77.41(17) . . . . ?
C36 C31 C32 C37 168.58(14) . . . . ?
C36 C31 C32 C33 -7.0(2) . . . . ?
C36 C35 C34 C33 -2.1(2) . . . . ?
C36 C35 C34 C38 -179.40(16) . . . . ?
C13 C8 C9 C10 -6.1(2) . . . . ?
C13 C8 C9 C14 172.92(14) . . . . ?
C13 C12 C11 C10 -4.4(2) . . . . ?
C13 C12 C11 C15 175.12(14) . . . . ?
C28 C23 C22 N1 -8.3(2) . . . . ?
C28 C23 C22 C27 171.94(15) . . . . ?
C28 C23 C24 C25 -175.74(15) . . . . ?
C11 C12 C13 C8 -0.6(2) . . . . ?
C11 C12 C13 C16 179.14(15) . . . . ?
C14 C9 C10 C11 -178.25(14) . . . . ?
C53 C50 C49 C48 177.07(15) . . . . ?
C51 C46 C47 C48 -177.43(14) . . . . ?
C30 C27 C26 C25 176.70(16) . . . . ?
C39 C36 C35 C34 178.44(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3231-3229-3227-3225
_database_code_depnum_ccdc_archive 'CCDC 2201798'
loop_
_audit_author_name
_audit_author_address
'Eric Reinheimer'
;Rigaku Oxford Diffraction
United States of America
;
_audit_update_record             
;
2022-08-16 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_audit_creation_date             2022-07-30
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H40 N2 O2'
_chemical_formula_sum            'C30 H40 N2 O2'
_chemical_formula_weight         460.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.56(13)
_cell_length_b                   19.48(12)
_cell_length_c                   15.5(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.1(2)
_cell_angle_gamma                90
_cell_volume                     2879(67)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1779
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.8710
_cell_measurement_theta_min      0.1170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.002
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.00015
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2406
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22427
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        0.749
_diffrn_reflns_theta_max         0.749
_diffrn_reflns_theta_min         0.099
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00  50.00   0.25    1.00    --    0.00   0.00   0.00  380
  2  ω    -35.00  75.00   0.25    0.50    --    0.00   0.00   0.00  440
  3  ω    -65.00  23.00   0.25    1.00    --    0.00   0.00   0.00  352
  4  ω    -15.00  60.00   0.25    1.00    --    0.00   0.00   0.00  300
;
_diffrn_measurement_device       'Electron diffractometer'
_diffrn_measurement_device_type  Synergy-ED
_diffrn_measurement_method       'continuous rotation'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0002066000
_diffrn_orient_matrix_UB_12      0.0001104000
_diffrn_orient_matrix_UB_13      0.0016044000
_diffrn_orient_matrix_UB_21      -0.0023058000
_diffrn_orient_matrix_UB_22      -0.0006113000
_diffrn_orient_matrix_UB_23      -0.0001489000
_diffrn_orient_matrix_UB_31      0.0012393000
_diffrn_orient_matrix_UB_32      -0.0011296000
_diffrn_orient_matrix_UB_33      0.0002211000
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200 keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'thermionic-emission electron gun'
_diffrn_source_type              LaB6
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2054
_reflns_number_total             3387
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       85(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   2.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2325
_refine_ls_R_factor_gt           0.1648
_refine_ls_restrained_S_all      2.063
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3778
_refine_ls_wR_factor_ref         0.4084
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7A,H7B), C4(H4A,H4B), C6(H6A,H6B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C23(H23), C25(H25)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C19(H19A,
 H19B,H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2208(7) 0.7302(5) 0.2939(5) 0.050(3) Uani 1 1 d . . . . .
H1 H 0.215483 0.739479 0.363637 0.061 Uiso 1 1 calc R U . . .
C21 C 0.3909(8) 0.8313(6) 0.3018(6) 0.059(3) Uani 1 1 d . . . . .
N1 N 0.0785(7) 0.7083(5) 0.2628(5) 0.056(2) Uani 1 1 d . . . . .
N2 N 0.2673(8) 0.7968(5) 0.2578(6) 0.063(3) Uani 1 1 d . . . . .
C15 C -0.0888(9) 0.5395(6) 0.3235(7) 0.070(3) Uani 1 1 d . . . . .
H15 H -0.113176 0.488906 0.294796 0.084 Uiso 1 1 calc R U . . .
C13 C -0.1022(8) 0.6205(7) 0.4408(6) 0.068(3) Uani 1 1 d . . . . .
H13 H -0.137971 0.633372 0.504778 0.081 Uiso 1 1 calc R U . . .
C10 C 0.2009(9) 0.8318(6) 0.1861(6) 0.062(3) Uani 1 1 d . . . . .
C11 C 0.0055(8) 0.6569(5) 0.3071(6) 0.055(3) Uani 1 1 d . . . . .
C22 C 0.3742(9) 0.8650(6) 0.3817(6) 0.073(3) Uani 1 1 d . . . . .
C26 C 0.5218(9) 0.8300(6) 0.2667(6) 0.063(3) Uani 1 1 d . . . . .
C14 C -0.1235(8) 0.5518(7) 0.4092(7) 0.077(4) Uani 1 1 d . . . . .
C29 C 0.5457(9) 0.8000(7) 0.1768(6) 0.089(4) Uani 1 1 d . . . . .
H29A H 0.452431 0.770935 0.152638 0.134 Uiso 1 1 calc R U . . .
H29B H 0.637278 0.765693 0.181978 0.134 Uiso 1 1 calc R U . . .
H29C H 0.564615 0.842096 0.131702 0.134 Uiso 1 1 calc R U . . .
C12 C -0.0397(8) 0.6709(5) 0.3956(6) 0.060(3) Uani 1 1 d . . . . .
C9 C 0.0660(8) 0.7953(6) 0.1410(6) 0.062(3) Uani 1 1 d . . . . .
C2 C 0.3394(9) 0.6725(5) 0.2871(6) 0.061(3) Uani 1 1 d . . . . .
H2 H 0.438516 0.699621 0.304112 0.073 Uiso 1 1 calc R U . . .
C8 C -0.0020(9) 0.7413(6) 0.1927(7) 0.071(3) Uani 1 1 d . . . . .
C16 C -0.0249(9) 0.5887(7) 0.2732(6) 0.077(3) Uani 1 1 d . . . . .
C30 C 0.1014(10) 0.7647(7) 0.0508(6) 0.082(4) Uani 1 1 d . . . . .
H30A H 0.146076 0.805296 0.011767 0.123 Uiso 1 1 calc R U . . .
H30B H 0.005025 0.744830 0.016690 0.123 Uiso 1 1 calc R U . . .
H30C H 0.177811 0.722805 0.061193 0.123 Uiso 1 1 calc R U . . .
C23 C 0.4959(11) 0.8961(6) 0.4264(7) 0.080(3) Uani 1 1 d . . . . .
H23 H 0.481207 0.923412 0.487171 0.096 Uiso 1 1 calc R U . . .
C25 C 0.6387(8) 0.8617(7) 0.3136(7) 0.080(4) Uani 1 1 d . . . . .
H25 H 0.740074 0.861843 0.284160 0.097 Uiso 1 1 calc R U . . .
C24 C 0.6314(11) 0.8937(7) 0.3977(8) 0.093(4) Uani 1 1 d . . . . .
C17 C -0.0364(13) 0.7461(7) 0.4290(9) 0.108(4) Uani 1 1 d . . . . .
H17A H -0.128441 0.755455 0.466104 0.162 Uiso 1 1 calc R U . . .
H17B H -0.038331 0.781531 0.373686 0.162 Uiso 1 1 calc R U . . .
H17C H 0.059793 0.754448 0.470932 0.162 Uiso 1 1 calc R U . . .
O2 O 0.2480(9) 0.8844(7) 0.1598(7) 0.088(3) Uani 1 1 d . . . . .
C18 C -0.1937(9) 0.4988(6) 0.4645(7) 0.088(4) Uani 1 1 d . . . . .
H18A H -0.308309 0.503809 0.454241 0.132 Uiso 1 1 calc R U . . .
H18B H -0.161478 0.507574 0.533163 0.132 Uiso 1 1 calc R U . . .
H18C H -0.162071 0.446914 0.445803 0.132 Uiso 1 1 calc R U . . .
C3 C 0.3336(11) 0.6148(7) 0.3577(8) 0.099(4) Uani 1 1 d . . . . .
H3A H 0.241156 0.582067 0.343023 0.119 Uiso 1 1 calc R U . . .
H3B H 0.324618 0.638193 0.421661 0.119 Uiso 1 1 calc R U . . .
C7 C 0.3568(10) 0.6433(7) 0.1974(6) 0.080(3) Uani 1 1 d . . . . .
H7A H 0.365821 0.685887 0.151431 0.096 Uiso 1 1 calc R U . . .
H7B H 0.262924 0.613438 0.176353 0.096 Uiso 1 1 calc R U . . .
O1 O -0.1247(8) 0.7260(7) 0.1760(7) 0.112(4) Uani 1 1 d . . . . .
C20 C -0.0445(10) 0.8559(7) 0.1230(8) 0.096(4) Uani 1 1 d . . . . .
H20A H -0.070491 0.878635 0.184803 0.145 Uiso 1 1 calc R U . . .
H20B H -0.140311 0.835367 0.088792 0.145 Uiso 1 1 calc R U . . .
H20C H 0.001133 0.895484 0.082840 0.145 Uiso 1 1 calc R U . . .
C4 C 0.4707(11) 0.5701(9) 0.3587(9) 0.113(5) Uani 1 1 d . . . . .
H4A H 0.561319 0.600685 0.383981 0.136 Uiso 1 1 calc R U . . .
H4B H 0.461121 0.525349 0.401135 0.136 Uiso 1 1 calc R U . . .
C27 C 0.2290(12) 0.8797(9) 0.4175(9) 0.123(5) Uani 1 1 d . . . . .
H27A H 0.165388 0.911316 0.370803 0.185 Uiso 1 1 calc R U . . .
