# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_1
_database_code_depnum_ccdc_archive 'CCDC 1939483'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch'
;University of Valencia
Spain
;
_audit_update_record             
;
2019-07-09 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;
_audit_creation_date             2019-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(Br), 2(H2 O), C36 H30 N3'
_chemical_formula_sum            'C36 H34 Br3 N3 O2'
_chemical_formula_weight         780.39
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'raf qui I 1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.4720(4)
_cell_length_b                   29.1025(13)
_cell_length_c                   11.8612(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.230(5)
_cell_angle_gamma                90
_cell_volume                     3227.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3649
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.4450
_cell_measurement_theta_min      3.7410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.788
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.044
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14239
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.309
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0133
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     62.00  95.00   0.75   25.00    --   20.73 178.00  60.00   44
  2  ω    -20.00  41.50   0.75   25.00    --   20.73 -99.00  60.00   82
  3  ω    -51.00  93.00   0.75   25.00    --   20.73   0.00  60.00  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0270462000
_diffrn_orient_matrix_UB_12      0.0217354000
_diffrn_orient_matrix_UB_13      -0.0200547000
_diffrn_orient_matrix_UB_21      0.0373908000
_diffrn_orient_matrix_UB_22      -0.0018007000
_diffrn_orient_matrix_UB_23      -0.0471070000
_diffrn_orient_matrix_UB_31      -0.0602271000
_diffrn_orient_matrix_UB_32      -0.0108385000
_diffrn_orient_matrix_UB_33      -0.0324562000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4887
_reflns_number_total             6331
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         2.088
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6331
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0462
_refine_ls_restrained_S_all      1.048
_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)+(0.0427P)²+4.2622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1081
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O2(H2a,H2b), O1(H1a,H1b)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C27(H27a,H27b), C17(H17a,H17b)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C18(H18), C6(H6), C32(H32), C28(H28), C19(H19), C30(H30), C8(H8),
 C4(H4), C33(H33), C35(H35), C34(H34), C9(H9), C29(H29), C10(H10), C23(H23),
 C25(H25), C12(H12), C24(H24), C13(H13), C15(H15), C22(H22), C14(H14), C20(H20)
;
_atom_sites_solution_hydrogens   mixed
_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
Br2 Br 0.33253(4) 0.94565(2) 0.48439(4) 0.02777(12) Uani 1 1 d . . . . .
Br3 Br -0.01417(5) 0.96633(2) 0.76400(4) 0.03591(14) Uani 1 1 d . . . . .
Br1 Br 0.62099(5) 0.77335(2) 0.86800(4) 0.03824(14) Uani 1 1 d . . . . .
O2 O 0.2374(3) 0.89792(11) 0.7117(3) 0.0384(8) Uani 1 1 d . . . . .
H2A H 0.1660 0.9132 0.7258 0.058 Uiso 1 1 d G . . . .
H2B H 0.2591 0.9065 0.6482 0.058 Uiso 1 1 d G . . . .
N20 N 0.4389(3) 0.62106(11) 0.8790(3) 0.0202(7) Uani 1 1 d . . . . .
N19 N 0.5531(3) 0.75849(12) 0.5143(3) 0.0237(8) Uani 1 1 d . . . . .
N18 N 0.8532(3) 0.53576(11) 0.5997(3) 0.0220(7) Uani 1 1 d . . . . .
O1 O 0.2858(4) 0.80899(13) 0.7999(4) 0.0528(10) Uani 1 1 d . . . . .
H1A H 0.2887 0.8351 0.7687 0.079 Uiso 1 1 d G . . . .
H1B H 0.3698 0.7980 0.8145 0.079 Uiso 1 1 d G . . . .
C2 C 0.6299(4) 0.63172(14) 0.5066(3) 0.0225(9) Uani 1 1 d . . . . .
H2 H 0.6411 0.6285 0.4305 0.027 Uiso 1 1 calc R . . . .
C18 C 0.4285(5) 0.77854(16) 0.5234(4) 0.0305(10) Uani 1 1 d . . . . .
H18 H 0.3437 0.7630 0.4972 0.037 Uiso 1 1 calc R . . . .
C6 C 0.6369(4) 0.59913(14) 0.6936(3) 0.0208(9) Uani 1 1 d . . . . .
H6 H 0.6527 0.5742 0.7432 0.025 Uiso 1 1 calc R . . . .
C32 C 0.0444(4) 0.63111(16) 0.8205(4) 0.0294(10) Uani 1 1 d . . . . .
H32 H -0.0361 0.6142 0.8300 0.035 Uiso 1 1 calc R . . . .
C5 C 0.5922(4) 0.64101(14) 0.7327(3) 0.0214(9) Uani 1 1 d . . . . .
C28 C 0.4551(4) 0.58046(14) 0.9326(3) 0.0231(9) Uani 1 1 d . . . . .
H28 H 0.5468 0.5687 0.9540 0.028 Uiso 1 1 calc R . . . .
C1 C 0.6581(4) 0.59444(14) 0.5812(4) 0.0217(9) Uani 1 1 d . . . . .
C7 C 0.7084(4) 0.54904(14) 0.5389(4) 0.0256(10) Uani 1 1 d . . . . .
H7A H 0.6404 0.5252 0.5499 0.031 Uiso 1 1 calc R . . . .
H7B H 0.7111 0.5513 0.4577 0.031 Uiso 1 1 calc R . . . .
C36 C 0.3035(4) 0.63943(14) 0.8436(3) 0.0228(9) Uani 1 1 d . . . . .
C19 C 0.4225(5) 0.82188(16) 0.5709(4) 0.0362(11) Uani 1 1 d . . . . .
H19 H 0.3345 0.8354 0.5745 0.043 Uiso 1 1 calc R . . . .
C27 C 0.5707(4) 0.64560(14) 0.8561(3) 0.0227(9) Uani 1 1 d . . . . .
H27A H 0.6535 0.6331 0.9054 0.027 Uiso 1 1 calc R . . . .
H27B H 0.5633 0.6779 0.8745 0.027 Uiso 1 1 calc R . . . .
C31 C 0.1830(4) 0.61362(14) 0.8621(3) 0.0212(9) Uani 1 1 d . . . . .
C26 C 0.6822(4) 0.78036(15) 0.5554(4) 0.0275(10) Uani 1 1 d . . . . .
C3 C 0.5852(4) 0.67387(14) 0.5452(4) 0.0234(9) Uani 1 1 d . . . . .
C30 C 0.2041(4) 0.57135(15) 0.9218(3) 0.0242(9) Uani 1 1 d . . . . .
H30 H 0.1257 0.5545 0.9369 0.029 Uiso 1 1 calc R . . . .
C8 C 0.8596(4) 0.50527(15) 0.6833(4) 0.0280(10) Uani 1 1 d . . . . .
H8 H 0.7746 0.4939 0.7021 0.034 Uiso 1 1 calc R . . . .
C4 C 0.5700(4) 0.67817(13) 0.6585(3) 0.0216(9) Uani 1 1 d . U . . .
H4 H 0.5445 0.7064 0.6857 0.026 Uiso 1 1 calc R . . . .
C33 C 0.0287(5) 0.67248(18) 0.7668(4) 0.0384(12) Uani 1 1 d . . . . .
H33 H -0.0622 0.6834 0.7379 0.046 Uiso 1 1 calc R . . . .
C35 C 0.2853(5) 0.68335(16) 0.7922(4) 0.0298(10) Uani 1 1 d . . . . .
H35 H 0.3641 0.7014 0.7839 0.036 Uiso 1 1 calc R . . . .
C34 C 0.1496(5) 0.69882(17) 0.7549(4) 0.0366(12) Uani 1 1 d . . . . .
H34 H 0.1370 0.7276 0.7208 0.044 Uiso 1 1 calc R . . . .
C9 C 0.9880(5) 0.48959(16) 0.7441(4) 0.0308(10) Uani 1 1 d . . . . .
H9 H 0.9895 0.4685 0.8031 0.037 Uiso 1 1 calc R . . . .
C29 C 0.3391(4) 0.55531(14) 0.9571(4) 0.0257(9) Uani 1 1 d . . . . .
H29 H 0.3534 0.5278 0.9973 0.031 Uiso 1 1 calc R . . . .
C10 C 1.1124(5) 0.50607(15) 0.7148(4) 0.0282(10) Uani 1 1 d . . . . .
H10 H 1.1996 0.4951 0.7525 0.034 Uiso 1 1 calc R . . . .
C11 C 1.1104(4) 0.53927(14) 0.6289(4) 0.0241(9) Uani 1 1 d . . . . .
C21 C 0.6771(5) 0.82439(15) 0.6057(4) 0.0327(11) Uani 1 1 d . . . . .
C17 C 0.5496(5) 0.71284(14) 0.4597(4) 0.0269(10) Uani 1 1 d . . . . .
H17A H 0.6174 0.7124 0.4065 0.032 Uiso 1 1 calc R . . . .
H17B H 0.4550 0.7077 0.4164 0.032 Uiso 1 1 calc R . . . .
C16 C 0.9763(4) 0.55494(14) 0.5699(3) 0.0221(9) Uani 1 1 d . . . . .
C23 C 0.9348(6) 0.8268(2) 0.6355(4) 0.0484(15) Uani 1 1 d . . . . .
H23 H 1.0204 0.8417 0.6627 0.058 Uiso 1 1 calc R . . . .
C25 C 0.8138(4) 0.75992(18) 0.5436(4) 0.0352(11) Uani 1 1 d . . . . .
H25 H 0.8168 0.7312 0.5097 0.042 Uiso 1 1 calc R . . . .
C12 C 1.2376(5) 0.55816(16) 0.6008(4) 0.0331(11) Uani 1 1 d . . . . .
H12 H 1.3258 0.5478 0.6379 0.040 Uiso 1 1 calc R . . . .
C24 C 0.9372(5) 0.7834(2) 0.5830(4) 0.0439(13) Uani 1 1 d . . . . .
H24 H 1.0247 0.7703 0.5751 0.053 Uiso 1 1 calc R . . . .
C13 C 1.2316(5) 0.59169(17) 0.5193(4) 0.0402(12) Uani 1 1 d . . . . .
H13 H 1.3154 0.6045 0.5018 0.048 Uiso 1 1 calc R . . . .
C15 C 0.9724(5) 0.58878(15) 0.4866(4) 0.0309(10) Uani 1 1 d . . . . .
H15 H 0.8852 0.5992 0.4476 0.037 Uiso 1 1 calc R . . . .
C22 C 0.8098(6) 0.84695(19) 0.6468(4) 0.0466(14) Uani 1 1 d . . . . .
H22 H 0.8096 0.8756 0.6814 0.056 Uiso 1 1 calc R . . . .
C14 C 1.0979(5) 0.60670(16) 0.4624(4) 0.0396(12) Uani 1 1 d . . . . .
H14 H 1.0946 0.6294 0.4068 0.048 Uiso 1 1 calc R . . . .
C20 C 0.5453(5) 0.84450(16) 0.6120(4) 0.0390(12) Uani 1 1 d . . . . .
H20 H 0.5413 0.8735 0.6444 0.047 Uiso 1 1 calc R . . . .


_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
O2 H2A 0.8487 . ?
O2 H2B 0.8502 . ?
N20 C28 1.339(5) . ?
N20 C36 1.391(5) . ?
N20 C27 1.500(5) . ?
N19 C18 1.337(5) . ?
N19 C26 1.395(5) . ?
N19 C17 1.476(5) . ?
N18 C7 1.495(5) . ?
N18 C8 1.325(5) . ?
N18 C16 1.388(5) . ?
O1 H1A 0.8486 . ?
O1 H1B 0.8494 . ?
C2 H2 0.9300 . ?
C2 C1 1.399(6) . ?
C2 C3 1.399(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.386(6) . ?
C6 H6 0.9300 . ?
C6 C5 1.394(5) . ?
C6 C1 1.386(6) . ?
C32 H32 0.9300 . ?
C32 C31 1.421(5) . ?
C32 C33 1.359(6) . ?
C5 C27 1.516(6) . ?
C5 C4 1.388(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.390(6) . ?
C1 C7 1.517(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C36 C31 1.413(6) . ?
C36 C35 1.415(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.357(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C31 C30 1.418(6) . ?
C26 C21 1.417(6) . ?
C26 C25 1.408(6) . ?
C3 C4 1.380(6) . ?
C3 C17 1.523(6) . ?
C30 H30 0.9300 . ?
C30 C29 1.363(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(6) . ?
C4 H4 0.9300 . ?
C33 H33 0.9300 . ?
C33 C34 1.403(7) . ?
C35 H35 0.9300 . ?
C35 C34 1.367(6) . ?
C34 H34 0.9300 . ?
C9 H9 0.9300 . ?
C9 C10 1.368(6) . ?
C29 H29 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.402(6) . ?
C11 C16 1.423(6) . ?
C11 C12 1.412(6) . ?
C21 C22 1.433(7) . ?
C21 C20 1.392(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C16 C15 1.391(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.412(8) . ?
C23 C22 1.346(8) . ?
C25 H25 0.9300 . ?
C25 C24 1.370(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.368(7) . ?
C24 H24 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.406(7) . ?
C15 H15 0.9300 . ?
C15 C14 1.370(6) . ?
C22 H22 0.9300 . ?
C14 H14 0.9300 . ?
C20 H20 0.9300 . ?

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
H2A O2 H2B 109.5 . . ?
C28 N20 C36 120.8(3) . . ?
C28 N20 C27 118.1(3) . . ?
C36 N20 C27 121.1(3) . . ?
C18 N19 C26 120.6(4) . . ?
C18 N19 C17 118.0(4) . . ?
C26 N19 C17 121.4(3) . . ?
C8 N18 C7 117.5(4) . . ?
C8 N18 C16 121.4(3) . . ?
C16 N18 C7 121.1(3) . . ?
H1A O1 H1B 109.5 . . ?
C1 C2 H2 119.7 . . ?
C1 C2 C3 120.7(4) . . ?
