# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2021

####################################################################### 
# 
# 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_exp_1755
_database_code_depnum_ccdc_archive 'CCDC 2071725'
loop_
_audit_author_name
_audit_author_address
M
;ECNU
China
;
_audit_update_record             
;
2021-03-20 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_audit_creation_date             2021-03-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H29 Br2 N O, C4 Cl N O'
_chemical_formula_sum            'C31 H29 Br2 Cl N2 O2'
_chemical_formula_weight         656.83
_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'
Cl Cl 0.3639 0.7018 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5868(5)
_cell_length_b                   10.6482(6)
_cell_length_c                   13.8870(6)
_cell_angle_alpha                107.508(5)
_cell_angle_beta                 104.966(4)
_cell_angle_gamma                94.584(4)
_cell_volume                     1421.06(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3855
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      73.0020
_cell_measurement_theta_min      4.3580
_shelx_estimated_absorpt_T_max   0.518
_shelx_estimated_absorpt_T_min   0.373
_exptl_absorpt_coefficient_mu    4.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13645
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         4.730
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  24.00   1.00    2.00    --    0.00 -19.00-120.00   57
  2  ω      9.00  84.00   1.00    2.00    --    0.00  38.00-120.00   75
  3  ω      3.00  86.00   1.00    2.00    --    0.00  38.00 150.00   83
  4  ω    -88.00 -42.00   1.00    2.00    --    0.00 -19.00-120.00   46
  5  ω    -30.00  -3.00   1.00    2.00    --    0.00 -57.00-180.00   27
  6  ω     26.00 116.00   1.00    2.00    --   95.80 -45.00  60.00   90
  7  ω     92.00 125.00   1.00    2.00    --   95.80 -77.00-150.00   33
  8  ω     98.00 135.00   1.00    2.00    --   95.80  45.00   0.00   37
  9  ω     50.00 115.00   1.00    2.00    --   95.80 -30.00  60.00   65
 10  ω      6.00  96.00   1.00    2.00    --   95.80 -61.00  60.00   90
 11  ω     50.00 105.00   1.00    2.00    --   95.80 -82.00 -30.00   55
 12  ω     76.00 104.00   1.00    2.00    --   95.80  30.00  60.00   28
 13  ω    140.00 185.00   1.00    2.00    --   95.80  30.00  60.00   45
 14  ω     10.00  72.00   1.00    2.00    --   95.80 -77.00-150.00   62
 15  ω     74.00 185.00   1.00    2.00    --   95.80  15.00   0.00  111
 16  ω     46.00  77.00   1.00    2.00    --   95.80 -77.00   0.00   31
 17  ω     56.00 121.00   1.00    2.00    --   95.80 -82.00-180.00   65
 18  ω     90.00 128.00   1.00    2.00    --   95.80 -82.00-120.00   38
 19  ω    153.00 182.00   1.00    2.00    --   95.80  45.00   0.00   29
 20  ω     77.00 104.00   1.00    2.00    --   95.80 -82.00  90.00   27
 21  ω     93.00 119.00   1.00    2.00    --   95.80 -82.00   0.00   26
 22  ω      6.00 115.00   1.00    2.00    --   95.80 -30.00-150.00  109
 23  ω     70.00 127.00   1.00    2.00    --   95.80 -82.00 150.00   57
 24  ω     11.00  96.00   1.00    2.00    --   95.80 -82.00  60.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0729151000
_diffrn_orient_matrix_UB_12      0.0541357000
_diffrn_orient_matrix_UB_13      0.1194875000
_diffrn_orient_matrix_UB_21      0.0620259000
_diffrn_orient_matrix_UB_22      0.1281410000
_diffrn_orient_matrix_UB_23      -0.0121181000
_diffrn_orient_matrix_UB_31      -0.1191991000
_diffrn_orient_matrix_UB_32      0.0660113000
_diffrn_orient_matrix_UB_33      0.0203904000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3742
_reflns_number_total             5043
_reflns_odcompleteness_completeness 99.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0700
_refine_ls_restrained_S_all      1.022
_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)+(0.0978P)²+2.7497P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1922
_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. Rigid bond restraints
 C23, C24, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C19, C20, C21, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C25 \\sim C26: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C19 \\sim C20 \\sim C21 \\sim C22: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C30 \\sim C29 \\sim C31 \\sim N2 \\sim Cl2 \\sim C32 \\sim Cl1 \\sim N3: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) N2(0.5) C31(0.5) N3(0.5) C32(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C14(H14), C18(H18)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_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
Br1 Br 0.05332(6) 0.53659(8) 0.39139(6) 0.0436(2) Uani 1 1 d . . . . .
Br2 Br 0.81040(7) 0.94280(8) 0.84872(5) 0.0479(3) Uani 1 1 d . . . . .
O1 O 0.8121(4) 0.4190(4) 0.0437(3) 0.0332(9) Uani 1 1 d . . . . .
N1 N 0.6181(4) 0.6231(5) 0.3842(4) 0.0289(11) Uani 1 1 d . . . . .
C1 C 0.4582(5) 0.6497(6) 0.4696(4) 0.0265(12) Uani 1 1 d . . . . .
C2 C 0.3299(6) 0.6329(6) 0.4751(5) 0.0319(13) Uani 1 1 d . . . . .
H2 H 0.311246 0.671130 0.538482 0.038 Uiso 1 1 calc R . . . .
C3 C 0.2297(5) 0.5584(7) 0.3848(5) 0.0348(14) Uani 1 1 d . . . . .
C4 C 0.2554(6) 0.4990(7) 0.2890(5) 0.0359(14) Uani 1 1 d . . . . .
H4 H 0.185732 0.448617 0.229838 0.043 Uiso 1 1 calc R . . . .
C5 C 0.3831(6) 0.5141(7) 0.2806(5) 0.0342(14) Uani 1 1 d . . . . .
H5 H 0.400936 0.474957 0.217096 0.041 Uiso 1 1 calc R . . . .
C6 C 0.4834(5) 0.5904(6) 0.3717(4) 0.0267(12) Uani 1 1 d . . . . .
C7 C 0.6808(5) 0.7007(6) 0.4897(4) 0.0275(12) Uani 1 1 d . . . . .
C8 C 0.8136(5) 0.7559(6) 0.5409(5) 0.0309(13) Uani 1 1 d . . . . .
H8 H 0.876050 0.744504 0.503958 0.037 Uiso 1 1 calc R . . . .
C9 C 0.8508(5) 0.8275(6) 0.6464(5) 0.0338(14) Uani 1 1 d . . . . .
H9 H 0.939358 0.864991 0.682054 0.041 Uiso 1 1 calc R . . . .
C10 C 0.7555(6) 0.8444(6) 0.7014(5) 0.0321(13) Uani 1 1 d . . . . .
C11 C 0.6234(5) 0.7904(6) 0.6515(4) 0.0292(13) Uani 1 1 d . . . . .
H11 H 0.561590 0.801911 0.689061 0.035 Uiso 1 1 calc R . . . .
C12 C 0.5846(5) 0.7187(6) 0.5448(5) 0.0262(12) Uani 1 1 d . . . . .
C13 C 0.6795(5) 0.5724(6) 0.3031(4) 0.0255(12) Uani 1 1 d . . . . .
C14 C 0.6755(5) 0.4378(6) 0.2627(5) 0.0286(12) Uani 1 1 d . . . . .
H14 H 0.636760 0.381932 0.291120 0.034 Uiso 1 1 calc R . . . .
C15 C 0.7276(5) 0.3815(6) 0.1802(4) 0.0282(12) Uani 1 1 d . . . . .
C16 C 0.7740(5) 0.4704(6) 0.1347(4) 0.0269(12) Uani 1 1 d . . . . .
C17 C 0.7914(5) 0.6092(6) 0.1805(5) 0.0295(13) Uani 1 1 d . . . . .
C18 C 0.7404(5) 0.6587(6) 0.2648(5) 0.0301(13) Uani 1 1 d . . . . .
H18 H 0.747250 0.750525 0.295614 0.036 Uiso 1 1 calc R . . . .
C19 C 0.7381(7) 0.2317(7) 0.1506(6) 0.0449(14) Uani 1 1 d . U . . .
C20 C 0.7660(10) 0.1939(9) 0.2555(7) 0.067(2) Uani 1 1 d . U . . .
H20A H 0.837267 0.258247 0.310038 0.101 Uiso 1 1 calc GR . . . .
H20B H 0.790159 0.106660 0.241956 0.101 Uiso 1 1 calc GR . . . .
H20C H 0.687549 0.193997 0.277992 0.101 Uiso 1 1 calc GR . . . .
C21 C 0.6130(9) 0.1450(9) 0.0776(9) 0.087(3) Uani 1 1 d . U . . .
H21A H 0.540873 0.168634 0.105502 0.130 Uiso 1 1 calc GR . . . .
H21B H 0.619617 0.053303 0.070022 0.130 Uiso 1 1 calc GR . . . .
H21C H 0.597185 0.156558 0.009782 0.130 Uiso 1 1 calc GR . . . .
C22 C 0.8589(7) 0.1982(7) 0.1158(6) 0.0462(15) Uani 1 1 d . U . . .
H22A H 0.851151 0.212552 0.049592 0.069 Uiso 1 1 calc GR . . . .
H22B H 0.865137 0.106297 0.107375 0.069 Uiso 1 1 calc GR . . . .
H22C H 0.937126 0.254494 0.168161 0.069 Uiso 1 1 calc GR . . . .
C23 C 0.8632(7) 0.7082(7) 0.1423(6) 0.0471(15) Uani 1 1 d . U . . .
C24 C 0.8894(12) 0.8490(9) 0.2169(10) 0.097(3) Uani 1 1 d . U . . .
H24A H 0.807303 0.874304 0.226556 0.145 Uiso 1 1 calc GR . . . .
H24B H 0.928519 0.907898 0.188023 0.145 Uiso 1 1 calc GR . . . .
H24C H 0.948978 0.854801 0.283769 0.145 Uiso 1 1 calc GR . . . .
C25 C 0.9960(8) 0.6717(8) 0.1321(8) 0.063(2) Uani 1 1 d . U . . .
H25A H 1.050665 0.672697 0.199420 0.094 Uiso 1 1 calc GR . . . .
H25B H 1.039263 0.735290 0.109404 0.094 Uiso 1 1 calc GR . . . .
H25C H 0.982126 0.583963 0.081161 0.094 Uiso 1 1 calc GR . . . .
C26 C 0.7781(11) 0.7031(13) 0.0317(9) 0.104(3) Uani 1 1 d . U . . .
H26A H 0.746320 0.611684 -0.012764 0.156 Uiso 1 1 calc GR . . . .
H26B H 0.831118 0.746880 0.000738 0.156 Uiso 1 1 calc GR . . . .
H26C H 0.703945 0.747726 0.038752 0.156 Uiso 1 1 calc GR . . . .
C27 C 0.7077(10) 0.3687(13) -0.0507(6) 0.097(4) Uani 1 1 d . . . . .
H27A H 0.714753 0.279093 -0.088388 0.145 Uiso 1 1 calc GR . . . .
H27B H 0.712154 0.423981 -0.093494 0.145 Uiso 1 1 calc GR . . . .
H27C H 0.624546 0.368660 -0.034976 0.145 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.5206(7) 0.8951(7) 0.2615(5) 0.0524(15) Uani 0.5 1 d . U P A 1
O2 O 0.7108(5) 1.1336(6) 0.6648(4) 0.0569(14) Uani 1 1 d . . . . .
C30 C 0.5180(7) 0.9577(7) 0.3978(6) 0.0445(15) Uani 1 1 d . U . . .
C29 C 0.6267(6) 1.0209(7) 0.4810(6) 0.0430(15) Uani 1 1 d . U . . .
C28 C 0.6144(6) 1.0695(8) 0.5892(6) 0.0470(18) Uani 1 1 d . . . . .
Cl2 Cl 0.7761(9) 1.0435(9) 0.4573(5) 0.0453(14) Uani 0.5 1 d . U P B 2
N2 N 0.8637(15) 1.0746(14) 0.4702(12) 0.057(3) Uani 0.5 1 d . U P B 1
C31 C 0.765(4) 1.054(4) 0.485(2) 0.040(4) Uani 0.5 1 d . U P B 1
N3 N 0.5354(19) 0.891(2) 0.2200(15) 0.054(5) Uani 0.5 1 d . U P A 2
C32 C 0.528(3) 0.925(3) 0.3041(19) 0.056(5) Uani 0.5 1 d . U P A 2


_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
Br1 C3 1.892(5) . ?
Br2 C10 1.903(6) . ?
O1 C16 1.394(6) . ?
O1 C27 1.401(9) . ?
N1 C6 1.394(7) . ?
N1 C7 1.397(7) . ?
N1 C13 1.432(7) . ?
C1 C2 1.381(7) . ?
C1 C6 1.420(8) . ?
C1 C12 1.442(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.381(8) . ?
C3 C4 1.398(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.388(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.391(8) . ?
C7 C8 1.389(8) . ?
C7 C12 1.416(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.366(9) . ?
C9 H9 0.9300 . ?
C9 C10 1.406(8) . ?
C10 C11 1.378(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.379(8) . ?
C13 C14 1.365(8) . ?
C13 C18 1.385(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.393(8) . ?
C15 C16 1.407(8) . ?
C15 C19 1.543(9) . ?
C16 C17 1.397(8) . ?
C17 C18 1.393(8) . ?
C17 C23 1.546(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.588(11) . ?
C19 C21 1.478(10) . ?
C19 C22 1.512(9) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.499(11) . ?
C23 C25 1.518(10) . ?
C23 C26 1.549(12) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
Cl1 C30 1.816(9) . ?
O2 C28 1.230(9) . ?
C30 C29 1.354(10) . ?
C30 C28 1.476(9) 2_676 ?
C30 C32 1.28(3) . ?
C29 C28 1.479(11) . ?
C29 Cl2 1.710(11) . ?
C29 C31 1.46(4) . ?
N2 C31 1.13(4) . ?
N3 C32 1.14(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
C16 O1 C27 115.1(5) . . ?
C6 N1 C7 108.2(4) . . ?
C6 N1 C13 124.1(5) . . ?
C7 N1 C13 127.4(4) . . ?
C2 C1 C6 119.3(5) . . ?
C2 C1 C12 134.3(5) . . ?
C6 C1 C12 106.4(5) . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C3 118.7(5) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 Br1 119.0(4) . . ?
C2 C3 C4 121.7(5) . . ?
C4 C3 Br1 119.3(5) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 121.1(6) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 121.5 . . ?
C4 C5 C6 117.0(5) . . ?
C6 C5 H5 121.5 . . ?
N1 C6 C1 109.3(5) . . ?
C5 C6 N1 128.4(5) . . ?
C5 C6 C1 122.3(5) . . ?
N1 C7 C12 108.9(5) . . ?
C8 C7 N1 130.0(5) . . ?
C8 C7 C12 121.1(5) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.7(5) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.1(5) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 Br2 119.2(4) . . ?
C11 C10 Br2 119.1(4) . . ?
C11 C10 C9 121.7(5) . . ?
C10 C11 H11 120.7 . . ?
C10 C11 C12 118.6(5) . . ?
C12 C11 H11 120.7 . . ?
C7 C12 C1 107.2(5) . . ?
C11 C12 C1 133.2(5) . . ?
C11 C12 C7 119.6(5) . . ?
C14 C13 N1 119.2(5) . . ?
C14 C13 C18 120.4(5) . . ?
C18 C13 N1 120.4(5) . . ?
C13 C14 H14 118.9 . . ?
C13 C14 C15 122.1(5) . . ?
C15 C14 H14 118.9 . . ?
C14 C15 C16 115.8(5) . . ?
C14 C15 C19 118.7(5) . . ?
C16 C15 C19 125.4(5) . . ?
O1 C16 C15 119.0(5) . . ?
O1 C16 C17 118.1(5) . . ?
C17 C16 C15 122.8(5) . . ?
C16 C17 C23 123.4(5) . . ?
C18 C17 C16 117.3(5) . . ?
C18 C17 C23 119.3(6) . . ?
C13 C18 C17 120.6(6) . . ?
C13 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C15 C19 C20 108.0(6) . . ?
C21 C19 C15 112.4(6) . . ?
C21 C19 C20 106.3(7) . . ?
C21 C19 C22 113.5(7) . . ?
C22 C19 C15 114.0(5) . . ?
C22 C19 C20 101.5(6) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17 C23 C26 109.7(6) . . ?
C24 C23 C17 112.1(6) . . ?
C24 C23 C25 107.4(7) . . ?
C24 C23 C26 108.9(9) . . ?
C25 C23 C17 111.0(6) . . ?
C25 C23 C26 107.6(8) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O1 C27 H27A 109.5 . . ?
O1 C27 H27B 109.5 . . ?
O1 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C30 Cl1 124.0(6) . . ?
C29 C30 C28 122.3(7) . 2_676 ?
C28 C30 Cl1 113.7(6) 2_676 . ?
C32 C30 C29 119.4(14) . . ?
C32 C30 C28 118.3(14) . 2_676 ?
C30 C29 C28 120.1(6) . . ?
C30 C29 Cl2 118.4(6) . . ?
C30 C29 C31 130.6(13) . . ?
C28 C29 Cl2 121.5(6) . . ?
C31 C29 C28 109.3(12) . . ?
O2 C28 C30 121.6(7) . 2_676 ?
O2 C28 C29 120.8(6) . . ?
C30 C28 C29 117.6(6) 2_676 . ?
N2 C31 C29 168(3) . . ?