H27B H 0.244424 0.907310 0.479405 0.185 Uiso 1 1 calc R U . . .
H27C H 0.174762 0.830879 0.427642 0.185 Uiso 1 1 calc R U . . .
C28 C 0.7558(13) 0.9263(7) 0.4425(9) 0.119(5) Uani 1 1 d . . . . .
H28A H 0.721965 0.964092 0.489491 0.178 Uiso 1 1 calc R U . . .
H28B H 0.817470 0.952207 0.394893 0.178 Uiso 1 1 calc R U . . .
H28C H 0.820670 0.886742 0.476679 0.178 Uiso 1 1 calc R U . . .
C6 C 0.4903(14) 0.5959(9) 0.1955(10) 0.124(5) Uani 1 1 d . . . . .
H6A H 0.488342 0.568604 0.133214 0.148 Uiso 1 1 calc R U . . .
H6B H 0.585699 0.627568 0.201792 0.148 Uiso 1 1 calc R U . . .
C19 C 0.0002(15) 0.5715(9) 0.1791(8) 0.137(6) Uani 1 1 d . . . . .
H19A H 0.098942 0.542804 0.176919 0.206 Uiso 1 1 calc R U . . .
H19B H 0.006593 0.619293 0.141802 0.206 Uiso 1 1 calc R U . . .
H19C H -0.087085 0.539990 0.150997 0.206 Uiso 1 1 calc R U . . .
C5 C 0.4929(16) 0.5461(10) 0.2662(12) 0.142(6) Uani 1 1 d . . . . .
H5A H 0.594851 0.519775 0.268171 0.170 Uiso 1 1 calc R U . . .
H5B H 0.412275 0.507289 0.248761 0.170 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 1.1000 . ?
C1 N1 1.47(2) . ?
C1 N2 1.493(15) . ?
C1 C2 1.605(17) . ?
C21 N2 1.482(18) . ?
C21 C22 1.42(2) . ?
C21 C26 1.40(2) . ?
N1 C11 1.423(15) . ?
N1 C8 1.44(2) . ?
N2 C10 1.41(2) . ?
C15 H15 1.1000 . ?
C15 C14 1.41(3) . ?
C15 C16 1.402(17) . ?
C13 H13 1.1000 . ?
C13 C14 1.435(18) . ?
C13 C12 1.368(16) . ?
C10 C9 1.59(2) . ?
C10 O2 1.203(14) . ?
C11 C12 1.49(3) . ?
C11 C16 1.451(17) . ?
C22 C23 1.444(19) . ?
C22 C27 1.56(2) . ?
C26 C29 1.54(3) . ?
C26 C25 1.429(18) . ?
C14 C18 1.526(18) . ?
C29 H29A 1.1001 . ?
C29 H29B 1.1001 . ?
C29 H29C 1.1001 . ?
C12 C17 1.553(18) . ?
C9 C8 1.498(17) . ?
C9 C30 1.58(3) . ?
C9 C20 1.596(18) . ?
C2 H2 1.1000 . ?
C2 C3 1.57(2) . ?
C2 C7 1.52(3) . ?
C8 O1 1.220(19) . ?
C16 C19 1.53(3) . ?
C30 H30A 1.1001 . ?
C30 H30B 1.1001 . ?
C30 H30C 1.1001 . ?
C23 H23 1.1000 . ?
C23 C24 1.40(2) . ?
C25 H25 1.1000 . ?
C25 C24 1.45(3) . ?
C24 C28 1.48(2) . ?
C17 H17A 1.1001 . ?
C17 H17B 1.1001 . ?
C17 H17C 1.1001 . ?
C18 H18A 1.1001 . ?
C18 H18B 1.1001 . ?
C18 H18C 1.1001 . ?
C3 H3A 1.1000 . ?
C3 H3B 1.1000 . ?
C3 C4 1.57(2) . ?
C7 H7A 1.1000 . ?
C7 H7B 1.1000 . ?
C7 C6 1.58(2) . ?
C20 H20A 1.1001 . ?
C20 H20B 1.1001 . ?
C20 H20C 1.1001 . ?
C4 H4A 1.1000 . ?
C4 H4B 1.1000 . ?
C4 C5 1.54(3) . ?
C27 H27A 1.1001 . ?
C27 H27B 1.1001 . ?
C27 H27C 1.1001 . ?
C28 H28A 1.1001 . ?
C28 H28B 1.1001 . ?
C28 H28C 1.1001 . ?
C6 H6A 1.1000 . ?
C6 H6B 1.1000 . ?
C6 C5 1.46(2) . ?
C19 H19A 1.1001 . ?
C19 H19B 1.1001 . ?
C19 H19C 1.1001 . ?
C5 H5A 1.1000 . ?
C5 H5B 1.1000 . ?

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
N1 C1 H1 105.2 . . ?
N1 C1 N2 115.0(8) . . ?
N1 C1 C2 114.5(10) . . ?
N2 C1 H1 105.2 . . ?
N2 C1 C2 110.7(9) . . ?
C2 C1 H1 105.2 . . ?
C22 C21 N2 118.3(9) . . ?
C26 C21 N2 121.2(12) . . ?
C26 C21 C22 120.4(9) . . ?
C11 N1 C1 121.3(10) . . ?
C11 N1 C8 115.0(10) . . ?
C8 N1 C1 123.3(9) . . ?
C21 N2 C1 118.0(10) . . ?
C10 N2 C1 125.7(9) . . ?
C10 N2 C21 116.2(10) . . ?
C14 C15 H15 118.4 . . ?
C16 C15 H15 118.4 . . ?
C16 C15 C14 123.3(12) . . ?
C14 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
C12 C13 C14 123.4(12) . . ?
N2 C10 C9 115.8(10) . . ?
O2 C10 N2 121.2(11) . . ?
O2 C10 C9 123.0(11) . . ?
N1 C11 C12 119.9(10) . . ?
N1 C11 C16 124.2(11) . . ?
C16 C11 C12 115.8(9) . . ?
C21 C22 C23 118.3(10) . . ?
C21 C22 C27 123.7(9) . . ?
C23 C22 C27 117.4(13) . . ?
C21 C26 C29 123.5(9) . . ?
C21 C26 C25 118.9(13) . . ?
C25 C26 C29 117.4(10) . . ?
C15 C14 C13 116.2(11) . . ?
C15 C14 C18 123.7(13) . . ?
C13 C14 C18 119.8(13) . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C13 C12 C11 120.4(11) . . ?
C13 C12 C17 120.3(12) . . ?
C11 C12 C17 118.6(10) . . ?
C10 C9 C20 104.6(11) . . ?
C8 C9 C10 116.6(11) . . ?
C8 C9 C30 109.8(12) . . ?
C8 C9 C20 107.8(10) . . ?
C30 C9 C10 109.8(10) . . ?
C30 C9 C20 107.8(10) . . ?
C1 C2 H2 104.4 . . ?
C3 C2 C1 113.3(9) . . ?
C3 C2 H2 104.4 . . ?
C7 C2 C1 116.4(8) . . ?
C7 C2 H2 104.4 . . ?
C7 C2 C3 112.3(13) . . ?
N1 C8 C9 119.2(11) . . ?
O1 C8 N1 120.4(11) . . ?
O1 C8 C9 120.4(11) . . ?
C15 C16 C11 120.6(12) . . ?
C15 C16 C19 118.9(13) . . ?
C11 C16 C19 120.3(11) . . ?
C9 C30 H30A 109.5 . . ?
C9 C30 H30B 109.5 . . ?
C9 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C22 C23 H23 117.7 . . ?
C24 C23 C22 124.5(13) . . ?
C24 C23 H23 117.7 . . ?
C26 C25 H25 118.1 . . ?
C26 C25 C24 123.7(10) . . ?
C24 C25 H25 118.1 . . ?
C23 C24 C25 113.8(10) . . ?
C23 C24 C28 124.7(15) . . ?
C25 C24 C28 121.2(13) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C2 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C2 C3 C4 109.4(10) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C2 C7 H7A 109.2 . . ?
C2 C7 H7B 109.2 . . ?
C2 C7 C6 112.2(9) . . ?
H7A C7 H7B 107.9 . . ?
C6 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
C9 C20 H20A 109.5 . . ?
C9 C20 H20B 109.5 . . ?
C9 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
C5 C4 C3 109.2(10) . . ?
C5 C4 H4A 109.8 . . ?
C5 C4 H4B 109.8 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C7 C6 H6A 109.6 . . ?
C7 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C5 C6 C7 110.2(11) . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C4 C5 H5A 107.3 . . ?
C4 C5 H5B 107.3 . . ?
C6 C5 C4 120.1(17) . . ?
C6 C5 H5A 107.3 . . ?
C6 C5 H5B 107.3 . . ?
H5A C5 H5B 106.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C11 C12 66.8(13) . . . . ?
C1 N1 C11 C16 -110.6(13) . . . . ?
C1 N1 C8 C9 7.6(13) . . . . ?
C1 N1 C8 O1 -171.8(11) . . . . ?
C1 N2 C10 C9 -0.6(12) . . . . ?
C1 N2 C10 O2 -177.8(10) . . . . ?
C1 C2 C3 C4 -168.0(10) . . . . ?
C1 C2 C7 C6 171.2(10) . . . . ?
C21 N2 C10 C9 -178.4(7) . . . . ?
C21 N2 C10 O2 4.3(14) . . . . ?
C21 C22 C23 C24 -1.8(18) . . . . ?
C21 C26 C25 C24 2.0(17) . . . . ?
N1 C1 N2 C21 164.3(7) . . . . ?
N1 C1 N2 C10 -13.5(12) . . . . ?
N1 C1 C2 C3 -74.6(13) . . . . ?
N1 C1 C2 C7 57.9(11) . . . . ?
N1 C11 C12 C13 -175.9(8) . . . . ?
N1 C11 C12 C17 13.7(13) . . . . ?
N1 C11 C16 C15 175.5(8) . . . . ?
N1 C11 C16 C19 -10.1(15) . . . . ?