C3 C2 H2 119.7 . . ?
N19 C18 H18 119.2 . . ?
N19 C18 C19 121.6(4) . . ?
C19 C18 H18 119.2 . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C1 C6 C5 120.3(4) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C33 C32 C31 120.4(4) . . ?
C6 C5 C27 119.5(4) . . ?
C4 C5 C6 119.6(4) . . ?
C4 C5 C27 120.9(4) . . ?
N20 C28 H28 119.0 . . ?
N20 C28 C29 122.0(4) . . ?
C29 C28 H28 119.0 . . ?
C2 C1 C7 120.3(4) . . ?
C6 C1 C2 119.4(4) . . ?
C6 C1 C7 120.3(4) . . ?
N18 C7 C1 112.3(3) . . ?
N18 C7 H7A 109.2 . . ?
N18 C7 H7B 109.2 . . ?
C1 C7 H7A 109.2 . . ?
C1 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N20 C36 C31 118.5(4) . . ?
N20 C36 C35 121.4(4) . . ?
C31 C36 C35 120.1(4) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 119.9(4) . . ?
C20 C19 H19 120.0 . . ?
N20 C27 C5 112.2(3) . . ?
N20 C27 H27A 109.2 . . ?
N20 C27 H27B 109.2 . . ?
C5 C27 H27A 109.2 . . ?
C5 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C36 C31 C32 118.7(4) . . ?
C36 C31 C30 119.1(4) . . ?
C30 C31 C32 122.2(4) . . ?
N19 C26 C21 118.2(4) . . ?
N19 C26 C25 120.8(4) . . ?
C25 C26 C21 121.0(4) . . ?
C2 C3 C17 118.7(4) . . ?
C4 C3 C2 118.9(4) . . ?
C4 C3 C17 122.3(4) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 C31 120.1(4) . . ?
C29 C30 H30 120.0 . . ?
N18 C8 H8 118.7 . . ?
N18 C8 C9 122.7(4) . . ?
C9 C8 H8 118.7 . . ?
C5 C4 H4 119.4 . . ?
C3 C4 C5 121.2(4) . . ?
C3 C4 H4 119.4 . . ?
C32 C33 H33 120.0 . . ?
C32 C33 C34 120.1(4) . . ?
C34 C33 H33 120.0 . . ?
C36 C35 H35 120.7 . . ?
C34 C35 C36 118.7(4) . . ?
C34 C35 H35 120.7 . . ?
C33 C34 H34 119.1 . . ?
C35 C34 C33 121.9(4) . . ?
C35 C34 H34 119.1 . . ?
C8 C9 H9 120.9 . . ?
C10 C9 C8 118.2(4) . . ?
C10 C9 H9 120.9 . . ?
C28 C29 H29 120.3 . . ?
C30 C29 C28 119.3(4) . . ?
C30 C29 H29 120.3 . . ?
C9 C10 H10 119.5 . . ?
C9 C10 C11 121.0(4) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C16 119.0(4) . . ?
C10 C11 C12 121.8(4) . . ?
C12 C11 C16 119.2(4) . . ?
C26 C21 C22 118.0(5) . . ?
C20 C21 C26 119.6(4) . . ?
C20 C21 C22 122.3(5) . . ?
N19 C17 C3 113.0(3) . . ?
N19 C17 H17A 109.0 . . ?
N19 C17 H17B 109.0 . . ?
C3 C17 H17A 109.0 . . ?
C3 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
N18 C16 C11 117.8(4) . . ?
N18 C16 C15 122.5(4) . . ?
C15 C16 C11 119.7(4) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.6(5) . . ?
C26 C25 H25 120.8 . . ?
C24 C25 C26 118.4(5) . . ?
C24 C25 H25 120.8 . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.3(4) . . ?
C13 C12 H12 119.9 . . ?
C23 C24 H24 119.2 . . ?
C25 C24 C23 121.6(5) . . ?
C25 C24 H24 119.2 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.6(4) . . ?
C14 C13 H13 120.2 . . ?
C16 C15 H15 120.2 . . ?
C14 C15 C16 119.6(4) . . ?
C14 C15 H15 120.2 . . ?
C21 C22 H22 119.8 . . ?
C23 C22 C21 120.3(5) . . ?
C23 C22 H22 119.8 . . ?
C13 C14 H14 119.1 . . ?
C15 C14 C13 121.7(5) . . ?
C15 C14 H14 119.1 . . ?
C19 C20 C21 120.1(5) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?


_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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.880
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: water, methanol'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_rafaiodo2(1)
_database_code_depnum_ccdc_archive 'CCDC 1939485'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch Jarque'
;University of Valencia
Spain
;
_audit_update_record             
;
2019-10-28 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;
_audit_creation_date             2019-10-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '9(Br), 3(C30 H30 N9), 4(H2 O)'
_chemical_formula_sum            'C90 H98 Br9 N27 O4'
_chemical_formula_weight         2341.14
_chemical_absolute_configuration unk
_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 0.0033 0.0016 '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 -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   20.7951(4)
_cell_length_b                   30.5457(6)
_cell_length_c                   14.9217(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9478.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5680
_cell_measurement_theta_min      3.6010
_shelx_estimated_absorpt_T_max   0.654
_shelx_estimated_absorpt_T_min   0.390
_exptl_absorpt_coefficient_mu    3.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            43674
_diffrn_reflns_point_group_measured_fraction_full 0.761
_diffrn_reflns_point_group_measured_fraction_max 0.754
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.309
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00 -35.00   1.00   30.46    --  -19.87-178.00  60.00   61
  2  ω    -81.00  15.00   1.00   30.46    --  -19.87   0.00   0.00   96
  3  ω     -5.00  83.00   1.00   30.46    --   20.73  38.00  30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0118789000
_diffrn_orient_matrix_UB_12      -0.0035546000
_diffrn_orient_matrix_UB_13      0.0405544000
_diffrn_orient_matrix_UB_21      -0.0090907000
_diffrn_orient_matrix_UB_22      0.0291477000
_diffrn_orient_matrix_UB_23      0.0161722000
_diffrn_orient_matrix_UB_31      -0.0177531000
_diffrn_orient_matrix_UB_32      -0.0173187000
_diffrn_orient_matrix_UB_33      0.0188957000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.453
_reflns_Friedel_fraction_full    0.505
_reflns_Friedel_fraction_max     0.491
_reflns_number_gt                11106
_reflns_number_total             14073
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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         0.897
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 
;
 Flack x determined using 2760 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         14073
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0450
_refine_ls_restrained_S_all      0.974
_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)+(0.0527P)²+8.9994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1128
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.979(12)
 0.021(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2a,H2b} of O2, {H1a,H1b} of O1, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H4a,H4b} of O4, {H3a,H3b} of O3
3. Restrained distances
 H1a-O1
 0.82 with sigma of 0.01
 O1-H1b
 0.82 with sigma of 0.01
 H1b-H1a
 1.39 with sigma of 0.01
 O2-H2a
 0.82 with sigma of 0.01
 H3b-Br5
 2.6 with sigma of 0.01
 H4a-C55_$1
 2.893 with sigma of 0.01
 H4b-Br9A
 1.5 with sigma of 0.01
 H4b-H44
 2.2 with sigma of 0.01
4. Rigid bond restraints
 C70, N20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N11, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68, N19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C76, C78
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C76, C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C84, C86
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C14 \\sim N2 \\sim N3: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N27 \\sim N26 \\sim C78: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N2 \\sim N3 \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N8 \\sim C30 \\sim C26 \\sim C24: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(N11)
\\sim Ueq, Uanis(N20) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.001
Uanis(N5) \\sim Ueq, Uanis(N21) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N27) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
6. Others
 Fixed Sof: Br8B(0.6) Br9B(0.7) Br9A(0.3) Br8A(0.4)
7.a Free rotating group:
 O3(H3a,H3b), O4(H4a,H4b)
7.b Rotating group with stretchable bonds:
 O1(H1a,H1b), O2(H2a,H2b)
7.c Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C23(H23a,H23b), C37(H37a,H37b), C83(H83a,H83b), C15(H15a,H15b),
 C53(H53a,H53b), C75(H75a,H75b), C67(H67a,H67b), C45(H45a,H45b)
7.d Me refined with riding coordinates:
 C55(H55a,H55b,H55c)
7.e Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C64(H64), C36(H36), C4(H4), C14(H14), C32(H32), C13(H13),
 C42(H42), C34(H34), C12(H12), C66(H66), C11(H11), C19(H19), C90(H90), C49(H49),
  C30(H30), C82(H82), C22(H22), C80(H80), C52(H52), C79(H79), C41(H41),
 C88(H88), C27(H27), C81(H81), C60(H60), C62(H62), C89(H89), C44(H44), C58(H58),
  C87(H87), C57(H57), C20(H20), C28(H28), C51(H51), C50(H50), C21(H21),
 C43(H43), C59(H59), C29(H29), C71(H71), C72(H72), C73(H73), C74(H74)
7.f Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C9(H9a,H9b,H9c), C39(H39a,H39b,H39c), C77(H77a,H77b,
 H77c), C47(H47a,H47b,H47c), C69(H69a,H69b,H69c), C85(H85a,H85b,H85c), C25(H25a,
 H25b,H25c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.42155(4) 1.10194(2) 0.59132(6) 0.0239(2) Uani 1 1 d . . . . .
Br7 Br 1.08205(4) 0.77385(3) 0.10589(5) 0.0245(2) Uani 1 1 d . . . . .
Br3 Br 0.87976(4) 0.91976(3) 0.93994(6) 0.0265(2) Uani 1 1 d . . . . .
Br2 Br 0.73877(4) 1.06473(3) 1.12006(6) 0.0279(2) Uani 1 1 d . . . . .
Br4 Br 0.87834(4) 0.25354(3) -0.04701(6) 0.0292(2) Uani 1 1 d . . . . .
Br6 Br 0.74424(4) 0.39752(3) 0.13398(6) 0.0310(3) Uani 1 1 d . . . . .
Br5 Br 0.24134(4) 0.26812(3) 0.11443(6) 0.0330(2) Uani 1 1 d D . . . .
Br8B Br 0.9109(4) 0.5611(2) 0.6314(4) 0.0196(7) Uani 0.6 1 d . . P A 2
Br9B Br 0.87553(7) 0.56656(4) 1.00352(10) 0.0269(3) Uani 0.7 1 d . . P B 2
N1 N 0.5508(3) 1.03746(19) 1.1217(4) 0.0167(14) Uani 1 1 d . . . . .
N4 N 0.5617(3) 1.11594(19) 0.7401(4) 0.0166(14) Uani 1 1 d . . . . .
N10 N 0.9492(3) 0.7092(2) 0.6152(4) 0.0206(15) Uani 1 1 d . . . . .
N13 N 0.9366(3) 0.78423(19) 0.2335(4) 0.0185(15) Uani 1 1 d . . . . .
N24 N 0.7156(3) 0.25191(19) -0.0522(5) 0.0239(15) Uani 1 1 d . . . . .
N14 N 0.9380(3) 0.84544(19) 0.2943(4) 0.0173(14) Uani 1 1 d . U . . .
N9 N 0.7176(3) 0.92151(19) 0.9367(5) 0.0206(15) Uani 1 1 d . . . . .
N5 N 0.5603(3) 1.17719(18) 0.8049(4) 0.0158(14) Uani 1 1 d . U . . .
O1 O 0.8691(3) 1.00615(19) 1.0778(4) 0.0391(16) Uani 1 1 d D . . . .
H1A H 0.8451(3) 1.0266(2) 1.0746(4) 0.047 Uiso 1 1 d DGR . . . .
H1B H 0.8666(3) 0.9876(2) 1.0371(5) 0.047 Uiso 1 1 d DGR . . . .
N8 N 0.7180(3) 0.8810(2) 0.9018(4) 0.0203(15) Uani 1 1 d . U . . .
N7 N 0.7348(3) 0.94602(19) 0.8673(5) 0.0184(15) Uani 1 1 d . . . . .
O2 O 0.8740(3) 0.3377(2) 0.0982(5) 0.0455(18) Uani 1 1 d D . . . .
H2A H 0.8706(3) 0.3192(3) 0.0584(8) 0.055 Uiso 1 1 d DGR . . . .
H2B H 0.8382(6) 0.3511(3) 0.1010(5) 0.055 Uiso 1 1 d GR . . . .
N3 N 0.5646(3) 1.0160(2) 1.1972(4) 0.0187(14) Uani 1 1 d . U . . .
N23 N 0.7173(3) 0.2117(2) -0.0889(5) 0.0218(16) Uani 1 1 d . . . . .
N6 N 0.5493(3) 1.13458(19) 0.8200(4) 0.0199(15) Uani 1 1 d . . . . .
N17 N 0.7819(3) 0.5474(2) 0.4117(5) 0.0208(15) Uani 1 1 d . . . . .
N18 N 0.7803(3) 0.5886(2) 0.4421(5) 0.0238(15) Uani 1 1 d . . . . .
N25 N 0.5566(3) 0.3687(2) 0.1506(5) 0.0246(17) Uani 1 1 d . . . . .
N15 N 0.9487(3) 0.80308(19) 0.3123(4) 0.0212(16) Uani 1 1 d . . . . .
N22 N 0.7336(3) 0.2775(2) -0.1189(5) 0.0213(16) Uani 1 1 d . . . . .
N2 N 0.5830(3) 1.0481(2) 1.2528(4) 0.0182(14) Uani 1 1 d . U . . .
N12 N 0.9328(3) 0.6895(2) 0.6913(5) 0.0243(16) Uani 1 1 d . . . . .
N16 N 0.7666(3) 0.6112(2) 0.3687(5) 0.0211(16) Uani 1 1 d . . . . .
N11 N 0.9152(3) 0.7227(2) 0.7431(5) 0.0250(15) Uani 1 1 d . U . . .
C16 C 0.5797(4) 1.1442(2) 0.6761(5) 0.0184(17) Uani 1 1 d . U . . .