N3 C32 C30 178(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.879
_oxdiff_exptl_absorpt_empirical_full_min 0.333
####################################################################### 
# 
# 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_exp_1861
_database_code_depnum_ccdc_archive 'CCDC 2073892'
loop_
_audit_author_name
_audit_author_address
SM ECNU
_audit_update_record             
;
2021-03-29 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_audit_creation_date             2021-03-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H29 Br2 N O'
_chemical_formula_sum            'C27 H29 Br2 N O'
_chemical_formula_weight         543.33
_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           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                   8.7418(2)
_cell_length_b                   40.2906(7)
_cell_length_c                   14.2849(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.339(2)
_cell_angle_gamma                90
_cell_volume                     4895.58(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    30044
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      73.9850
_cell_measurement_theta_min      3.8330
_shelx_estimated_absorpt_T_max   0.338
_shelx_estimated_absorpt_T_min   0.251
_exptl_absorpt_coefficient_mu    4.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1220
_diffrn_reflns_av_unetI/netI     0.0545
_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       -10
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49730
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.364
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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    -88.00  19.00   1.00    1.00    --    0.00 -38.00 -30.00  107
  2  ω    -47.00   8.00   1.00    1.00    --    0.00 -38.00 120.00   55
  3  ω    -88.00 -29.00   1.00    1.00    --    0.00 -38.00  60.00   59
  4  ω    -67.00   3.00   1.00    1.00    --    0.00 -19.00-150.00   70
  5  ω    -23.00  19.00   1.00    1.00    --    0.00 -38.00  60.00   42
  6  ω     91.00 184.00   1.00    1.00    --   95.80  30.00-120.00   93
  7  ω     35.00 106.00   1.00    1.00    --   95.80 -61.00 -60.00   71
  8  ω     15.00 112.00   1.00    1.00    --   95.80 -30.00 -90.00   97
  9  ω      6.00 120.00   1.00    1.00    --   95.80 -61.00-180.00  114
 10  ω      8.00 107.00   1.00    1.00    --   95.80 -61.00  60.00   99
 11  ω    133.00 162.00   1.00    1.00    --   95.80  30.00 150.00   29
 12  ω     68.00 139.00   1.00    1.00    --   95.80  15.00  60.00   71
 13  ω    157.00 183.00   1.00    1.00    --   95.80  15.00  60.00   26
 14  ω    123.00 168.00   1.00    1.00    --   95.80  45.00 -60.00   45
 15  ω     33.00 119.00   1.00    1.00    --   95.80 -82.00  60.00   86
 16  ω     71.00 118.00   1.00    1.00    --   95.80 -82.00 -60.00   47
 17  ω     89.00 115.00   1.00    1.00    --   95.80 -82.00 150.00   26
 18  ω     12.00  45.00   1.00    1.00    --   95.80 -82.00 150.00   33
 19  ω     21.00  47.00   1.00    1.00    --   95.80 -82.00-120.00   26
 20  ω     95.00 121.00   1.00    1.00    --   95.80 -82.00-120.00   26
 21  ω     15.00  48.00   1.00    1.00    --   95.80 -82.00 -60.00   33
 22  ω     80.00 106.00   1.00    1.00    --   95.80  30.00 150.00   26
 23  ω     22.00 128.00   1.00    1.00    --   95.80 -82.00-180.00  106
 24  ω     80.00 105.00   1.00    1.00    --   95.80 -82.00  30.00   25
 25  ω     83.00 125.00   1.00    1.00    --   95.80  82.00-120.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0284150000
_diffrn_orient_matrix_UB_12      0.0268228000
_diffrn_orient_matrix_UB_13      -0.0710359000
_diffrn_orient_matrix_UB_21      0.0386536000
_diffrn_orient_matrix_UB_22      -0.0271980000
_diffrn_orient_matrix_UB_23      -0.0667147000
_diffrn_orient_matrix_UB_31      -0.1746273000
_diffrn_orient_matrix_UB_32      -0.0016587000
_diffrn_orient_matrix_UB_33      -0.0528058000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8256
_reflns_number_total             8703
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.887
_refine_diff_density_min         -1.473
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         8703
_refine_ls_number_restraints     210
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0758
_refine_ls_restrained_S_all      1.111
_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)+(0.1102P)²+27.9044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.1988
_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. Restrained distances
 C19-C21
 1.52 with sigma of 0.01
 C19-C20
 1.52 with sigma of 0.01
 C19-C22
 1.52 with sigma of 0.01
 C23-C24
 1.52 with sigma of 0.01
 C23-C25
 1.52 with sigma of 0.01
 C23-C26
 1.52 with sigma of 0.01
 C46-C47
 1.52 with sigma of 0.01
 C46-C48
 1.52 with sigma of 0.01
 C46-C49
 1.52 with sigma of 0.01
 C50-C51
 1.52 with sigma of 0.01
 C50-C53
 1.52 with sigma of 0.01
 C50-C52
 1.52 with sigma of 0.01
3. Rigid bond restraints
 C46, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C49
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C19, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C19, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C23, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C25, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C26, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34, C35, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C20 \\sim C19: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C19 \\sim C22: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C19 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C23 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C23 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C23 \\sim C25: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C46 \\sim C47: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C46 \\sim C49: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C46 \\sim C48: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C50 \\sim C51: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C53 \\sim C50: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C50 \\sim C52: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C21) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C22) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C46) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C48) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C49) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C47) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C50) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C53) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C52) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C20) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), C14(H14), C18(H18),
 C29(H29), C30(H30), C32(H32), C36(H36), C38(H38), C39(H39), C41(H41), C45(H45)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_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
Br1 Br -0.05711(7) 0.41564(2) 0.32770(4) 0.02694(18) Uani 1 1 d . . . . .
Br2 Br 0.25862(8) 0.24159(2) 0.67502(5) 0.0367(2) Uani 1 1 d . . . . .
C1 C 0.4338(6) 0.35050(12) 0.6836(3) 0.0149(10) Uani 1 1 d . . . . .
C2 C 0.5120(6) 0.32828(14) 0.7524(4) 0.0204(11) Uani 1 1 d . . . . .
H2 H 0.598644 0.334984 0.799522 0.024 Uiso 1 1 calc R . . . .
C3 C 0.4586(6) 0.29611(14) 0.7492(4) 0.0213(11) Uani 1 1 d . . . . .
H3 H 0.510177 0.280760 0.794135 0.026 Uiso 1 1 calc R . . . .
C4 C 0.3272(6) 0.28634(13) 0.6786(4) 0.0199(10) Uani 1 1 d . . . . .
C5 C 0.2459(6) 0.30817(13) 0.6109(3) 0.0172(10) Uani 1 1 d . . . . .
H5 H 0.157716 0.301341 0.565144 0.021 Uiso 1 1 calc R . . . .
C6 C 0.2995(5) 0.34076(12) 0.6131(3) 0.0138(9) Uani 1 1 d . . . . .
C7 C 0.2502(6) 0.36954(12) 0.5527(3) 0.0143(9) Uani 1 1 d . . . . .
C8 C 0.3598(6) 0.39479(12) 0.5873(3) 0.0141(9) Uani 1 1 d . . . . .
C9 C 0.3469(6) 0.42598(13) 0.5433(4) 0.0193(10) Uani 1 1 d . . . . .
H9 H 0.419629 0.442615 0.566215 0.023 Uiso 1 1 calc R . . . .
C10 C 0.2241(6) 0.43146(13) 0.4654(4) 0.0202(10) Uani 1 1 d . . . . .
H10 H 0.213508 0.451920 0.434460 0.024 Uiso 1 1 calc R . . . .
C11 C 0.1153(6) 0.40629(13) 0.4329(3) 0.0167(10) Uani 1 1 d . . . . .
C12 C 0.1250(6) 0.37518(12) 0.4749(3) 0.0148(9) Uani 1 1 d . . . . .
H12 H 0.050821 0.358799 0.452018 0.018 Uiso 1 1 calc R . . . .
C13 C 0.5868(6) 0.40324(12) 0.7273(3) 0.0158(10) Uani 1 1 d . . . . .
C14 C 0.7000(6) 0.41814(13) 0.6891(4) 0.0179(10) Uani 1 1 d . . . . .
H14 H 0.702025 0.413872 0.625452 0.021 Uiso 1 1 calc R . . . .
C15 C 0.8118(6) 0.43946(12) 0.7430(3) 0.0152(10) Uani 1 1 d . . . . .
C16 C 0.8079(5) 0.44388(12) 0.8406(3) 0.0136(9) Uani 1 1 d . . . . .
C17 C 0.6904(6) 0.42970(12) 0.8811(3) 0.0152(10) Uani 1 1 d . . . . .
C18 C 0.5808(5) 0.40894(12) 0.8216(3) 0.0141(9) Uani 1 1 d . . . . .
H18 H 0.502709 0.398835 0.846144 0.017 Uiso 1 1 calc R . . . .
C19 C 0.6717(7) 0.43590(15) 0.9843(4) 0.0371(12) Uani 1 1 d D U . . .
C20 C 0.6973(13) 0.4718(2) 1.0155(7) 0.069(2) Uani 1 1 d D U . . .
H20A H 0.804164 0.477925 1.017807 0.103 Uiso 1 1 calc GR . . . .
H20B H 0.676214 0.474404 1.078103 0.103 Uiso 1 1 calc GR . . . .
H20C H 0.627617 0.485713 0.970302 0.103 Uiso 1 1 calc GR . . . .
C21 C 0.7956(13) 0.4172(3) 1.0564(7) 0.079(3) Uani 1 1 d D U . . .
H21A H 0.786476 0.393890 1.042321 0.119 Uiso 1 1 calc GR . . . .
H21B H 0.780831 0.421054 1.120022 0.119 Uiso 1 1 calc GR . . . .
H21C H 0.898040 0.424798 1.052540 0.119 Uiso 1 1 calc GR . . . .
C22 C 0.5157(10) 0.4248(3) 0.9991(7) 0.067(2) Uani 1 1 d D U . . .
H22A H 0.433900 0.438039 0.960289 0.101 Uiso 1 1 calc GR . . . .
H22B H 0.513857 0.427257 1.065664 0.101 Uiso 1 1 calc GR . . . .
H22C H 0.499304 0.401885 0.980861 0.101 Uiso 1 1 calc GR . . . .
C23 C 0.9295(6) 0.45638(13) 0.6920(4) 0.0256(11) Uani 1 1 d D U . . .
C24 C 0.9700(9) 0.49195(15) 0.7242(5) 0.0414(16) Uani 1 1 d D U . . .
H24A H 0.875307 0.503777 0.725924 0.062 Uiso 1 1 calc GR . . . .
H24B H 1.021571 0.502616 0.679884 0.062 Uiso 1 1 calc GR . . . .
H24C H 1.038583 0.491896 0.787295 0.062 Uiso 1 1 calc GR . . . .
C25 C 1.0785(8) 0.43520(19) 0.7081(7) 0.057(2) Uani 1 1 d D U . . .
H25A H 1.135889 0.437289 0.773804 0.086 Uiso 1 1 calc GR . . . .
H25B H 1.142928 0.442646 0.666181 0.086 Uiso 1 1 calc GR . . . .
H25C H 1.050305 0.412386 0.694542 0.086 Uiso 1 1 calc GR . . . .
C26 C 0.8613(11) 0.4581(3) 0.5831(5) 0.073(3) Uani 1 1 d D U . . .
H26A H 0.861228 0.436264 0.555951 0.109 Uiso 1 1 calc GR . . . .
H26B H 0.924328 0.472633 0.554382 0.109 Uiso 1 1 calc GR . . . .
H26C H 0.755517 0.466332 0.570846 0.109 Uiso 1 1 calc GR . . . .
C27 C 1.0599(8) 0.4500(2) 0.9456(6) 0.0504(19) Uani 1 1 d . . . . .
H27A H 1.134690 0.451651 0.906045 0.076 Uiso 1 1 calc GR . . . .
H27B H 1.042506 0.427025 0.957885 0.076 Uiso 1 1 calc GR . . . .
H27C H 1.100021 0.461238 1.005488 0.076 Uiso 1 1 calc GR . . . .
N1 N 0.4691(5) 0.38299(11) 0.6674(3) 0.0160(8) Uani 1 1 d . . . . .
O1 O 0.9162(4) 0.46478(10) 0.8976(3) 0.0246(8) Uani 1 1 d . . . . .
Br3 Br 0.79855(8) 0.31970(2) 0.59097(4) 0.0362(2) Uani 1 1 d . . . . .
Br4 Br 0.55650(8) 0.50311(2) 0.27715(5) 0.0346(2) Uani 1 1 d . . . . .
C28 C 0.3333(6) 0.39789(13) 0.2508(3) 0.0152(10) Uani 1 1 d . . . . .
C29 C 0.2627(6) 0.42272(14) 0.1887(4) 0.0201(10) Uani 1 1 d . . . . .
H29 H 0.171705 0.418418 0.141873 0.024 Uiso 1 1 calc R . . . .
C30 C 0.3293(6) 0.45394(14) 0.1972(4) 0.0219(11) Uani 1 1 d . . . . .
H30 H 0.283244 0.470940 0.156219 0.026 Uiso 1 1 calc R . . . .
C31 C 0.4672(6) 0.45989(12) 0.2680(4) 0.0192(10) Uani 1 1 d . . . . .
C32 C 0.5396(6) 0.43570(13) 0.3312(4) 0.0181(10) Uani 1 1 d . . . . .
H32 H 0.630894 0.440179 0.377633 0.022 Uiso 1 1 calc R . . . .
C33 C 0.4709(6) 0.40421(12) 0.3228(3) 0.0146(9) Uani 1 1 d . . . . .
C34 C 0.3902(6) 0.35067(13) 0.3360(3) 0.0162(8) Uani 1 1 d . U . . .
C35 C 0.5088(6) 0.37379(13) 0.3764(3) 0.0158(8) Uani 1 1 d . U . . .
C36 C 0.6304(6) 0.36492(13) 0.4530(3) 0.0180(8) Uani 1 1 d . U . . .
H36 H 0.709385 0.379876 0.479808 0.022 Uiso 1 1 calc R . . . .
C37 C 0.6295(6) 0.33288(14) 0.4880(4) 0.0224(9) Uani 1 1 d . U . . .
C38 C 0.5114(7) 0.30970(14) 0.4495(4) 0.0238(9) Uani 1 1 d . U . . .
H38 H 0.514347 0.288490 0.475518 0.029 Uiso 1 1 calc R . . . .
C39 C 0.3912(7) 0.31865(13) 0.3728(4) 0.0219(9) Uani 1 1 d . U . . .
H39 H 0.312403 0.303612 0.346176 0.026 Uiso 1 1 calc R . . . .
C40 C 0.1687(6) 0.34860(12) 0.1878(3) 0.0148(9) Uani 1 1 d . . . . .
C41 C 0.0368(6) 0.33567(13) 0.2099(4) 0.0202(11) Uani 1 1 d . . . . .
H41 H 0.024010 0.337561 0.272531 0.024 Uiso 1 1 calc R . . . .
C42 C -0.0796(6) 0.31966(12) 0.1409(4) 0.0189(10) Uani 1 1 d . . . . .
C43 C -0.0527(6) 0.31671(12) 0.0482(4) 0.0181(10) Uani 1 1 d . . . . .
C44 C 0.0781(6) 0.33166(12) 0.0210(3) 0.0156(10) Uani 1 1 d . . . . .
C45 C 0.1890(6) 0.34726(13) 0.0942(3) 0.0155(10) Uani 1 1 d . . . . .
H45 H 0.277667 0.356888 0.079951 0.019 Uiso 1 1 calc R . . . .
C46 C -0.2306(8) 0.30780(16) 0.1701(5) 0.0404(13) Uani 1 1 d D U . . .
C47 C -0.2720(14) 0.3314(3) 0.2411(9) 0.086(3) Uani 1 1 d D U . . .
H47A H -0.207954 0.326841 0.303962 0.129 Uiso 1 1 calc GR . . . .
H47B H -0.380834 0.328738 0.241898 0.129 Uiso 1 1 calc GR . . . .
H47C H -0.253837 0.353735 0.223030 0.129 Uiso 1 1 calc GR . . . .
C48 C -0.2132(12) 0.2725(2) 0.2051(8) 0.066(2) Uani 1 1 d D U . . .
H48A H -0.244256 0.257695 0.151349 0.099 Uiso 1 1 calc GR . . . .
H48B H -0.278713 0.268859 0.249592 0.099 Uiso 1 1 calc GR . . . .
H48C H -0.105479 0.268342 0.236618 0.099 Uiso 1 1 calc GR . . . .
C49 C -0.3788(10) 0.3089(3) 0.0865(7) 0.069(2) Uani 1 1 d D U . . .
H49A H -0.381657 0.329529 0.052619 0.103 Uiso 1 1 calc GR . . . .
H49B H -0.471042 0.306946 0.111789 0.103 Uiso 1 1 calc GR . . . .
H49C H -0.375604 0.290813 0.043144 0.103 Uiso 1 1 calc GR . . . .
C50 C 0.1001(6) 0.33242(14) -0.0826(4) 0.0281(11) Uani 1 1 d D U . . .
C51 C 0.2381(7) 0.35430(17) -0.0919(4) 0.0310(13) Uani 1 1 d D U . . .
H51A H 0.223924 0.376184 -0.068712 0.047 Uiso 1 1 calc GR . . . .
H51B H 0.243330 0.355498 -0.158201 0.047 Uiso 1 1 calc GR . . . .
H51C H 0.334042 0.344987 -0.054580 0.047 Uiso 1 1 calc GR . . . .
C52 C 0.1339(11) 0.29805(18) -0.1179(6) 0.0536(18) Uani 1 1 d D U . . .
H52A H 0.223470 0.288668 -0.074022 0.080 Uiso 1 1 calc GR . . . .
H52B H 0.155431 0.299871 -0.180602 0.080 Uiso 1 1 calc GR . . . .
H52C H 0.044200 0.283995 -0.121128 0.080 Uiso 1 1 calc GR . . . .
C53 C -0.0456(8) 0.3469(2) -0.1510(5) 0.0489(16) Uani 1 1 d D U . . .
H53A H -0.131311 0.331544 -0.157894 0.073 Uiso 1 1 calc GR . . . .
H53B H -0.023219 0.350936 -0.212700 0.073 Uiso 1 1 calc GR . . . .
H53C H -0.073759 0.367462 -0.125150 0.073 Uiso 1 1 calc GR . . . .
C54 C -0.1470(10) 0.26540(19) -0.0258(5) 0.048(2) Uani 1 1 d . . . . .
H54A H -0.185782 0.257616 -0.090440 0.073 Uiso 1 1 calc GR . . . .
H54B H -0.207199 0.255606 0.015388 0.073 Uiso 1 1 calc GR . . . .
H54C H -0.038532 0.259264 -0.003815 0.073 Uiso 1 1 calc GR . . . .
N2 N 0.2863(5) 0.36543(11) 0.2591(3) 0.0176(9) Uani 1 1 d . . . . .
O2 O -0.1610(5) 0.30037(11) -0.0236(3) 0.0340(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C11 1.905(5) . ?
Br2 C4 1.897(5) . ?
C1 C2 1.387(8) . ?
C1 C6 1.415(6) . ?
C1 N1 1.377(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.375(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.399(8) . ?
C4 C5 1.377(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(7) . ?
C6 C7 1.450(7) . ?
C7 C8 1.406(7) . ?
C7 C12 1.388(7) . ?
C8 C9 1.398(7) . ?
C8 N1 1.394(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.374(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.395(7) . ?
C11 C12 1.383(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.374(7) . ?
C13 C18 1.379(7) . ?
C13 N1 1.432(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.392(7) . ?
C15 C16 1.414(7) . ?
C15 C23 1.549(7) . ?
C16 C17 1.411(7) . ?
C16 O1 1.383(6) . ?
C17 C18 1.401(7) . ?
C17 C19 1.540(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.514(7) . ?
C19 C21 1.512(8) . ?
C19 C22 1.496(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.522(6) . ?
C23 C25 1.530(7) . ?
C23 C26 1.533(7) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27 O1 1.417(8) . ?
Br3 C37 1.904(5) . ?
Br4 C31 1.901(5) . ?
C28 C29 1.384(7) . ?
C28 C33 1.413(7) . ?
C28 N2 1.384(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.380(8) . ?
C30 H30 0.9300 . ?
C30 C31 1.404(7) . ?
C31 C32 1.378(8) . ?
C32 H32 0.9300 . ?
C32 C33 1.397(7) . ?
C33 C35 1.443(7) . ?
C34 C35 1.414(7) . ?
C34 C39 1.392(8) . ?
C34 N2 1.388(6) . ?
C35 C36 1.385(7) . ?
C36 H36 0.9300 . ?
C36 C37 1.386(8) . ?
C37 C38 1.406(8) . ?
C38 H38 0.9300 . ?
C38 C39 1.380(8) . ?
C39 H39 0.9300 . ?
C40 C41 1.367(7) . ?
C40 C45 1.389(7) . ?
C40 N2 1.439(6) . ?
C41 H41 0.9300 . ?
C41 C42 1.401(8) . ?
C42 C43 1.402(8) . ?
C42 C46 1.549(8) . ?
C43 C44 1.424(7) . ?
C43 O2 1.391(6) . ?
C44 C45 1.400(7) . ?
C44 C50 1.536(7) . ?
C45 H45 0.9300 . ?
C46 C47 1.493(8) . ?