N2 C1 N1 C11 -163.0(8) . . . . ?
N2 C1 N1 C8 10.0(11) . . . . ?
N2 C1 C2 C3 153.5(8) . . . . ?
N2 C1 C2 C7 -74.1(12) . . . . ?
N2 C21 C22 C23 177.4(10) . . . . ?
N2 C21 C22 C27 -11.7(17) . . . . ?
N2 C21 C26 C29 6.4(16) . . . . ?
N2 C21 C26 C25 -177.5(10) . . . . ?
N2 C10 C9 C8 18.2(12) . . . . ?
N2 C10 C9 C30 -107.4(13) . . . . ?
N2 C10 C9 C20 137.1(9) . . . . ?
C10 C9 C8 N1 -21.7(13) . . . . ?
C10 C9 C8 O1 157.6(11) . . . . ?
C11 N1 C8 C9 -179.0(8) . . . . ?
C11 N1 C8 O1 1.7(15) . . . . ?
C22 C21 N2 C1 -74.9(14) . . . . ?
C22 C21 N2 C10 103.1(13) . . . . ?
C22 C21 C26 C29 -174.5(10) . . . . ?
C22 C21 C26 C25 1.5(15) . . . . ?
C22 C23 C24 C25 4.9(18) . . . . ?
C22 C23 C24 C28 179.1(12) . . . . ?
C26 C21 N2 C1 104.2(13) . . . . ?
C26 C21 N2 C10 -77.8(14) . . . . ?
C26 C21 C22 C23 -1.7(15) . . . . ?
C26 C21 C22 C27 169.2(12) . . . . ?
C26 C25 C24 C23 -5.1(17) . . . . ?
C26 C25 C24 C28 -179.4(12) . . . . ?
C14 C15 C16 C11 -1.9(14) . . . . ?
C14 C15 C16 C19 -176.4(10) . . . . ?
C14 C13 C12 C11 2.5(14) . . . . ?
C14 C13 C12 C17 172.7(10) . . . . ?
C29 C26 C25 C24 178.3(11) . . . . ?
C12 C13 C14 C15 -6.1(13) . . . . ?
C12 C13 C14 C18 179.8(8) . . . . ?
C12 C11 C16 C15 -2.0(12) . . . . ?
C12 C11 C16 C19 172.4(10) . . . . ?
C2 C1 N1 C11 67.1(13) . . . . ?
C2 C1 N1 C8 -119.8(12) . . . . ?
C2 C1 N2 C21 -64.0(13) . . . . ?
C2 C1 N2 C10 118.2(12) . . . . ?
C2 C3 C4 C5 -51.5(17) . . . . ?
C2 C7 C6 C5 49.0(19) . . . . ?
C8 N1 C11 C12 -106.8(12) . . . . ?
C8 N1 C11 C16 75.8(14) . . . . ?
C16 C15 C14 C13 5.8(13) . . . . ?
C16 C15 C14 C18 179.7(8) . . . . ?
C16 C11 C12 C13 1.7(12) . . . . ?
C16 C11 C12 C17 -168.7(9) . . . . ?
C30 C9 C8 N1 104.0(12) . . . . ?
C30 C9 C8 O1 -76.7(15) . . . . ?
O2 C10 C9 C8 -164.6(11) . . . . ?
O2 C10 C9 C30 69.7(16) . . . . ?
O2 C10 C9 C20 -45.7(14) . . . . ?
C3 C2 C7 C6 -55.9(13) . . . . ?
C3 C4 C5 C6 51.5(19) . . . . ?
C7 C2 C3 C4 57.5(12) . . . . ?
C7 C6 C5 C4 -49(2) . . . . ?
C20 C9 C8 N1 -138.9(11) . . . . ?
C20 C9 C8 O1 40.4(15) . . . . ?
C27 C22 C23 C24 -173.3(13) . . . . ?

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

# start Validation Reply Form
_vrf_THETM01_3231-3229-3227-3225 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength =    0.5208  
RESPONSE: This is a dataset completed using electron diffraction.  
The wavelength is different from that conventional X-ray.  Based on
NMR, the structural model is correct.
;
_vrf_RINTA01_3231-3229-3227-3225 
;
PROBLEM: The value of Rint is greater than 0.18
            Rint given   0.241  
RESPONSE: This is a dataset completed using electron diffraction.  
Based on NMR, the structural model is correct.
;
_vrf_PLAT020_3231-3229-3227-3225 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.241 Report  
RESPONSE: This is a dataset completed using electron diffraction.  
Based on NMR, the structural model is correct.
;
_vrf_PLAT082_3231-3229-3227-3225 
;
PROBLEM: High R1 Value ..................................       0.16 Report  
RESPONSE: This is a dataset completed using electron diffraction.  
Based on NMR, the structural model is correct.
;
_vrf_PLAT084_3231-3229-3227-3225 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.41 Report  
RESPONSE: This is a dataset completed using electron diffraction.  
Based on NMR, the structural model is correct.
;
_vrf_PLAT149_3231-3229-3227-3225 
;
PROBLEM:  s.u. on the   beta    Angle is Too Large .......       0.20 Degree  
RESPONSE: This is a dataset completed using electron diffraction.  
Based on NMR, the structural model is correct.
;
_vrf_PLAT340_3231-3229-3227-3225 
;
PROBLEM:  Low Bond Precision on  C-C Bonds ...............    0.03138 Ang.  
RESPONSE: This is a dataset completed using electron diffraction.  
Based on NMR, the structural model is correct.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_proc_notwin
_database_code_depnum_ccdc_archive 'CCDC 2201799'
loop_
_audit_author_name
_audit_author_address
'Eric Reinheimer'
;Rigaku Oxford Diffraction
United States of America
;
_audit_update_record             
;
2022-08-16 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_audit_creation_date             2022-08-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C58 H63 Br N4 O4'
_chemical_formula_sum            'C58 H63 Br N4 O4'
_chemical_formula_weight         960.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   14.89710(10)
_cell_length_b                   23.3372(2)
_cell_length_c                   33.3618(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.4690(10)
_cell_angle_gamma                90
_cell_volume                     11587.68(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    22348
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.9920
_cell_measurement_theta_min      3.5170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.1d (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4048
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 -1 -1 0.0893
0 -12 14 0.0385
10 -1 3 0.0783
7 9 -9 0.0825
-2 11 -14 0.0606
-9 5 0 0.0872
0 -2 21 0.0467
-1 3 -21 0.0502
-9 7 0 0.0914
6 -2 16 0.0799
8 -6 7 0.0761
7 -8 -9 0.0793
-1 -4 -21 0.0523
0 3 5 0.0627
0 -3 -5 0.0627
0 -1 0 0.0467

_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            31898
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         5.841
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  45.00   0.50    1.96    --   46.72 -19.00   0.00  118
  2  ω     28.00  98.00   0.50    7.83    --   99.96 -94.00   0.00  140
  3  ω     31.00  57.00   0.50    7.83    --   99.96 -30.00   0.00   52
  4  ω     26.00  54.00   0.50    7.83    --   99.96 -30.00  60.00   56
  5  ω     23.00  55.00   0.50    7.83    --   99.96 -30.00 120.00   64
  6  ω     25.00  51.00   0.50    7.83    --   99.96 -15.00 120.00   52
  7  ω     23.00  79.00   0.50    7.83    --   99.96 -45.00  60.00  112
  8  ω     25.00  50.00   0.50    7.83    --   99.96 -15.00   0.00   50
  9  ω     25.00  57.00   0.50    7.83    --   99.96 -30.00 -60.00   64
 10  ω     22.00  56.00   0.50    7.83    --   99.96 -30.00-120.00   68
 11  ω     22.00  54.00   0.50    7.83    --   99.96 -15.00 -90.00   64
 12  ω     29.00  54.00   0.50    7.83    --   99.96 -15.00-120.00   50
 13  ω     19.00  44.00   0.50    7.83    --   99.96 -15.00-150.00   50
 14  ω     68.00 113.00   0.50    7.83    --   99.96-111.00-180.00   90
 15  ω     17.00  43.00   0.50    7.83    --   99.96 -15.00  30.00   52
 16  ω     17.00  50.00   0.50    7.83    --   99.96 -15.00  90.00   66
 17  ω     20.00 112.00   0.50    7.83    --   99.96-111.00  60.00  184
 18  ω    -32.00  94.00   0.50    1.96    --   46.72   0.00-120.00  252
 19  ω    -68.00 -21.00   0.50    7.83    --  -84.50  61.00-180.00   94
 20  ω   -126.00 -86.00   0.50    1.96    --  -46.72 -99.00  90.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9552
_reflns_number_total             10182
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.1d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.1d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.1d (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         10182
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0518
_refine_ls_restrained_S_all      1.068
_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)+(0.0567P)²+25.9344P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1389
_refine_special_details          ?
_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. Uiso/Uaniso restraints and constraints
C5B \\sim C3A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C5A \\sim C2B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C11A \\sim C8B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C9A \\sim C10B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C10B \\sim C9B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C12A) = Uanis(C6B)
Uanis(C6A) = Uanis(C3B)
3. Rigid body (RIGU) restrains
 Br1A, C5A, C3A, C2A, C12A, C7A, C6A, C8A, C9A, C10A, C11A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: Br1A(0.5) Br1B(0.5) C2B(0.5) H2B(0.5) C5B(0.5) H5B(0.5) C3B(0.5)
 H3B(0.5) C6B(0.5) H6B(0.5) C12B(0.5) C7B(0.5) C11B(0.5) C8B(0.5) H8B(0.5)
 C9B(0.5) H9B(0.5) C10B(0.5) H10B(0.5) C5A(0.5) H5A(0.5) C3A(0.5) H3A(0.5)
 C2A(0.5) H2A(0.5) C12A(0.5) C7A(0.5) C6A(0.5) H6A(0.5) C8A(0.5) H8A(0.5)
 C9A(0.5) H9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5)
5.a Ternary CH refined with riding coordinates:
 C2B(H2B), C5B(H5B), C3B(H3B), C6B(H6B), C5A(H5A), C3A(H3A), C2A(H2A), C6A(H6A)
5.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C17(H17), C38(H38), C15(H15), C52(H52), C31(H31), C29(H29),
 C54(H54), C8B(H8B), C9B(H9B), C10B(H10B), C8A(H8A), C9A(H9A), C10A(H10A)
5.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C26(H26A,H26B,
 H26C), C56(H56A,H56B,H56C), C35(H35A,H35B,H35C), C58(H58A,H58B,H58C), C48(H48A,
 H48B,H48C), C33(H33A,H33B,H33C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C),
 C19(H19A,H19B,H19C), C43(H43A,H43B,H43C), C20(H20A,H20B,H20C), C57(H57A,H57B,
 H57C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1A Br 0.42615(3) 0.84482(2) 0.28491(2) 0.03284(12) Uani 0.5 1 d . U P A 1
Br1B Br 0.69730(4) 0.65561(3) 0.26839(2) 0.04577(15) Uani 0.5 1 d . . P B 2
O4 O 0.85468(10) 0.60355(7) 0.41908(5) 0.0309(3) Uani 1 1 d . . . . .