C5 C 0.6696(4) 1.0110(2) 0.8869(5) 0.0127(15) Uani 1 1 d . . . . .
N19 N 0.5508(4) 0.4435(2) -0.2318(5) 0.0298(17) Uani 1 1 d . U . . .
C7 C 0.5273(4) 1.0114(2) 1.0452(5) 0.0162(16) Uani 1 1 d . . . . .
H7A H 0.483258 1.019607 1.031806 0.019 Uiso 1 1 calc R . . . .
H7B H 0.527596 0.980572 1.061145 0.019 Uiso 1 1 calc R . . . .
C46 C 0.9193(4) 0.8118(2) 0.1680(5) 0.0210(18) Uani 1 1 d . U . . .
N27 N 0.5901(3) 0.3805(2) 0.2799(5) 0.0284(16) Uani 1 1 d . U . . .
C1 C 0.5687(4) 1.0184(2) 0.9629(5) 0.0159(17) Uani 1 1 d . . . . .
C8 C 0.5593(4) 1.0810(2) 1.1266(5) 0.0173(17) Uani 1 1 d . U . . .
O3 O 0.3717(3) 0.3249(3) 0.0571(7) 0.071(3) Uani 1 1 d . . . . .
H3A H 0.378850 0.350414 0.036616 0.106 Uiso 1 1 d G . . . .
H3B H 0.331354 0.320170 0.058098 0.106 Uiso 1 1 d DG . . . .
C6 C 0.6322(4) 1.0055(2) 0.9635(5) 0.0148(16) Uani 1 1 d . . . . .
H6 H 0.650011 0.993278 1.014897 0.018 Uiso 1 1 calc R . . . .
C68 C 0.5682(4) 0.4729(3) -0.2930(6) 0.0290(19) Uani 1 1 d . U . . .
N26 N 0.5705(4) 0.3479(2) 0.2263(5) 0.0286(17) Uani 1 1 d . U . . .
C18 C 0.5791(4) 1.1852(2) 0.7169(5) 0.0147(16) Uani 1 1 d . U . . .
C2 C 0.5424(4) 1.0375(2) 0.8873(5) 0.0139(16) Uani 1 1 d . . . . .
H2 H 0.499235 1.045459 0.886933 0.017 Uiso 1 1 calc R . . . .
N20 N 0.5476(4) 0.5032(2) -0.1627(6) 0.0393(19) Uani 1 1 d . U . . .
C64 C 0.6329(4) 0.3363(2) -0.0153(5) 0.0214(19) Uani 1 1 d . . . . .
H64 H 0.652838 0.324542 0.035080 0.026 Uiso 1 1 calc R . . . .
C36 C 0.8681(4) 0.6730(2) 0.4586(5) 0.0169(17) Uani 1 1 d . . . . .
H36 H 0.850322 0.660623 0.509819 0.020 Uiso 1 1 calc R . . . .
C48 C 0.9195(4) 0.8528(2) 0.2066(5) 0.0179(17) Uani 1 1 d . . . . .
N21 N 0.5368(4) 0.4604(2) -0.1508(5) 0.0341(19) Uani 1 1 d . U . . .
C65 C 0.6676(4) 0.3416(2) -0.0926(5) 0.0204(18) Uani 1 1 d . . . . .
C63 C 0.5685(4) 0.3483(2) -0.0108(6) 0.0207(19) Uani 1 1 d . . . . .
C35 C 0.8306(4) 0.6778(2) 0.3813(5) 0.0149(16) Uani 1 1 d . . . . .
C31 C 0.9319(4) 0.6867(2) 0.4588(5) 0.0180(17) Uani 1 1 d . . . . .
C23 C 0.7368(4) 0.9932(2) 0.8832(6) 0.0205(18) Uani 1 1 d . . . . .
H23A H 0.760460 1.007459 0.835423 0.025 Uiso 1 1 calc R . . . .
H23B H 0.758635 0.999132 0.939322 0.025 Uiso 1 1 calc R . . . .
C37 C 0.9724(4) 0.6810(2) 0.5412(5) 0.0220(18) Uani 1 1 d . . . . .
H37A H 0.971204 0.650657 0.559967 0.026 Uiso 1 1 calc R . . . .
H37B H 1.016653 0.688469 0.527377 0.026 Uiso 1 1 calc R . . . .
C83 C 0.7355(4) 0.3247(2) -0.1000(6) 0.024(2) Uani 1 1 d . . . . .
H83A H 0.757865 0.339891 -0.147758 0.029 Uiso 1 1 calc R . . . .
H83B H 0.758319 0.329995 -0.044341 0.029 Uiso 1 1 calc R . . . .
C4 C 0.6438(4) 1.0311(2) 0.8117(5) 0.0166(17) Uani 1 1 d . . . . .
H4 H 0.669144 1.035265 0.761109 0.020 Uiso 1 1 calc R . . . .
C10 C 0.5806(4) 1.0889(3) 1.2124(5) 0.0184(17) Uani 1 1 d . U . . .
C38 C 0.9425(4) 0.7537(2) 0.6158(5) 0.0202(18) Uani 1 1 d . U . . .
C17 C 0.5974(4) 1.1323(2) 0.5825(5) 0.0246(19) Uani 1 1 d . . . . .
H17A H 0.637472 1.116673 0.582658 0.037 Uiso 1 1 calc GR . . . .
H17B H 0.601792 1.158467 0.547368 0.037 Uiso 1 1 calc GR . . . .
H17C H 0.564441 1.114142 0.557120 0.037 Uiso 1 1 calc GR . . . .
C86 C 0.7371(4) 0.2123(2) -0.1771(6) 0.0198(18) Uani 1 1 d . U . . .
C9 C 0.5474(4) 1.1118(2) 1.0510(5) 0.0209(18) Uani 1 1 d . . . . .
H9A H 0.580449 1.108399 1.006660 0.031 Uiso 1 1 calc GR . . . .
H9B H 0.547711 1.141373 1.072992 0.031 Uiso 1 1 calc GR . . . .
H9C H 0.506277 1.105616 1.024561 0.031 Uiso 1 1 calc GR . . . .
C14 C 0.6030(4) 1.0418(3) 1.3392(6) 0.027(2) Uani 1 1 d . U . . .
H14 H 0.604253 1.013953 1.364410 0.032 Uiso 1 1 calc R . . . .
O4 O 0.8798(4) 0.6191(2) 0.8153(6) 0.056(2) Uani 1 1 d . U . C 3
H4A H 0.873920 0.594069 0.791532 0.084 Uiso 1 1 d DG . . C 3
H4B H 0.850778 0.623608 0.854543 0.084 Uiso 1 1 d DG . . C 3
C32 C 0.9574(4) 0.7062(2) 0.3824(5) 0.0170(17) Uani 1 1 d . . . . .
H32 H 1.000279 0.714812 0.381961 0.020 Uiso 1 1 calc R . . . .
C26 C 0.7365(4) 0.8801(2) 0.8133(6) 0.0227(18) Uani 1 1 d . U . . .
C56 C 0.7696(4) 0.5447(3) 0.3215(6) 0.0232(18) Uani 1 1 d . U . . .
C24 C 0.7473(4) 0.9239(3) 0.7916(6) 0.0225(18) Uani 1 1 d . U . . .
C13 C 0.6207(5) 1.0769(3) 1.3860(6) 0.033(2) Uani 1 1 d . . . . .
H13 H 0.635641 1.073218 1.444291 0.039 Uiso 1 1 calc R . . . .
C42 C 0.8825(4) 0.7967(3) 0.8340(6) 0.030(2) Uani 1 1 d . . . . .
H42 H 0.871730 0.821420 0.867086 0.036 Uiso 1 1 calc R . . . .
C34 C 0.8568(4) 0.6981(2) 0.3063(5) 0.0190(17) Uani 1 1 d . . . . .
H34 H 0.831783 0.701815 0.255186 0.023 Uiso 1 1 calc R . . . .
C12 C 0.6175(4) 1.1204(3) 1.3491(6) 0.030(2) Uani 1 1 d . . . . .
H12 H 0.628807 1.144446 1.383891 0.036 Uiso 1 1 calc R . . . .
C66 C 0.6390(4) 0.3607(2) -0.1669(6) 0.0213(19) Uani 1 1 d . . . . .
H66 H 0.662346 0.365305 -0.219194 0.026 Uiso 1 1 calc R . . . .
C39 C 0.9566(4) 0.7829(2) 0.5407(5) 0.0249(19) Uani 1 1 d . U . . .
H39A H 0.998759 0.776573 0.517878 0.037 Uiso 1 1 calc GR . . . .
H39B H 0.954911 0.812731 0.560600 0.037 Uiso 1 1 calc GR . . . .
H39C H 0.925376 0.778451 0.494124 0.037 Uiso 1 1 calc GR . . . .
C76 C 0.5663(4) 0.4125(3) 0.1517(7) 0.028(2) Uani 1 1 d . U . . .
C11 C 0.5979(4) 1.1259(3) 1.2636(6) 0.0229(19) Uani 1 1 d . . . . .
H11 H 0.595772 1.153785 1.238682 0.027 Uiso 1 1 calc R . . . .
C19 C 0.5907(4) 1.2286(2) 0.6912(5) 0.0211(18) Uani 1 1 d . . . . .
H19 H 0.602429 1.235263 0.632677 0.025 Uiso 1 1 calc R . . . .
C90 C 0.7037(4) 0.1739(2) -0.0415(6) 0.027(2) Uani 1 1 d . . . . .
H90 H 0.692016 0.174697 0.018628 0.033 Uiso 1 1 calc R . . . .
C49 C 0.9065(4) 0.8961(2) 0.1784(6) 0.0226(19) Uani 1 1 d . . . . .
H49 H 0.894047 0.902045 0.119773 0.027 Uiso 1 1 calc R . . . .
C30 C 0.7038(4) 0.8437(2) 0.9512(6) 0.0264(18) Uani 1 1 d . U . . .
H30 H 0.692250 0.845258 1.011369 0.032 Uiso 1 1 calc R . . . .
C84 C 0.7471(4) 0.2566(3) -0.1966(6) 0.0228(19) Uani 1 1 d . U . . .
C77 C 0.5546(4) 0.4429(2) 0.0758(6) 0.033(2) Uani 1 1 d . U . . .
H77A H 0.584632 0.436780 0.028505 0.049 Uiso 1 1 calc GR . . . .
H77B H 0.560138 0.472507 0.095762 0.049 Uiso 1 1 calc GR . . . .
H77C H 0.511570 0.438973 0.054000 0.049 Uiso 1 1 calc GR . . . .
C47 C 0.9024(5) 0.7984(3) 0.0759(5) 0.029(2) Uani 1 1 d . U . . .
H47A H 0.936254 0.780570 0.051702 0.043 Uiso 1 1 calc GR . . . .
H47B H 0.896903 0.823917 0.039195 0.043 Uiso 1 1 calc GR . . . .
H47C H 0.863094 0.781906 0.076899 0.043 Uiso 1 1 calc GR . . . .
C82 C 0.6101(4) 0.3743(3) 0.3670(6) 0.030(2) Uani 1 1 d . . . . .
H82 H 0.611278 0.346571 0.392771 0.036 Uiso 1 1 calc R . . . .
C69 C 0.5881(4) 0.4618(3) -0.3876(7) 0.038(2) Uani 1 1 d . U . . .
H69A H 0.628872 0.447023 -0.386586 0.057 Uiso 1 1 calc GR . . . .
H69B H 0.591739 0.488199 -0.422010 0.057 Uiso 1 1 calc GR . . . .
H69C H 0.556393 0.443024 -0.414300 0.057 Uiso 1 1 calc GR . . . .
C15 C 0.5515(4) 1.0682(2) 0.7315(5) 0.0188(17) Uani 1 1 d . . . . .
H15A H 0.571639 1.057620 0.677056 0.023 Uiso 1 1 calc R . . . .
H15B H 0.505777 1.062021 0.727900 0.023 Uiso 1 1 calc R . . . .
C22 C 0.5546(4) 1.2087(2) 0.8692(5) 0.0202(18) Uani 1 1 d . . . . .
H22 H 0.543870 1.201924 0.928123 0.024 Uiso 1 1 calc R . . . .
C80 C 0.6263(4) 0.4531(3) 0.3737(7) 0.036(2) Uani 1 1 d . . . . .
H80 H 0.638649 0.477187 0.407851 0.043 Uiso 1 1 calc R . . . .
C54 C 0.7612(4) 0.5874(3) 0.2930(6) 0.0265(19) Uani 1 1 d . U . . .
C85 C 0.7702(5) 0.2767(3) -0.2807(6) 0.036(2) Uani 1 1 d . . . . .
H85A H 0.751061 0.305054 -0.287792 0.053 Uiso 1 1 calc GR . . . .
H85B H 0.758434 0.258428 -0.330477 0.053 Uiso 1 1 calc GR . . . .
H85C H 0.816155 0.279562 -0.278562 0.053 Uiso 1 1 calc GR . . . .
C53 C 0.7634(4) 0.6591(2) 0.3800(6) 0.0222(19) Uani 1 1 d . . . . .
H53A H 0.741627 0.666140 0.435634 0.027 Uiso 1 1 calc R . . . .
H53B H 0.739204 0.671936 0.331037 0.027 Uiso 1 1 calc R . . . .
C52 C 0.9427(4) 0.8782(2) 0.3578(5) 0.0219(18) Uani 1 1 d . . . . .
H52 H 0.953126 0.872371 0.417179 0.026 Uiso 1 1 calc R . . . .
C70 C 0.5661(4) 0.5131(2) -0.2470(6) 0.0256(17) Uani 1 1 d . U . . .
C78 C 0.5880(4) 0.4210(3) 0.2370(7) 0.029(2) Uani 1 1 d . U . . .
C75 C 0.5305(4) 0.3423(3) 0.0742(6) 0.031(2) Uani 1 1 d . . . . .
H75A H 0.486207 0.350849 0.063496 0.037 Uiso 1 1 calc R . . . .