C46 C48 1.504(7) . ?
C46 C49 1.547(8) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C51 1.524(6) . ?
C50 C52 1.525(7) . ?
C50 C53 1.531(7) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C54 O2 1.415(9) . ?

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
C2 C1 C6 121.2(5) . . ?
N1 C1 C2 129.8(4) . . ?
N1 C1 C6 109.0(4) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.5(5) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(5) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 Br2 119.3(4) . . ?
C5 C4 Br2 118.7(4) . . ?
C5 C4 C3 122.1(5) . . ?
C4 C5 H5 121.0 . . ?
C4 C5 C6 118.0(5) . . ?
C6 C5 H5 121.0 . . ?
C1 C6 C7 106.6(4) . . ?
C5 C6 C1 119.8(5) . . ?
C5 C6 C7 133.5(4) . . ?
C8 C7 C6 106.6(4) . . ?
C12 C7 C6 132.7(4) . . ?
C12 C7 C8 120.7(5) . . ?
C9 C8 C7 121.0(5) . . ?
N1 C8 C7 108.9(4) . . ?
N1 C8 C9 130.1(4) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 C8 118.4(5) . . ?
C10 C9 H9 120.8 . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.9(5) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 Br1 118.3(4) . . ?
C12 C11 Br1 118.6(4) . . ?
C12 C11 C10 123.1(5) . . ?
C7 C12 H12 121.5 . . ?
C11 C12 C7 117.0(4) . . ?
C11 C12 H12 121.5 . . ?
C14 C13 C18 120.5(4) . . ?
C14 C13 N1 119.8(4) . . ?
C18 C13 N1 119.6(4) . . ?
C13 C14 H14 119.0 . . ?
C13 C14 C15 121.9(4) . . ?
C15 C14 H14 119.0 . . ?
C14 C15 C16 116.7(4) . . ?
C14 C15 C23 118.0(4) . . ?
C16 C15 C23 125.3(4) . . ?
C17 C16 C15 122.6(4) . . ?
O1 C16 C15 119.2(4) . . ?
O1 C16 C17 118.0(4) . . ?
C16 C17 C19 125.1(4) . . ?
C18 C17 C16 117.0(4) . . ?
C18 C17 C19 117.9(4) . . ?
C13 C18 C17 121.1(4) . . ?
C13 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C20 C19 C17 113.3(6) . . ?
C21 C19 C17 110.7(6) . . ?
C21 C19 C20 104.0(8) . . ?
C22 C19 C17 112.8(6) . . ?
C22 C19 C20 108.8(7) . . ?
C22 C19 C21 106.7(8) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C15 113.9(4) . . ?
C24 C23 C25 110.4(6) . . ?
C24 C23 C26 105.9(6) . . ?
C25 C23 C15 108.6(5) . . ?
C25 C23 C26 107.2(7) . . ?
C26 C23 C15 110.6(5) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C27 H27A 109.5 . . ?
O1 C27 H27B 109.5 . . ?
O1 C27 H27C 109.5 . . ?
C1 N1 C8 108.9(4) . . ?
C1 N1 C13 126.8(4) . . ?
C8 N1 C13 123.9(4) . . ?
C16 O1 C27 116.0(5) . . ?
C29 C28 C33 121.0(5) . . ?
N2 C28 C29 129.8(4) . . ?
N2 C28 C33 109.1(4) . . ?
C28 C29 H29 120.5 . . ?
C30 C29 C28 119.1(5) . . ?
C30 C29 H29 120.5 . . ?
C29 C30 H30 120.2 . . ?
C29 C30 C31 119.6(5) . . ?
C31 C30 H30 120.2 . . ?
C30 C31 Br4 118.4(4) . . ?
C32 C31 Br4 118.9(4) . . ?
C32 C31 C30 122.6(5) . . ?
C31 C32 H32 121.2 . . ?
C31 C32 C33 117.5(5) . . ?
C33 C32 H32 121.2 . . ?
C28 C33 C35 106.6(4) . . ?
C32 C33 C28 120.2(5) . . ?
C32 C33 C35 133.2(5) . . ?
C39 C34 C35 121.1(5) . . ?
N2 C34 C35 109.0(4) . . ?
N2 C34 C39 129.9(5) . . ?
C34 C35 C33 106.6(4) . . ?
C36 C35 C33 132.8(5) . . ?
C36 C35 C34 120.6(5) . . ?
C35 C36 H36 121.3 . . ?
C35 C36 C37 117.3(5) . . ?
C37 C36 H36 121.3 . . ?
C36 C37 Br3 118.1(4) . . ?
C36 C37 C38 122.8(5) . . ?
C38 C37 Br3 119.1(4) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 C37 119.5(5) . . ?
C39 C38 H38 120.2 . . ?
C34 C39 H39 120.7 . . ?
C38 C39 C34 118.6(5) . . ?
C38 C39 H39 120.7 . . ?
C41 C40 C45 120.6(5) . . ?
C41 C40 N2 121.2(4) . . ?
C45 C40 N2 118.1(4) . . ?
C40 C41 H41 119.1 . . ?
C40 C41 C42 121.8(5) . . ?
C42 C41 H41 119.1 . . ?
C41 C42 C43 116.8(5) . . ?
C41 C42 C46 118.5(5) . . ?
C43 C42 C46 124.6(5) . . ?
C42 C43 C44 122.9(5) . . ?
O2 C43 C42 120.1(5) . . ?
O2 C43 C44 116.9(5) . . ?
C43 C44 C50 124.0(4) . . ?
C45 C44 C43 116.6(4) . . ?
C45 C44 C50 119.5(4) . . ?
C40 C45 C44 121.1(5) . . ?
C40 C45 H45 119.5 . . ?
C44 C45 H45 119.5 . . ?
C47 C46 C42 110.0(6) . . ?
C47 C46 C48 113.5(8) . . ?
C47 C46 C49 102.5(8) . . ?
C48 C46 C42 110.7(6) . . ?
C48 C46 C49 106.6(7) . . ?
C49 C46 C42 113.4(6) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
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 . . ?
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 . . ?
C51 C50 C44 111.9(4) . . ?
C51 C50 C52 106.2(5) . . ?
C51 C50 C53 106.4(5) . . ?
C52 C50 C44 112.1(5) . . ?
C52 C50 C53 109.4(6) . . ?
C53 C50 C44 110.6(5) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O2 C54 H54A 109.5 . . ?
O2 C54 H54B 109.5 . . ?
O2 C54 H54C 109.5 . . ?
C28 N2 C34 108.6(4) . . ?
C28 N2 C40 124.2(4) . . ?
C34 N2 C40 126.1(4) . . ?
C43 O2 C54 116.1(5) . . ?

_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 0.056 0.213 0.900 19.5 0.4 ?
2 0.056 0.287 0.400 19.5 0.4 ?
3 -0.056 0.713 0.600 19.5 0.4 ?
4 -0.056 0.787 0.100 19.5 0.7 ?
5 0.500 0.000 0.000 20.7 0.8 ?
6 0.500 0.500 0.500 20.7 0.8 ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.440
_oxdiff_exptl_absorpt_empirical_full_min 0.411
####################################################################### 
# 
# 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_mlj_h4_0m
_database_code_depnum_ccdc_archive 'CCDC 2071727'
loop_
_audit_author_name
_audit_author_address
H-four
;ECNU
China
;
_audit_update_record             
;
2021-03-20 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_audit_creation_date             2020-10-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C108 H116 N4 O4'
_chemical_formula_sum            'C108 H116 N4 O4'
_chemical_formula_weight         1534.04
_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 0.0052 0.0023 '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 0.0094 0.0046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0163 0.0086 '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        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   26.709(3)
_cell_length_b                   24.342(3)
_cell_length_c                   20.0808(16)
_cell_angle_alpha                90
_cell_angle_beta                 113.763(2)
_cell_angle_gamma                90
_cell_volume                     11948.8(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7806
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      30.760
_cell_measurement_theta_min      2.683
_shelx_estimated_absorpt_T_max   0.989
_shelx_estimated_absorpt_T_min   0.982
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0789 before and 0.0661 after correction. The Ratio of minimum to maximum transmission is 0.8215. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.853
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.883
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38346
_diffrn_reflns_point_group_measured_fraction_full 0.883
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        29.750
_diffrn_reflns_theta_max         31.238
_diffrn_reflns_theta_min         1.939
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.82704
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4521
_reflns_number_total             10295
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10295
_refine_ls_number_restraints     334
_refine_ls_R_factor_all          0.2529
_refine_ls_R_factor_gt           0.1790
_refine_ls_restrained_S_all      1.120
_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)+(0.0350P)²+115.5487P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3630
_refine_ls_wR_factor_ref         0.3894
_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. Restrained distances
 C31-C34
 1.52 with sigma of 0.01
 C31-C32
 1.52 with sigma of 0.01
 C33-C31
 1.52 with sigma of 0.01
 C35-C38
 1.52 with sigma of 0.01
 C35-C37
 1.52 with sigma of 0.01
 C46-C48
 1.52 with sigma of 0.01
 C46-C49
 1.52 with sigma of 0.01
 C46-C47
 1.52 with sigma of 0.01
 C50-C52
 1.52 with sigma of 0.01
 C50-C51
 1.52 with sigma of 0.01
 C52-C51
 2.1 with sigma of 0.02
 C50-C53
 1.52 with sigma of 0.001
 C35-C36
 1.52 with sigma of 0.001
 C51-C52 \\sim C52-C53 \\sim C53-C51
 with sigma of 0.02
 C51-C52 \\sim C52-C53
 with sigma of 0.02
3. Rigid bond restraints
 C6, C5, C4, C3, C2, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C29, C28, C27, C26, C25, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C39, O12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C44, C51, C52, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C32, C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C49
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C44, C42, C43, C41, C40, C45
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C42, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C27 \\sim C26 \\sim C25 \\sim C30 \\sim C29 \\sim C28: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C48 \\sim C46: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C46 \\sim C47: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C49 \\sim C46: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C31 \\sim C32: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C35 \\sim C38: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C35 \\sim C37: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C35 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C39 \\sim O12: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C50 \\sim C52 \\sim C53 \\sim C51: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C31 \\sim C33: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C31 \\sim C34: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C32 \\sim C31: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C50 \\sim C52: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C50 \\sim C51: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C50 \\sim C53: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C43 \\sim C42 \\sim C41 \\sim C40 \\sim C45 \\sim C44: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C14 \\sim C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C53)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C51) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C39) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C31) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C52) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C33) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), C14(H14), C16(H16),
 C17(H17), C20(H20), C21(H21), C23(H23), C26(H26), C30(H30), C41(H41), C43(H43)
5.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_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
N1 N 0.26414(19) 0.5234(2) 0.7943(3) 0.0504(15) Uani 1 1 d . . . . .
N2 N 0.3582(2) 0.6258(3) 0.3833(4) 0.0627(16) Uani 1 1 d . U . . .
C1 C 0.3137(2) 0.5336(3) 0.8500(4) 0.0409(12) Uani 1 1 d . U . . .
C2 C 0.3326(2) 0.5267(3) 0.9250(4) 0.0488(14) Uani 1 1 d . U . . .
H2 H 0.310500 0.510911 0.945698 0.059 Uiso 1 1 calc R . . . .
C3 C 0.3841(2) 0.5435(3) 0.9669(4) 0.0505(14) Uani 1 1 d . U . . .
H3 H 0.396071 0.539433 1.017020 0.061 Uiso 1 1 calc R . . . .
C4 C 0.4218(2) 0.5674(3) 0.9397(4) 0.0510(14) Uani 1 1 d . U . . .
C5 C 0.4012(2) 0.5713(3) 0.8649(4) 0.0467(13) Uani 1 1 d . U . . .
H5 H 0.424837 0.583813 0.844616 0.056 Uiso 1 1 calc R . . . .
C6 C 0.3507(2) 0.5587(3) 0.8195(4) 0.0444(13) Uani 1 1 d . U . . .
C7 C 0.3193(2) 0.5583(3) 0.7420(4) 0.0515(19) Uani 1 1 d . . . . .
C8 C 0.2678(2) 0.5386(3) 0.7277(4) 0.0523(19) Uani 1 1 d . . . . .
C9 C 0.2276(2) 0.5343(4) 0.6559(4) 0.068(3) Uani 1 1 d . . . . .
H9 H 0.193033 0.520412 0.646827 0.081 Uiso 1 1 calc R . . . .
C10 C 0.2410(3) 0.5511(4) 0.5998(4) 0.071(2) Uani 1 1 d . . . . .
H10 H 0.214463 0.550270 0.552415 0.085 Uiso 1 1 calc R . . . .
C11 C 0.2934(2) 0.5695(4) 0.6127(4) 0.063(2) Uani 1 1 d . . . . .
C12 C 0.3334(2) 0.5756(3) 0.6843(4) 0.055(2) Uani 1 1 d . . . . .
H12 H 0.367631 0.590428 0.693257 0.067 Uiso 1 1 calc R . . . .
C13 C 0.4275(2) 0.5933(3) 0.4920(4) 0.0520(17) Uani 1 1 d . U . . .
C14 C 0.4799(2) 0.5774(3) 0.5356(4) 0.0468(15) Uani 1 1 d . U . . .
H14 H 0.487359 0.563406 0.581674 0.056 Uiso 1 1 calc R . . . .
C15 C 0.5236(2) 0.5822(3) 0.5110(4) 0.0483(16) Uani 1 1 d . U . . .
C16 C 0.5098(3) 0.6008(3) 0.4402(4) 0.0615(19) Uani 1 1 d . U . . .
H16 H 0.537366 0.604706 0.423354 0.074 Uiso 1 1 calc R . . . .
C17 C 0.4559(3) 0.6139(4) 0.3932(4) 0.068(2) Uani 1 1 d . U . . .
H17 H 0.446992 0.622269 0.344554 0.082 Uiso 1 1 calc R . . . .
C18 C 0.4165(3) 0.6141(4) 0.4213(4) 0.0628(19) Uani 1 1 d . U . . .
C19 C 0.3350(3) 0.6137(3) 0.4336(4) 0.0493(18) Uani 1 1 d . . . . .
C20 C 0.2833(3) 0.6195(4) 0.4279(4) 0.071(2) Uani 1 1 d . . . . .
H20 H 0.256649 0.633023 0.384883 0.085 Uiso 1 1 calc R . . . .
C21 C 0.2697(3) 0.6060(4) 0.4837(4) 0.068(2) Uani 1 1 d . . . . .
H21 H 0.233601 0.610237 0.478125 0.082 Uiso 1 1 calc R . . . .
C22 C 0.3085(2) 0.5859(3) 0.5501(4) 0.054(2) Uani 1 1 d . . . . .
C23 C 0.3637(3) 0.5788(3) 0.5587(4) 0.057(2) Uani 1 1 d . . . . .
H23 H 0.390077 0.564460 0.601373 0.068 Uiso 1 1 calc R . . . .
C24 C 0.3769(2) 0.5943(3) 0.4999(4) 0.0467(17) Uani 1 1 d . . . . .
C25 C 0.2155(2) 0.5019(5) 0.7964(4) 0.084(2) Uani 1 1 d . U . . .
C26 C 0.1907(3) 0.4583(5) 0.7640(5) 0.092(2) Uani 1 1 d . U . . .
H26 H 0.206207 0.438569 0.737348 0.111 Uiso 1 1 calc R . . . .
C27 C 0.1421(3) 0.4381(5) 0.7655(5) 0.100(2) Uani 1 1 d . U . . .
C28 C 0.1258(3) 0.4621(6) 0.8132(6) 0.107(2) Uani 1 1 d . U . . .
C29 C 0.1449(3) 0.5106(6) 0.8451(5) 0.102(2) Uani 1 1 d . U . . .
C30 C 0.1926(3) 0.5323(5) 0.8374(5) 0.094(2) Uani 1 1 d . U . . .
H30 H 0.207920 0.565558 0.858918 0.112 Uiso 1 1 calc R . . . .
C31 C 0.1185(5) 0.5574(5) 0.8862(6) 0.129(3) Uani 1 1 d D U . . .
C32 C 0.1209(5) 0.5348(7) 0.9586(8) 0.170(5) Uani 1 1 d D U . . .
H32A H 0.108510 0.497399 0.952203 0.256 Uiso 1 1 calc GR . . . .
H32B H 0.097833 0.556522 0.974576 0.256 Uiso 1 1 calc GR . . . .
H32C H 0.157894 0.536385 0.994397 0.256 Uiso 1 1 calc GR . . . .
C33 C 0.0587(4) 0.5593(6) 0.8300(7) 0.131(3) Uani 1 1 d D U . . .
H33A H 0.052108 0.529225 0.796600 0.197 Uiso 1 1 calc GR . . . .
H33B H 0.052281 0.593370 0.803656 0.197 Uiso 1 1 calc GR . . . .
H33C H 0.034600 0.556627 0.854574 0.197 Uiso 1 1 calc GR . . . .
C34 C 0.1426(4) 0.6148(4) 0.8942(8) 0.127(4) Uani 1 1 d D U . . .
H34A H 0.179819 0.614223 0.929489 0.190 Uiso 1 1 calc GR . . . .
H34B H 0.121637 0.639548 0.909959 0.190 Uiso 1 1 calc GR . . . .
H34C H 0.141683 0.626820 0.848169 0.190 Uiso 1 1 calc GR . . . .
C35 C 0.1155(4) 0.3844(6) 0.7118(7) 0.156(5) Uani 1 1 d D U . . .
C36 C 0.1510(5) 0.3332(6) 0.7296(8) 0.175(7) Uani 1 1 d D U . . .
H36A H 0.182792 0.339848 0.719644 0.262 Uiso 1 1 calc GR . . . .
H36B H 0.130580 0.303121 0.700196 0.262 Uiso 1 1 calc GR . . . .
H36C H 0.162225 0.324171 0.780082 0.262 Uiso 1 1 calc GR . . . .
C37 C 0.0544(4) 0.3791(7) 0.6920(8) 0.193(7) Uani 1 1 d D U . . .
H37A H 0.045926 0.394182 0.730412 0.289 Uiso 1 1 calc GR . . . .
H37B H 0.044148 0.341096 0.685310 0.289 Uiso 1 1 calc GR . . . .
H37C H 0.034628 0.398871 0.647720 0.289 Uiso 1 1 calc GR . . . .
C38 C 0.1161(5) 0.3987(7) 0.6386(7) 0.167(6) Uani 1 1 d D U . . .
H38A H 0.081424 0.414188 0.607633 0.250 Uiso 1 1 calc GR . . . .
H38B H 0.122608 0.366048 0.616445 0.250 Uiso 1 1 calc GR . . . .
H38C H 0.144586 0.424884 0.645313 0.250 Uiso 1 1 calc GR . . . .
C39 C 0.0948(7) 0.4010(7) 0.8756(10) 0.190(6) Uani 1 1 d . U . . .
H39A H 0.103917 0.368625 0.855551 0.285 Uiso 1 1 calc GR . . . .
H39B H 0.065326 0.392875 0.889856 0.285 Uiso 1 1 calc GR . . . .
H39C H 0.126118 0.412932 0.917246 0.285 Uiso 1 1 calc GR . . . .
C40 C 0.3128(3) 0.6504(5) 0.1858(5) 0.0887(18) Uani 1 1 d . U . . .
C41 C 0.3370(3) 0.6269(4) 0.2554(4) 0.0649(17) Uani 1 1 d . U . . .
H41 H 0.355492 0.593726 0.260900 0.078 Uiso 1 1 calc R . . . .