O3 O 0.82050(11) 0.79781(7) 0.41272(6) 0.0395(4) Uani 1 1 d . . . . .
O2 O 0.24047(11) 0.61599(8) 0.32400(5) 0.0410(4) Uani 1 1 d . . . . .
O1 O 0.17361(11) 0.76524(10) 0.40181(5) 0.0477(5) Uani 1 1 d . . . . .
N4 N 0.71554(12) 0.64137(8) 0.40791(5) 0.0260(4) Uani 1 1 d . . . . .
N3 N 0.69787(12) 0.74323(8) 0.39840(6) 0.0267(4) Uani 1 1 d . . . . .
N2 N 0.35862(12) 0.66457(8) 0.35267(6) 0.0286(4) Uani 1 1 d . . . . .
N1 N 0.32057(12) 0.74196(9) 0.39740(6) 0.0313(4) Uani 1 1 d . . . . .
C4 C 0.65778(14) 0.68722(10) 0.39096(6) 0.0250(4) Uani 1 1 d . . . . .
C45 C 0.80787(14) 0.64449(10) 0.40872(6) 0.0250(4) Uani 1 1 d . . . . .
C2B C 0.558(3) 0.6731(18) 0.3905(10) 0.0240(12) Uani 0.5 1 d . U P B 2
H2B H 0.5447 0.6375 0.4046 0.029 Uiso 0.5 1 calc R U P B 2
C5B C 0.485(3) 0.7213(14) 0.3950(11) 0.0253(13) Uani 0.5 1 d . U P B 2
H5B H 0.4889 0.7435 0.4200 0.030 Uiso 0.5 1 calc R U P B 2
C3B C 0.6046(11) 0.6641(5) 0.3531(4) 0.0240(9) Uani 0.5 1 d . . P B 2
H3B H 0.6163 0.6240 0.3464 0.029 Uiso 0.5 1 calc R U P B 2
C36 C 0.67973(14) 0.58487(10) 0.41671(7) 0.0269(5) Uani 1 1 d . . . . .
C41 C 0.64117(14) 0.57638(10) 0.45416(7) 0.0288(5) Uani 1 1 d . . . . .
C47 C 0.78887(15) 0.75096(10) 0.40354(7) 0.0305(5) Uani 1 1 d . . . . .
C40 C 0.61353(16) 0.52165(11) 0.46415(7) 0.0350(5) Uani 1 1 d . . . . .
H40 H 0.5867 0.5159 0.4885 0.042 Uiso 1 1 calc R U . . .
C46 C 0.84917(14) 0.70030(10) 0.39606(7) 0.0293(5) Uani 1 1 d . . . . .
C50 C 0.64697(14) 0.79650(10) 0.40131(7) 0.0293(5) Uani 1 1 d . . . . .
C27 C 0.41036(15) 0.61384(10) 0.34380(7) 0.0317(5) Uani 1 1 d . . . . .
C6B C 0.4642(11) 0.7553(7) 0.3560(3) 0.0276(14) Uani 0.5 1 d . . P B 2
H6B H 0.4526 0.7960 0.3608 0.033 Uiso 0.5 1 calc R U P B 2
C13 C 0.34093(15) 0.78134(11) 0.43037(7) 0.0325(5) Uani 1 1 d . . . . .
C37 C 0.69257(15) 0.53903(10) 0.39077(7) 0.0309(5) Uani 1 1 d . . . . .
C1 C 0.39214(14) 0.71455(10) 0.37474(7) 0.0282(5) Uani 1 1 d . . . . .
C18 C 0.33281(16) 0.84006(11) 0.42415(8) 0.0377(6) Uani 1 1 d . . . . .
C44 C 0.62864(16) 0.62434(11) 0.48307(7) 0.0338(5) Uani 1 1 d . . . . .
H44A H 0.6782 0.6505 0.4819 0.051 Uiso 1 1 calc R U . . .
H44B H 0.6259 0.6092 0.5097 0.051 Uiso 1 1 calc R U . . .
H44C H 0.5737 0.6442 0.4761 0.051 Uiso 1 1 calc R U . . .
C12B C 0.5838(7) 0.7022(3) 0.3182(3) 0.0216(19) Uani 0.5 1 d . . P B 2
C7B C 0.5174(7) 0.7448(4) 0.3189(2) 0.0234(18) Uani 0.5 1 d . . P B 2
C24 C 0.27001(16) 0.66007(11) 0.33910(7) 0.0328(5) Uani 1 1 d . . . . .
C42 C 0.73568(17) 0.54465(11) 0.35067(7) 0.0365(5) Uani 1 1 d . . . . .
H42A H 0.6897 0.5461 0.3296 0.055 Uiso 1 1 calc R U . . .
H42B H 0.7739 0.5122 0.3466 0.055 Uiso 1 1 calc R U . . .
H42C H 0.7708 0.5791 0.3504 0.055 Uiso 1 1 calc R U . . .
C22 C 0.23274(15) 0.74195(11) 0.38328(7) 0.0347(5) Uani 1 1 d . . . . .
C51 C 0.61035(15) 0.81161(10) 0.43756(8) 0.0333(5) Uani 1 1 d . . . . .
C14 C 0.35887(15) 0.75905(12) 0.46928(7) 0.0365(6) Uani 1 1 d . . . . .
C55 C 0.64722(16) 0.83507(11) 0.36888(8) 0.0345(5) Uani 1 1 d . . . . .
C49 C 0.93955(15) 0.70911(11) 0.41878(8) 0.0346(5) Uani 1 1 d . . . . .
H49A H 0.9305 0.7104 0.4471 0.052 Uiso 1 1 calc R U . . .
H49B H 0.9658 0.7445 0.4105 0.052 Uiso 1 1 calc R U . . .
H49C H 0.9791 0.6780 0.4130 0.052 Uiso 1 1 calc R U . . .
C32 C 0.42156(15) 0.57030(11) 0.37235(8) 0.0371(6) Uani 1 1 d . . . . .
C26 C 0.11263(16) 0.69475(14) 0.34054(8) 0.0451(7) Uani 1 1 d . . . . .
H26A H 0.1006 0.6748 0.3157 0.068 Uiso 1 1 calc R U . . .
H26B H 0.0752 0.7282 0.3414 0.068 Uiso 1 1 calc R U . . .
H26C H 0.1001 0.6700 0.3626 0.068 Uiso 1 1 calc R U . . .
C56 C 0.62142(17) 0.77533(12) 0.47454(8) 0.0375(6) Uani 1 1 d . . . . .
H56A H 0.5729 0.7483 0.4752 0.056 Uiso 1 1 calc R U . . .
H56B H 0.6210 0.7994 0.4979 0.056 Uiso 1 1 calc R U . . .
H56C H 0.6774 0.7551 0.4742 0.056 Uiso 1 1 calc R U . . .
C17 C 0.34594(18) 0.87631(13) 0.45699(9) 0.0442(6) Uani 1 1 d . . . . .
H17 H 0.3405 0.9156 0.4530 0.053 Uiso 1 1 calc R U . . .
C38 C 0.66449(16) 0.48480(11) 0.40254(8) 0.0352(5) Uani 1 1 d . . . . .
H38 H 0.6726 0.4539 0.3854 0.042 Uiso 1 1 calc R U . . .
C28 C 0.43344(15) 0.60486(11) 0.30392(8) 0.0360(5) Uani 1 1 d . . . . .
C35 C 0.38655(17) 0.57538(12) 0.41374(8) 0.0420(6) Uani 1 1 d . . . . .
H35A H 0.4336 0.5889 0.4319 0.063 Uiso 1 1 calc R U . . .
H35B H 0.3663 0.5385 0.4224 0.063 Uiso 1 1 calc R U . . .
H35C H 0.3374 0.6020 0.4133 0.063 Uiso 1 1 calc R U . . .
C15 C 0.37271(16) 0.79757(13) 0.50077(8) 0.0419(6) Uani 1 1 d . . . . .
H15 H 0.3864 0.7834 0.5263 0.050 Uiso 1 1 calc R U . . .
C23 C 0.21139(15) 0.71273(12) 0.34355(7) 0.0349(5) Uani 1 1 d . . . . .
C16 C 0.36678(18) 0.85617(13) 0.49539(9) 0.0449(6) Uani 1 1 d . . . . .
C39 C 0.62479(17) 0.47519(11) 0.43885(8) 0.0384(6) Uani 1 1 d . . . . .
C58 C 0.70273(17) 0.82596(12) 0.33285(8) 0.0393(6) Uani 1 1 d . . . . .
H58A H 0.7610 0.8428 0.3376 0.059 Uiso 1 1 calc R U . . .
H58B H 0.6735 0.8436 0.3098 0.059 Uiso 1 1 calc R U . . .
H58C H 0.7092 0.7856 0.3281 0.059 Uiso 1 1 calc R U . . .
C53 C 0.56061(18) 0.90182(12) 0.40791(10) 0.0481(7) Uani 1 1 d . . . . .