H75B H 0.530736 0.311605 0.090573 0.037 Uiso 1 1 calc R . . . .
C79 C 0.6068(4) 0.4587(3) 0.2872(6) 0.029(2) Uani 1 1 d . . . . .
H79 H 0.605722 0.486426 0.261521 0.035 Uiso 1 1 calc R . . . .
C41 C 0.9039(4) 0.8011(3) 0.7503(6) 0.027(2) Uani 1 1 d . . . . .
H41 H 0.908707 0.828625 0.724622 0.033 Uiso 1 1 calc R . . . .
C40 C 0.9193(4) 0.7628(3) 0.7014(6) 0.0229(17) Uani 1 1 d . U . . .
C3 C 0.5800(4) 1.0449(2) 0.8117(5) 0.0163(17) Uani 1 1 d . . . . .
C25 C 0.7695(4) 0.9425(3) 0.7067(6) 0.034(2) Uani 1 1 d . . . . .
H25A H 0.751315 0.971157 0.698924 0.051 Uiso 1 1 calc GR . . . .
H25B H 0.756198 0.923980 0.658127 0.051 Uiso 1 1 calc GR . . . .
H25C H 0.815553 0.944607 0.707244 0.051 Uiso 1 1 calc GR . . . .
C33 C 0.9197(4) 0.7129(2) 0.3069(5) 0.0210(18) Uani 1 1 d . . . . .
C88 C 0.7258(4) 0.1351(3) -0.1797(6) 0.028(2) Uani 1 1 d . . . . .
H88 H 0.727252 0.108523 -0.210076 0.034 Uiso 1 1 calc R . . . .
C27 C 0.7381(4) 0.8389(3) 0.7695(6) 0.029(2) Uani 1 1 d . . . . .
H27 H 0.748758 0.837204 0.709084 0.035 Uiso 1 1 calc R . . . .
C81 C 0.6277(5) 0.4096(3) 0.4124(7) 0.042(3) Uani 1 1 d . . . . .
H81 H 0.641500 0.406358 0.471288 0.050 Uiso 1 1 calc R . . . .
C60 C 0.7932(4) 0.5115(3) 0.4661(6) 0.031(2) Uani 1 1 d . . . . .
H60 H 0.800832 0.514531 0.527176 0.037 Uiso 1 1 calc R . . . .
C62 C 0.5390(4) 0.3666(2) -0.0855(6) 0.024(2) Uani 1 1 d . . . . .
H62 H 0.495757 0.374130 -0.083407 0.029 Uiso 1 1 calc R . . . .
C89 C 0.7082(4) 0.1359(3) -0.0868(6) 0.031(2) Uani 1 1 d . . . . .
H89 H 0.699777 0.109722 -0.057358 0.037 Uiso 1 1 calc R . . . .
C44 C 0.8928(4) 0.7180(3) 0.8294(6) 0.032(2) Uani 1 1 d . . . . .
H44 H 0.889714 0.690520 0.856017 0.038 Uiso 1 1 calc DR . . . .
C58 C 0.7808(4) 0.4669(3) 0.3345(7) 0.035(2) Uani 1 1 d . . . . .
H58 H 0.780693 0.439030 0.309370 0.042 Uiso 1 1 calc R . . . .
C87 C 0.7404(4) 0.1725(3) -0.2237(6) 0.0265(19) Uani 1 1 d . . . . .
H87 H 0.752411 0.171798 -0.283736 0.032 Uiso 1 1 calc R . . . .
C57 C 0.7693(4) 0.5023(3) 0.2810(6) 0.034(2) Uani 1 1 d . . . . .
H57 H 0.761391 0.498957 0.220014 0.040 Uiso 1 1 calc R . . . .
C20 C 0.5845(4) 1.2605(3) 0.7535(6) 0.026(2) Uani 1 1 d . . . . .
H20 H 0.592751 1.289474 0.737920 0.031 Uiso 1 1 calc R . . . .
C28 C 0.7242(4) 0.8026(3) 0.8153(7) 0.033(2) Uani 1 1 d . . . . .
H28 H 0.725529 0.775590 0.786745 0.039 Uiso 1 1 calc R . . . .
C51 C 0.9311(4) 0.9198(2) 0.3280(6) 0.024(2) Uani 1 1 d . . . . .
H51 H 0.935465 0.943031 0.367878 0.028 Uiso 1 1 calc R . . . .
C50 C 0.9128(4) 0.9288(2) 0.2396(6) 0.026(2) Uani 1 1 d . . . . .
H50 H 0.904916 0.957530 0.222482 0.031 Uiso 1 1 calc R . . . .
C21 C 0.5655(4) 1.2502(3) 0.8424(6) 0.028(2) Uani 1 1 d . . . . .
H21 H 0.560442 1.272825 0.883549 0.034 Uiso 1 1 calc R . . . .
C43 C 0.8757(5) 0.7542(3) 0.8736(6) 0.034(2) Uani 1 1 d . . . . .
H43 H 0.859156 0.751731 0.931250 0.041 Uiso 1 1 calc R . . . .
C55 C 0.7486(5) 0.6046(3) 0.2021(7) 0.044(3) Uani 1 1 d D . . . .
H55A H 0.747005 0.580735 0.160293 0.066 Uiso 1 1 calc R . . . .
H55B H 0.708156 0.619785 0.201720 0.066 Uiso 1 1 calc R . . . .
H55C H 0.782317 0.624391 0.185381 0.066 Uiso 1 1 calc R . . . .
C61 C 0.5733(4) 0.3733(2) -0.1613(6) 0.0227(19) Uani 1 1 d . U . . .
C59 C 0.7927(4) 0.4716(3) 0.4262(7) 0.036(2) Uani 1 1 d . . . . .
H59 H 0.800513 0.446800 0.460686 0.043 Uiso 1 1 calc R . . . .
C29 C 0.7075(4) 0.8050(3) 0.9078(7) 0.033(2) Uani 1 1 d . . . . .
H29 H 0.698843 0.779319 0.938983 0.039 Uiso 1 1 calc R . . . .
C67 C 0.5445(4) 0.3960(2) -0.2434(6) 0.028(2) Uani 1 1 d . . . . .
H67A H 0.567032 0.386732 -0.297075 0.034 Uiso 1 1 calc R . . . .
H67B H 0.499554 0.388115 -0.249523 0.034 Uiso 1 1 calc R . . . .
C45 C 0.9478(4) 0.7365(2) 0.2272(5) 0.0238(19) Uani 1 1 d . . . . .
H45A H 0.993671 0.730846 0.224213 0.029 Uiso 1 1 calc R . . . .
H45B H 0.928367 0.725362 0.172654 0.029 Uiso 1 1 calc R . . . .
C71 C 0.5782(4) 0.5574(3) -0.2699(8) 0.043(3) Uani 1 1 d . . . . .
H71 H 0.590280 0.565897 -0.327400 0.051 Uiso 1 1 calc R . . . .
C72 C 0.5707(4) 0.5874(3) -0.2001(7) 0.036(2) Uani 1 1 d . U . . .
H72 H 0.577052 0.616965 -0.211952 0.043 Uiso 1 1 calc R . . . .
C73 C 0.5543(5) 0.5749(3) -0.1141(8) 0.047(3) Uani 1 1 d . . . . .
H73 H 0.551191 0.596007 -0.069525 0.056 Uiso 1 1 calc R . . . .
C74 C 0.5430(5) 0.5338(3) -0.0941(7) 0.046(3) Uani 1 1 d . U . . .
H74 H 0.532302 0.525442 -0.036086 0.056 Uiso 1 1 calc R . . . .
Br9A Br 0.87868(17) 0.58441(16) 0.9518(5) 0.0636(12) Uani 0.3 1 d D . P D 1
Br8A Br 0.9161(6) 0.5619(4) 0.6124(7) 0.054(3) Uani 0.4 1 d . . P E 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 N3 1.335(8) . ?
N1 C7 1.476(9) . ?
N1 C8 1.343(9) . ?
N4 N6 1.347(8) . ?
N4 C16 1.339(10) . ?
N4 C15 1.480(9) . ?
N10 N12 1.330(9) . ?
N10 C37 1.481(9) . ?
N10 C38 1.367(9) . ?
N13 N15 1.333(8) . ?
N13 C46 1.340(10) . ?
N13 C45 1.480(9) . ?
N24 N23 1.345(8) . ?
N24 N22 1.319(9) . ?
N14 N15 1.340(8) . ?
N14 C48 1.382(9) . ?
N14 C52 1.382(9) . ?
N9 N8 1.343(8) . ?
N9 N7 1.327(9) . ?
N5 N6 1.341(8) . ?
N5 C18 1.392(9) . ?
N5 C22 1.364(9) . ?
O1 H1A 0.801(6) . ?
O1 H1B 0.833(6) . ?
N8 C26 1.376(10) . ?
N8 C30 1.389(10) . ?
N7 C23 1.461(9) . ?
N7 C24 1.342(10) . ?
O2 H2A 0.822(13) . ?
O2 H2B 0.851(13) . ?
N3 N2 1.339(9) . ?
N23 C86 1.380(10) . ?
N23 C90 1.383(10) . ?
N17 N18 1.337(8) . ?
N17 C56 1.373(10) . ?
N17 C60 1.385(10) . ?
N18 N16 1.326(9) . ?
N25 N26 1.327(10) . ?
N25 C76 1.353(10) . ?
N25 C75 1.497(11) . ?
N22 C83 1.470(9) . ?
N22 C84 1.353(10) . ?
N2 C10 1.387(10) . ?
N2 C14 1.369(11) . ?
N12 N11 1.326(9) . ?
N16 C54 1.348(10) . ?
N16 C53 1.475(9) . ?
N11 C40 1.376(10) . ?
N11 C44 1.377(12) . ?
C16 C18 1.393(10) . ?
C16 C17 1.490(10) . ?
C5 C6 1.393(10) . ?
C5 C23 1.499(10) . ?
C5 C4 1.386(10) . ?
N19 C68 1.329(11) . ?
N19 N21 1.345(10) . ?
N19 C67 1.469(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C1 1.515(10) . ?
C46 C48 1.377(10) . ?
C46 C47 1.477(11) . ?
N27 N26 1.341(10) . ?
N27 C82 1.377(11) . ?
N27 C78 1.394(11) . ?
C1 C6 1.378(10) . ?
C1 C2 1.383(10) . ?
C8 C10 1.376(11) . ?
C8 C9 1.491(10) . ?
O3 H3A 0.8499 . ?
O3 H3B 0.8516 . ?
C6 H6 0.9300 . ?
C68 C69 1.510(13) . ?
C68 C70 1.410(11) . ?
C18 C19 1.400(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.390(10) . ?
N20 N21 1.340(10) . ?
N20 C70 1.349(12) . ?
N20 C74 1.389(11) . ?
C64 H64 0.9300 . ?
C64 C65 1.370(11) . ?
C64 C63 1.391(11) . ?
C36 H36 0.9300 . ?
C36 C35 1.399(10) . ?
C36 C31 1.391(10) . ?
C48 C49 1.415(10) . ?
C65 C83 1.506(11) . ?
C65 C66 1.387(11) . ?
C63 C75 1.507(11) . ?
C63 C62 1.388(11) . ?
C35 C34 1.391(10) . ?
C35 C53 1.509(10) . ?
C31 C37 1.499(11) . ?
C31 C32 1.391(11) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C4 H4 0.9300 . ?
C4 C3 1.393(10) . ?
C10 C11 1.409(11) . ?
C38 C39 1.461(11) . ?
C38 C40 1.392(11) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C86 C84 1.400(11) . ?
C86 C87 1.402(11) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C14 H14 0.9300 . ?
C14 C13 1.332(12) . ?
O4 H4A 0.8517 . ?
O4 H4B 0.8521 . ?
C32 H32 0.9300 . ?
C32 C33 1.388(11) . ?
C26 C24 1.394(11) . ?
C26 C27 1.419(11) . ?
C56 C54 1.383(11) . ?
C56 C57 1.428(11) . ?
C24 C25 1.463(12) . ?
C13 H13 0.9300 . ?
C13 C12 1.439(12) . ?
C42 H42 0.9300 . ?
C42 C41 1.334(13) . ?
C42 C43 1.433(13) . ?
C34 H34 0.9300 . ?
C34 C33 1.383(11) . ?
C12 H12 0.9300 . ?
C12 C11 1.351(12) . ?
C66 H66 0.9300 . ?
C66 C61 1.421(11) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C76 C77 1.485(12) . ?
C76 C78 1.375(13) . ?
C11 H11 0.9300 . ?
C19 H19 0.9300 . ?
C19 C20 1.355(11) . ?
C90 H90 0.9300 . ?
C90 C89 1.347(11) . ?
C49 H49 0.9300 . ?
C49 C50 1.359(11) . ?
C30 H30 0.9300 . ?
C30 C29 1.348(11) . ?
C84 C85 1.478(12) . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C82 H82 0.9300 . ?
C82 C81 1.326(13) . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C3 1.513(10) . ?
C22 H22 0.9300 . ?
C22 C21 1.349(11) . ?
C80 H80 0.9300 . ?
C80 C79 1.364(13) . ?
C80 C81 1.449(14) . ?
C54 C55 1.478(13) . ?
C85 H85A 0.9600 . ?
C85 H85B 0.9600 . ?
C85 H85C 0.9600 . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C52 H52 0.9300 . ?
C52 C51 1.368(11) . ?
C70 C71 1.418(12) . ?
C78 C79 1.429(12) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C79 H79 0.9300 . ?
C41 H41 0.9300 . ?
C41 C40 1.416(11) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C33 C45 1.509(11) . ?
C88 H88 0.9300 . ?
C88 C89 1.434(12) . ?
C88 C87 1.351(11) . ?
C27 H27 0.9300 . ?
C27 C28 1.334(12) . ?
C81 H81 0.9300 . ?
C60 H60 0.9300 . ?
C60 C59 1.355(11) . ?
C62 H62 0.9300 . ?
C62 C61 1.352(12) . ?