C42 C 0.3344(3) 0.6516(4) 0.3167(5) 0.0751(18) Uani 1 1 d . U . . .
C43 C 0.3110(4) 0.7012(5) 0.3107(5) 0.097(2) Uani 1 1 d . U . . .
H43 H 0.311735 0.720063 0.351374 0.117 Uiso 1 1 calc R . . . .
C44 C 0.2838(5) 0.7244(6) 0.2366(7) 0.127(3) Uani 1 1 d . U . . .
C45 C 0.2887(4) 0.7023(5) 0.1814(6) 0.107(2) Uani 1 1 d . U . . .
C46 C 0.3222(4) 0.6215(4) 0.1227(6) 0.105(3) Uani 1 1 d D U . . .
C47 C 0.3443(5) 0.6607(5) 0.0831(7) 0.124(4) Uani 1 1 d D U . . .
H47A H 0.330057 0.696810 0.083518 0.186 Uiso 1 1 calc GR . . . .
H47B H 0.333487 0.648631 0.033719 0.186 Uiso 1 1 calc GR . . . .
H47C H 0.383514 0.661509 0.106816 0.186 Uiso 1 1 calc GR . . . .
C48 C 0.3704(5) 0.5835(6) 0.1506(7) 0.143(5) Uani 1 1 d D U . . .
H48A H 0.397746 0.598158 0.194545 0.215 Uiso 1 1 calc GR . . . .
H48B H 0.385403 0.579765 0.114638 0.215 Uiso 1 1 calc GR . . . .
H48C H 0.358942 0.548095 0.160316 0.215 Uiso 1 1 calc GR . . . .
C49 C 0.2663(5) 0.6051(6) 0.0670(7) 0.153(5) Uani 1 1 d D U . . .
H49A H 0.238558 0.624456 0.076557 0.229 Uiso 1 1 calc GR . . . .
H49B H 0.261340 0.566295 0.069928 0.229 Uiso 1 1 calc GR . . . .
H49C H 0.263562 0.614289 0.019133 0.229 Uiso 1 1 calc GR . . . .
C50 C 0.2519(6) 0.7786(5) 0.2313(8) 0.166(3) Uani 1 1 d D U . . .
C51 C 0.2658(6) 0.8010(7) 0.3075(8) 0.199(4) Uani 1 1 d D U . . .
H51A H 0.243905 0.782688 0.328692 0.299 Uiso 1 1 calc GR . . . .
H51B H 0.258300 0.839739 0.304707 0.299 Uiso 1 1 calc GR . . . .
H51C H 0.303798 0.794833 0.337084 0.299 Uiso 1 1 calc GR . . . .
C52 C 0.1926(5) 0.7747(7) 0.2232(9) 0.191(4) Uani 1 1 d D U . . .
H52A H 0.171218 0.802580 0.190073 0.287 Uiso 1 1 calc GR . . . .
H52B H 0.191211 0.780028 0.269745 0.287 Uiso 1 1 calc GR . . . .
H52C H 0.178161 0.739172 0.204531 0.287 Uiso 1 1 calc GR . . . .
C53 C 0.2447(7) 0.8350(5) 0.1963(9) 0.197(4) Uani 1 1 d D U . . .
H53A H 0.279849 0.849887 0.203987 0.295 Uiso 1 1 calc GR . . . .
H53B H 0.226709 0.858879 0.217828 0.295 Uiso 1 1 calc GR . . . .
H53C H 0.222869 0.831869 0.145053 0.295 Uiso 1 1 calc GR . . . .
C54 C 0.2001(5) 0.7062(8) 0.0763(6) 0.176(8) Uani 1 1 d . . . . .
H54A H 0.190059 0.700546 0.025212 0.264 Uiso 1 1 calc GR . . . .
H54B H 0.178446 0.735413 0.083084 0.264 Uiso 1 1 calc GR . . . .
H54C H 0.193609 0.673058 0.097582 0.264 Uiso 1 1 calc GR . . . .
O12 O 0.0791(3) 0.4413(5) 0.8249(6) 0.164(4) Uani 1 1 d . U . . .
O011 O 0.2537(4) 0.7196(5) 0.1088(5) 0.169(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.369(8) . ?
N1 C8 1.427(9) . ?
N1 C25 1.416(8) . ?
N2 C18 1.459(8) . ?
N2 C19 1.414(9) . ?
N2 C42 1.379(10) . ?
C1 C2 1.392(9) . ?
C1 C6 1.488(8) . ?
C2 C3 1.355(9) . ?
C3 C4 1.449(8) . ?
C4 C5 1.379(9) . ?
C4 C15 1.439(9) 2_656 ?
C5 C6 1.325(9) . ?
C6 C7 1.440(9) . ?
C7 C8 1.375(8) . ?
C7 C12 1.419(9) . ?
C8 C9 1.412(9) . ?
C9 C10 1.373(10) . ?
C10 C11 1.392(9) . ?
C11 C12 1.411(10) . ?
C11 C22 1.520(10) . ?
C13 C14 1.374(9) . ?
C13 C18 1.422(10) . ?
C13 C24 1.425(8) . ?
C14 C15 1.442(8) . ?
C15 C16 1.394(10) . ?
C16 C17 1.403(9) . ?
C17 C18 1.379(10) . ?
C19 C20 1.345(9) . ?
C19 C24 1.430(9) . ?
C20 C21 1.353(10) . ?
C21 C22 1.406(10) . ?
C22 C23 1.424(8) . ?
C23 C24 1.412(9) . ?
C25 C26 1.282(13) . ?
C25 C30 1.417(12) . ?
C26 C27 1.402(11) . ?
C27 C28 1.335(14) . ?
C27 C35 1.662(17) . ?
C28 C29 1.341(16) . ?
C28 O12 1.450(11) . ?
C29 C30 1.445(11) . ?
C29 C31 1.715(17) . ?
C31 C32 1.531(9) . ?
C31 C33 1.541(9) . ?
C31 C34 1.519(9) . ?
C35 C36 1.5201(10) . ?
C35 C37 1.520(9) . ?
C35 C38 1.519(9) . ?
C39 O12 1.352(17) . ?
C40 C41 1.404(10) . ?
C40 C45 1.403(14) . ?
C40 C46 1.554(14) . ?
C41 C42 1.397(11) . ?
C42 C43 1.342(12) . ?
C43 C44 1.481(14) . ?
C44 C45 1.285(16) . ?
C44 C50 1.550(17) . ?
C45 O011 1.443(12) . ?
C46 C47 1.506(8) . ?
C46 C48 1.500(8) . ?
C46 C49 1.514(9) . ?
C50 C51 1.524(9) . ?
C50 C52 1.528(9) . ?
C50 C53 1.5195(10) . ?
C54 O011 1.355(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C8 108.1(5) . . ?
C1 N1 C25 129.6(6) . . ?
C25 N1 C8 122.2(5) . . ?
C19 N2 C18 105.6(6) . . ?
C42 N2 C18 125.1(6) . . ?
C42 N2 C19 128.6(6) . . ?
N1 C1 C2 132.3(6) . . ?
N1 C1 C6 108.7(6) . . ?
C2 C1 C6 119.0(6) . . ?
C3 C2 C1 118.0(6) . . ?
C2 C3 C4 125.0(7) . . ?
C5 C4 C3 113.9(6) . . ?
C5 C4 C15 125.5(6) . 2_656 ?
C15 C4 C3 120.5(7) 2_656 . ?
C6 C5 C4 125.7(6) . . ?
C5 C6 C1 118.2(7) . . ?
C5 C6 C7 137.2(6) . . ?
C7 C6 C1 104.4(5) . . ?
C8 C7 C6 109.0(6) . . ?
C8 C7 C12 120.4(6) . . ?
C12 C7 C6 130.6(6) . . ?
C7 C8 N1 109.6(6) . . ?
C7 C8 C9 121.5(6) . . ?
C9 C8 N1 128.8(6) . . ?
C10 C9 C8 118.3(6) . . ?
C9 C10 C11 121.2(6) . . ?
C10 C11 C12 121.0(6) . . ?
C10 C11 C22 120.9(6) . . ?
C12 C11 C22 118.0(6) . . ?
C11 C12 C7 117.3(6) . . ?
C14 C13 C18 118.9(6) . . ?
C14 C13 C24 134.6(7) . . ?
C18 C13 C24 106.4(6) . . ?
C13 C14 C15 121.1(7) . . ?
C4 C15 C14 118.7(7) 2_656 . ?
C16 C15 C4 124.1(6) . 2_656 ?
C16 C15 C14 117.2(6) . . ?
C15 C16 C17 122.5(6) . . ?
C18 C17 C16 118.1(7) . . ?
C13 C18 N2 109.8(6) . . ?
C17 C18 N2 128.0(7) . . ?
C17 C18 C13 121.5(6) . . ?
N2 C19 C24 109.3(5) . . ?
C20 C19 N2 130.3(7) . . ?
C20 C19 C24 120.4(6) . . ?
C19 C20 C21 120.9(7) . . ?
C20 C21 C22 121.9(6) . . ?
C21 C22 C11 122.4(5) . . ?
C21 C22 C23 119.3(7) . . ?
C23 C22 C11 118.3(6) . . ?
C24 C23 C22 117.4(7) . . ?
C13 C24 C19 108.8(6) . . ?
C23 C24 C13 131.0(7) . . ?
C23 C24 C19 120.1(6) . . ?
N1 C25 C30 116.2(9) . . ?
C26 C25 N1 125.6(8) . . ?
C26 C25 C30 118.2(8) . . ?
C25 C26 C27 125.0(10) . . ?
C26 C27 C35 114.8(9) . . ?
C28 C27 C26 115.8(10) . . ?
C28 C27 C35 129.2(9) . . ?
C27 C28 C29 123.9(10) . . ?
C27 C28 O12 120.8(11) . . ?
C29 C28 O12 114.6(10) . . ?
C28 C29 C30 116.9(10) . . ?
C28 C29 C31 131.6(8) . . ?
C30 C29 C31 111.0(10) . . ?
C25 C30 C29 118.5(10) . . ?
C32 C31 C29 110.5(10) . . ?
C32 C31 C33 110.0(11) . . ?
C33 C31 C29 99.9(9) . . ?
C34 C31 C29 115.0(9) . . ?
C34 C31 C32 112.1(11) . . ?
C34 C31 C33 108.6(10) . . ?
C36 C35 C27 115.5(9) . . ?
C36 C35 C37 119.7(12) . . ?
C37 C35 C27 111.7(11) . . ?
C38 C35 C27 106.2(10) . . ?
C38 C35 C36 99.5(12) . . ?
C38 C35 C37 101.2(10) . . ?
C41 C40 C45 116.3(10) . . ?
C41 C40 C46 117.8(9) . . ?
C45 C40 C46 125.2(8) . . ?
C42 C41 C40 122.4(9) . . ?
N2 C42 C41 119.4(8) . . ?
C43 C42 N2 120.9(8) . . ?
C43 C42 C41 119.6(8) . . ?
C42 C43 C44 117.1(10) . . ?
C43 C44 C50 115.3(11) . . ?
C45 C44 C43 121.8(12) . . ?
C45 C44 C50 122.8(10) . . ?
C40 C45 O011 114.8(11) . . ?
C44 C45 C40 121.9(9) . . ?
C44 C45 O011 119.9(11) . . ?
C47 C46 C40 111.8(9) . . ?
C47 C46 C49 104.9(10) . . ?
C48 C46 C40 111.8(8) . . ?
C48 C46 C47 97.3(9) . . ?
C48 C46 C49 123.7(12) . . ?
C49 C46 C40 106.7(8) . . ?
C51 C50 C44 109.4(12) . . ?
C51 C50 C52 87.2(8) . . ?
C52 C50 C44 118.3(12) . . ?
C53 C50 C44 139.9(12) . . ?
C53 C50 C51 94.2(10) . . ?
C53 C50 C52 94.1(10) . . ?
C39 O12 C28 110.5(10) . . ?
C54 O011 C45 123.0(10) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_1216
_database_code_depnum_ccdc_archive 'CCDC 2071729'
loop_
_audit_author_name
_audit_author_address
H-five ECNU
_audit_update_record             
;
2021-03-20 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_audit_creation_date             2020-07-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C135 H145 N5 O5, 8(C H Cl3)'
_chemical_formula_sum            'C143 H153 Cl24 N5 O5'
_chemical_formula_weight         2872.49
_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'
Cl Cl 0.3639 0.7018 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.9844(3)
_cell_length_b                   20.5203(4)
_cell_length_c                   22.5310(4)
_cell_angle_alpha                113.094(2)
_cell_angle_beta                 90.2810(10)
_cell_angle_gamma                104.994(2)
_cell_volume                     7335.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    29910
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.1720
_cell_measurement_theta_min      3.2550
_shelx_estimated_absorpt_T_max   0.327
_shelx_estimated_absorpt_T_min   0.254
_exptl_absorpt_coefficient_mu    4.502
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2988
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            189783
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.997
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     43.00  73.00   1.00    1.00    --    0.00  82.00 -90.00   30
  2  ω    -23.00  84.00   1.00    1.00    --    0.00  57.00-180.00  107
  3  ω    -19.00  88.00   1.00    1.00    --    0.00  38.00 -30.00  107
  4  ω    -32.00  -4.00   1.00    1.00    --    0.00  82.00 -90.00   28
  5  ω     24.00  87.00   1.00    1.00    --    0.00  38.00 150.00   63
  6  ω    -32.00  36.00   1.00    1.00    --    0.00  82.00-120.00   68
  7  ω    -18.00  33.00   1.00    1.00    --    0.00  38.00  90.00   51
  8  ω    -30.00  14.00   1.00    1.00    --    0.00  77.00   0.00   44
  9  ω     42.00  69.00   1.00    1.00    --    0.00  82.00-120.00   27
 10  ω    -79.00 -54.00   1.00    1.00    --    0.00 -57.00-120.00   25
 11  ω      5.00  39.00   1.00    1.00    --    0.00  82.00 -90.00   34
 12  ω     39.00  89.00   1.00    1.00    --    0.00  38.00  90.00   50
 13  ω    -19.00  17.00   1.00    1.00    --    0.00  38.00 150.00   36
 14  ω     22.00  64.00   1.00    1.00    --    0.00  77.00   0.00   42
 15  ω    -32.00   5.00   1.00    1.00    --    0.00 -57.00-120.00   37
 16  ω     66.00  91.00   1.00    1.00    --   95.80  75.00 -96.64   25
 17  ω     70.00  95.00   1.00    1.00    --   95.80  64.00  94.81   25
 18  ω    115.00 141.00   1.00    1.00    --   95.80  57.00 127.75   26
 19  ω     65.00 170.00   1.00    1.00    --   95.80  76.00 170.76  105
 20  ω     68.00 125.00   1.00    1.00    --   95.80  68.00   0.79   57
 21  ω     72.00 105.00   1.00    1.00    --   95.80  57.00 127.75   33
 22  ω     69.00  97.00   1.00    1.00    --   95.80  65.00 131.58   28
 23  ω     63.00  89.00   1.00    1.00    --   95.80  81.00 137.11   26
 24  ω    112.00 139.00   1.00    1.00    --   95.80  81.00 137.11   27
 25  ω     63.00  89.00   1.00    1.00    --   95.80  82.00  30.00   26
 26  ω     65.00  91.00   1.00    1.00    --   95.80  77.00 -60.00   26
 27  ω     60.00 128.00   1.00    1.00    --   95.80 -82.00-180.00   68
 28  ω     65.00  92.00   1.00    1.00    --   95.80  77.00-150.00   27
 29  ω     30.00 128.00   1.00    1.00    --   95.80 -82.00 -30.00   98
 30  ω     63.00  89.00   1.00    1.00    --   95.80  82.00 -60.00   26
 31  ω     65.00  91.00   1.00    1.00    --   95.80  76.00 178.31   26
 32  ω    124.00 185.00   1.00    1.00    --   95.80  80.00  23.73   61
 33  ω    160.00 185.00   1.00    1.00    --   95.80  70.00  65.32   25
 34  ω     64.00  89.00   1.00    1.00    --   95.80  80.00  23.73   25
 35  ω     65.00  91.00   1.00    1.00    --   95.80  76.00 106.85   26
 36  ω     68.00  94.00   1.00    1.00    --   95.80  70.00  65.32   26
 37  ω     71.00  97.00   1.00    1.00    --   95.80  62.00  61.58   26
 38  ω     62.00 127.00   1.00    1.00    --   95.80 -82.00-150.00   65
 39  ω     63.00  89.00   1.00    1.00    --   95.80  82.00 150.00   26
 40  ω     65.00  90.00   1.00    1.00    --   95.80  77.00 -30.00   25
 41  ω     63.00  99.00   1.00    1.00    --   95.80  82.00 -90.00   36
 42  ω    110.00 185.00   1.00    1.00    --   95.80  82.00 -90.00   75
 43  ω     63.00  88.00   1.00    1.00    --   95.80  82.00  60.00   25
 44  ω     63.00  89.00   1.00    1.00    --   95.80  82.00-150.00   26
 45  ω     65.00  90.00   1.00    1.00    --   95.80  77.00  90.00   25
 46  ω     95.00 184.00   1.00    1.00    --   95.80  82.00 120.00   89
 47  ω     65.00  91.00   1.00    1.00    --   95.80  77.00 -90.00   26
 48  ω     63.00  89.00   1.00    1.00    --   95.80  82.00-120.00   26
 49  ω    116.00 183.00   1.00    1.00    --   95.80  81.00 -73.55   67
 50  ω     63.00  89.00   1.00    1.00    --   95.80  82.00 120.00   26
 51  ω    113.00 185.00   1.00    1.00    --   95.80  82.00-180.00   72
 52  ω     71.00  97.00   1.00    1.00    --   95.80  61.00 -30.00   26
 53  ω     63.00  88.00   1.00    1.00    --   95.80  81.00 -73.55   25
 54  ω     76.00 184.00   1.00    1.00    --   95.80  45.00-120.00  108
 55  ω    132.00 178.00   1.00    1.00    --   95.80  58.00-105.89   46
 56  ω     63.00  89.00   1.00    1.00    --   95.80  82.00-180.00   26
 57  ω     65.00  90.00   1.00    1.00    --   95.80  77.00   0.00   25
 58  ω      6.00  75.00   1.00    1.00    --   95.80 -82.00-120.00   69
 59  ω     96.00 128.00   1.00    1.00    --   95.80 -82.00-120.00   32
 60  ω     75.00 102.00   1.00    1.00    --   95.80  45.00 -60.00   27
 61  ω     75.00 101.00   1.00    1.00    --   95.80  45.00 -30.00   26
 62  ω    132.00 185.00   1.00    1.00    --   95.80  45.00 -30.00   53
 63  ω     39.00 125.00   1.00    1.00    --   95.80 -82.00 120.00   86
 64  ω     67.00  93.00   1.00    1.00    --   95.80  72.00-120.60   26
 65  ω     78.00 182.00   1.00    1.00    --   95.80  45.00  90.00  104
 66  ω     76.00 165.00   1.00    1.00    --   95.80  45.00   0.00   89
 67  ω    160.00 185.00   1.00    1.00    --   95.80  82.00 -30.00   25
 68  ω     63.00  89.00   1.00    1.00    --   95.80  82.00 -30.00   26
 69  ω     71.00 185.00   1.00    1.00    --   95.80  61.00-150.00  114
 70  ω     47.00 127.00   1.00    1.00    --   95.80 -82.00  30.00   80
 71  ω     65.00  90.00   1.00    1.00    --   95.80  77.00-120.00   25
 72  ω     65.00  96.00   1.00    1.00    --   95.80  77.00 150.00   31
 73  ω    119.00 144.00   1.00    1.00    --   95.80  77.00 150.00   25
 74  ω     73.00  99.00   1.00    1.00    --   95.80  61.00  30.00   26
 75  ω     63.00  89.00   1.00    1.00    --   95.80  82.00   0.00   26
 76  ω     70.00 185.00   1.00    1.00    --   95.80  66.00  98.02  115
 77  ω     71.00  97.00   1.00    1.00    --   95.80  58.00-105.89   26
 78  ω    149.00 174.00   1.00    1.00    --   95.80  65.00 131.58   25
 79  ω    116.00 176.00   1.00    1.00    --   95.80  48.00  62.75   60
 80  ω     74.00 110.00   1.00    1.00    --   95.80  48.00  62.75   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0790263000
_diffrn_orient_matrix_UB_12      -0.0107214000
_diffrn_orient_matrix_UB_13      -0.0206827000
_diffrn_orient_matrix_UB_21      0.0330355000
_diffrn_orient_matrix_UB_22      0.0304474000
_diffrn_orient_matrix_UB_23      0.0719190000
_diffrn_orient_matrix_UB_31      -0.0253396000
_diffrn_orient_matrix_UB_32      -0.0787435000
_diffrn_orient_matrix_UB_33      -0.0023392000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                19741
_reflns_number_total             26011
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.271
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1629
_refine_ls_number_reflns         26011
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.1062
_refine_ls_restrained_S_all      1.027
_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)+(0.1684P)²+21.7544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2803
_refine_ls_wR_factor_ref         0.3004
_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. Rigid bond restraints
 C81, C83, C82, C84
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C81 \\sim C83 \\sim C82 \\sim C84: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C139(H139),
 C140(H140), C141(H141)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C14(H14), C16(H16),
 C17(H17), C20(H20), C21(H21), C23(H23), C26(H26), C28(H28), C29(H29), C32(H32),
  C33(H33), C35(H35), C035(H035), C39(H39), C41(H41), C42(H42), C44(H44),
 C45(H45), C47(H47), C50(H50), C52(H52), C53(H53), C56(H56), C57(H57), C59(H59),
  C62(H62), C66(H66), C77(H77), C91(H91), C95(H95), C106(H106), C110(H110),
 C120(H120), C124(H124)
4.c Idealised Me refined as rotating group:
 C04A(H04A,H04B,H04C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,
 H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,
 H75B,H75C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C),
 C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,
 H89C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C),
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C103(H10G,H10H,H10I), C104(H10J,
 H10K,H10L), C112(H11A,H11B,H11C), C113(H11D,H11E,H11F), C114(H11G,H11H,H11I),
 C116(H11J,H11K,H11L), C117(H11M,H11N,H11O), C118(H11P,H11Q,H11R), C126(H12A,
 H12B,H12C), C127(H12D,H12E,H12F), C128(H12G,H12H,H12I), C130(H13A,H13B,H13C),
 C131(H13D,H13E,H13F), C132(H13G,H13H,H13I), C133(H13J,H13K,H13L)
;
_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
C0AA C 0.6760(3) 0.6297(3) -0.0111(2) 0.0210(9) Uani 1 1 d . . . . .