C48 C 0.86290(17) 0.69698(12) 0.35047(7) 0.0383(6) Uani 1 1 d . . . . .
H48A H 0.9001 0.6646 0.3449 0.058 Uiso 1 1 calc R U . . .
H48B H 0.8914 0.7314 0.3418 0.058 Uiso 1 1 calc R U . . .
H48C H 0.8057 0.6928 0.3364 0.058 Uiso 1 1 calc R U . . .
C33 C 0.40648(17) 0.64570(12) 0.27029(8) 0.0398(6) Uani 1 1 d . . . . .
H33A H 0.3477 0.6357 0.2595 0.060 Uiso 1 1 calc R U . . .
H33B H 0.4489 0.6431 0.2495 0.060 Uiso 1 1 calc R U . . .
H33C H 0.4057 0.6842 0.2805 0.060 Uiso 1 1 calc R U . . .
C52 C 0.56611(17) 0.86397(11) 0.43989(9) 0.0426(6) Uani 1 1 d . . . . .
H52 H 0.5395 0.8738 0.4636 0.051 Uiso 1 1 calc R U . . .
C31 C 0.46172(17) 0.51947(12) 0.36122(10) 0.0456(7) Uani 1 1 d . . . . .
H31 H 0.4702 0.4906 0.3802 0.055 Uiso 1 1 calc R U . . .
C21 C 0.3077(2) 0.86612(13) 0.38382(9) 0.0494(7) Uani 1 1 d . . . . .
H21A H 0.3119 0.8375 0.3633 0.074 Uiso 1 1 calc R U . . .
H21B H 0.3479 0.8971 0.3786 0.074 Uiso 1 1 calc R U . . .
H21C H 0.2472 0.8803 0.3839 0.074 Uiso 1 1 calc R U . . .
C25 C 0.23108(18) 0.75396(13) 0.30894(8) 0.0425(6) Uani 1 1 d . . . . .
H25A H 0.2942 0.7624 0.3094 0.064 Uiso 1 1 calc R U . . .
H25B H 0.1979 0.7888 0.3120 0.064 Uiso 1 1 calc R U . . .
H25C H 0.2135 0.7364 0.2838 0.064 Uiso 1 1 calc R U . . .
C19 C 0.36035(18) 0.69642(12) 0.47734(9) 0.0443(6) Uani 1 1 d . . . . .
H19A H 0.3093 0.6787 0.4638 0.067 Uiso 1 1 calc R U . . .
H19B H 0.3581 0.6899 0.5057 0.067 Uiso 1 1 calc R U . . .
H19C H 0.4146 0.6802 0.4677 0.067 Uiso 1 1 calc R U . . .
C29 C 0.47475(17) 0.55356(12) 0.29447(9) 0.0451(6) Uani 1 1 d . . . . .
H29 H 0.4931 0.5480 0.2685 0.054 Uiso 1 1 calc R U . . .
C30 C 0.48967(19) 0.51025(13) 0.32262(10) 0.0508(7) Uani 1 1 d . . . . .
C54 C 0.60157(18) 0.88662(12) 0.37252(9) 0.0451(6) Uani 1 1 d . . . . .
H54 H 0.5982 0.9117 0.3508 0.054 Uiso 1 1 calc R U . . .
C43 C 0.5932(2) 0.41631(13) 0.45065(11) 0.0576(8) Uani 1 1 d . . . . .
H43A H 0.6004 0.4119 0.4792 0.086 Uiso 1 1 calc R U . . .
H43B H 0.6281 0.3877 0.4377 0.086 Uiso 1 1 calc R U . . .
H43C H 0.5310 0.4118 0.4425 0.086 Uiso 1 1 calc R U . . .
C11B C 0.6302(4) 0.6941(3) 0.28318(17) 0.0262(12) Uani 0.5 1 d . . P B 2
C20 C 0.3816(2) 0.89680(17) 0.53006(10) 0.0627(9) Uani 1 1 d . . . . .
H20A H 0.4449 0.9012 0.5359 0.094 Uiso 1 1 calc R U . . .
H20B H 0.3536 0.8818 0.5532 0.094 Uiso 1 1 calc R U . . .
H20C H 0.3558 0.9334 0.5232 0.094 Uiso 1 1 calc R U . . .
C57 C 0.5172(2) 0.95972(14) 0.41214(14) 0.0719(11) Uani 1 1 d . . . . .
H57A H 0.4880 0.9615 0.4372 0.108 Uiso 1 1 calc R U . . .
H57B H 0.4737 0.9655 0.3904 0.108 Uiso 1 1 calc R U . . .
H57C H 0.5623 0.9890 0.4115 0.108 Uiso 1 1 calc R U . . .
C8B C 0.5067(4) 0.7801(3) 0.28505(17) 0.0311(8) Uani 0.5 1 d . U P B 2
H8B H 0.4649 0.8097 0.2854 0.037 Uiso 0.5 1 calc R U P B 2
C34 C 0.5292(2) 0.45331(15) 0.31108(14) 0.0725(11) Uani 1 1 d . . . . .
H34A H 0.5936 0.4555 0.3132 0.109 Uiso 1 1 calc R U . . .
H34B H 0.5104 0.4442 0.2839 0.109 Uiso 1 1 calc R U . . .
H34C H 0.5088 0.4240 0.3287 0.109 Uiso 1 1 calc R U . . .
C9B C 0.5559(4) 0.7727(3) 0.25115(14) 0.0270(8) Uani 0.5 1 d . U P B 2
H9B H 0.5481 0.7972 0.2293 0.032 Uiso 0.5 1 calc R U P B 2
C10B C 0.6165(4) 0.7284(3) 0.25031(15) 0.0294(8) Uani 0.5 1 d . U P B 2
H10B H 0.6482 0.7218 0.2274 0.035 Uiso 0.5 1 calc R U P B 2
C5A C 0.557(3) 0.6765(18) 0.3919(10) 0.0242(12) Uani 0.5 1 d . U P A 1
H5A H 0.5420 0.6386 0.4024 0.029 Uiso 0.5 1 calc R U P A 1
C3A C 0.486(3) 0.7171(14) 0.3941(11) 0.0254(13) Uani 0.5 1 d . U P A 1
H3A H 0.4855 0.7347 0.4207 0.030 Uiso 0.5 1 calc R U P A 1
C2A C 0.4620(11) 0.7595(6) 0.3622(3) 0.0279(16) Uani 0.5 1 d . U P A 1
H2A H 0.4515 0.7985 0.3718 0.033 Uiso 0.5 1 calc R U P A 1
C12A C 0.5083(9) 0.7559(5) 0.3248(3) 0.0276(14) Uani 0.5 1 d . U P A 1
C7A C 0.5742(10) 0.7159(4) 0.3191(3) 0.0272(16) Uani 0.5 1 d . U P A 1
C6A C 0.6040(11) 0.6741(5) 0.3508(4) 0.0240(9) Uani 0.5 1 d . U P A 1
H6A H 0.6129 0.6351 0.3407 0.029 Uiso 0.5 1 calc R U P A 1
C8A C 0.6116(5) 0.7139(3) 0.2809(2) 0.0325(13) Uani 0.5 1 d . U P A 1
H8A H 0.6532 0.6852 0.2761 0.039 Uiso 0.5 1 calc R U P A 1
C9A C 0.5906(5) 0.7510(3) 0.25067(15) 0.0319(8) Uani 0.5 1 d . U P A 1
H9A H 0.6176 0.7481 0.2261 0.038 Uiso 0.5 1 calc R U P A 1
C10A C 0.5281(4) 0.7930(3) 0.25731(18) 0.0382(12) Uani 0.5 1 d . U P A 1
H10A H 0.5139 0.8201 0.2376 0.046 Uiso 0.5 1 calc R U P A 1
C11A C 0.4864(4) 0.7947(3) 0.29400(18) 0.0325(8) Uani 0.5 1 d . U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1A C11A 1.498(6) . ?
Br1B C11B 1.446(6) . ?
O4 C45 1.224(3) . ?
O3 C47 1.224(3) . ?
O2 C24 1.219(3) . ?
O1 C22 1.225(3) . ?
N4 C4 1.471(3) . ?
N4 C45 1.376(3) . ?
N4 C36 1.457(3) . ?
N3 C4 1.454(3) . ?
N3 C47 1.371(3) . ?
N3 C50 1.462(3) . ?
N2 C27 1.450(3) . ?
N2 C1 1.456(3) . ?
N2 C24 1.381(3) . ?
N1 C13 1.455(3) . ?
N1 C1 1.479(3) . ?
N1 C22 1.371(3) . ?
C4 C2B 1.52(5) . ?
C4 C3B 1.558(17) . ?
C4 C5A 1.52(5) . ?
C4 C6A 1.561(16) . ?
C45 C46 1.509(3) . ?
C2B H2B 0.9800 . ?
C2B C5B 1.58(6) . ?
C2B C3B 1.47(3) . ?
C5B H5B 0.9800 . ?
C5B C6B 1.55(3) . ?
C5B C1 1.53(5) . ?
C3B H3B 0.9800 . ?
C3B C12B 1.487(11) . ?
C36 C41 1.411(3) . ?
C36 C37 1.394(3) . ?
C41 C40 1.387(3) . ?
C41 C44 1.494(3) . ?
C47 C46 1.512(3) . ?
C40 H40 0.9300 . ?
C40 C39 1.389(4) . ?
C46 C49 1.530(3) . ?
C46 C48 1.545(3) . ?
C50 C51 1.393(3) . ?
C50 C55 1.408(3) . ?
C27 C32 1.398(3) . ?
C27 C28 1.404(4) . ?
C6B H6B 0.9800 . ?
C6B C1 1.582(16) . ?
C6B C7B 1.518(10) . ?
C13 C18 1.390(4) . ?
C13 C14 1.413(3) . ?
C37 C42 1.514(3) . ?
C37 C38 1.395(4) . ?
C1 C3A 1.52(5) . ?
C1 C2A 1.547(17) . ?