C89 H89 0.9300 . ?
C44 H44 0.9300 . ?
C44 C43 1.335(12) . ?
C58 H58 0.9300 . ?
C58 C57 1.366(12) . ?
C58 C59 1.399(13) . ?
C87 H87 0.9300 . ?
C57 H57 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.419(12) . ?
C28 H28 0.9300 . ?
C28 C29 1.425(13) . ?
C51 H51 0.9300 . ?
C51 C50 1.398(12) . ?
C50 H50 0.9300 . ?
C21 H21 0.9300 . ?
C43 H43 0.9300 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C61 C67 1.529(12) . ?
C59 H59 0.9300 . ?
C29 H29 0.9300 . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C71 H71 0.9300 . ?
C71 C72 1.395(13) . ?
C72 H72 0.9300 . ?
C72 C73 1.382(14) . ?
C73 H73 0.9300 . ?
C73 C74 1.310(14) . ?
C74 H74 0.9300 . ?

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
N3 N1 C7 117.3(6) . . ?
N3 N1 C8 114.3(6) . . ?
C8 N1 C7 128.4(6) . . ?
N6 N4 C15 117.7(6) . . ?
C16 N4 N6 114.4(6) . . ?
C16 N4 C15 127.8(6) . . ?
N12 N10 C37 117.2(6) . . ?
N12 N10 C38 114.7(6) . . ?
C38 N10 C37 128.1(7) . . ?
N15 N13 C46 115.0(6) . . ?
N15 N13 C45 116.9(6) . . ?
C46 N13 C45 128.0(7) . . ?
N22 N24 N23 103.1(6) . . ?
N15 N14 C48 113.1(6) . . ?
N15 N14 C52 123.4(7) . . ?
C52 N14 C48 123.4(6) . . ?
N7 N9 N8 102.5(6) . . ?
N6 N5 C18 112.1(6) . . ?
N6 N5 C22 123.5(6) . . ?
C22 N5 C18 124.4(6) . . ?
H1A O1 H1B 116.7 . . ?
N9 N8 C26 113.0(6) . . ?
N9 N8 C30 123.3(7) . . ?
C26 N8 C30 123.6(7) . . ?
N9 N7 C23 115.9(6) . . ?
N9 N7 C24 115.2(6) . . ?
C24 N7 C23 128.9(7) . . ?
H2A O2 H2B 107.0 . . ?
N1 N3 N2 103.0(6) . . ?
N24 N23 C86 112.6(6) . . ?
N24 N23 C90 123.3(7) . . ?
C86 N23 C90 124.0(7) . . ?
N5 N6 N4 103.2(6) . . ?
N18 N17 C56 112.6(7) . . ?
N18 N17 C60 123.5(7) . . ?
C56 N17 C60 123.9(7) . . ?
N16 N18 N17 102.5(6) . . ?
N26 N25 C76 115.5(7) . . ?
N26 N25 C75 118.0(6) . . ?
C76 N25 C75 126.5(8) . . ?
N13 N15 N14 102.0(6) . . ?
N24 N22 C83 116.4(7) . . ?
N24 N22 C84 115.2(6) . . ?
C84 N22 C83 128.5(7) . . ?
N3 N2 C10 112.3(6) . . ?
N3 N2 C14 124.6(7) . . ?
C14 N2 C10 123.1(7) . . ?
N11 N12 N10 102.8(6) . . ?
N18 N16 C54 115.4(7) . . ?
N18 N16 C53 115.7(6) . . ?
C54 N16 C53 128.8(7) . . ?
N12 N11 C40 113.5(7) . . ?
N12 N11 C44 124.0(7) . . ?
C40 N11 C44 122.5(7) . . ?
N4 C16 C18 105.4(7) . . ?
N4 C16 C17 125.5(7) . . ?
C18 C16 C17 129.1(7) . . ?
C6 C5 C23 120.4(7) . . ?
C4 C5 C6 120.0(7) . . ?
C4 C5 C23 119.4(7) . . ?
C68 N19 N21 114.7(7) . . ?
C68 N19 C67 127.6(8) . . ?
N21 N19 C67 117.7(7) . . ?
N1 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
N1 C7 C1 111.2(6) . . ?
H7A C7 H7B 108.0 . . ?
C1 C7 H7A 109.4 . . ?
C1 C7 H7B 109.4 . . ?
N13 C46 C48 105.4(7) . . ?
N13 C46 C47 124.6(7) . . ?
C48 C46 C47 130.0(7) . . ?
N26 N27 C82 123.6(7) . . ?
N26 N27 C78 112.0(8) . . ?
C82 N27 C78 124.4(8) . . ?
C6 C1 C7 119.9(7) . . ?
C6 C1 C2 120.3(7) . . ?
C2 C1 C7 119.8(7) . . ?
N1 C8 C10 105.5(7) . . ?
N1 C8 C9 124.2(7) . . ?
C10 C8 C9 130.3(7) . . ?
H3A O3 H3B 109.5 . . ?
C5 C6 H6 120.1 . . ?
C1 C6 C5 119.7(7) . . ?
C1 C6 H6 120.1 . . ?
N19 C68 C69 124.5(7) . . ?
N19 C68 C70 104.2(8) . . ?
C70 C68 C69 131.2(8) . . ?
N25 N26 N27 102.6(6) . . ?
N5 C18 C16 104.9(6) . . ?
N5 C18 C19 118.2(7) . . ?
C16 C18 C19 136.9(7) . . ?
C1 C2 H2 119.7 . . ?
C1 C2 C3 120.6(7) . . ?
C3 C2 H2 119.7 . . ?
N21 N20 C70 113.0(7) . . ?
N21 N20 C74 123.2(9) . . ?
C70 N20 C74 123.8(8) . . ?
C65 C64 H64 119.5 . . ?
C65 C64 C63 121.0(8) . . ?
C63 C64 H64 119.5 . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C31 C36 C35 120.2(7) . . ?
N14 C48 C49 119.1(7) . . ?
C46 C48 N14 104.5(6) . . ?
C46 C48 C49 136.4(7) . . ?
N20 N21 N19 102.6(7) . . ?
C64 C65 C83 120.9(7) . . ?
C64 C65 C66 119.8(8) . . ?
C66 C65 C83 119.2(8) . . ?
C64 C63 C75 120.9(8) . . ?
C62 C63 C64 119.5(8) . . ?
C62 C63 C75 119.6(8) . . ?
C36 C35 C53 119.1(7) . . ?
C34 C35 C36 119.4(7) . . ?
C34 C35 C53 121.4(7) . . ?
C36 C31 C37 120.3(7) . . ?
C36 C31 C32 119.3(7) . . ?
C32 C31 C37 120.4(7) . . ?
N7 C23 C5 109.7(6) . . ?
N7 C23 H23A 109.7 . . ?
N7 C23 H23B 109.7 . . ?
C5 C23 H23A 109.7 . . ?
C5 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
N10 C37 C31 111.2(6) . . ?
N10 C37 H37A 109.4 . . ?
N10 C37 H37B 109.4 . . ?
C31 C37 H37A 109.4 . . ?
C31 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
N22 C83 C65 108.9(6) . . ?
N22 C83 H83A 109.9 . . ?
N22 C83 H83B 109.9 . . ?
C65 C83 H83A 109.9 . . ?
C65 C83 H83B 109.9 . . ?
H83A C83 H83B 108.3 . . ?
C5 C4 H4 119.9 . . ?
C5 C4 C3 120.2(7) . . ?
C3 C4 H4 119.9 . . ?
N2 C10 C11 118.5(7) . . ?
C8 C10 N2 104.9(7) . . ?
C8 C10 C11 136.6(8) . . ?
N10 C38 C39 125.4(7) . . ?
N10 C38 C40 103.8(7) . . ?
C40 C38 C39 130.8(7) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N23 C86 C84 104.7(7) . . ?
N23 C86 C87 118.5(7) . . ?
C84 C86 C87 136.8(8) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C14 H14 121.1 . . ?
C13 C14 N2 117.7(8) . . ?
C13 C14 H14 121.1 . . ?
H4A O4 H4B 109.2 . . ?
C31 C32 H32 119.6 . . ?
C33 C32 C31 120.9(8) . . ?
C33 C32 H32 119.6 . . ?
N8 C26 C24 104.5(7) . . ?
N8 C26 C27 117.7(7) . . ?
C24 C26 C27 137.8(8) . . ?
N17 C56 C54 105.5(7) . . ?
N17 C56 C57 118.1(8) . . ?
C54 C56 C57 136.3(8) . . ?
N7 C24 C26 104.8(7) . . ?
N7 C24 C25 126.5(7) . . ?
C26 C24 C25 128.6(8) . . ?
C14 C13 H13 119.0 . . ?
C14 C13 C12 122.0(9) . . ?
C12 C13 H13 119.0 . . ?
C41 C42 H42 119.7 . . ?
C41 C42 C43 120.6(8) . . ?
C43 C42 H42 119.7 . . ?
C35 C34 H34 119.7 . . ?
C33 C34 C35 120.7(7) . . ?
C33 C34 H34 119.7 . . ?
C13 C12 H12 120.3 . . ?
C11 C12 C13 119.4(8) . . ?
C11 C12 H12 120.3 . . ?
C65 C66 H66 120.7 . . ?
C65 C66 C61 118.6(8) . . ?
C61 C66 H66 120.7 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N25 C76 C77 125.8(8) . . ?
N25 C76 C78 104.3(8) . . ?
C78 C76 C77 129.9(8) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.2(8) . . ?
C12 C11 H11 120.4 . . ?
C18 C19 H19 120.7 . . ?
C20 C19 C18 118.6(8) . . ?
C20 C19 H19 120.7 . . ?
N23 C90 H90 121.7 . . ?
C89 C90 N23 116.6(8) . . ?
C89 C90 H90 121.7 . . ?
C48 C49 H49 121.1 . . ?
C50 C49 C48 117.9(8) . . ?
C50 C49 H49 121.1 . . ?
N8 C30 H30 121.6 . . ?
C29 C30 N8 116.8(8) . . ?
C29 C30 H30 121.6 . . ?
N22 C84 C86 104.4(7) . . ?
N22 C84 C85 126.8(7) . . ?
C86 C84 C85 128.7(8) . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
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 . . ?
N27 C82 H82 121.5 . . ?
C81 C82 N27 117.0(9) . . ?
C81 C82 H82 121.5 . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
N4 C15 H15A 109.7 . . ?
N4 C15 H15B 109.7 . . ?
N4 C15 C3 109.8(6) . . ?
H15A C15 H15B 108.2 . . ?
C3 C15 H15A 109.7 . . ?
C3 C15 H15B 109.7 . . ?
N5 C22 H22 122.0 . . ?
C21 C22 N5 116.1(7) . . ?
C21 C22 H22 122.0 . . ?
C79 C80 H80 120.1 . . ?
C79 C80 C81 119.8(9) . . ?
C81 C80 H80 120.1 . . ?
N16 C54 C56 103.9(8) . . ?
N16 C54 C55 126.3(8) . . ?
C56 C54 C55 129.8(8) . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
N16 C53 C35 109.7(6) . . ?
N16 C53 H53A 109.7 . . ?
N16 C53 H53B 109.7 . . ?
C35 C53 H53A 109.7 . . ?
C35 C53 H53B 109.7 . . ?
H53A C53 H53B 108.2 . . ?
N14 C52 H52 122.0 . . ?
C51 C52 N14 116.0(7) . . ?
C51 C52 H52 122.0 . . ?
C68 C70 C71 135.2(9) . . ?
N20 C70 C68 105.5(7) . . ?
N20 C70 C71 119.3(8) . . ?
N27 C78 C79 117.8(9) . . ?
C76 C78 N27 105.5(8) . . ?
C76 C78 C79 136.7(9) . . ?
N25 C75 C63 112.7(7) . . ?
N25 C75 H75A 109.1 . . ?
N25 C75 H75B 109.1 . . ?
C63 C75 H75A 109.1 . . ?
C63 C75 H75B 109.1 . . ?
H75A C75 H75B 107.8 . . ?
C80 C79 C78 118.5(9) . . ?
C80 C79 H79 120.8 . . ?
C78 C79 H79 120.8 . . ?
C42 C41 H41 120.8 . . ?
C42 C41 C40 118.4(9) . . ?
C40 C41 H41 120.8 . . ?
N11 C40 C38 105.1(7) . . ?
N11 C40 C41 119.2(8) . . ?
C38 C40 C41 135.6(8) . . ?
C2 C3 C4 119.1(7) . . ?
C2 C3 C15 119.8(7) . . ?
C4 C3 C15 121.1(7) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C32 C33 C45 119.4(8) . . ?
C34 C33 C32 119.4(7) . . ?
C34 C33 C45 121.1(8) . . ?
C89 C88 H88 119.6 . . ?
C87 C88 H88 119.6 . . ?
C87 C88 C89 120.8(8) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.8(9) . . ?
C28 C27 H27 120.1 . . ?
C82 C81 C80 122.6(10) . . ?
C82 C81 H81 118.7 . . ?
C80 C81 H81 118.7 . . ?
N17 C60 H60 121.5 . . ?
C59 C60 N17 117.0(9) . . ?
C59 C60 H60 121.5 . . ?
C63 C62 H62 120.0 . . ?
C61 C62 C63 120.0(8) . . ?
C61 C62 H62 120.0 . . ?
C90 C89 C88 121.2(8) . . ?
C90 C89 H89 119.4 . . ?
C88 C89 H89 119.4 . . ?
N11 C44 H44 121.1 . . ?
C43 C44 N11 117.7(9) . . ?
C43 C44 H44 121.1 . . ?
C57 C58 H58 119.3 . . ?
C57 C58 C59 121.4(8) . . ?
C59 C58 H58 119.3 . . ?
C86 C87 H87 120.6 . . ?
C88 C87 C86 118.7(8) . . ?
C88 C87 H87 120.6 . . ?
C56 C57 H57 121.0 . . ?
C58 C57 C56 118.0(9) . . ?