C2 C 0.6401(3) 0.5657(3) -0.0015(2) 0.0222(9) Uani 1 1 d . . . . .
H2 H 0.608591 0.568654 0.031546 0.027 Uiso 1 1 calc R . . . .
C3 C 0.6512(3) 0.4978(3) -0.0410(2) 0.0221(9) Uani 1 1 d . . . . .
C4 C 0.6986(3) 0.4965(3) -0.0915(2) 0.0305(11) Uani 1 1 d . . . . .
H4 H 0.706261 0.451602 -0.118485 0.037 Uiso 1 1 calc R . . . .
C04A C 0.2674(4) 0.2516(3) 0.5733(3) 0.0445(14) Uani 1 1 d . . . . .
H04A H 0.219606 0.222587 0.545565 0.067 Uiso 1 1 calc GR . . . .
H04B H 0.269119 0.238864 0.609873 0.067 Uiso 1 1 calc GR . . . .
H04C H 0.310208 0.241744 0.549381 0.067 Uiso 1 1 calc GR . . . .
C5 C 0.7338(3) 0.5579(3) -0.1024(2) 0.0296(10) Uani 1 1 d . . . . .
H5 H 0.764459 0.554692 -0.136058 0.036 Uiso 1 1 calc R . . . .
C6 C 0.7226(3) 0.6247(3) -0.0622(2) 0.0232(9) Uani 1 1 d . . . . .
C7 C 0.7282(3) 0.7437(3) -0.0120(2) 0.0235(9) Uani 1 1 d . . . . .
C8 C 0.7495(3) 0.8201(3) 0.0083(2) 0.0267(10) Uani 1 1 d . . . . .
H8 H 0.778706 0.842825 -0.015887 0.032 Uiso 1 1 calc R . . . .
C9 C 0.7253(3) 0.8607(3) 0.0656(2) 0.0259(10) Uani 1 1 d . . . . .
H9 H 0.740308 0.911904 0.081054 0.031 Uiso 1 1 calc R . . . .
C10 C 0.6783(3) 0.8267(3) 0.1017(2) 0.0238(9) Uani 1 1 d . . . . .
C11 C 0.6551(3) 0.7503(2) 0.0788(2) 0.0215(9) Uani 1 1 d . . . . .
H11 H 0.622640 0.727391 0.101233 0.026 Uiso 1 1 calc R . . . .
C12 C 0.6806(3) 0.7081(3) 0.0219(2) 0.0223(9) Uani 1 1 d . . . . .
C13 C 0.5678(3) 0.9140(2) 0.2384(2) 0.0232(9) Uani 1 1 d . . . . .
C14 C 0.5842(3) 0.8623(2) 0.1815(2) 0.0224(9) Uani 1 1 d . . . . .
H14 H 0.545847 0.819651 0.155590 0.027 Uiso 1 1 calc R . . . .
C15 C 0.6595(3) 0.8763(2) 0.1643(2) 0.0216(9) Uani 1 1 d . . . . .
C16 C 0.7170(3) 0.9394(3) 0.2056(2) 0.0260(10) Uani 1 1 d . . . . .
H16 H 0.767265 0.947109 0.194357 0.031 Uiso 1 1 calc R . . . .
C17 C 0.7020(3) 0.9910(2) 0.2626(2) 0.0247(9) Uani 1 1 d . . . . .
H17 H 0.740907 1.032539 0.289432 0.030 Uiso 1 1 calc R . . . .
C18 C 0.6265(3) 0.9778(2) 0.2777(2) 0.0233(9) Uani 1 1 d . . . . .
C19 C 0.5158(3) 0.9892(3) 0.3212(2) 0.0257(10) Uani 1 1 d . . . . .
C20 C 0.4586(3) 1.0126(3) 0.3596(2) 0.0323(11) Uani 1 1 d . . . . .
H20 H 0.470930 1.057421 0.395802 0.039 Uiso 1 1 calc R . . . .
C21 C 0.3839(3) 0.9672(3) 0.3422(2) 0.0329(11) Uani 1 1 d . . . . .
H21 H 0.345574 0.982422 0.367042 0.039 Uiso 1 1 calc R . . . .
C22 C 0.3630(3) 0.8985(3) 0.2879(2) 0.0292(10) Uani 1 1 d . . . . .
C23 C 0.4207(3) 0.8756(3) 0.2507(2) 0.0258(10) Uani 1 1 d . . . . .
H23 H 0.408282 0.830080 0.215182 0.031 Uiso 1 1 calc R . . . .
C24 C 0.4962(3) 0.9205(3) 0.2665(2) 0.0243(9) Uani 1 1 d . . . . .
C25 C 0.1879(3) 0.7408(3) 0.2656(2) 0.0268(10) Uani 1 1 d . . . . .
C26 C 0.2646(3) 0.7795(3) 0.2688(2) 0.0263(10) Uani 1 1 d . . . . .
H26 H 0.303853 0.757208 0.267418 0.032 Uiso 1 1 calc R . . . .
C27 C 0.2825(3) 0.8517(3) 0.2742(2) 0.0287(10) Uani 1 1 d . . . . .
C28 C 0.2207(3) 0.8818(3) 0.2707(2) 0.0310(11) Uani 1 1 d . . . . .
H28 H 0.232545 0.929325 0.272078 0.037 Uiso 1 1 calc R . . . .
C29 C 0.1443(3) 0.8438(3) 0.2655(2) 0.0303(11) Uani 1 1 d . . . . .
H29 H 0.104770 0.864226 0.262213 0.036 Uiso 1 1 calc R . . . .
C30 C 0.1282(3) 0.7736(3) 0.2652(2) 0.0269(10) Uani 1 1 d . . . . .
C31 C 0.0728(3) 0.6665(3) 0.2756(2) 0.0259(10) Uani 1 1 d . . . . .
C32 C 0.0251(3) 0.6127(3) 0.2923(2) 0.0258(10) Uani 1 1 d . . . . .
H32 H -0.027719 0.607724 0.293508 0.031 Uiso 1 1 calc R . . . .
C33 C 0.0592(3) 0.5669(3) 0.3070(2) 0.0265(10) Uani 1 1 d . . . . .
H33 H 0.028857 0.532032 0.320100 0.032 Uiso 1 1 calc R . . . .
C34 C 0.1382(3) 0.5711(3) 0.3028(2) 0.0247(9) Uani 1 1 d . . . . .
C35 C 0.1839(3) 0.6229(3) 0.2835(2) 0.0264(10) Uani 1 1 d . . . . .
H35 H 0.235534 0.624467 0.278371 0.032 Uiso 1 1 calc R . . . .
C035 C 0.6084(3) 1.1548(3) 0.3764(2) 0.0311(11) Uani 1 1 d . . . . .
H035 H 0.568320 1.147008 0.346032 0.037 Uiso 1 1 calc R . . . .
C36 C 0.1527(3) 0.6725(3) 0.2718(2) 0.0243(9) Uani 1 1 d . . . . .
C37 C 0.2494(3) 0.4514(2) 0.3735(2) 0.0233(9) Uani 1 1 d . . . . .
C38 C 0.2668(3) 0.4564(2) 0.3143(2) 0.0224(9) Uani 1 1 d . . . . .
C39 C 0.2286(3) 0.4926(2) 0.2898(2) 0.0236(9) Uani 1 1 d . . . . .
H39 H 0.239268 0.495405 0.250362 0.028 Uiso 1 1 calc R . . . .
C40 C 0.1738(3) 0.5251(3) 0.3244(2) 0.0245(9) Uani 1 1 d . . . . .
C41 C 0.1580(3) 0.5189(3) 0.3835(2) 0.0273(10) Uani 1 1 d . . . . .
H41 H 0.121158 0.539954 0.406120 0.033 Uiso 1 1 calc R . . . .
C42 C 0.1948(3) 0.4830(3) 0.4090(2) 0.0259(10) Uani 1 1 d . . . . .
H42 H 0.183843 0.479975 0.448319 0.031 Uiso 1 1 calc R . . . .
C43 C 0.3393(3) 0.3907(2) 0.3376(2) 0.0225(9) Uani 1 1 d . . . . .
C44 C 0.3899(3) 0.3475(3) 0.3285(2) 0.0264(10) Uani 1 1 d . . . . .
H44 H 0.401301 0.331573 0.359969 0.032 Uiso 1 1 calc R . . . .
C45 C 0.4226(3) 0.3291(3) 0.2709(2) 0.0270(10) Uani 1 1 d . . . . .
H45 H 0.456431 0.300102 0.263991 0.032 Uiso 1 1 calc R . . . .
C46 C 0.4070(3) 0.3524(2) 0.2222(2) 0.0221(9) Uani 1 1 d . . . . .
C47 C 0.3579(3) 0.3979(2) 0.2332(2) 0.0218(9) Uani 1 1 d . . . . .
H47 H 0.348143 0.415628 0.202708 0.026 Uiso 1 1 calc R . . . .
C48 C 0.3236(2) 0.4162(2) 0.2911(2) 0.0212(9) Uani 1 1 d . . . . .
C49 C 0.4998(3) 0.3287(2) 0.0661(2) 0.0208(9) Uani 1 1 d . . . . .
C50 C 0.4707(3) 0.3627(3) 0.1240(2) 0.0234(9) Uani 1 1 d . . . . .
H50 H 0.474671 0.412838 0.140049 0.028 Uiso 1 1 calc R . . . .
C51 C 0.4353(3) 0.3206(3) 0.1579(2) 0.0239(9) Uani 1 1 d . . . . .
C52 C 0.4254(3) 0.2445(3) 0.1310(2) 0.0250(9) Uani 1 1 d . . . . .
H52 H 0.400330 0.216958 0.153199 0.030 Uiso 1 1 calc R . . . .
C53 C 0.4514(3) 0.2083(2) 0.0726(2) 0.0224(9) Uani 1 1 d . . . . .
H53 H 0.442921 0.157366 0.054536 0.027 Uiso 1 1 calc R . . . .
C54 C 0.4907(3) 0.2521(3) 0.0426(2) 0.0230(9) Uani 1 1 d . . . . .
C55 C 0.5620(3) 0.2917(3) -0.0246(2) 0.0260(10) Uani 1 1 d . . . . .
C56 C 0.6073(3) 0.2960(3) -0.0733(2) 0.0361(12) Uani 1 1 d . . . . .
H56 H 0.619498 0.254657 -0.102730 0.043 Uiso 1 1 calc R . . . .
C57 C 0.6334(3) 0.3630(3) -0.0767(2) 0.0376(13) Uani 1 1 d . . . . .
H57 H 0.662782 0.365907 -0.109892 0.045 Uiso 1 1 calc R . . . .
C58 C 0.6183(3) 0.4282(3) -0.0326(2) 0.0228(9) Uani 1 1 d . . . . .
C59 C 0.5724(3) 0.4219(2) 0.0166(2) 0.0217(9) Uani 1 1 d . . . . .
H59 H 0.560490 0.463419 0.046190 0.026 Uiso 1 1 calc R . . . .
C60 C 0.5449(3) 0.3548(2) 0.0214(2) 0.0208(9) Uani 1 1 d . . . . .
C61 C 0.8107(3) 0.7098(3) -0.1025(2) 0.0244(9) Uani 1 1 d . . . . .
C62 C 0.8786(3) 0.6911(3) -0.0996(2) 0.0253(10) Uani 1 1 d . . . . .
H62 H 0.886059 0.669320 -0.071626 0.030 Uiso 1 1 calc R . . . .
C63 C 0.9364(3) 0.7046(3) -0.1383(2) 0.0247(9) Uani 1 1 d . . . . .
C64 C 0.9198(3) 0.7352(3) -0.1805(2) 0.0240(9) Uani 1 1 d . . . . .
C65 C 0.8547(3) 0.7620(3) -0.1790(2) 0.0248(9) Uani 1 1 d . . . . .
C66 C 0.7998(3) 0.7471(3) -0.1393(2) 0.0252(10) Uani 1 1 d . . . . .
H66 H 0.755203 0.762427 -0.137742 0.030 Uiso 1 1 calc R . . . .
C67 C 1.0119(3) 0.6858(3) -0.1281(2) 0.0306(11) Uani 1 1 d . . . . .
C68 C 1.0354(3) 0.7145(4) -0.0544(3) 0.0404(13) Uani 1 1 d . . . . .
H68A H 1.038905 0.766114 -0.033873 0.061 Uiso 1 1 calc GR . . . .
H68B H 1.084836 0.707416 -0.047101 0.061 Uiso 1 1 calc GR . . . .
H68C H 0.997175 0.687721 -0.036387 0.061 Uiso 1 1 calc GR . . . .
C69 C 0.9975(3) 0.6012(3) -0.1576(3) 0.0417(13) Uani 1 1 d . . . . .
H69A H 0.956934 0.579539 -0.137780 0.063 Uiso 1 1 calc GR . . . .
H69B H 1.044148 0.589858 -0.149917 0.063 Uiso 1 1 calc GR . . . .
H69C H 0.982355 0.581719 -0.203589 0.063 Uiso 1 1 calc GR . . . .
C70 C 1.0815(3) 0.7212(3) -0.1545(3) 0.0401(13) Uani 1 1 d . . . . .
H70A H 1.074365 0.697848 -0.201170 0.060 Uiso 1 1 calc GR . . . .
H70B H 1.127747 0.715263 -0.138481 0.060 Uiso 1 1 calc GR . . . .
H70C H 1.086309 0.772913 -0.140615 0.060 Uiso 1 1 calc GR . . . .
C71 C 0.8453(3) 0.8099(3) -0.2150(2) 0.0267(10) Uani 1 1 d . . . . .
C72 C 0.7705(3) 0.8330(3) -0.2025(3) 0.0371(12) Uani 1 1 d . . . . .
H72A H 0.726646 0.790189 -0.221620 0.056 Uiso 1 1 calc GR . . . .
H72B H 0.769239 0.867270 -0.221474 0.056 Uiso 1 1 calc GR . . . .
H72C H 0.768793 0.856088 -0.156513 0.056 Uiso 1 1 calc GR . . . .
C73 C 0.9139(3) 0.8802(3) -0.1908(3) 0.0382(12) Uani 1 1 d . . . . .
H73A H 0.914860 0.907074 -0.144867 0.057 Uiso 1 1 calc GR . . . .
H73B H 0.908329 0.910465 -0.212946 0.057 Uiso 1 1 calc GR . . . .
H73C H 0.961377 0.866902 -0.199308 0.057 Uiso 1 1 calc GR . . . .
C74 C 0.8420(3) 0.7687(3) -0.2894(2) 0.0337(11) Uani 1 1 d . . . . .
H74A H 0.892485 0.763776 -0.300121 0.051 Uiso 1 1 calc GR . . . .
H74B H 0.826025 0.796167 -0.310600 0.051 Uiso 1 1 calc GR . . . .
H74C H 0.805630 0.720579 -0.303769 0.051 Uiso 1 1 calc GR . . . .
C75 C 0.9550(3) 0.6701(3) -0.2830(2) 0.0336(11) Uani 1 1 d . . . . .
H75A H 0.981853 0.677240 -0.317716 0.050 Uiso 1 1 calc GR . . . .
H75B H 0.900355 0.650036 -0.297253 0.050 Uiso 1 1 calc GR . . . .
H75C H 0.973283 0.636535 -0.270942 0.050 Uiso 1 1 calc GR . . . .
C76 C 0.6332(3) 1.0957(3) 0.3745(2) 0.0277(10) Uani 1 1 d . . . . .
C77 C 0.6950(3) 1.1060(3) 0.4167(2) 0.0303(10) Uani 1 1 d . . . . .
H77 H 0.713268 1.066212 0.412708 0.036 Uiso 1 1 calc R . . . .
C78 C 0.7305(3) 1.1758(3) 0.4653(2) 0.0330(11) Uani 1 1 d . . . . .
C79 C 0.6991(3) 1.2333(3) 0.4699(2) 0.0358(12) Uani 1 1 d . . . . .
C80 C 0.6428(3) 1.2259(3) 0.4234(2) 0.0348(12) Uani 1 1 d . . . . .
C81 C 0.8009(3) 1.1833(4) 0.5101(3) 0.0475(13) Uani 1 1 d . U . . .
C82 C 0.8426(5) 1.1262(5) 0.4759(4) 0.084(3) Uani 1 1 d . U . . .