C18 C17 1.392(4) . ?
C18 C21 1.509(4) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C12B C7B 1.403(8) . ?
C12B C11B 1.397(10) . ?
C7B C8B 1.402(10) . ?
C24 C23 1.519(4) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C22 C23 1.512(4) . ?
C51 C56 1.500(4) . ?
C51 C52 1.392(4) . ?
C14 C15 1.391(4) . ?
C14 C19 1.486(4) . ?
C55 C58 1.503(4) . ?
C55 C54 1.390(4) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C32 C35 1.502(4) . ?
C32 C31 1.386(4) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C26 C23 1.529(3) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C17 H17 0.9300 . ?
C17 C16 1.387(4) . ?
C38 H38 0.9300 . ?
C38 C39 1.389(4) . ?
C28 C33 1.513(4) . ?
C28 C29 1.389(4) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C15 H15 0.9300 . ?
C15 C16 1.381(4) . ?
C23 C25 1.541(3) . ?
C16 C20 1.505(4) . ?
C39 C43 1.510(4) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C53 C52 1.385(4) . ?
C53 C54 1.398(4) . ?
C53 C57 1.507(4) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C52 H52 0.9300 . ?
C31 H31 0.9300 . ?
C31 C30 1.387(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C29 H29 0.9300 . ?
C29 C30 1.391(4) . ?
C30 C34 1.510(4) . ?
C54 H54 0.9300 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C11B C10B 1.366(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C8B H8B 0.9300 . ?
C8B C9B 1.385(8) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C9B H9B 0.9300 . ?
C9B C10B 1.373(7) . ?
C10B H10B 0.9300 . ?
C5A H5A 0.9800 . ?
C5A C3A 1.43(6) . ?
C5A C6A 1.57(3) . ?
C3A H3A 0.9800 . ?
C3A C2A 1.48(3) . ?
C2A H2A 0.9800 . ?
C2A C12A 1.455(13) . ?
C12A C7A 1.373(12) . ?
C12A C11A 1.398(12) . ?
C7A C6A 1.493(13) . ?
C7A C8A 1.415(13) . ?
C6A H6A 0.9800 . ?
C8A H8A 0.9300 . ?
C8A C9A 1.355(9) . ?
C9A H9A 0.9300 . ?
C9A C10A 1.377(8) . ?
C10A H10A 0.9300 . ?
C10A C11A 1.397(8) . ?

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
C45 N4 C4 122.47(18) . . ?
C45 N4 C36 114.71(18) . . ?
C36 N4 C4 121.51(17) . . ?
C4 N3 C50 124.45(17) . . ?
C47 N3 C4 122.43(19) . . ?
C47 N3 C50 113.12(19) . . ?
C27 N2 C1 125.70(18) . . ?
C24 N2 C27 112.33(19) . . ?
C24 N2 C1 121.9(2) . . ?
C13 N1 C1 121.89(18) . . ?
C22 N1 C13 115.11(19) . . ?
C22 N1 C1 121.5(2) . . ?
N4 C4 C2B 113.7(15) . . ?
N4 C4 C3B 109.2(4) . . ?
N4 C4 C5A 115.7(15) . . ?
N4 C4 C6A 117.2(4) . . ?
N3 C4 N4 111.05(17) . . ?
N3 C4 C2B 126.2(15) . . ?
N3 C4 C3B 129.8(4) . . ?
N3 C4 C5A 122.8(15) . . ?
N3 C4 C6A 121.0(4) . . ?
C2B C4 C3B 56.9(13) . . ?
C5A C4 C6A 61.1(13) . . ?
O4 C45 N4 121.4(2) . . ?
O4 C45 C46 121.24(19) . . ?
N4 C45 C46 117.34(19) . . ?
C4 C2B H2B 113.6 . . ?
C4 C2B C5B 121(4) . . ?
C5B C2B H2B 113.6 . . ?
C3B C2B C4 62.9(17) . . ?
C3B C2B H2B 113.6 . . ?
C3B C2B C5B 122(3) . . ?
C2B C5B H5B 116.5 . . ?
C6B C5B C2B 114(3) . . ?
C6B C5B H5B 116.5 . . ?
C1 C5B C2B 120(4) . . ?
C1 C5B H5B 116.5 . . ?
C1 C5B C6B 62.0(16) . . ?
C4 C3B H3B 115.2 . . ?
C2B C3B C4 60(2) . . ?
C2B C3B H3B 115.2 . . ?
C2B C3B C12B 119.4(16) . . ?
C12B C3B C4 120.6(9) . . ?
C12B C3B H3B 115.2 . . ?
C41 C36 N4 118.2(2) . . ?
C37 C36 N4 120.5(2) . . ?
C37 C36 C41 120.9(2) . . ?
C36 C41 C44 122.2(2) . . ?
C40 C41 C36 118.6(2) . . ?
C40 C41 C44 119.2(2) . . ?
O3 C47 N3 121.1(2) . . ?
O3 C47 C46 121.0(2) . . ?
N3 C47 C46 117.9(2) . . ?
C41 C40 H40 119.1 . . ?
C41 C40 C39 121.9(2) . . ?
C39 C40 H40 119.1 . . ?
C45 C46 C47 112.12(18) . . ?
C45 C46 C49 109.77(19) . . ?
C45 C46 C48 107.8(2) . . ?
C47 C46 C49 109.2(2) . . ?
C47 C46 C48 107.83(19) . . ?
C49 C46 C48 110.08(19) . . ?
C51 C50 N3 119.8(2) . . ?
C51 C50 C55 121.3(2) . . ?
C55 C50 N3 118.3(2) . . ?
C32 C27 N2 120.2(2) . . ?
C32 C27 C28 120.7(2) . . ?
C28 C27 N2 118.0(2) . . ?
C5B C6B H6B 113.0 . . ?
C5B C6B C1 58.4(17) . . ?
C1 C6B H6B 113.0 . . ?
C7B C6B C5B 120.6(16) . . ?
C7B C6B H6B 113.0 . . ?
C7B C6B C1 127.7(10) . . ?
C18 C13 N1 119.7(2) . . ?
C18 C13 C14 120.8(2) . . ?
C14 C13 N1 119.1(2) . . ?
C36 C37 C42 123.8(2) . . ?
C36 C37 C38 118.1(2) . . ?
C38 C37 C42 118.1(2) . . ?
N2 C1 N1 111.47(18) . . ?
N2 C1 C5B 126.4(12) . . ?
N2 C1 C6B 120.3(5) . . ?
N2 C1 C3A 122.4(13) . . ?
N2 C1 C2A 128.8(5) . . ?
N1 C1 C5B 113.0(12) . . ?
N1 C1 C6B 117.3(5) . . ?
N1 C1 C3A 116.0(13) . . ?
N1 C1 C2A 110.7(5) . . ?
C5B C1 C6B 59.6(13) . . ?
C3A C1 C2A 57.9(14) . . ?
C13 C18 C17 118.2(2) . . ?
C13 C18 C21 123.2(2) . . ?
C17 C18 C21 118.6(2) . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C7B C12B C3B 122.3(8) . . ?
C11B C12B C3B 118.7(6) . . ?
C11B C12B C7B 119.0(7) . . ?
C12B C7B C6B 121.4(8) . . ?
C8B C7B C6B 121.1(6) . . ?
C8B C7B C12B 117.3(6) . . ?
O2 C24 N2 121.5(2) . . ?
O2 C24 C23 121.6(2) . . ?
N2 C24 C23 116.9(2) . . ?
C37 C42 H42A 109.5 . . ?
C37 C42 H42B 109.5 . . ?
C37 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O1 C22 N1 121.5(2) . . ?
O1 C22 C23 120.9(2) . . ?
N1 C22 C23 117.6(2) . . ?
C50 C51 C56 122.6(2) . . ?
C52 C51 C50 118.3(2) . . ?
C52 C51 C56 119.0(2) . . ?
C13 C14 C19 121.9(2) . . ?
C15 C14 C13 118.1(3) . . ?
C15 C14 C19 119.9(2) . . ?
C50 C55 C58 123.0(2) . . ?
C54 C55 C50 118.0(2) . . ?
C54 C55 C58 118.7(2) . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C27 C32 C35 122.2(2) . . ?
C31 C32 C27 118.7(3) . . ?
C31 C32 C35 119.0(2) . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
C51 C56 H56A 109.5 . . ?
C51 C56 H56B 109.5 . . ?
C51 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C18 C17 H17 118.7 . . ?
C16 C17 C18 122.6(3) . . ?
C16 C17 H17 118.7 . . ?
C37 C38 H38 118.8 . . ?
C39 C38 C37 122.4(2) . . ?
C39 C38 H38 118.8 . . ?
C27 C28 C33 122.7(2) . . ?
C29 C28 C27 118.2(2) . . ?
C29 C28 C33 118.7(2) . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C14 C15 H15 118.8 . . ?
C16 C15 C14 122.3(3) . . ?
C16 C15 H15 118.8 . . ?
C24 C23 C26 109.1(2) . . ?
C24 C23 C25 107.67(19) . . ?
C22 C23 C24 110.51(19) . . ?
C22 C23 C26 110.3(2) . . ?
C22 C23 C25 109.6(2) . . ?
C26 C23 C25 109.6(2) . . ?
C17 C16 C20 121.1(3) . . ?
C15 C16 C17 117.8(3) . . ?
C15 C16 C20 121.2(3) . . ?
C40 C39 C38 118.1(2) . . ?
C40 C39 C43 120.3(3) . . ?
C38 C39 C43 121.6(3) . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C52 C53 C54 118.4(2) . . ?
C52 C53 C57 120.7(3) . . ?
C54 C53 C57 120.7(3) . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C51 C52 H52 119.0 . . ?
C53 C52 C51 122.0(3) . . ?
C53 C52 H52 119.0 . . ?
C32 C31 H31 118.9 . . ?
C32 C31 C30 122.1(3) . . ?
C30 C31 H31 118.9 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C28 C29 H29 118.9 . . ?
C28 C29 C30 122.2(3) . . ?