C58 C57 H57 121.0 . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.5(8) . . ?
C21 C20 H20 119.8 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.4(8) . . ?
C29 C28 H28 119.8 . . ?
C52 C51 H51 118.8 . . ?
C52 C51 C50 122.4(7) . . ?
C50 C51 H51 118.8 . . ?
C49 C50 C51 121.1(7) . . ?
C49 C50 H50 119.4 . . ?
C51 C50 H50 119.4 . . ?
C22 C21 C20 122.2(8) . . ?
C22 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
C42 C43 H43 119.3 . . ?
C44 C43 C42 121.4(9) . . ?
C44 C43 H43 119.3 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C66 C61 C67 116.8(8) . . ?
C62 C61 C66 121.0(8) . . ?
C62 C61 C67 122.2(8) . . ?
C60 C59 C58 121.6(9) . . ?
C60 C59 H59 119.2 . . ?
C58 C59 H59 119.2 . . ?
C30 C29 C28 121.6(8) . . ?
C30 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
N19 C67 C61 108.6(6) . . ?
N19 C67 H67A 110.0 . . ?
N19 C67 H67B 110.0 . . ?
C61 C67 H67A 110.0 . . ?
C61 C67 H67B 110.0 . . ?
H67A C67 H67B 108.4 . . ?
N13 C45 C33 111.1(6) . . ?
N13 C45 H45A 109.4 . . ?
N13 C45 H45B 109.4 . . ?
C33 C45 H45A 109.4 . . ?
C33 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
C70 C71 H71 122.4 . . ?
C72 C71 C70 115.2(10) . . ?
C72 C71 H71 122.4 . . ?
C71 C72 H72 118.7 . . ?
C73 C72 C71 122.6(9) . . ?
C73 C72 H72 118.7 . . ?
C72 C73 H73 119.3 . . ?
C74 C73 C72 121.4(10) . . ?
C74 C73 H73 119.3 . . ?
N20 C74 H74 121.2 . . ?
C73 C74 N20 117.6(11) . . ?
C73 C74 H74 121.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N3 N2 C10 -0.1(8) . . . . ?
N1 N3 N2 C14 -178.9(7) . . . . ?
N1 C7 C1 C6 64.3(8) . . . . ?
N1 C7 C1 C2 -116.0(7) . . . . ?
N1 C8 C10 N2 -0.2(8) . . . . ?
N1 C8 C10 C11 -179.0(9) . . . . ?
N4 C16 C18 N5 0.3(8) . . . . ?
N4 C16 C18 C19 -178.3(9) . . . . ?
N4 C15 C3 C2 90.3(8) . . . . ?
N4 C15 C3 C4 -89.1(8) . . . . ?
N10 N12 N11 C40 0.6(9) . . . . ?
N10 N12 N11 C44 178.7(8) . . . . ?
N10 C38 C40 N11 0.5(8) . . . . ?
N10 C38 C40 C41 176.9(9) . . . . ?
N13 C46 C48 N14 0.5(8) . . . . ?
N13 C46 C48 C49 180.0(9) . . . . ?
N24 N23 C86 C84 -1.3(9) . . . . ?
N24 N23 C86 C87 -179.4(7) . . . . ?
N24 N23 C90 C89 -179.1(7) . . . . ?
N24 N22 C83 C65 -72.0(9) . . . . ?
N24 N22 C84 C86 -0.6(9) . . . . ?
N24 N22 C84 C85 -177.9(8) . . . . ?
N14 C48 C49 C50 -0.2(11) . . . . ?
N14 C52 C51 C50 2.7(12) . . . . ?
N9 N8 C26 C24 -1.1(9) . . . . ?
N9 N8 C26 C27 -179.5(7) . . . . ?
N9 N8 C30 C29 -178.6(7) . . . . ?
N9 N7 C23 C5 -74.8(8) . . . . ?
N9 N7 C24 C26 0.7(9) . . . . ?
N9 N7 C24 C25 -177.4(8) . . . . ?
N5 C18 C19 C20 1.3(11) . . . . ?
N5 C22 C21 C20 -2.6(12) . . . . ?
N8 N9 N7 C23 178.0(6) . . . . ?
N8 N9 N7 C24 -1.3(8) . . . . ?
N8 C26 C24 N7 0.2(8) . . . . ?
N8 C26 C24 C25 178.2(8) . . . . ?
N8 C26 C27 C28 -2.4(12) . . . . ?
N8 C30 C29 C28 -0.9(12) . . . . ?
N7 N9 N8 C26 1.4(8) . . . . ?
N7 N9 N8 C30 179.0(7) . . . . ?
N3 N1 C7 C1 -124.1(7) . . . . ?
N3 N1 C8 C10 0.1(9) . . . . ?
N3 N1 C8 C9 179.6(7) . . . . ?
N3 N2 C10 C8 0.2(9) . . . . ?
N3 N2 C10 C11 179.2(7) . . . . ?
N3 N2 C14 C13 179.0(8) . . . . ?
N23 N24 N22 C83 178.9(6) . . . . ?
N23 N24 N22 C84 -0.1(9) . . . . ?
N23 C86 C84 N22 1.1(8) . . . . ?
N23 C86 C84 C85 178.3(9) . . . . ?
N23 C86 C87 C88 -1.9(12) . . . . ?
N23 C90 C89 C88 -0.5(12) . . . . ?
N6 N4 C16 C18 -0.1(9) . . . . ?
N6 N4 C16 C17 178.7(7) . . . . ?
N6 N4 C15 C3 -45.5(9) . . . . ?
N6 N5 C18 C16 -0.3(8) . . . . ?
N6 N5 C18 C19 178.5(7) . . . . ?
N6 N5 C22 C21 -178.1(7) . . . . ?
N17 N18 N16 C54 -1.8(9) . . . . ?
N17 N18 N16 C53 -178.0(6) . . . . ?
N17 C56 C54 N16 -2.4(9) . . . . ?
N17 C56 C54 C55 178.1(9) . . . . ?
N17 C56 C57 C58 0.4(12) . . . . ?
N17 C60 C59 C58 -0.5(13) . . . . ?
N18 N17 C56 C54 1.5(9) . . . . ?
N18 N17 C56 C57 -179.3(7) . . . . ?
N18 N17 C60 C59 179.2(7) . . . . ?
N18 N16 C54 C56 2.7(9) . . . . ?
N18 N16 C54 C55 -177.7(8) . . . . ?
N18 N16 C53 C35 79.3(8) . . . . ?
N25 C76 C78 N27 0.6(9) . . . . ?
N25 C76 C78 C79 -178.8(9) . . . . ?
N15 N13 C46 C48 -0.3(9) . . . . ?
N15 N13 C46 C47 -178.8(8) . . . . ?
N15 N13 C45 C33 46.0(10) . . . . ?
N15 N14 C48 C46 -0.5(9) . . . . ?
N15 N14 C48 C49 179.9(7) . . . . ?
N15 N14 C52 C51 179.2(7) . . . . ?
N22 N24 N23 C86 0.9(8) . . . . ?
N22 N24 N23 C90 177.9(7) . . . . ?
N2 C10 C11 C12 1.5(12) . . . . ?
N2 C14 C13 C12 1.8(13) . . . . ?
N12 N10 C37 C31 122.3(7) . . . . ?
N12 N10 C38 C39 -179.5(7) . . . . ?
N12 N10 C38 C40 -0.2(9) . . . . ?
N12 N11 C40 C38 -0.8(9) . . . . ?
N12 N11 C40 C41 -177.8(7) . . . . ?
N12 N11 C44 C43 -179.0(8) . . . . ?
N11 C44 C43 C42 -2.1(13) . . . . ?
C16 N4 N6 N5 -0.1(9) . . . . ?
C16 N4 C15 C3 137.7(8) . . . . ?
C16 C18 C19 C20 179.8(9) . . . . ?
C5 C4 C3 C2 -1.4(10) . . . . ?
C5 C4 C3 C15 178.0(6) . . . . ?
N19 C68 C70 N20 0.0(9) . . . . ?
N19 C68 C70 C71 -179.7(9) . . . . ?
C7 N1 N3 N2 -178.8(6) . . . . ?
C7 N1 C8 C10 178.7(7) . . . . ?
C7 N1 C8 C9 -1.8(12) . . . . ?
C7 C1 C6 C5 178.3(6) . . . . ?
C7 C1 C2 C3 178.8(6) . . . . ?
C46 N13 N15 N14 0.0(9) . . . . ?
C46 N13 C45 C33 -138.4(8) . . . . ?
C46 C48 C49 C50 -179.6(9) . . . . ?
N27 C82 C81 C80 0.1(14) . . . . ?
N27 C78 C79 C80 0.7(12) . . . . ?
C1 C2 C3 C4 2.9(11) . . . . ?
C1 C2 C3 C15 -176.5(6) . . . . ?
C8 N1 N3 N2 0.0(8) . . . . ?
C8 N1 C7 C1 57.3(10) . . . . ?
C8 C10 C11 C12 -179.8(9) . . . . ?
C6 C5 C23 N7 77.8(8) . . . . ?
C6 C5 C4 C3 -1.5(10) . . . . ?
C6 C1 C2 C3 -1.5(11) . . . . ?
C68 N19 N21 N20 -1.4(10) . . . . ?
C68 N19 C67 C61 137.7(9) . . . . ?
C68 C70 C71 C72 -179.1(9) . . . . ?
N26 N25 C76 C77 179.9(8) . . . . ?
N26 N25 C76 C78 -0.6(9) . . . . ?
N26 N25 C75 C63 -126.1(8) . . . . ?
N26 N27 C82 C81 -179.4(8) . . . . ?
N26 N27 C78 C76 -0.5(9) . . . . ?
N26 N27 C78 C79 179.0(7) . . . . ?
C18 N5 N6 N4 0.3(8) . . . . ?
C18 N5 C22 C21 3.0(11) . . . . ?
C18 C19 C20 C21 -1.1(12) . . . . ?
C2 C1 C6 C5 -1.4(10) . . . . ?
N20 C70 C71 C72 1.2(12) . . . . ?
C64 C65 C83 N22 80.5(9) . . . . ?
C64 C65 C66 C61 -2.0(11) . . . . ?
C64 C63 C75 N25 62.1(10) . . . . ?
C64 C63 C62 C61 -1.3(11) . . . . ?
C36 C35 C34 C33 1.1(10) . . . . ?
C36 C35 C53 N16 -76.0(8) . . . . ?
C36 C31 C37 N10 -66.9(9) . . . . ?
C36 C31 C32 C33 1.3(11) . . . . ?
C48 N14 N15 N13 0.3(8) . . . . ?
C48 N14 C52 C51 -3.4(11) . . . . ?
C48 C49 C50 C51 -0.5(12) . . . . ?
N21 N19 C68 C69 178.0(8) . . . . ?
N21 N19 C68 C70 0.9(10) . . . . ?
N21 N19 C67 C61 -43.5(10) . . . . ?
N21 N20 C70 C68 -0.9(10) . . . . ?
N21 N20 C70 C71 178.9(7) . . . . ?
N21 N20 C74 C73 -179.5(9) . . . . ?
C65 C64 C63 C75 179.7(7) . . . . ?
C65 C64 C63 C62 -1.0(11) . . . . ?
C65 C66 C61 C62 -0.3(11) . . . . ?
C65 C66 C61 C67 177.6(6) . . . . ?
C63 C64 C65 C83 -174.3(7) . . . . ?
C63 C64 C65 C66 2.6(11) . . . . ?
C63 C62 C61 C66 1.9(11) . . . . ?
C63 C62 C61 C67 -175.9(7) . . . . ?
C35 C36 C31 C37 -179.3(6) . . . . ?
C35 C36 C31 C32 1.6(10) . . . . ?
C35 C34 C33 C32 1.8(11) . . . . ?
C35 C34 C33 C45 -177.6(7) . . . . ?
C31 C36 C35 C34 -2.8(10) . . . . ?
C31 C36 C35 C53 174.6(6) . . . . ?
C31 C32 C33 C34 -3.0(11) . . . . ?
C31 C32 C33 C45 176.4(7) . . . . ?
C23 N7 C24 C26 -178.5(7) . . . . ?
C23 N7 C24 C25 3.4(14) . . . . ?
C23 C5 C6 C1 -173.9(6) . . . . ?
C23 C5 C4 C3 175.3(6) . . . . ?
C37 N10 N12 N11 179.4(6) . . . . ?
C37 N10 C38 C39 0.9(13) . . . . ?
C37 N10 C38 C40 -179.8(7) . . . . ?
C37 C31 C32 C33 -177.8(6) . . . . ?
C83 N22 C84 C86 -179.5(7) . . . . ?
C83 N22 C84 C85 3.2(14) . . . . ?
C83 C65 C66 C61 175.0(6) . . . . ?
C4 C5 C6 C1 2.9(10) . . . . ?
C4 C5 C23 N7 -99.0(8) . . . . ?
C10 N2 C14 C13 0.3(12) . . . . ?
C38 N10 N12 N11 -0.2(9) . . . . ?
C38 N10 C37 C31 -58.1(10) . . . . ?
C17 C16 C18 N5 -178.5(8) . . . . ?
C17 C16 C18 C19 2.9(16) . . . . ?
C86 N23 C90 C89 -2.5(12) . . . . ?
C9 C8 C10 N2 -179.6(8) . . . . ?
C9 C8 C10 C11 1.6(16) . . . . ?
C14 N2 C10 C8 179.0(7) . . . . ?
C14 N2 C10 C11 -2.0(11) . . . . ?
C14 C13 C12 C11 -2.1(14) . . . . ?
C32 C31 C37 N10 112.2(8) . . . . ?
C32 C33 C45 N13 -90.4(9) . . . . ?
C26 N8 C30 C29 -1.3(11) . . . . ?
C26 C27 C28 C29 0.4(13) . . . . ?
C56 N17 N18 N16 0.1(8) . . . . ?
C56 N17 C60 C59 0.9(12) . . . . ?
C24 N7 C23 C5 104.4(9) . . . . ?