H82A H 0.807946 1.077679 0.464227 0.126 Uiso 1 1 calc GR . . . .
H82B H 0.886540 1.133079 0.504366 0.126 Uiso 1 1 calc GR . . . .
H82C H 0.859872 1.131593 0.437386 0.126 Uiso 1 1 calc GR . . . .
C83 C 0.8596(5) 1.2590(5) 0.5321(7) 0.113(3) Uani 1 1 d . U . . .
H83A H 0.892421 1.259555 0.498712 0.170 Uiso 1 1 calc GR . . . .
H83B H 0.890643 1.269172 0.571190 0.170 Uiso 1 1 calc GR . . . .
H83C H 0.832791 1.295890 0.540233 0.170 Uiso 1 1 calc GR . . . .
C84 C 0.7727(6) 1.1722(8) 0.5688(4) 0.107(3) Uani 1 1 d . U . . .
H84A H 0.733162 1.196598 0.583313 0.161 Uiso 1 1 calc GR . . . .
H84B H 0.815165 1.192654 0.602802 0.161 Uiso 1 1 calc GR . . . .
H84C H 0.751823 1.120381 0.557930 0.161 Uiso 1 1 calc GR . . . .
C85 C 0.6137(4) 1.2882(3) 0.4169(3) 0.0474(15) Uani 1 1 d . . . . .
C86 C 0.6533(5) 1.3670(4) 0.4641(4) 0.068(2) Uani 1 1 d . . . . .
H86A H 0.641295 1.373414 0.507187 0.102 Uiso 1 1 calc GR . . . .
H86B H 0.635275 1.400502 0.451716 0.102 Uiso 1 1 calc GR . . . .
H86C H 0.708390 1.376932 0.463388 0.102 Uiso 1 1 calc GR . . . .
C87 C 0.5257(4) 1.2730(4) 0.4257(4) 0.0637(19) Uani 1 1 d . . . . .
H87A H 0.497249 1.226588 0.392106 0.096 Uiso 1 1 calc GR . . . .
H87B H 0.507120 1.311811 0.423171 0.096 Uiso 1 1 calc GR . . . .
H87C H 0.518615 1.271405 0.467391 0.096 Uiso 1 1 calc GR . . . .
C88 C 0.6198(6) 1.2836(4) 0.3489(3) 0.068(2) Uani 1 1 d . . . . .
H88A H 0.671814 1.284629 0.338813 0.103 Uiso 1 1 calc GR . . . .
H88B H 0.607084 1.324808 0.345635 0.103 Uiso 1 1 calc GR . . . .
H88C H 0.584462 1.238409 0.318739 0.103 Uiso 1 1 calc GR . . . .
C89 C 0.6756(4) 1.3085(4) 0.5735(3) 0.0512(16) Uani 1 1 d . . . . .
H89A H 0.623661 1.299447 0.555381 0.077 Uiso 1 1 calc GR . . . .
H89B H 0.693068 1.357758 0.606803 0.077 Uiso 1 1 calc GR . . . .
H89C H 0.676681 1.273664 0.591827 0.077 Uiso 1 1 calc GR . . . .
C90 C -0.0146(3) 0.7433(3) 0.2753(2) 0.0258(10) Uani 1 1 d . . . . .
C91 C -0.0178(3) 0.8132(3) 0.3176(2) 0.0267(10) Uani 1 1 d . . . . .
H91 H 0.027369 0.847951 0.342499 0.032 Uiso 1 1 calc R . . . .
C92 C -0.0870(3) 0.8319(3) 0.3234(2) 0.0317(11) Uani 1 1 d . . . . .
C93 C -0.1542(3) 0.7758(3) 0.2875(2) 0.0299(11) Uani 1 1 d . . . . .
C94 C -0.1542(3) 0.7028(3) 0.2491(2) 0.0291(10) Uani 1 1 d . . . . .
C95 C -0.0811(3) 0.6898(3) 0.2413(2) 0.0277(10) Uani 1 1 d . . . . .
H95 H -0.077869 0.643770 0.212359 0.033 Uiso 1 1 calc R . . . .
C96 C -0.2250(3) 0.6338(3) 0.2145(3) 0.0375(12) Uani 1 1 d . . . . .
C97 C -0.2331(4) 0.6140(4) 0.1423(3) 0.0607(19) Uani 1 1 d . . . . .
H97A H -0.248417 0.651519 0.134227 0.091 Uiso 1 1 calc GR . . . .
H97B H -0.271725 0.567403 0.120578 0.091 Uiso 1 1 calc GR . . . .
H97C H -0.184337 0.610416 0.126204 0.091 Uiso 1 1 calc GR . . . .
C98 C -0.2112(4) 0.5694(4) 0.2274(4) 0.0588(18) Uani 1 1 d . . . . .
H98A H -0.163081 0.561203 0.212687 0.088 Uiso 1 1 calc GR . . . .
H98B H -0.252875 0.525485 0.204483 0.088 Uiso 1 1 calc GR . . . .
H98C H -0.209055 0.581206 0.273181 0.088 Uiso 1 1 calc GR . . . .
C99 C -0.3019(3) 0.6409(4) 0.2418(3) 0.0483(15) Uani 1 1 d . . . . .
H99A H -0.296105 0.652088 0.287375 0.072 Uiso 1 1 calc GR . . . .
H99B H -0.341670 0.595206 0.219657 0.072 Uiso 1 1 calc GR . . . .
H99C H -0.316094 0.679848 0.235283 0.072 Uiso 1 1 calc GR . . . .
C100 C -0.0859(3) 0.9117(3) 0.3695(3) 0.0374(12) Uani 1 1 d . . . . .
C101 C -0.0027(4) 0.9598(3) 0.4012(3) 0.0547(17) Uani 1 1 d . . . . .
H10A H 0.016976 0.939596 0.427665 0.082 Uiso 1 1 calc GR . . . .
H10B H -0.003598 1.009329 0.427700 0.082 Uiso 1 1 calc GR . . . .
H10C H 0.030141 0.960375 0.367824 0.082 Uiso 1 1 calc GR . . . .
C102 C -0.1147(5) 0.9511(4) 0.3320(3) 0.0553(17) Uani 1 1 d . . . . .
H10D H -0.088149 0.945311 0.294128 0.083 Uiso 1 1 calc GR . . . .
H10E H -0.104236 1.002706 0.359450 0.083 Uiso 1 1 calc GR . . . .
H10F H -0.169438 0.929784 0.318926 0.083 Uiso 1 1 calc GR . . . .
C103 C -0.1348(4) 0.9110(3) 0.4243(3) 0.0440(14) Uani 1 1 d . . . . .
H10G H -0.187429 0.882885 0.406298 0.066 Uiso 1 1 calc GR . . . .
H10H H -0.133418 0.960704 0.452337 0.066 Uiso 1 1 calc GR . . . .
H10I H -0.114573 0.888894 0.448730 0.066 Uiso 1 1 calc GR . . . .
C104 C -0.2499(4) 0.8037(4) 0.2371(3) 0.0506(16) Uani 1 1 d . . . . .
H10J H -0.255395 0.759197 0.198881 0.076 Uiso 1 1 calc GR . . . .
H10K H -0.212698 0.843944 0.232515 0.076 Uiso 1 1 calc GR . . . .
H10L H -0.298976 0.814235 0.242788 0.076 Uiso 1 1 calc GR . . . .
C105 C 0.2885(3) 0.3922(3) 0.4425(2) 0.0258(10) Uani 1 1 d . . . . .
C106 C 0.2173(3) 0.3546(3) 0.4516(2) 0.0259(10) Uani 1 1 d . . . . .
H106 H 0.174738 0.341280 0.421341 0.031 Uiso 1 1 calc R . . . .
C107 C 0.2072(3) 0.3360(3) 0.5050(2) 0.0287(10) Uani 1 1 d . . . . .
C108 C 0.2756(3) 0.3514(3) 0.5453(2) 0.0298(10) Uani 1 1 d . . . . .
C109 C 0.3483(3) 0.3926(3) 0.5383(2) 0.0292(10) Uani 1 1 d . . . . .
C110 C 0.3534(3) 0.4124(3) 0.4859(2) 0.0275(10) Uani 1 1 d . . . . .
H110 H 0.400752 0.439409 0.479996 0.033 Uiso 1 1 calc R . . . .
C111 C 0.4199(3) 0.4202(3) 0.5897(2) 0.0330(11) Uani 1 1 d . . . . .
C112 C 0.4422(4) 0.3577(4) 0.5985(3) 0.0458(14) Uani 1 1 d . . . . .
H11A H 0.405397 0.337868 0.622159 0.069 Uiso 1 1 calc GR . . . .
H11B H 0.492973 0.376250 0.622262 0.069 Uiso 1 1 calc GR . . . .
H11C H 0.442180 0.319632 0.556699 0.069 Uiso 1 1 calc GR . . . .
C113 C 0.4042(4) 0.4738(3) 0.6548(3) 0.0441(14) Uani 1 1 d . . . . .
H11D H 0.393875 0.514926 0.649532 0.066 Uiso 1 1 calc GR . . . .
H11E H 0.448732 0.491156 0.686347 0.066 Uiso 1 1 calc GR . . . .
H11F H 0.360115 0.448849 0.669338 0.066 Uiso 1 1 calc GR . . . .
C114 C 0.4916(3) 0.4634(3) 0.5695(3) 0.0380(12) Uani 1 1 d . . . . .
H11G H 0.503972 0.431387 0.528941 0.057 Uiso 1 1 calc GR . . . .
H11H H 0.534921 0.481209 0.602295 0.057 Uiso 1 1 calc GR . . . .
H11I H 0.480531 0.504471 0.564598 0.057 Uiso 1 1 calc GR . . . .
C115 C 0.1228(3) 0.3012(3) 0.5138(3) 0.0390(12) Uani 1 1 d . . . . .
C116 C 0.0944(4) 0.2196(4) 0.4638(3) 0.0585(18) Uani 1 1 d . . . . .
H11J H 0.098410 0.217563 0.420648 0.088 Uiso 1 1 calc GR . . . .
H11K H 0.041290 0.198851 0.467793 0.088 Uiso 1 1 calc GR . . . .
H11L H 0.125801 0.192025 0.471967 0.088 Uiso 1 1 calc GR . . . .
C117 C 0.1106(3) 0.3057(4) 0.5823(3) 0.0467(15) Uani 1 1 d . . . . .
H11M H 0.134659 0.273248 0.591025 0.070 Uiso 1 1 calc GR . . . .
H11N H 0.056034 0.291313 0.585544 0.070 Uiso 1 1 calc GR . . . .
H11O H 0.133330 0.355518 0.613472 0.070 Uiso 1 1 calc GR . . . .
C118 C 0.0709(4) 0.3431(5) 0.4985(4) 0.0599(19) Uani 1 1 d . . . . .
H11P H 0.090495 0.394886 0.525668 0.090 Uiso 1 1 calc GR . . . .
H11Q H 0.018915 0.324930 0.506680 0.090 Uiso 1 1 calc GR . . . .
H11R H 0.070909 0.335633 0.453705 0.090 Uiso 1 1 calc GR . . . .
C119 C 0.5464(3) 0.1607(3) -0.0423(2) 0.0250(10) Uani 1 1 d . . . . .
C120 C 0.4865(3) 0.0959(3) -0.0702(2) 0.0242(9) Uani 1 1 d . . . . .
H120 H 0.435204 0.097090 -0.068088 0.029 Uiso 1 1 calc R . . . .
C121 C 0.5035(3) 0.0292(3) -0.1014(2) 0.0284(10) Uani 1 1 d . . . . .
C122 C 0.5828(3) 0.0306(3) -0.1059(2) 0.0289(10) Uani 1 1 d . . . . .
C123 C 0.6429(3) 0.0939(3) -0.0718(2) 0.0321(11) Uani 1 1 d . . . . .
C124 C 0.6225(3) 0.1601(3) -0.0413(2) 0.0282(10) Uani 1 1 d . . . . .
H124 H 0.661323 0.204171 -0.020180 0.034 Uiso 1 1 calc R . . . .
C125 C 0.7305(3) 0.1001(3) -0.0618(3) 0.0405(13) Uani 1 1 d . . . . .
C126 C 0.7493(4) 0.0248(4) -0.0812(4) 0.071(2) Uani 1 1 d . . . . .
H12A H 0.713729 -0.005464 -0.064293 0.107 Uiso 1 1 calc GR . . . .
H12B H 0.801334 0.033464 -0.063471 0.107 Uiso 1 1 calc GR . . . .
H12C H 0.744319 0.000099 -0.127667 0.107 Uiso 1 1 calc GR . . . .
C127 C 0.7595(3) 0.1419(3) 0.0102(3) 0.0448(14) Uani 1 1 d . . . . .
H12D H 0.755076 0.191286 0.024844 0.067 Uiso 1 1 calc GR . . . .
H12E H 0.812847 0.143713 0.017286 0.067 Uiso 1 1 calc GR . . . .
H12F H 0.728981 0.117166 0.034102 0.067 Uiso 1 1 calc GR . . . .
C128 C 0.7775(4) 0.1426(5) -0.0981(4) 0.067(2) Uani 1 1 d . . . . .
H12G H 0.759218 0.117526 -0.143682 0.101 Uiso 1 1 calc GR . . . .
H12H H 0.831261 0.145534 -0.091580 0.101 Uiso 1 1 calc GR . . . .
H12I H 0.771600 0.191589 -0.081946 0.101 Uiso 1 1 calc GR . . . .
C129 C 0.4370(3) -0.0437(3) -0.1258(2) 0.0313(11) Uani 1 1 d . . . . .
C130 C 0.4308(4) -0.0882(3) -0.2004(2) 0.0382(12) Uani 1 1 d . . . . .
H13A H 0.437791 -0.055085 -0.221744 0.057 Uiso 1 1 calc GR . . . .
H13B H 0.380662 -0.123632 -0.215666 0.057 Uiso 1 1 calc GR . . . .
H13C H 0.470213 -0.113543 -0.210024 0.057 Uiso 1 1 calc GR . . . .
C131 C 0.4529(4) -0.0904(3) -0.0910(3) 0.0414(13) Uani 1 1 d . . . . .
H13D H 0.499611 -0.103902 -0.103549 0.062 Uiso 1 1 calc GR . . . .
H13E H 0.410303 -0.134293 -0.102932 0.062 Uiso 1 1 calc GR . . . .
H13F H 0.458879 -0.062424 -0.044887 0.062 Uiso 1 1 calc GR . . . .
C132 C 0.3584(3) -0.0300(3) -0.1104(3) 0.0371(12) Uani 1 1 d . . . . .
H13G H 0.360875 -0.000998 -0.064655 0.056 Uiso 1 1 calc GR . . . .
H13H H 0.319502 -0.076428 -0.122420 0.056 Uiso 1 1 calc GR . . . .
H13I H 0.345406 -0.003930 -0.134319 0.056 Uiso 1 1 calc GR . . . .
C133 C 0.6187(4) -0.0358(4) -0.2073(3) 0.0511(16) Uani 1 1 d . . . . .
H13J H 0.624375 -0.083321 -0.234428 0.077 Uiso 1 1 calc GR . . . .
H13K H 0.666623 0.001532 -0.200944 0.077 Uiso 1 1 calc GR . . . .
H13L H 0.578468 -0.025916 -0.227772 0.077 Uiso 1 1 calc GR . . . .
N1 N 0.7521(2) 0.6926(2) -0.06361(18) 0.0237(8) Uani 1 1 d . . . . .
N2 N 0.5937(2) 1.0228(2) 0.32807(18) 0.0265(8) Uani 1 1 d . . . . .
N3 N 0.0582(2) 0.7271(2) 0.26901(19) 0.0265(8) Uani 1 1 d . . . . .
N4 N 0.2949(2) 0.4127(2) 0.38859(17) 0.0232(8) Uani 1 1 d . . . . .
N5 N 0.5285(2) 0.2301(2) -0.01236(17) 0.0252(8) Uani 1 1 d . . . . .
O1 O 0.96912(19) 0.73956(18) -0.22821(15) 0.0284(7) Uani 1 1 d . . . . .
O2 O 0.7254(2) 1.3006(2) 0.52367(18) 0.0432(9) Uani 1 1 d . . . . .
O3 O -0.2237(2) 0.7944(2) 0.29269(18) 0.0368(8) Uani 1 1 d . . . . .
O4 O 0.2724(2) 0.3279(2) 0.59546(17) 0.0372(8) Uani 1 1 d . . . . .
O5 O 0.5983(2) -0.0351(2) -0.14498(17) 0.0395(9) Uani 1 1 d . . . . .
C134 C 0.8820(4) 1.1576(5) 0.2489(5) 0.080(3) Uani 1 1 d . . . . .
H134 H 0.922584 1.198334 0.246122 0.096 Uiso 1 1 calc R . . . .
Cl4 Cl 0.85456(13) 1.08515(14) 0.17114(16) 0.1014(8) Uani 1 1 d . . . . .
Cl5 Cl 0.80065(14) 1.18867(15) 0.27583(17) 0.1009(8) Uani 1 1 d . . . . .
Cl6 Cl 0.91823(14) 1.1265(2) 0.30079(17) 0.1367(15) Uani 1 1 d . . . . .
C135 C 0.9556(4) 0.7998(4) 0.1469(3) 0.0564(18) Uani 1 1 d . . . . .
H135 H 0.937495 0.794207 0.186110 0.068 Uiso 1 1 calc R . . . .
Cl1 Cl 1.01612(10) 0.74271(12) 0.11544(7) 0.0642(5) Uani 1 1 d . . . . .
Cl2 Cl 0.87437(11) 0.77313(16) 0.09011(10) 0.0866(7) Uani 1 1 d . . . . .
Cl3 Cl 1.00785(15) 0.89354(15) 0.16863(12) 0.0880(7) Uani 1 1 d . . . . .
C136 C 0.8195(5) 0.4218(4) 0.3428(4) 0.0649(19) Uani 1 1 d . . . . .
H136 H 0.779158 0.374946 0.320346 0.078 Uiso 1 1 calc R . . . .
Cl10 Cl 0.77330(12) 0.48800(11) 0.38784(9) 0.0697(5) Uani 1 1 d . . . . .
Cl11 Cl 0.8812(3) 0.4083(2) 0.39277(17) 0.1476(15) Uani 1 1 d . . . . .
Cl12 Cl 0.86644(11) 0.44562(12) 0.28324(11) 0.0799(6) Uani 1 1 d . . . . .
C137 C 0.6612(3) 0.3141(3) 0.1600(3) 0.0437(13) Uani 1 1 d . . . . .
H137 H 0.611921 0.279621 0.134981 0.052 Uiso 1 1 calc R . . . .
Cl7 Cl 0.71490(10) 0.34980(9) 0.10975(7) 0.0518(4) Uani 1 1 d . . . . .
Cl8 Cl 0.71132(9) 0.26573(8) 0.18739(7) 0.0466(3) Uani 1 1 d . . . . .
Cl9 Cl 0.64107(9) 0.38554(10) 0.22773(8) 0.0551(4) Uani 1 1 d . . . . .
C138 C 0.4926(4) 0.6454(4) 0.2424(4) 0.0567(17) Uani 1 1 d . . . . .
H138 H 0.532679 0.648783 0.273903 0.068 Uiso 1 1 calc R . . . .
Cl13 Cl 0.49649(13) 0.57529(13) 0.16676(12) 0.0893(7) Uani 1 1 d . . . . .