C30 C29 H29 118.9 . . ?
C31 C30 C29 117.9(3) . . ?
C31 C30 C34 120.6(3) . . ?
C29 C30 C34 121.3(3) . . ?
C55 C54 C53 121.8(3) . . ?
C55 C54 H54 119.1 . . ?
C53 C54 H54 119.1 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C12B C11B Br1B 138.1(5) . . ?
C10B C11B Br1B 99.9(4) . . ?
C10B C11B C12B 122.0(5) . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C53 C57 H57A 109.5 . . ?
C53 C57 H57B 109.5 . . ?
C53 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C7B C8B H8B 118.7 . . ?
C9B C8B C7B 122.6(5) . . ?
C9B C8B H8B 118.7 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C8B C9B H9B 120.6 . . ?
C10B C9B C8B 118.8(5) . . ?
C10B C9B H9B 120.6 . . ?
C11B C10B C9B 120.0(5) . . ?
C11B C10B H10B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
C4 C5A H5A 113.5 . . ?
C4 C5A C6A 60.7(16) . . ?
C3A C5A C4 129(4) . . ?
C3A C5A H5A 113.5 . . ?
C3A C5A C6A 115(3) . . ?
C6A C5A H5A 113.5 . . ?
C1 C3A H3A 111.0 . . ?
C5A C3A C1 129(4) . . ?
C5A C3A H3A 111.0 . . ?
C5A C3A C2A 124(3) . . ?
C2A C3A C1 62.1(16) . . ?
C2A C3A H3A 111.0 . . ?
C1 C2A H2A 115.0 . . ?
C3A C2A C1 60.0(18) . . ?
C3A C2A H2A 115.0 . . ?
C12A C2A C1 122.8(9) . . ?
C12A C2A C3A 117.9(16) . . ?
C12A C2A H2A 115.0 . . ?
C7A C12A C2A 121.7(10) . . ?
C7A C12A C11A 118.9(9) . . ?
C11A C12A C2A 119.3(8) . . ?
C12A C7A C6A 122.6(11) . . ?
C12A C7A C8A 117.3(9) . . ?
C8A C7A C6A 120.0(10) . . ?
C4 C6A C5A 58.2(19) . . ?
C4 C6A H6A 113.9 . . ?
C5A C6A H6A 113.9 . . ?
C7A C6A C4 127.3(10) . . ?
C7A C6A C5A 117.8(15) . . ?
C7A C6A H6A 113.9 . . ?
C7A C8A H8A 117.9 . . ?
C9A C8A C7A 124.2(8) . . ?
C9A C8A H8A 117.9 . . ?
C8A C9A H9A 120.9 . . ?
C8A C9A C10A 118.2(5) . . ?
C10A C9A H9A 120.9 . . ?
C9A C10A H10A 120.3 . . ?
C9A C10A C11A 119.3(5) . . ?
C11A C10A H10A 120.3 . . ?
C12A C11A Br1A 140.7(6) . . ?
C10A C11A Br1A 97.4(4) . . ?
C10A C11A C12A 121.9(6) . . ?

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
Br1B C11B C10B C9B -179.8(5) . . . . ?
O4 C45 C46 C47 -152.7(2) . . . . ?
O4 C45 C46 C49 -31.1(3) . . . . ?
O4 C45 C46 C48 88.8(2) . . . . ?
O3 C47 C46 C45 146.8(2) . . . . ?
O3 C47 C46 C49 24.9(3) . . . . ?
O3 C47 C46 C48 -94.7(3) . . . . ?
O2 C24 C23 C22 140.7(2) . . . . ?
O2 C24 C23 C26 19.3(3) . . . . ?
O2 C24 C23 C25 -99.6(3) . . . . ?
O1 C22 C23 C24 -144.9(2) . . . . ?
O1 C22 C23 C26 -24.2(3) . . . . ?
O1 C22 C23 C25 96.6(3) . . . . ?
N4 C4 C2B C5B 149(3) . . . . ?
N4 C4 C2B C3B -98.2(11) . . . . ?
N4 C4 C3B C2B 106.3(18) . . . . ?
N4 C4 C3B C12B -145.2(8) . . . . ?
N4 C4 C5A C3A 151(3) . . . . ?
N4 C4 C5A C6A -108.3(9) . . . . ?
N4 C4 C6A C5A 105.8(17) . . . . ?
N4 C4 C6A C7A -151.6(10) . . . . ?
N4 C45 C46 C47 27.7(3) . . . . ?
N4 C45 C46 C49 149.28(19) . . . . ?
N4 C45 C46 C48 -90.8(2) . . . . ?
N4 C36 C41 C40 -174.85(19) . . . . ?
N4 C36 C41 C44 5.6(3) . . . . ?
N4 C36 C37 C42 -5.7(3) . . . . ?
N4 C36 C37 C38 173.95(19) . . . . ?
N3 C4 C2B C5B 5(4) . . . . ?
N3 C4 C2B C3B 118.0(10) . . . . ?
N3 C4 C3B C2B -112.0(19) . . . . ?
N3 C4 C3B C12B -3.5(14) . . . . ?
N3 C4 C5A C3A 10(4) . . . . ?
N3 C4 C5A C6A 110.1(10) . . . . ?
N3 C4 C6A C5A -113.0(18) . . . . ?
N3 C4 C6A C7A -10.4(15) . . . . ?
N3 C47 C46 C45 -35.4(3) . . . . ?
N3 C47 C46 C49 -157.3(2) . . . . ?
N3 C47 C46 C48 83.1(2) . . . . ?
N3 C50 C51 C56 0.5(3) . . . . ?
N3 C50 C51 C52 176.8(2) . . . . ?
N3 C50 C55 C58 -4.6(3) . . . . ?
N3 C50 C55 C54 -177.5(2) . . . . ?
N2 C27 C32 C35 -4.0(3) . . . . ?
N2 C27 C32 C31 172.1(2) . . . . ?
N2 C27 C28 C33 -0.1(3) . . . . ?
N2 C27 C28 C29 -173.4(2) . . . . ?
N2 C1 C3A C5A 5(4) . . . . ?
N2 C1 C3A C2A 118.5(10) . . . . ?
N2 C1 C2A C3A -108.0(15) . . . . ?
N2 C1 C2A C12A -2.3(13) . . . . ?
N2 C24 C23 C22 -39.8(3) . . . . ?
N2 C24 C23 C26 -161.2(2) . . . . ?
N2 C24 C23 C25 79.9(3) . . . . ?
N1 C13 C18 C17 175.1(2) . . . . ?
N1 C13 C18 C21 -3.0(4) . . . . ?
N1 C13 C14 C15 -176.1(2) . . . . ?
N1 C13 C14 C19 1.9(3) . . . . ?
N1 C1 C3A C5A 148(3) . . . . ?
N1 C1 C3A C2A -99.1(11) . . . . ?
N1 C1 C2A C3A 108.4(16) . . . . ?
N1 C1 C2A C12A -145.9(8) . . . . ?
N1 C22 C23 C24 35.9(3) . . . . ?
N1 C22 C23 C26 156.6(2) . . . . ?
N1 C22 C23 C25 -82.6(3) . . . . ?
C4 N4 C45 O4 -172.31(19) . . . . ?
C4 N4 C45 C46 7.3(3) . . . . ?
C4 N4 C36 C41 -85.6(2) . . . . ?
C4 N4 C36 C37 101.6(2) . . . . ?
C4 N3 C47 O3 -174.5(2) . . . . ?
C4 N3 C47 C46 7.7(3) . . . . ?
C4 N3 C50 C51 83.7(3) . . . . ?
C4 N3 C50 C55 -105.2(2) . . . . ?
C4 C2B C5B C6B 79(4) . . . . ?
C4 C2B C5B C1 149(2) . . . . ?
C4 C2B C3B C12B -110.5(17) . . . . ?
C4 C3B C12B C7B -74.4(14) . . . . ?
C4 C3B C12B C11B 107.6(11) . . . . ?
C4 C5A C3A C1 145(3) . . . . ?
C4 C5A C3A C2A 65(6) . . . . ?
C4 C5A C6A C7A -118.6(16) . . . . ?
C45 N4 C4 N3 -34.8(3) . . . . ?
C45 N4 C4 C2B 175.9(14) . . . . ?
C45 N4 C4 C3B 114.5(6) . . . . ?
C45 N4 C4 C5A 179.2(14) . . . . ?
C45 N4 C4 C6A 110.0(6) . . . . ?
C45 N4 C36 C41 107.2(2) . . . . ?
C45 N4 C36 C37 -65.6(3) . . . . ?
C2B C4 C3B C12B 108.5(19) . . . . ?
C2B C5B C6B C1 113(4) . . . . ?
C2B C5B C6B C7B -5(5) . . . . ?
C2B C5B C1 N2 5(4) . . . . ?
C2B C5B C1 N1 148(2) . . . . ?
C2B C5B C1 C6B -103(3) . . . . ?
C2B C3B C12B C7B -4(3) . . . . ?
C2B C3B C12B C11B 178(3) . . . . ?
C5B C2B C3B C4 112(5) . . . . ?
C5B C2B C3B C12B 1(6) . . . . ?
C5B C6B C1 N2 -116.9(14) . . . . ?
C5B C6B C1 N1 101.9(15) . . . . ?
C5B C6B C7B C12B 3(3) . . . . ?
C5B C6B C7B C8B -172(2) . . . . ?
C3B C4 C2B C5B -113(3) . . . . ?
C3B C2B C5B C6B 3(7) . . . . ?
C3B C2B C5B C1 73(6) . . . . ?
C3B C12B C7B C6B 1.5(16) . . . . ?
C3B C12B C7B C8B 176.8(11) . . . . ?
C3B C12B C11B Br1B 2.1(16) . . . . ?
C3B C12B C11B C10B -178.2(9) . . . . ?
C36 N4 C4 N3 158.96(18) . . . . ?
C36 N4 C4 C2B 9.7(14) . . . . ?
C36 N4 C4 C3B -51.7(6) . . . . ?