C24 C26 C27 C28 179.9(10) . . . . ?
C13 C12 C11 C10 0.4(13) . . . . ?
C42 C41 C40 N11 -3.7(12) . . . . ?
C42 C41 C40 C38 -179.7(9) . . . . ?
C34 C35 C53 N16 101.3(8) . . . . ?
C34 C33 C45 N13 89.0(9) . . . . ?
C66 C65 C83 N22 -96.4(8) . . . . ?
C66 C61 C67 N19 -93.0(8) . . . . ?
C39 C38 C40 N11 179.8(8) . . . . ?
C39 C38 C40 C41 -3.9(17) . . . . ?
C76 N25 N26 N27 0.3(9) . . . . ?
C76 N25 C75 C63 55.8(10) . . . . ?
C76 C78 C79 C80 -179.9(10) . . . . ?
C19 C20 C21 C22 1.8(13) . . . . ?
C90 N23 C86 C84 -178.2(7) . . . . ?
C90 N23 C86 C87 3.7(12) . . . . ?
C30 N8 C26 C24 -178.6(7) . . . . ?
C30 N8 C26 C27 3.0(11) . . . . ?
C84 N22 C83 C65 107.0(9) . . . . ?
C84 C86 C87 C88 -179.1(9) . . . . ?
C77 C76 C78 N27 -179.8(8) . . . . ?
C77 C76 C78 C79 0.7(17) . . . . ?
C47 C46 C48 N14 178.8(8) . . . . ?
C47 C46 C48 C49 -1.7(16) . . . . ?
C82 N27 N26 N25 -179.6(8) . . . . ?
C82 N27 C78 C76 179.2(8) . . . . ?
C82 N27 C78 C79 -1.2(12) . . . . ?
C69 C68 C70 N20 -176.9(9) . . . . ?
C69 C68 C70 C71 3.4(17) . . . . ?
C15 N4 N6 N5 -177.4(6) . . . . ?
C15 N4 C16 C18 176.8(7) . . . . ?
C15 N4 C16 C17 -4.3(13) . . . . ?
C22 N5 N6 N4 -178.8(7) . . . . ?
C22 N5 C18 C16 178.7(7) . . . . ?
C22 N5 C18 C19 -2.4(11) . . . . ?
C54 N16 C53 C35 -96.4(9) . . . . ?
C54 C56 C57 C58 179.3(10) . . . . ?
C53 N16 C54 C56 178.4(7) . . . . ?
C53 N16 C54 C55 -2.1(14) . . . . ?
C53 C35 C34 C33 -176.3(6) . . . . ?
C52 N14 N15 N13 177.9(7) . . . . ?
C52 N14 C48 C46 -178.1(7) . . . . ?
C52 N14 C48 C49 2.3(11) . . . . ?
C52 C51 C50 C49 -0.8(13) . . . . ?
C70 N20 N21 N19 1.3(10) . . . . ?
C70 N20 C74 C73 3.5(15) . . . . ?
C70 C71 C72 C73 1.6(13) . . . . ?
C78 N27 N26 N25 0.2(9) . . . . ?
C78 N27 C82 C81 0.8(13) . . . . ?
C75 N25 N26 N27 -178.0(6) . . . . ?
C75 N25 C76 C77 -2.0(13) . . . . ?
C75 N25 C76 C78 177.5(7) . . . . ?
C75 C63 C62 C61 178.0(7) . . . . ?
C79 C80 C81 C82 -0.6(14) . . . . ?
C41 C42 C43 C44 2.4(14) . . . . ?
C40 N11 C44 C43 -1.1(13) . . . . ?
C27 C26 C24 N7 178.1(9) . . . . ?
C27 C26 C24 C25 -3.9(16) . . . . ?
C27 C28 C29 C30 1.4(14) . . . . ?
C81 C80 C79 C78 0.1(13) . . . . ?
C60 N17 N18 N16 -178.3(7) . . . . ?
C60 N17 C56 C54 179.9(7) . . . . ?
C60 N17 C56 C57 -0.8(12) . . . . ?
C62 C63 C75 N25 -117.1(8) . . . . ?
C62 C61 C67 N19 84.9(9) . . . . ?
C89 C88 C87 C86 -0.9(12) . . . . ?
C44 N11 C40 C38 -178.8(8) . . . . ?
C44 N11 C40 C41 4.1(12) . . . . ?
C87 C86 C84 N22 178.6(9) . . . . ?
C87 C86 C84 C85 -4.2(16) . . . . ?
C87 C88 C89 C90 2.1(13) . . . . ?
C57 C56 C54 N16 178.6(10) . . . . ?
C57 C56 C54 C55 -1.0(17) . . . . ?
C57 C58 C59 C60 0.2(14) . . . . ?
C43 C42 C41 C40 0.6(13) . . . . ?
C59 C58 C57 C56 -0.1(13) . . . . ?
C67 N19 C68 C69 -3.1(14) . . . . ?
C67 N19 C68 C70 179.8(8) . . . . ?
C67 N19 N21 N20 179.6(7) . . . . ?
C45 N13 N15 N14 176.2(6) . . . . ?
C45 N13 C46 C48 -176.0(7) . . . . ?
C45 N13 C46 C47 5.6(13) . . . . ?
C71 C72 C73 C74 -2.0(16) . . . . ?
C72 C73 C74 N20 -0.5(15) . . . . ?
C74 N20 N21 N19 -176.0(8) . . . . ?
C74 N20 C70 C68 176.4(8) . . . . ?
C74 N20 C70 C71 -3.8(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.622
_oxdiff_exptl_absorpt_empirical_full_min 0.756
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.979(12)
2 0.021(12)

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1939484'
loop_
_audit_author_name
_audit_author_address
'Javier Pitarch'
;University of Valencia
Spain
;
_audit_update_record             
;
2019-07-09 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;
_audit_creation_date             2019-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '6(Br), 2(C39 H30 N9), 3(H2 O)'
_chemical_formula_sum            'C78 H66 Br6 N18 O3'
_chemical_formula_weight         1782.94
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'raf qui I 1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   12.3635(9)
_cell_length_b                   23.3233(15)
_cell_length_c                   13.8839(12)
_cell_angle_alpha                90
_cell_angle_beta                 113.410(10)
_cell_angle_gamma                90
_cell_volume                     3674.0(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3300
_cell_measurement_temperature    119.9(3)
_cell_measurement_theta_max      24.4530
_cell_measurement_theta_min      3.6910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17947
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.315
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0133
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  90.00   1.00   45.00    --   20.73  57.00  30.00   90
  2  ω     -6.00  63.00   1.00   45.00    --   20.73  77.00  60.00   69
  3  ω    -48.00  42.00   1.00   45.00    --   20.73 -57.00-120.00   90
  4  ω    -82.00 -38.00   1.00   45.00    --  -19.95 178.00 -30.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0063757000
_diffrn_orient_matrix_UB_12      0.0300787000
_diffrn_orient_matrix_UB_13      -0.0026527000
_diffrn_orient_matrix_UB_21      0.0046157000
_diffrn_orient_matrix_UB_22      0.0027320000
_diffrn_orient_matrix_UB_23      0.0524270000
_diffrn_orient_matrix_UB_31      0.0620286000
_diffrn_orient_matrix_UB_32      -0.0032664000
_diffrn_orient_matrix_UB_33      0.0186761000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4654
_reflns_number_total             6452
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         0.896
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6452
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0588
_refine_ls_restrained_S_all      1.104
_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)+(0.0355P)²+7.9776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1261
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Br2_$1-H2a
 3.5 with sigma of 0.01
 Br2_$1-H3b
 3.2 with sigma of 0.01
 Br3-H3a
 3.2 with sigma of 0.01
 H2a-H8_$1
 2.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: O2(0.75) H2a(0.75) H2b(0.75) O1(0.5) H1a(0.5) H1b(0.5) O3(0.25)
 H3a(0.25) H3b(0.25)
5.a Free rotating group:
 O2(H2a,H2b), O1(H1a,H1b), O3(H3a,H3b)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C18(H18a,H18b), C29(H29a,H29b)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C24(H24), C8(H8), C26(H26), C19(H19), C22(H22),
 C27(H27), C15(H15), C14(H14), C21(H21), C30(H30), C10(H10), C16(H16), C25(H25),
  C32(H32), C11(H11), C13(H13), C35(H35), C38(H38), C36(H36), C37(H37), C33(H33)
;
_atom_sites_solution_hydrogens   mixed
_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
Br2 Br 0.60555(5) 0.37254(3) 0.64249(5) 0.03475(18) Uani 1 1 d D . . . .
Br3 Br 0.71539(5) 0.48073(3) 0.23152(5) 0.03603(19) Uani 1 1 d D . . . .
Br1 Br 0.39162(5) 0.13035(3) 0.75183(5) 0.03618(19) Uani 1 1 d . . . . .
N1 N 0.3099(4) 0.2784(2) 0.5092(3) 0.0212(11) Uani 1 1 d . . . . .
N6 N 0.8890(4) 0.31948(18) 0.5045(3) 0.0185(10) Uani 1 1 d . . . . .
O2 O 0.7091(4) 0.5339(2) 0.4496(4) 0.0195(11) Uani 0.75 1 d . . P A 1
H2A H 0.6420 0.5380 0.4521 0.029 Uiso 0.75 1 d DG . P A 1
H2B H 0.7000 0.5255 0.3872 0.029 Uiso 0.75 1 d G . P A 1
N5 N 0.8224(4) 0.27472(19) 0.4555(3) 0.0212(11) Uani 1 1 d . . . . .
N2 N 0.2180(4) 0.2466(2) 0.4506(3) 0.0232(11) Uani 1 1 d . . . . .
N3 N 0.1373(4) 0.2870(2) 0.4013(3) 0.0229(11) Uani 1 1 d . . . . .
N4 N 0.7202(4) 0.29961(19) 0.3977(3) 0.0194(10) Uani 1 1 d . . . . .
N7 N 0.6378(4) 0.0499(2) 0.4170(4) 0.0254(12) Uani 1 1 d . . . . .
N9 N 0.8026(4) 0.05049(19) 0.4087(4) 0.0251(12) Uani 1 1 d . . . . .
N8 N 0.7476(4) 0.0690(2) 0.4684(4) 0.0282(12) Uani 1 1 d . . . . .
C7 C 0.4176(4) 0.2481(2) 0.5770(4) 0.0223(13) Uani 1 1 d . . . . .
H7A H 0.3979 0.2197 0.6185 0.027 Uiso 1 1 calc R . . . .
H7B H 0.4722 0.2752 0.6248 0.027 Uiso 1 1 calc R . . . .
C3 C 0.5718(4) 0.2271(2) 0.3930(4) 0.0186(12) Uani 1 1 d . . . . .
C2 C 0.5184(4) 0.2529(2) 0.4534(4) 0.0192(13) Uani 1 1 d . . . . .
H2 H 0.5113 0.2926 0.4538 0.023 Uiso 1 1 calc R . . . .
C18 C 0.6212(4) 0.2628(2) 0.3296(4) 0.0220(13) Uani 1 1 d . . . . .
H18A H 0.6487 0.2377 0.2884 0.026 Uiso 1 1 calc R . . . .
H18B H 0.5592 0.2869 0.2814 0.026 Uiso 1 1 calc R . . . .
C23 C 1.0641(4) 0.3645(2) 0.6224(4) 0.0217(13) Uani 1 1 d . . . . .
C4 C 0.5803(4) 0.1676(2) 0.3918(4) 0.0224(13) Uani 1 1 d . . . . .
H4 H 0.6140 0.1503 0.3500 0.027 Uiso 1 1 calc R . . . .
C28 C 1.0069(4) 0.3136(2) 0.5771(4) 0.0207(13) Uani 1 1 d . . . . .
C6 C 0.4872(4) 0.1605(2) 0.5138(4) 0.0206(13) Uani 1 1 d . . . . .
H6 H 0.4603 0.1384 0.5555 0.025 Uiso 1 1 calc R . . . .
C5 C 0.5388(4) 0.1336(2) 0.4526(4) 0.0228(13) Uani 1 1 d . . . . .
C24 C 1.1815(5) 0.3598(3) 0.6974(4) 0.0274(14) Uani 1 1 d . . . . .
H24 H 1.2227 0.3925 0.7299 0.033 Uiso 1 1 calc R . . . .
C8 C 0.2932(5) 0.3349(2) 0.4999(4) 0.0261(14) Uani 1 1 d . . . . .
H8 H 0.3470 0.3635 0.5343 0.031 Uiso 1 1 calc DR . . . .
C9 C 0.1773(5) 0.3416(2) 0.4275(4) 0.0239(13) Uani 1 1 d . . . . .
C26 C 1.1758(5) 0.2573(3) 0.6757(4) 0.0263(14) Uani 1 1 d . . . . .
H26 H 1.2137 0.2221 0.6942 0.032 Uiso 1 1 calc R . . . .
C19 C 0.7194(5) 0.3561(2) 0.4072(4) 0.0253(14) Uani 1 1 d . . . . .
H19 H 0.6567 0.3808 0.3731 0.030 Uiso 1 1 calc R . . . .
C1 C 0.4755(4) 0.2190(2) 0.5133(4) 0.0209(13) Uani 1 1 d . . . . .
C22 C 1.0051(5) 0.4184(3) 0.5928(4) 0.0279(14) Uani 1 1 d . . . . .
H22 H 1.0461 0.4518 0.6217 0.034 Uiso 1 1 calc R . . . .
C17 C 0.0226(5) 0.2730(3) 0.3305(4) 0.0252(14) Uani 1 1 d . . . . .
C27 C 1.0605(5) 0.2596(3) 0.6016(4) 0.0246(13) Uani 1 1 d . . . . .
H27 H 1.0203 0.2265 0.5694 0.030 Uiso 1 1 calc R . . . .
C20 C 0.8312(5) 0.3708(2) 0.4784(4) 0.0228(13) Uani 1 1 d . . . . .