Cl14 Cl 0.5143(2) 0.72681(13) 0.23399(15) 0.1090(9) Uani 1 1 d . . . . .
Cl15 Cl 0.40291(12) 0.6190(2) 0.26758(12) 0.1146(11) Uani 1 1 d . . . . .
C139 C 0.1509(5) 0.5379(5) 0.0232(4) 0.071(2) Uani 1 1 d . . . . .
H139 H 0.204372 0.534752 0.022058 0.086 Uiso 1 1 calc R . . . .
Cl22 Cl 0.08861(15) 0.44792(15) -0.00604(13) 0.0938(7) Uani 1 1 d . . . . .
Cl23 Cl 0.13559(18) 0.5801(2) -0.02714(19) 0.1252(12) Uani 1 1 d . . . . .
Cl24 Cl 0.13832(17) 0.58603(19) 0.10377(12) 0.1159(11) Uani 1 1 d . . . . .
C140 C 0.5607(5) 0.8941(5) 0.4122(4) 0.079(2) Uani 1 1 d . . . . .
H140 H 0.528811 0.898203 0.379165 0.095 Uiso 1 1 calc R . . . .
Cl16 Cl 0.6443(2) 0.8732(2) 0.37955(14) 0.1243(12) Uani 1 1 d . . . . .
Cl17 Cl 0.5060(3) 0.8280(3) 0.4352(3) 0.192(2) Uani 1 1 d . . . . .
Cl18 Cl 0.58964(18) 0.97763(16) 0.47633(14) 0.1004(8) Uani 1 1 d . . . . .
C141 C 0.7452(9) 0.9028(8) 0.6262(6) 0.130(5) Uani 1 1 d . . . . .
H141 H 0.710800 0.931057 0.650766 0.156 Uiso 1 1 calc R . . . .
Cl19 Cl 0.75495(17) 0.92780(13) 0.55970(10) 0.0878(7) Uani 1 1 d . . . . .
Cl20 Cl 0.82794(14) 0.94085(12) 0.67904(12) 0.0823(6) Uani 1 1 d . . . . .
Cl21 Cl 0.69465(18) 0.8169(2) 0.61039(17) 0.1232(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C0AA C2 1.404(7) . ?
C0AA C6 1.415(6) . ?
C0AA C12 1.463(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.396(6) . ?
C3 C4 1.420(6) . ?
C3 C58 1.485(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.372(7) . ?
C04A H04A 0.9600 . ?
C04A H04B 0.9600 . ?
C04A H04C 0.9600 . ?
C04A O4 1.422(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.382(6) . ?
C6 N1 1.370(6) . ?
C7 C8 1.393(7) . ?
C7 C12 1.405(6) . ?
C7 N1 1.384(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.378(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.418(6) . ?
C10 C11 1.385(7) . ?
C10 C15 1.482(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.395(6) . ?
C13 C14 1.399(6) . ?
C13 C18 1.406(7) . ?
C13 C24 1.452(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.400(6) . ?
C15 C16 1.403(7) . ?
C16 H16 0.9300 . ?
C16 C17 1.388(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.387(7) . ?
C18 N2 1.397(6) . ?
C19 C20 1.405(7) . ?
C19 C24 1.417(6) . ?
C19 N2 1.371(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.373(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.412(7) . ?
C22 C23 1.398(6) . ?
C22 C27 1.468(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.382(7) . ?
C25 C26 1.388(7) . ?
C25 C30 1.409(6) . ?
C25 C36 1.443(7) . ?
C26 H26 0.9300 . ?
C26 C27 1.388(7) . ?
C27 C28 1.419(7) . ?
C28 H28 0.9300 . ?
C28 C29 1.372(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.392(7) . ?
C30 N3 1.395(6) . ?
C31 C32 1.391(7) . ?
C31 C36 1.416(6) . ?
C31 N3 1.396(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.381(7) . ?
C33 H33 0.9300 . ?
C33 C34 1.405(6) . ?
C34 C35 1.381(7) . ?
C34 C40 1.487(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.386(7) . ?
C035 H035 0.9300 . ?
C035 C76 1.382(7) . ?
C035 C80 1.396(7) . ?
C37 C38 1.408(6) . ?
C37 C42 1.398(6) . ?
C37 N4 1.401(6) . ?
C38 C39 1.383(6) . ?
C38 C48 1.449(6) . ?
C39 H39 0.9300 . ?
C39 C40 1.402(6) . ?
C40 C41 1.408(6) . ?
C41 H41 0.9300 . ?
C41 C42 1.376(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.390(6) . ?
C43 C48 1.399(6) . ?
C43 N4 1.397(5) . ?
C44 H44 0.9300 . ?
C44 C45 1.382(6) . ?
C45 H45 0.9300 . ?
C45 C46 1.412(6) . ?
C46 C47 1.399(6) . ?
C46 C51 1.489(6) . ?
C47 H47 0.9300 . ?
C47 C48 1.401(6) . ?
C49 C50 1.394(6) . ?
C49 C54 1.412(6) . ?
C49 C60 1.471(6) . ?
C50 H50 0.9300 . ?
C50 C51 1.404(6) . ?
C51 C52 1.397(7) . ?
C52 H52 0.9300 . ?
C52 C53 1.386(6) . ?
C53 H53 0.9300 . ?
C53 C54 1.384(6) . ?
C54 N5 1.387(5) . ?
C55 C56 1.387(7) . ?
C55 C60 1.414(6) . ?
C55 N5 1.386(6) . ?
C56 H56 0.9300 . ?
C56 C57 1.365(7) . ?
C57 H57 0.9300 . ?
C57 C58 1.413(6) . ?
C58 C59 1.412(6) . ?
C59 H59 0.9300 . ?
C59 C60 1.386(6) . ?
C61 C62 1.378(7) . ?
C61 C66 1.375(7) . ?
C61 N1 1.436(5) . ?
C62 H62 0.9300 . ?
C62 C63 1.404(6) . ?
C63 C64 1.396(7) . ?
C63 C67 1.543(6) . ?
C64 C65 1.413(7) . ?
C64 O1 1.412(5) . ?
C65 C66 1.390(6) . ?
C65 C71 1.539(7) . ?
C66 H66 0.9300 . ?
C67 C68 1.543(7) . ?
C67 C69 1.543(8) . ?
C67 C70 1.526(7) . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 C72 1.530(7) . ?
C71 C73 1.534(7) . ?
C71 C74 1.546(6) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?
C75 O1 1.432(6) . ?
C76 C77 1.376(7) . ?
C76 N2 1.432(6) . ?
C77 H77 0.9300 . ?
C77 C78 1.395(7) . ?
C78 C79 1.405(8) . ?
C78 C81 1.552(8) . ?
C79 C80 1.391(8) . ?
C79 O2 1.394(6) . ?
C80 C85 1.554(8) . ?
C81 C82 1.510(9) . ?
C81 C83 1.520(11) . ?
C81 C84 1.497(11) . ?
C82 H82A 0.9600 . ?
C82 H82B 0.9600 . ?
C82 H82C 0.9600 . ?
C83 H83A 0.9600 . ?
C83 H83B 0.9600 . ?
C83 H83C 0.9600 . ?
C84 H84A 0.9600 . ?
C84 H84B 0.9600 . ?
C84 H84C 0.9600 . ?
C85 C86 1.518(9) . ?
C85 C87 1.562(10) . ?
C85 C88 1.504(9) . ?
C86 H86A 0.9600 . ?
C86 H86B 0.9600 . ?
C86 H86C 0.9600 . ?
C87 H87A 0.9600 . ?
C87 H87B 0.9600 . ?
C87 H87C 0.9600 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 0.9600 . ?
C89 H89A 0.9600 . ?
C89 H89B 0.9600 . ?
C89 H89C 0.9600 . ?
C89 O2 1.424(7) . ?
C90 C91 1.393(7) . ?
C90 C95 1.369(7) . ?
C90 N3 1.427(6) . ?
C91 H91 0.9300 . ?
C91 C92 1.387(7) . ?
C92 C93 1.407(8) . ?
C92 C100 1.554(7) . ?
C93 C94 1.406(7) . ?
C93 O3 1.390(5) . ?
C94 C95 1.406(7) . ?
C94 C96 1.558(7) . ?
C95 H95 0.9300 . ?
C96 C97 1.510(8) . ?
C96 C98 1.538(9) . ?
C96 C99 1.535(7) . ?
C97 H97A 0.9600 . ?
C97 H97B 0.9600 . ?
C97 H97C 0.9600 . ?
C98 H98A 0.9600 . ?
C98 H98B 0.9600 . ?
C98 H98C 0.9600 . ?
C99 H99A 0.9600 . ?
C99 H99B 0.9600 . ?
C99 H99C 0.9600 . ?
C100 C101 1.548(9) . ?
C100 C102 1.544(8) . ?
C100 C103 1.521(7) . ?
C101 H10A 0.9600 . ?
C101 H10B 0.9600 . ?
C101 H10C 0.9600 . ?
C102 H10D 0.9600 . ?
C102 H10E 0.9600 . ?
C102 H10F 0.9600 . ?
C103 H10G 0.9600 . ?
C103 H10H 0.9600 . ?
C103 H10I 0.9600 . ?
C104 H10J 0.9600 . ?
C104 H10K 0.9600 . ?
C104 H10L 0.9600 . ?
C104 O3 1.433(7) . ?
C105 C106 1.376(7) . ?
C105 C110 1.383(7) . ?
C105 N4 1.428(6) . ?
C106 H106 0.9300 . ?
C106 C107 1.398(7) . ?
C107 C108 1.414(7) . ?
C107 C115 1.552(7) . ?
C108 C109 1.409(7) . ?
C108 O4 1.390(6) . ?
C109 C110 1.387(7) . ?
C109 C111 1.554(7) . ?
C110 H110 0.9300 . ?
C111 C112 1.517(8) . ?
C111 C113 1.529(7) . ?
C111 C114 1.546(7) . ?
C112 H11A 0.9600 . ?
C112 H11B 0.9600 . ?
C112 H11C 0.9600 . ?
C113 H11D 0.9600 . ?
C113 H11E 0.9600 . ?
C113 H11F 0.9600 . ?
C114 H11G 0.9600 . ?
C114 H11H 0.9600 . ?
C114 H11I 0.9600 . ?
C115 C116 1.550(9) . ?
C115 C117 1.531(7) . ?
C115 C118 1.540(9) . ?
C116 H11J 0.9600 . ?
C116 H11K 0.9600 . ?
C116 H11L 0.9600 . ?
C117 H11M 0.9600 . ?
C117 H11N 0.9600 . ?
C117 H11O 0.9600 . ?
C118 H11P 0.9600 . ?
C118 H11Q 0.9600 . ?
C118 H11R 0.9600 . ?
C119 C120 1.386(7) . ?
C119 C124 1.372(7) . ?
C119 N5 1.439(6) . ?
C120 H120 0.9300 . ?
C120 C121 1.388(6) . ?
C121 C122 1.422(7) . ?
C121 C129 1.546(7) . ?
C122 C123 1.388(7) . ?
C122 O5 1.393(6) . ?
C123 C124 1.407(7) . ?
C123 C125 1.555(7) . ?
C124 H124 0.9300 . ?
C125 C126 1.560(9) . ?
C125 C127 1.520(8) . ?
C125 C128 1.527(9) . ?
C126 H12A 0.9600 . ?
C126 H12B 0.9600 . ?
C126 H12C 0.9600 . ?
C127 H12D 0.9600 . ?
C127 H12E 0.9600 . ?
C127 H12F 0.9600 . ?
C128 H12G 0.9600 . ?
C128 H12H 0.9600 . ?
C128 H12I 0.9600 . ?
C129 C130 1.555(7) . ?
C129 C131 1.531(7) . ?
C129 C132 1.527(8) . ?
C130 H13A 0.9600 . ?
C130 H13B 0.9600 . ?
C130 H13C 0.9600 . ?
C131 H13D 0.9600 . ?
C131 H13E 0.9600 . ?
C131 H13F 0.9600 . ?
C132 H13G 0.9600 . ?
C132 H13H 0.9600 . ?
C132 H13I 0.9600 . ?
C133 H13J 0.9600 . ?
C133 H13K 0.9600 . ?
C133 H13L 0.9600 . ?
C133 O5 1.448(7) . ?
C134 H134 0.9800 . ?
C134 Cl4 1.758(11) . ?
C134 Cl5 1.761(9) . ?
C134 Cl6 1.730(8) . ?
C135 H135 0.9800 . ?
C135 Cl1 1.754(7) . ?
C135 Cl2 1.758(6) . ?
C135 Cl3 1.774(8) . ?
C136 H136 0.9800 . ?
C136 Cl10 1.754(7) . ?
C136 Cl11 1.723(9) . ?
C136 Cl12 1.750(8) . ?
C137 H137 0.9800 . ?
C137 Cl7 1.746(7) . ?
C137 Cl8 1.765(6) . ?
C137 Cl9 1.771(6) . ?
C138 H138 0.9800 . ?
C138 Cl13 1.764(8) . ?
C138 Cl14 1.699(8) . ?
C138 Cl15 1.736(7) . ?
C139 H139 0.9800 . ?
C139 Cl22 1.751(9) . ?
C139 Cl23 1.732(9) . ?
C139 Cl24 1.742(8) . ?
C140 H140 0.9800 . ?
C140 Cl16 1.756(10) . ?
C140 Cl17 1.715(9) . ?
C140 Cl18 1.699(10) . ?
C141 H141 0.9800 . ?
C141 Cl19 1.760(10) . ?
C141 Cl20 1.701(13) . ?
C141 Cl21 1.655(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C0AA C6 119.5(4) . . ?
C2 C0AA C12 135.3(4) . . ?
C6 C0AA C12 105.2(4) . . ?
C0AA C2 H2 119.7 . . ?
C3 C2 C0AA 120.6(4) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C4 117.2(4) . . ?
C2 C3 C58 124.2(4) . . ?
C4 C3 C58 118.6(4) . . ?
C3 C4 H4 118.2 . . ?
C5 C4 C3 123.5(4) . . ?
C5 C4 H4 118.2 . . ?
H04A C04A H04B 109.5 . . ?
H04A C04A H04C 109.5 . . ?
H04B C04A H04C 109.5 . . ?
O4 C04A H04A 109.5 . . ?
O4 C04A H04B 109.5 . . ?
O4 C04A H04C 109.5 . . ?
C4 C5 H5 120.9 . . ?
C4 C5 C6 118.2(4) . . ?
C6 C5 H5 120.9 . . ?
C5 C6 C0AA 121.0(4) . . ?
N1 C6 C0AA 110.6(4) . . ?
N1 C6 C5 128.4(4) . . ?
C8 C7 C12 122.2(4) . . ?
N1 C7 C8 127.7(4) . . ?
N1 C7 C12 110.1(4) . . ?
C7 C8 H8 121.4 . . ?
C9 C8 C7 117.2(4) . . ?
C9 C8 H8 121.4 . . ?
C8 C9 H9 119.0 . . ?
C8 C9 C10 122.0(4) . . ?
C10 C9 H9 119.0 . . ?
C9 C10 C15 117.0(4) . . ?
C11 C10 C9 119.4(4) . . ?
C11 C10 C15 123.5(4) . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.6(4) . . ?
C12 C11 H11 120.2 . . ?
C7 C12 C0AA 106.2(4) . . ?
C11 C12 C0AA 134.2(4) . . ?
C11 C12 C7 119.4(4) . . ?
C14 C13 C18 120.3(4) . . ?
C14 C13 C24 132.6(4) . . ?
C18 C13 C24 106.9(4) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 C13 118.5(4) . . ?
C15 C14 H14 120.8 . . ?
C14 C15 C10 120.7(4) . . ?
C14 C15 C16 119.6(4) . . ?
C16 C15 C10 119.7(4) . . ?
C15 C16 H16 118.7 . . ?
C17 C16 C15 122.6(4) . . ?
C17 C16 H16 118.7 . . ?
C16 C17 H17 121.5 . . ?
C16 C17 C18 117.0(4) . . ?
C18 C17 H17 121.5 . . ?
C17 C18 C13 121.9(4) . . ?
C17 C18 N2 129.2(4) . . ?
N2 C18 C13 108.8(4) . . ?
C20 C19 C24 120.3(4) . . ?
N2 C19 C20 130.0(4) . . ?
N2 C19 C24 109.7(4) . . ?
C19 C20 H20 121.0 . . ?
C21 C20 C19 118.1(4) . . ?
C21 C20 H20 121.0 . . ?
C20 C21 H21 118.7 . . ?
C20 C21 C22 122.6(4) . . ?
C22 C21 H21 118.7 . . ?
C21 C22 C27 119.3(4) . . ?
C23 C22 C21 118.6(5) . . ?
C23 C22 C27 122.0(4) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.0(4) . . ?
C24 C23 H23 120.0 . . ?
C19 C24 C13 105.9(4) . . ?
C23 C24 C13 133.8(4) . . ?
C23 C24 C19 120.3(4) . . ?
C26 C25 C30 120.1(4) . . ?
C26 C25 C36 132.4(4) . . ?
C30 C25 C36 106.8(4) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.7(4) . . ?
C27 C26 H26 120.1 . . ?
C26 C27 C22 121.4(4) . . ?
C26 C27 C28 118.5(5) . . ?
C28 C27 C22 119.9(5) . . ?
C27 C28 H28 118.6 . . ?
C29 C28 C27 122.7(5) . . ?
C29 C28 H28 118.6 . . ?
C28 C29 H29 121.2 . . ?
C28 C29 C30 117.6(4) . . ?
C30 C29 H29 121.2 . . ?
C29 C30 C25 121.1(4) . . ?
C29 C30 N3 129.9(4) . . ?
N3 C30 C25 108.9(4) . . ?
C32 C31 C36 121.2(4) . . ?
C32 C31 N3 130.0(4) . . ?
N3 C31 C36 108.2(4) . . ?
C31 C32 H32 121.4 . . ?
C33 C32 C31 117.3(4) . . ?
C33 C32 H32 121.4 . . ?
C32 C33 H33 118.7 . . ?
C32 C33 C34 122.5(4) . . ?
C34 C33 H33 118.7 . . ?
C33 C34 C40 120.5(4) . . ?
C35 C34 C33 119.3(4) . . ?
C35 C34 C40 120.0(4) . . ?
C34 C35 H35 120.1 . . ?
C34 C35 C36 119.9(4) . . ?
C36 C35 H35 120.1 . . ?
C76 C035 H035 119.5 . . ?
C76 C035 C80 120.9(5) . . ?
C80 C035 H035 119.5 . . ?
C31 C36 C25 107.2(4) . . ?
C35 C36 C25 132.3(4) . . ?
C35 C36 C31 119.6(4) . . ?
C42 C37 C38 121.7(4) . . ?
C42 C37 N4 128.7(4) . . ?
N4 C37 C38 109.5(4) . . ?
C37 C38 C48 106.3(4) . . ?
C39 C38 C37 119.7(4) . . ?
C39 C38 C48 134.0(4) . . ?
C38 C39 H39 120.1 . . ?
C38 C39 C40 119.9(4) . . ?
C40 C39 H39 120.1 . . ?
C39 C40 C34 120.9(4) . . ?
C39 C40 C41 118.7(4) . . ?
C41 C40 C34 120.1(4) . . ?
C40 C41 H41 118.6 . . ?
C42 C41 C40 122.8(4) . . ?
C42 C41 H41 118.6 . . ?
C37 C42 H42 121.4 . . ?
C41 C42 C37 117.2(4) . . ?