C36 N4 C4 C5A 12.9(15) . . . . ?
C36 N4 C4 C6A -56.2(6) . . . . ?
C36 N4 C45 O4 -5.2(3) . . . . ?
C36 N4 C45 C46 174.38(18) . . . . ?
C36 C41 C40 C39 1.6(3) . . . . ?
C36 C37 C38 C39 -0.1(3) . . . . ?
C41 C36 C37 C42 -178.3(2) . . . . ?
C41 C36 C37 C38 1.3(3) . . . . ?
C41 C40 C39 C38 -0.4(4) . . . . ?
C41 C40 C39 C43 -179.5(2) . . . . ?
C47 N3 C4 N4 26.7(3) . . . . ?
C47 N3 C4 C2B 171.2(16) . . . . ?
C47 N3 C4 C3B -114.6(7) . . . . ?
C47 N3 C4 C5A 169.8(16) . . . . ?
C47 N3 C4 C6A -116.7(6) . . . . ?
C47 N3 C50 C51 -96.1(2) . . . . ?
C47 N3 C50 C55 75.0(3) . . . . ?
C50 N3 C4 N4 -153.17(19) . . . . ?
C50 N3 C4 C2B -8.6(16) . . . . ?
C50 N3 C4 C3B 65.6(7) . . . . ?
C50 N3 C4 C5A -10.0(16) . . . . ?
C50 N3 C4 C6A 63.5(6) . . . . ?
C50 N3 C47 O3 5.3(3) . . . . ?
C50 N3 C47 C46 -172.51(19) . . . . ?
C50 C51 C52 C53 -2.4(4) . . . . ?
C50 C55 C54 C53 3.6(4) . . . . ?
C27 N2 C1 N1 -148.6(2) . . . . ?
C27 N2 C1 C5B -4.5(15) . . . . ?
C27 N2 C1 C6B 68.2(6) . . . . ?
C27 N2 C1 C3A -4.8(15) . . . . ?
C27 N2 C1 C2A 68.0(7) . . . . ?
C27 N2 C24 O2 4.6(3) . . . . ?
C27 N2 C24 C23 -174.87(19) . . . . ?
C27 C32 C31 C30 -1.0(4) . . . . ?
C27 C28 C29 C30 3.2(4) . . . . ?
C6B C5B C1 N2 107.2(11) . . . . ?
C6B C5B C1 N1 -109.1(10) . . . . ?
C6B C7B C8B C9B 178.2(8) . . . . ?
C13 N1 C1 N2 161.76(19) . . . . ?
C13 N1 C1 C5B 12.6(13) . . . . ?
C13 N1 C1 C6B -53.8(6) . . . . ?
C13 N1 C1 C3A 15.4(14) . . . . ?
C13 N1 C1 C2A -48.0(5) . . . . ?
C13 N1 C22 O1 -12.8(3) . . . . ?
C13 N1 C22 C23 166.4(2) . . . . ?
C13 C18 C17 C16 0.1(4) . . . . ?
C13 C14 C15 C16 2.0(4) . . . . ?
C37 C36 C41 C40 -2.1(3) . . . . ?
C37 C36 C41 C44 178.4(2) . . . . ?
C37 C38 C39 C40 -0.3(4) . . . . ?
C37 C38 C39 C43 178.8(2) . . . . ?
C1 N2 C27 C32 83.1(3) . . . . ?
C1 N2 C27 C28 -108.9(2) . . . . ?
C1 N2 C24 O2 -173.0(2) . . . . ?
C1 N2 C24 C23 7.5(3) . . . . ?
C1 N1 C13 C18 101.6(3) . . . . ?
C1 N1 C13 C14 -85.4(3) . . . . ?
C1 N1 C22 O1 -179.1(2) . . . . ?
C1 N1 C22 C23 0.1(3) . . . . ?
C1 C5B C6B C7B -118.1(14) . . . . ?
C1 C6B C7B C12B -68.5(14) . . . . ?
C1 C6B C7B C8B 116.3(11) . . . . ?
C1 C3A C2A C12A -113.7(14) . . . . ?
C1 C2A C12A C7A -72.4(14) . . . . ?
C1 C2A C12A C11A 108.5(11) . . . . ?
C18 C13 C14 C15 -3.2(3) . . . . ?
C18 C13 C14 C19 174.8(2) . . . . ?
C18 C17 C16 C15 -1.3(4) . . . . ?
C18 C17 C16 C20 179.2(3) . . . . ?
C44 C41 C40 C39 -178.9(2) . . . . ?
C12B C7B C8B C9B 2.8(12) . . . . ?
C12B C11B C10B C9B 0.4(10) . . . . ?
C7B C6B C1 N2 -10.7(12) . . . . ?
C7B C6B C1 N1 -151.8(8) . . . . ?
C7B C6B C1 C5B 106.3(19) . . . . ?
C7B C12B C11B Br1B -176.0(7) . . . . ?
C7B C12B C11B C10B 3.7(13) . . . . ?
C7B C8B C9B C10B 1.2(10) . . . . ?
C24 N2 C27 C32 -94.4(2) . . . . ?
C24 N2 C27 C28 73.6(3) . . . . ?
C24 N2 C1 N1 28.7(3) . . . . ?
C24 N2 C1 C5B 172.8(15) . . . . ?
C24 N2 C1 C6B -114.5(6) . . . . ?
C24 N2 C1 C3A 172.5(15) . . . . ?
C24 N2 C1 C2A -114.7(7) . . . . ?
C42 C37 C38 C39 179.6(2) . . . . ?
C22 N1 C13 C18 -64.6(3) . . . . ?
C22 N1 C13 C14 108.3(2) . . . . ?
C22 N1 C1 N2 -32.9(3) . . . . ?
C22 N1 C1 C5B 178.0(13) . . . . ?
C22 N1 C1 C6B 111.5(6) . . . . ?
C22 N1 C1 C3A -179.3(13) . . . . ?
C22 N1 C1 C2A 117.3(5) . . . . ?
C51 C50 C55 C58 166.3(2) . . . . ?
C51 C50 C55 C54 -6.6(3) . . . . ?
C14 C13 C18 C17 2.2(3) . . . . ?
C14 C13 C18 C21 -175.8(2) . . . . ?
C14 C15 C16 C17 0.2(4) . . . . ?
C14 C15 C16 C20 179.7(2) . . . . ?
C55 C50 C51 C56 -170.4(2) . . . . ?
C55 C50 C51 C52 6.0(3) . . . . ?
C32 C27 C28 C33 167.9(2) . . . . ?
C32 C27 C28 C29 -5.5(3) . . . . ?
C32 C31 C30 C29 -1.2(4) . . . . ?
C32 C31 C30 C34 -177.1(3) . . . . ?
C56 C51 C52 C53 174.1(2) . . . . ?
C28 C27 C32 C35 -171.7(2) . . . . ?
C28 C27 C32 C31 4.5(3) . . . . ?
C28 C29 C30 C31 0.1(4) . . . . ?
C28 C29 C30 C34 176.0(3) . . . . ?
C35 C32 C31 C30 175.2(2) . . . . ?
C58 C55 C54 C53 -169.6(3) . . . . ?
C33 C28 C29 C30 -170.4(2) . . . . ?
C52 C53 C54 C55 -0.1(4) . . . . ?
C21 C18 C17 C16 178.2(3) . . . . ?
C19 C14 C15 C16 -176.1(2) . . . . ?
C54 C53 C52 C51 -0.5(4) . . . . ?
C11B C12B C7B C6B 179.5(9) . . . . ?
C11B C12B C7B C8B -5.1(14) . . . . ?
C57 C53 C52 C51 -176.2(3) . . . . ?
C57 C53 C54 C55 175.6(3) . . . . ?
C8B C9B C10B C11B -2.8(8) . . . . ?
C5A C4 C6A C7A 102.5(19) . . . . ?
C5A C3A C2A C1 120(5) . . . . ?
C5A C3A C2A C12A 6(6) . . . . ?
C3A C1 C2A C12A 106(2) . . . . ?
C3A C5A C6A C4 122(5) . . . . ?
C3A C5A C6A C7A 3(6) . . . . ?
C3A C2A C12A C7A -2(3) . . . . ?
C3A C2A C12A C11A 179(2) . . . . ?
C2A C1 C3A C5A -113(4) . . . . ?
C2A C12A C7A C6A -1.0(18) . . . . ?
C2A C12A C7A C8A 176.5(9) . . . . ?
C2A C12A C11A Br1A 1.2(16) . . . . ?
C2A C12A C11A C10A -179.5(8) . . . . ?
C12A C7A C6A C4 -69.4(17) . . . . ?
C12A C7A C6A C5A 0(3) . . . . ?
C12A C7A C8A C9A 4.3(15) . . . . ?
C7A C12A C11A Br1A -177.9(9) . . . . ?
C7A C12A C11A C10A 1.4(14) . . . . ?
C7A C8A C9A C10A -0.8(11) . . . . ?
C6A C4 C5A C3A -100(4) . . . . ?
C6A C5A C3A C1 73(6) . . . . ?
C6A C5A C3A C2A -7(7) . . . . ?
C6A C7A C8A C9A -178.1(10) . . . . ?
C8A C7A C6A C4 113.1(12) . . . . ?
C8A C7A C6A C5A -177(2) . . . . ?
C8A C9A C10A C11A -2.5(9) . . . . ?
C9A C10A C11A Br1A -178.3(5) . . . . ?
C9A C10A C11A C12A 2.2(11) . . . . ?
C11A C12A C7A C6A 178.0(11) . . . . ?
C11A C12A C7A C8A -4.5(16) . . . . ?

_smtbx_masks_special_details     ?
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 -0.531 0.000 0.500 1371.7 609.8 ?
2 -0.515 0.500 0.000 1371.7 609.8 ?


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

# start Validation Reply Form
_vrf_PLAT910_proc_notwin         
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: The beam stop was checked and re-configured but this did 
not fix this issue.  From the NMR data, we know that the provided 
structural model is correct.
;
# end Validation Reply Form