C15 C -0.1266(5) 0.2061(3) 0.2377(4) 0.0311(15) Uani 1 1 d . . . . .
H15 H -0.1539 0.1686 0.2223 0.037 Uiso 1 1 calc R . . . .
C12 C -0.0514(5) 0.3201(3) 0.2836(4) 0.0282(14) Uani 1 1 d . . . . .
C14 C -0.2006(5) 0.2520(3) 0.1871(5) 0.0333(16) Uani 1 1 d . . . . .
H14 H -0.2757 0.2443 0.1371 0.040 Uiso 1 1 calc R . . . .
C21 C 0.8916(5) 0.4223(2) 0.5243(5) 0.0290(15) Uani 1 1 d . . . . .
H21 H 0.8539 0.4576 0.5076 0.035 Uiso 1 1 calc R . . . .
C30 C 0.6233(5) 0.0198(2) 0.3309(5) 0.0282(14) Uani 1 1 d . . . . .
H30 H 0.5542 0.0026 0.2850 0.034 Uiso 1 1 calc R . . . .
C10 C 0.1005(5) 0.3884(3) 0.3833(5) 0.0330(16) Uani 1 1 d . . . . .
H10 H 0.1257 0.4259 0.4026 0.040 Uiso 1 1 calc R . . . .
C16 C -0.0141(5) 0.2161(3) 0.3100(4) 0.0289(15) Uani 1 1 d . . . . .
H16 H 0.0358 0.1861 0.3440 0.035 Uiso 1 1 calc R . . . .
C39 C 0.9225(5) 0.0628(3) 0.4328(5) 0.0290(15) Uani 1 1 d . . . . .
C25 C 1.2350(5) 0.3070(3) 0.7226(4) 0.0289(15) Uani 1 1 d . . . . .
H25 H 1.3122 0.3045 0.7719 0.035 Uiso 1 1 calc R . . . .
C31 C 0.7313(5) 0.0196(2) 0.3239(5) 0.0290(14) Uani 1 1 d . . . . .
C29 C 0.5496(5) 0.0689(2) 0.4564(5) 0.0302(15) Uani 1 1 d . . . . .
H29A H 0.5723 0.0558 0.5282 0.036 Uiso 1 1 calc R . . . .
H29B H 0.4738 0.0519 0.4142 0.036 Uiso 1 1 calc R . . . .
C32 C 0.7776(6) -0.0011(3) 0.2527(5) 0.0344(16) Uani 1 1 d . . . . .
H32 H 0.7304 -0.0216 0.1934 0.041 Uiso 1 1 calc R . . . .
C11 C -0.0106(5) 0.3777(3) 0.3124(5) 0.0331(16) Uani 1 1 d . . . . .
H11 H -0.0611 0.4082 0.2819 0.040 Uiso 1 1 calc R . . . .
C34 C 0.9663(5) 0.0412(2) 0.3619(5) 0.0305(15) Uani 1 1 d . . . . .
C13 C -0.1662(5) 0.3074(3) 0.2086(5) 0.0365(17) Uani 1 1 d . . . . .
H13 H -0.2177 0.3369 0.1743 0.044 Uiso 1 1 calc R . . . .
C35 C 1.0877(5) 0.0519(3) 0.3858(5) 0.0373(17) Uani 1 1 d . . . . .
H35 H 1.1217 0.0384 0.3412 0.045 Uiso 1 1 calc R . . . .
C38 C 0.9898(5) 0.0930(3) 0.5219(5) 0.0317(15) Uani 1 1 d . . . . .
H38 H 0.9571 0.1064 0.5674 0.038 Uiso 1 1 calc R . . . .
C36 C 1.1545(6) 0.0820(3) 0.4741(5) 0.0410(18) Uani 1 1 d . . . . .
H36 H 1.2337 0.0885 0.4889 0.049 Uiso 1 1 calc R . . . .
C37 C 1.1067(6) 0.1030(3) 0.5419(5) 0.0406(18) Uani 1 1 d . . . . .
H37 H 1.1533 0.1238 0.6010 0.049 Uiso 1 1 calc R . . . .
C33 C 0.8917(6) 0.0094(3) 0.2724(5) 0.0360(16) Uani 1 1 d . . . . .
H33 H 0.9229 -0.0046 0.2261 0.043 Uiso 1 1 calc R . . . .
O1 O 0.5148(9) 0.4606(4) 0.4307(8) 0.051(3) Uani 0.5 1 d . . P B 3
H1A H 0.5678 0.4496 0.4886 0.076 Uiso 0.5 1 d G . P B 3
H1B H 0.4954 0.4328 0.3875 0.076 Uiso 0.5 1 d G . P B 3
O3 O 0.6201(14) 0.5070(7) 0.4652(13) 0.035(4) Uani 0.25 1 d . U P C 2
H3A H 0.6068 0.4933 0.4048 0.053 Uiso 0.25 1 d DG . P C 2
H3B H 0.5560 0.5193 0.4666 0.053 Uiso 0.25 1 d DG . P C 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
N1 N2 1.330(6) . ?
N1 C7 1.471(6) . ?
N1 C8 1.331(7) . ?
N6 N5 1.336(6) . ?
N6 C28 1.412(6) . ?
N6 C20 1.367(7) . ?
O2 H2A 0.8500 . ?
O2 H2B 0.8503 . ?
N5 N4 1.331(6) . ?
N2 N3 1.346(6) . ?
N3 C9 1.361(7) . ?
N3 C17 1.406(7) . ?
N4 C18 1.486(6) . ?
N4 C19 1.324(7) . ?
N7 N8 1.334(6) . ?
N7 C30 1.334(7) . ?
N7 C29 1.470(7) . ?
N9 N8 1.335(7) . ?
N9 C39 1.413(7) . ?
N9 C31 1.363(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C1 1.504(8) . ?
C3 C2 1.392(7) . ?
C3 C18 1.506(8) . ?
C3 C4 1.393(7) . ?
C2 H2 0.9300 . ?
C2 C1 1.396(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C23 C28 1.397(8) . ?
C23 C24 1.415(7) . ?
C23 C22 1.429(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.395(8) . ?
C28 C27 1.402(8) . ?
C6 H6 0.9300 . ?
C6 C5 1.398(8) . ?
C6 C1 1.372(7) . ?
C5 C29 1.514(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.376(8) . ?
C8 H8 0.9300 . ?
C8 C9 1.394(7) . ?
C9 C10 1.417(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.389(7) . ?
C26 C25 1.386(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.386(7) . ?
C22 H22 0.9300 . ?
C22 C21 1.349(7) . ?
C17 C12 1.414(8) . ?
C17 C16 1.393(8) . ?
C27 H27 0.9300 . ?
C20 C21 1.424(8) . ?
C15 H15 0.9300 . ?
C15 C14 1.403(8) . ?
C15 C16 1.374(7) . ?
C12 C11 1.435(8) . ?
C12 C13 1.419(8) . ?
C14 H14 0.9300 . ?
C14 C13 1.354(9) . ?
C21 H21 0.9300 . ?
C30 H30 0.9300 . ?
C30 C31 1.376(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.358(8) . ?
C16 H16 0.9300 . ?
C39 C34 1.392(9) . ?
C39 C38 1.379(8) . ?
C25 H25 0.9300 . ?
C31 C32 1.411(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C32 H32 0.9300 . ?
C32 C33 1.349(8) . ?
C11 H11 0.9300 . ?
C34 C35 1.425(8) . ?
C34 C33 1.426(8) . ?
C13 H13 0.9300 . ?
C35 H35 0.9300 . ?
C35 C36 1.369(9) . ?
C38 H38 0.9300 . ?
C38 C37 1.378(8) . ?
C36 H36 0.9300 . ?
C36 C37 1.385(9) . ?
C37 H37 0.9300 . ?
C33 H33 0.9300 . ?
O1 H1A 0.8501 . ?
O1 H1B 0.8499 . ?
O3 H3A 0.8498 . ?
O3 H3B 0.8502 . ?

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
N2 N1 C7 117.3(4) . . ?
N2 N1 C8 115.5(4) . . ?
C8 N1 C7 127.1(5) . . ?
N5 N6 C28 122.7(4) . . ?
N5 N6 C20 113.5(4) . . ?
C20 N6 C28 123.8(4) . . ?
H2A O2 H2B 109.4 . . ?
N4 N5 N6 102.2(4) . . ?
N1 N2 N3 101.6(4) . . ?
N2 N3 C9 113.7(4) . . ?
N2 N3 C17 122.0(5) . . ?
C9 N3 C17 124.3(5) . . ?
N5 N4 C18 118.5(4) . . ?
C19 N4 N5 114.6(4) . . ?
C19 N4 C18 126.9(4) . . ?
N8 N7 C30 113.7(5) . . ?
N8 N7 C29 116.6(5) . . ?
C30 N7 C29 129.5(5) . . ?
N8 N9 C39 122.2(5) . . ?
N8 N9 C31 113.1(5) . . ?
C31 N9 C39 124.7(5) . . ?
N7 N8 N9 102.7(4) . . ?
N1 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
N1 C7 C1 111.2(4) . . ?
H7A C7 H7B 108.0 . . ?
C1 C7 H7A 109.4 . . ?
C1 C7 H7B 109.4 . . ?
C2 C3 C18 120.8(5) . . ?
C2 C3 C4 119.6(5) . . ?
C4 C3 C18 119.6(5) . . ?
C3 C2 H2 120.1 . . ?
C3 C2 C1 119.8(5) . . ?
C1 C2 H2 120.1 . . ?
N4 C18 C3 111.7(4) . . ?
N4 C18 H18A 109.3 . . ?
N4 C18 H18B 109.3 . . ?
C3 C18 H18A 109.3 . . ?
C3 C18 H18B 109.3 . . ?
H18A C18 H18B 107.9 . . ?
C28 C23 C24 116.9(5) . . ?
C28 C23 C22 120.6(5) . . ?
C24 C23 C22 122.5(5) . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.8(5) . . ?
C5 C4 H4 119.6 . . ?
C23 C28 N6 115.7(5) . . ?
C23 C28 C27 123.4(5) . . ?
C27 C28 N6 120.9(5) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C1 C6 C5 121.1(5) . . ?
C4 C5 C6 118.6(5) . . ?
C4 C5 C29 122.7(5) . . ?
C6 C5 C29 118.8(5) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.4(5) . . ?
C25 C24 H24 119.8 . . ?
N1 C8 H8 127.6 . . ?
N1 C8 C9 104.9(5) . . ?
C9 C8 H8 127.6 . . ?
N3 C9 C8 104.3(5) . . ?
N3 C9 C10 119.7(5) . . ?
C8 C9 C10 136.0(6) . . ?
C27 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.7(5) . . ?
N4 C19 H19 127.1 . . ?
N4 C19 C20 105.8(5) . . ?
C20 C19 H19 127.1 . . ?
C2 C1 C7 118.5(5) . . ?
C6 C1 C7 121.3(5) . . ?
C6 C1 C2 120.2(5) . . ?
C23 C22 H22 119.0 . . ?
C21 C22 C23 122.1(5) . . ?
C21 C22 H22 119.0 . . ?
N3 C17 C12 115.4(5) . . ?
C16 C17 N3 121.4(5) . . ?
C16 C17 C12 123.1(5) . . ?
C28 C27 H27 121.3 . . ?
C26 C27 C28 117.4(5) . . ?
C26 C27 H27 121.3 . . ?
N6 C20 C19 103.9(5) . . ?
N6 C20 C21 119.6(5) . . ?
C19 C20 C21 136.5(5) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C16 C15 C14 120.3(6) . . ?
C17 C12 C11 120.6(5) . . ?
C17 C12 C13 116.8(6) . . ?
C13 C12 C11 122.6(5) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 C15 122.2(5) . . ?
C13 C14 H14 118.9 . . ?
C22 C21 C20 118.2(5) . . ?
C22 C21 H21 120.9 . . ?
C20 C21 H21 120.9 . . ?
N7 C30 H30 127.0 . . ?
N7 C30 C31 106.0(5) . . ?
C31 C30 H30 127.0 . . ?
C9 C10 H10 120.5 . . ?
C11 C10 C9 118.9(6) . . ?
C11 C10 H10 120.5 . . ?
C17 C16 H16 121.1 . . ?
C15 C16 C17 117.7(6) . . ?
C15 C16 H16 121.1 . . ?
C34 C39 N9 115.2(5) . . ?
C38 C39 N9 121.3(6) . . ?
C38 C39 C34 123.6(6) . . ?
C24 C25 C26 121.2(5) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
N9 C31 C30 104.5(5) . . ?
N9 C31 C32 118.9(6) . . ?
C30 C31 C32 136.6(6) . . ?
N7 C29 C5 110.8(5) . . ?
N7 C29 H29A 109.5 . . ?
N7 C29 H29B 109.5 . . ?
C5 C29 H29A 109.5 . . ?
C5 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
C31 C32 H32 120.7 . . ?
C33 C32 C31 118.6(6) . . ?
C33 C32 H32 120.7 . . ?
C12 C11 H11 119.5 . . ?
C10 C11 C12 121.1(5) . . ?
C10 C11 H11 119.5 . . ?
C39 C34 C35 116.2(6) . . ?
C39 C34 C33 120.4(6) . . ?
C35 C34 C33 123.4(6) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.7(6) . . ?
C14 C13 H13 120.1 . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.2(7) . . ?
C36 C35 H35 119.9 . . ?
C39 C38 H38 120.7 . . ?
C37 C38 C39 118.6(6) . . ?
C37 C38 H38 120.7 . . ?
C35 C36 H36 119.3 . . ?
C35 C36 C37 121.4(6) . . ?
C37 C36 H36 119.3 . . ?
C38 C37 C36 119.9(6) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C33 C34 122.2(6) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 H33 118.9 . . ?
H1A O1 H1B 109.5 . . ?
H3A O3 H3B 109.5 . . ?


_olex2_date_sample_data_collection 2017-07-10
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.869
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: water, methanol'
_exptl_crystal_preparation       Luminescent