C41 C42 H42 121.4 . . ?
C44 C43 C48 121.4(4) . . ?
C44 C43 N4 129.0(4) . . ?
N4 C43 C48 109.5(4) . . ?
C43 C44 H44 121.3 . . ?
C45 C44 C43 117.3(4) . . ?
C45 C44 H44 121.3 . . ?
C44 C45 H45 118.5 . . ?
C44 C45 C46 123.0(4) . . ?
C46 C45 H45 118.5 . . ?
C45 C46 C51 118.9(4) . . ?
C47 C46 C45 118.6(4) . . ?
C47 C46 C51 122.0(4) . . ?
C46 C47 H47 120.5 . . ?
C46 C47 C48 118.9(4) . . ?
C48 C47 H47 120.5 . . ?
C43 C48 C38 107.1(4) . . ?
C43 C48 C47 120.6(4) . . ?
C47 C48 C38 132.2(4) . . ?
C50 C49 C54 118.4(4) . . ?
C50 C49 C60 134.8(4) . . ?
C54 C49 C60 106.6(4) . . ?
C49 C50 H50 120.2 . . ?
C49 C50 C51 119.6(4) . . ?
C51 C50 H50 120.2 . . ?
C50 C51 C46 123.8(4) . . ?
C52 C51 C46 116.9(4) . . ?
C52 C51 C50 119.4(4) . . ?
C51 C52 H52 118.6 . . ?
C53 C52 C51 122.7(4) . . ?
C53 C52 H52 118.6 . . ?
C52 C53 H53 121.8 . . ?
C54 C53 C52 116.4(4) . . ?
C54 C53 H53 121.8 . . ?
C53 C54 C49 123.3(4) . . ?
C53 C54 N5 127.1(4) . . ?
N5 C54 C49 109.6(4) . . ?
C56 C55 C60 121.4(4) . . ?
N5 C55 C56 128.0(4) . . ?
N5 C55 C60 110.5(4) . . ?
C55 C56 H56 121.1 . . ?
C57 C56 C55 117.9(4) . . ?
C57 C56 H56 121.1 . . ?
C56 C57 H57 118.1 . . ?
C56 C57 C58 123.7(4) . . ?
C58 C57 H57 118.1 . . ?
C57 C58 C3 118.4(4) . . ?
C57 C58 C59 116.9(4) . . ?
C59 C58 C3 124.6(4) . . ?
C58 C59 H59 119.6 . . ?
C60 C59 C58 120.8(4) . . ?
C60 C59 H59 119.6 . . ?
C55 C60 C49 105.1(4) . . ?
C59 C60 C49 135.7(4) . . ?
C59 C60 C55 119.2(4) . . ?
C62 C61 N1 118.7(4) . . ?
C66 C61 C62 121.5(4) . . ?
C66 C61 N1 119.7(4) . . ?
C61 C62 H62 119.6 . . ?
C61 C62 C63 120.7(4) . . ?
C63 C62 H62 119.6 . . ?
C62 C63 C67 116.3(4) . . ?
C64 C63 C62 116.3(4) . . ?
C64 C63 C67 127.4(4) . . ?
C63 C64 C65 123.4(4) . . ?
C63 C64 O1 119.7(4) . . ?
O1 C64 C65 116.8(4) . . ?
C64 C65 C71 123.2(4) . . ?
C66 C65 C64 116.7(4) . . ?
C66 C65 C71 120.0(4) . . ?
C61 C66 C65 120.6(4) . . ?
C61 C66 H66 119.7 . . ?
C65 C66 H66 119.7 . . ?
C63 C67 C68 108.4(4) . . ?
C63 C67 C69 109.9(4) . . ?
C69 C67 C68 107.5(4) . . ?
C70 C67 C63 115.2(4) . . ?
C70 C67 C68 105.9(4) . . ?
C70 C67 C69 109.7(4) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C67 C70 H70A 109.5 . . ?
C67 C70 H70B 109.5 . . ?
C67 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C65 C71 C74 112.1(4) . . ?
C72 C71 C65 111.5(4) . . ?
C72 C71 C73 108.1(4) . . ?
C72 C71 C74 107.0(4) . . ?
C73 C71 C65 109.0(4) . . ?
C73 C71 C74 109.1(4) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
O1 C75 H75A 109.5 . . ?
O1 C75 H75B 109.5 . . ?
O1 C75 H75C 109.5 . . ?
C035 C76 N2 119.4(4) . . ?
C77 C76 C035 120.8(4) . . ?
C77 C76 N2 119.8(4) . . ?
C76 C77 H77 119.7 . . ?
C76 C77 C78 120.5(5) . . ?
C78 C77 H77 119.7 . . ?
C77 C78 C79 117.1(5) . . ?
C77 C78 C81 117.5(5) . . ?
C79 C78 C81 125.4(5) . . ?
C80 C79 C78 122.9(5) . . ?
C80 C79 O2 118.6(5) . . ?
O2 C79 C78 118.5(5) . . ?
C035 C80 C85 115.6(5) . . ?
C79 C80 C035 116.9(5) . . ?
C79 C80 C85 127.5(5) . . ?
C82 C81 C78 111.4(5) . . ?
C82 C81 C83 107.5(7) . . ?
C83 C81 C78 111.7(6) . . ?
C84 C81 C78 109.0(5) . . ?
C84 C81 C82 108.3(8) . . ?
C84 C81 C83 108.8(8) . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C81 C84 H84A 109.5 . . ?
C81 C84 H84B 109.5 . . ?
C81 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C80 C85 C87 108.4(5) . . ?
C86 C85 C80 117.4(6) . . ?
C86 C85 C87 106.8(6) . . ?
C88 C85 C80 108.9(5) . . ?
C88 C85 C86 108.3(6) . . ?
C88 C85 C87 106.6(6) . . ?
C85 C86 H86A 109.5 . . ?
C85 C86 H86B 109.5 . . ?
C85 C86 H86C 109.5 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C85 C87 H87A 109.5 . . ?
C85 C87 H87B 109.5 . . ?
C85 C87 H87C 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C85 C88 H88A 109.5 . . ?
C85 C88 H88B 109.5 . . ?
C85 C88 H88C 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
O2 C89 H89A 109.5 . . ?
O2 C89 H89B 109.5 . . ?
O2 C89 H89C 109.5 . . ?
C91 C90 N3 119.5(4) . . ?
C95 C90 C91 120.3(4) . . ?
C95 C90 N3 120.1(4) . . ?
C90 C91 H91 119.4 . . ?
C92 C91 C90 121.3(5) . . ?
C92 C91 H91 119.4 . . ?
C91 C92 C93 117.0(5) . . ?
C91 C92 C100 118.7(5) . . ?
C93 C92 C100 124.4(4) . . ?
C94 C93 C92 123.2(4) . . ?
O3 C93 C92 117.2(4) . . ?
O3 C93 C94 119.6(5) . . ?
C93 C94 C96 128.3(4) . . ?
C95 C94 C93 116.3(5) . . ?
C95 C94 C96 115.4(4) . . ?
C90 C95 C94 121.5(5) . . ?
C90 C95 H95 119.3 . . ?
C94 C95 H95 119.3 . . ?
C97 C96 C94 110.0(5) . . ?
C97 C96 C98 109.9(6) . . ?
C97 C96 C99 110.6(5) . . ?
C98 C96 C94 108.1(4) . . ?
C99 C96 C94 114.8(5) . . ?
C99 C96 C98 103.1(5) . . ?
C96 C97 H97A 109.5 . . ?
C96 C97 H97B 109.5 . . ?
C96 C97 H97C 109.5 . . ?
H97A C97 H97B 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C96 C98 H98A 109.5 . . ?
C96 C98 H98B 109.5 . . ?
C96 C98 H98C 109.5 . . ?
H98A C98 H98B 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
C96 C99 H99A 109.5 . . ?
C96 C99 H99B 109.5 . . ?
C96 C99 H99C 109.5 . . ?
H99A C99 H99B 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?
C101 C100 C92 111.4(4) . . ?
C102 C100 C92 111.2(5) . . ?
C102 C100 C101 105.8(5) . . ?
C103 C100 C92 110.6(4) . . ?
C103 C100 C101 107.3(5) . . ?
C103 C100 C102 110.3(5) . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10B 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C100 C102 H10D 109.5 . . ?
C100 C102 H10E 109.5 . . ?
C100 C102 H10F 109.5 . . ?
H10D C102 H10E 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
C100 C103 H10G 109.5 . . ?
C100 C103 H10H 109.5 . . ?
C100 C103 H10I 109.5 . . ?
H10G C103 H10H 109.5 . . ?
H10G C103 H10I 109.5 . . ?
H10H C103 H10I 109.5 . . ?
H10J C104 H10K 109.5 . . ?
H10J C104 H10L 109.5 . . ?
H10K C104 H10L 109.5 . . ?
O3 C104 H10J 109.5 . . ?
O3 C104 H10K 109.5 . . ?
O3 C104 H10L 109.5 . . ?
C106 C105 C110 120.9(4) . . ?
C106 C105 N4 119.4(4) . . ?
C110 C105 N4 119.7(4) . . ?
C105 C106 H106 119.1 . . ?
C105 C106 C107 121.8(4) . . ?
C107 C106 H106 119.1 . . ?
C106 C107 C108 115.9(4) . . ?
C106 C107 C115 116.9(4) . . ?
C108 C107 C115 127.2(4) . . ?
C109 C108 C107 122.6(4) . . ?
O4 C108 C107 120.1(4) . . ?
O4 C108 C109 117.3(4) . . ?
C108 C109 C111 121.8(4) . . ?
C110 C109 C108 117.9(4) . . ?
C110 C109 C111 120.2(4) . . ?
C105 C110 C109 120.4(5) . . ?
C105 C110 H110 119.8 . . ?
C109 C110 H110 119.8 . . ?
C112 C111 C109 113.0(5) . . ?
C112 C111 C113 109.9(4) . . ?
C112 C111 C114 106.7(4) . . ?
C113 C111 C109 109.6(4) . . ?
C113 C111 C114 106.8(5) . . ?
C114 C111 C109 110.5(4) . . ?
C111 C112 H11A 109.5 . . ?
C111 C112 H11B 109.5 . . ?
C111 C112 H11C 109.5 . . ?
H11A C112 H11B 109.5 . . ?
H11A C112 H11C 109.5 . . ?
H11B C112 H11C 109.5 . . ?
C111 C113 H11D 109.5 . . ?
C111 C113 H11E 109.5 . . ?
C111 C113 H11F 109.5 . . ?
H11D C113 H11E 109.5 . . ?
H11D C113 H11F 109.5 . . ?
H11E C113 H11F 109.5 . . ?
C111 C114 H11G 109.5 . . ?
C111 C114 H11H 109.5 . . ?
C111 C114 H11I 109.5 . . ?
H11G C114 H11H 109.5 . . ?
H11G C114 H11I 109.5 . . ?
H11H C114 H11I 109.5 . . ?
C116 C115 C107 109.5(5) . . ?
C117 C115 C107 115.1(4) . . ?
C117 C115 C116 109.9(5) . . ?
C117 C115 C118 106.7(5) . . ?
C118 C115 C107 107.9(5) . . ?
C118 C115 C116 107.5(5) . . ?
C115 C116 H11J 109.5 . . ?
C115 C116 H11K 109.5 . . ?
C115 C116 H11L 109.5 . . ?
H11J C116 H11K 109.5 . . ?
H11J C116 H11L 109.5 . . ?
H11K C116 H11L 109.5 . . ?
C115 C117 H11M 109.5 . . ?
C115 C117 H11N 109.5 . . ?
C115 C117 H11O 109.5 . . ?
H11M C117 H11N 109.5 . . ?
H11M C117 H11O 109.5 . . ?
H11N C117 H11O 109.5 . . ?
C115 C118 H11P 109.5 . . ?
C115 C118 H11Q 109.5 . . ?
C115 C118 H11R 109.5 . . ?
H11P C118 H11Q 109.5 . . ?
H11P C118 H11R 109.5 . . ?
H11Q C118 H11R 109.5 . . ?
C120 C119 N5 119.4(4) . . ?
C124 C119 C120 121.4(4) . . ?
C124 C119 N5 119.2(4) . . ?
C119 C120 H120 120.2 . . ?
C119 C120 C121 119.6(4) . . ?
C121 C120 H120 120.2 . . ?
C120 C121 C122 118.0(5) . . ?
C120 C121 C129 119.3(5) . . ?
C122 C121 C129 122.5(4) . . ?
C123 C122 C121 122.3(4) . . ?
C123 C122 O5 120.5(4) . . ?
O5 C122 C121 117.2(4) . . ?
C122 C123 C124 116.6(5) . . ?
C122 C123 C125 127.7(4) . . ?
C124 C123 C125 115.7(5) . . ?
C119 C124 C123 121.2(5) . . ?
C119 C124 H124 119.4 . . ?
C123 C124 H124 119.4 . . ?
C123 C125 C126 114.7(5) . . ?
C127 C125 C123 108.7(4) . . ?
C127 C125 C126 104.5(5) . . ?
C127 C125 C128 108.3(5) . . ?
C128 C125 C123 110.9(5) . . ?
C128 C125 C126 109.3(6) . . ?
C125 C126 H12A 109.5 . . ?
C125 C126 H12B 109.5 . . ?
C125 C126 H12C 109.5 . . ?
H12A C126 H12B 109.5 . . ?
H12A C126 H12C 109.5 . . ?
H12B C126 H12C 109.5 . . ?
C125 C127 H12D 109.5 . . ?
C125 C127 H12E 109.5 . . ?
C125 C127 H12F 109.5 . . ?
H12D C127 H12E 109.5 . . ?
H12D C127 H12F 109.5 . . ?
H12E C127 H12F 109.5 . . ?
C125 C128 H12G 109.5 . . ?
C125 C128 H12H 109.5 . . ?
C125 C128 H12I 109.5 . . ?
H12G C128 H12H 109.5 . . ?
H12G C128 H12I 109.5 . . ?
H12H C128 H12I 109.5 . . ?
C121 C129 C130 112.1(4) . . ?
C131 C129 C121 108.0(4) . . ?
C131 C129 C130 109.1(4) . . ?
C132 C129 C121 112.0(4) . . ?
C132 C129 C130 107.4(4) . . ?
C132 C129 C131 108.0(5) . . ?
C129 C130 H13A 109.5 . . ?
C129 C130 H13B 109.5 . . ?
C129 C130 H13C 109.5 . . ?
H13A C130 H13B 109.5 . . ?
H13A C130 H13C 109.5 . . ?
H13B C130 H13C 109.5 . . ?
C129 C131 H13D 109.5 . . ?
C129 C131 H13E 109.5 . . ?
C129 C131 H13F 109.5 . . ?
H13D C131 H13E 109.5 . . ?
H13D C131 H13F 109.5 . . ?
H13E C131 H13F 109.5 . . ?
C129 C132 H13G 109.5 . . ?
C129 C132 H13H 109.5 . . ?
C129 C132 H13I 109.5 . . ?
H13G C132 H13H 109.5 . . ?
H13G C132 H13I 109.5 . . ?
H13H C132 H13I 109.5 . . ?
H13J C133 H13K 109.5 . . ?
H13J C133 H13L 109.5 . . ?
H13K C133 H13L 109.5 . . ?
O5 C133 H13J 109.5 . . ?
O5 C133 H13K 109.5 . . ?
O5 C133 H13L 109.5 . . ?
C6 N1 C7 107.9(4) . . ?
C6 N1 C61 125.3(4) . . ?
C7 N1 C61 125.6(4) . . ?
C18 N2 C76 125.5(4) . . ?
C19 N2 C18 108.7(4) . . ?
C19 N2 C76 125.4(4) . . ?
C30 N3 C31 108.8(4) . . ?
C30 N3 C90 126.0(4) . . ?
C31 N3 C90 124.5(4) . . ?
C37 N4 C105 125.0(4) . . ?
C43 N4 C37 107.5(3) . . ?
C43 N4 C105 127.1(4) . . ?
C54 N5 C119 126.1(4) . . ?
C55 N5 C54 108.1(4) . . ?
C55 N5 C119 124.2(4) . . ?
C64 O1 C75 111.9(3) . . ?
C79 O2 C89 113.1(4) . . ?
C93 O3 C104 113.5(4) . . ?
C108 O4 C04A 112.7(4) . . ?
C122 O5 C133 111.6(4) . . ?
Cl4 C134 H134 109.1 . . ?
Cl4 C134 Cl5 108.6(4) . . ?
Cl5 C134 H134 109.1 . . ?
Cl6 C134 H134 109.1 . . ?
Cl6 C134 Cl4 109.2(5) . . ?
Cl6 C134 Cl5 111.8(5) . . ?
Cl1 C135 H135 108.5 . . ?
Cl1 C135 Cl2 110.3(4) . . ?
Cl1 C135 Cl3 110.2(4) . . ?
Cl2 C135 H135 108.5 . . ?
Cl2 C135 Cl3 110.9(4) . . ?
Cl3 C135 H135 108.5 . . ?
Cl10 C136 H136 107.4 . . ?
Cl11 C136 H136 107.4 . . ?
Cl11 C136 Cl10 111.3(4) . . ?
Cl11 C136 Cl12 112.4(5) . . ?
Cl12 C136 H136 107.4 . . ?
Cl12 C136 Cl10 110.6(4) . . ?
Cl7 C137 H137 108.6 . . ?
Cl7 C137 Cl8 110.8(3) . . ?
Cl7 C137 Cl9 110.8(3) . . ?
Cl8 C137 H137 108.6 . . ?
Cl8 C137 Cl9 109.4(3) . . ?
Cl9 C137 H137 108.6 . . ?
Cl13 C138 H138 108.1 . . ?
Cl14 C138 H138 108.1 . . ?
Cl14 C138 Cl13 108.0(4) . . ?
Cl14 C138 Cl15 116.3(4) . . ?
Cl15 C138 H138 108.1 . . ?
Cl15 C138 Cl13 108.0(4) . . ?
Cl22 C139 H139 108.1 . . ?
Cl23 C139 H139 108.1 . . ?
Cl23 C139 Cl22 109.8(5) . . ?
Cl23 C139 Cl24 113.4(5) . . ?
Cl24 C139 H139 108.1 . . ?
Cl24 C139 Cl22 109.3(5) . . ?
Cl16 C140 H140 108.5 . . ?
Cl17 C140 H140 108.5 . . ?
Cl17 C140 Cl16 113.0(5) . . ?
Cl18 C140 H140 108.5 . . ?
Cl18 C140 Cl16 107.4(5) . . ?
Cl18 C140 Cl17 111.0(5) . . ?
Cl19 C141 H141 102.1 . . ?
Cl20 C141 H141 102.1 . . ?
Cl20 C141 Cl19 112.1(7) . . ?
Cl21 C141 H141 102.1 . . ?
Cl21 C141 Cl19 116.5(7) . . ?
Cl21 C141 Cl20 118.7(7) . . ?

_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 0.000 0.000 0.000 215.0 56.2 ?
2 -0.072 0.280 0.399 11.6 0.9 ?
3 0.033 0.460 0.854 13.7 0.1 ?
4 0.000 0.500 0.500 33.9 2.1 ?
5 -0.033 0.540 0.146 13.7 0.0 ?
6 0.072 0.720 0.601 11.6 0.8 ?
7 0.458 0.769 0.783 7.2 0.0 ?
8 0.542 0.231 0.217 7.2 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.828
_oxdiff_exptl_absorpt_empirical_full_min 0.475
