# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_klb-1
_database_code_depnum_ccdc_archive 'CCDC 1977878'
loop_
_audit_author_name
_audit_author_address
'Lingbing Kong'
;Shandong University
China
;
_audit_update_record             
;
2020-05-25 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_audit_creation_date             2020-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C18 H14 B Br N)'
_chemical_formula_sum            'C36 H28 B2 Br2 N2'
_chemical_formula_weight         670.04
_chemical_melting_point          ?
_chemical_oxdiff_formula         BrNBC
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   18.5040(3)
_cell_length_b                   17.9348(3)
_cell_length_c                   19.6933(7)
_cell_angle_alpha                90
_cell_angle_beta                 108.694(2)
_cell_angle_gamma                90
_cell_volume                     6190.7(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9371
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.0510
_cell_measurement_theta_min      3.4760
_shelx_estimated_absorpt_T_max   0.719
_shelx_estimated_absorpt_T_min   0.418
_exptl_absorpt_coefficient_mu    3.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14639
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.582
_diffrn_reflns_theta_max         66.582
_diffrn_reflns_theta_min         3.418
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00 -53.00   1.00    0.35    --  -48.45 113.00  99.00   33
  2  ω     23.00  86.00   1.00    0.35    --   48.45-113.00   7.00   63
  3  ω    -74.00 -49.00   1.00    1.40    --  -86.25 113.00  99.00   25
  4  ω   -132.00-102.00   1.00    1.40    --  -86.25-113.00   7.00   30
  5  ω     99.00 138.00   1.00    1.40    --  106.49 113.00  99.00   39
  6  ω     45.00 112.00   1.00    1.40    --  106.49-113.00   7.00   67
  7  ω   -108.00 -75.00   1.00    0.35    --  -48.45-125.00  30.00   33
  8  ω   -120.00 -72.00   1.00    0.35    --  -48.45-125.00 120.00   48
  9  ω    -61.00  27.00   1.00    0.35    --  -48.45  19.00-150.00   88
 10  ω     34.00 109.00   1.00    1.40    --  106.49 -99.00-150.00   75
 11  ω     36.00 120.00   1.00    1.40    --  106.49 -38.00-180.00   84
 12  ω     35.00 117.00   1.00    1.40    --  106.49-125.00-150.00   82
 13  ω     31.00 119.00   1.00    1.40    --  106.49 -19.00-180.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0681869000
_diffrn_orient_matrix_UB_12      -0.0498284000
_diffrn_orient_matrix_UB_13      0.0008381000
_diffrn_orient_matrix_UB_21      -0.0533168000
_diffrn_orient_matrix_UB_22      -0.0681836000
_diffrn_orient_matrix_UB_23      -0.0191374000
_diffrn_orient_matrix_UB_31      -0.0155835000
_diffrn_orient_matrix_UB_32      0.0157703000
_diffrn_orient_matrix_UB_33      -0.0802746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4624
_reflns_number_total             5361
_reflns_odcompleteness_completeness 97.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5361
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0730
_refine_ls_restrained_S_all      1.206
_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)+(0.1700P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2095
_refine_ls_wR_factor_ref         0.2527
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N1-H1
 0.9 with sigma of 0.02
 N2-H2
 0.9 with sigma of 0.02
3. Rigid bond restraints
 C31, C32, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C21(H21), C22(H22), C23(H23),
  C30(H30), C29(H29), C28(H28), C27(H27), C26(H26), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36)
;
_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
Br1 Br -0.09773(3) 0.27855(3) 0.16089(3) 0.0637(3) Uani 1 1 d . . . . .
N1 N -0.2154(2) 0.2611(2) 0.0277(2) 0.0475(8) Uani 1 1 d D . . . .
H1 H -0.189(3) 0.226(3) 0.014(3) 0.057 Uiso 1 1 d DR . . . .
C1 C -0.2430(3) 0.3548(3) 0.1239(3) 0.0480(10) Uani 1 1 d . . . . .
C2 C -0.2222(3) 0.4300(3) 0.1396(3) 0.0520(11) Uani 1 1 d . . . . .
C3 C -0.2661(3) 0.4796(3) 0.1623(3) 0.0565(12) Uani 1 1 d . . . . .
H3 H -0.2508 0.5289 0.1723 0.068 Uiso 1 1 calc R . . . .
C4 C -0.3302(3) 0.4557(3) 0.1696(3) 0.0627(14) Uani 1 1 d . . . . .
H4 H -0.3614 0.4886 0.1840 0.075 Uiso 1 1 calc R . . . .
C5 C -0.3512(3) 0.3827(3) 0.1562(3) 0.0560(12) Uani 1 1 d . . . . .
H5 H -0.3963 0.3668 0.1629 0.067 Uiso 1 1 calc R . . . .
C6 C -0.3081(3) 0.3312(3) 0.1329(3) 0.0525(11) Uani 1 1 d . . . . .
C7 C -0.3333(3) 0.2533(3) 0.1182(3) 0.0496(10) Uani 1 1 d . . . . .
C8 C -0.4021(3) 0.2379(3) 0.0661(3) 0.0565(12) Uani 1 1 d . . . . .
H8 H -0.4326 0.2769 0.0417 0.068 Uiso 1 1 calc R . . . .
C9 C -0.4258(3) 0.1659(3) 0.0503(3) 0.0643(14) Uani 1 1 d . . . . .
H9 H -0.4715 0.1564 0.0142 0.077 Uiso 1 1 calc R . . . .
C10 C -0.3828(4) 0.1075(3) 0.0869(4) 0.0675(15) Uani 1 1 d . . . . .
H10 H -0.3993 0.0587 0.0755 0.081 Uiso 1 1 calc R . . . .
C11 C -0.3165(4) 0.1211(3) 0.1397(4) 0.0675(15) Uani 1 1 d . . . . .
H11 H -0.2877 0.0819 0.1655 0.081 Uiso 1 1 calc R . . . .
C12 C -0.2920(3) 0.1930(3) 0.1549(3) 0.0543(11) Uani 1 1 d . . . . .
H12 H -0.2462 0.2018 0.1910 0.065 Uiso 1 1 calc R . . . .
C13 C -0.1552(3) 0.4590(3) 0.1293(3) 0.0522(11) Uani 1 1 d . . . . .
C18 C -0.1001(3) 0.4884(3) 0.1901(3) 0.0605(13) Uani 1 1 d . . . . .
H18 H -0.1065 0.4884 0.2351 0.073 Uiso 1 1 calc R . . . .
C17 C -0.0390(3) 0.5160(4) 0.1795(4) 0.0699(15) Uani 1 1 d . . . . .
H17 H -0.0002 0.5356 0.2181 0.084 Uiso 1 1 calc R . . . .
C16 C -0.0306(4) 0.5167(4) 0.1087(4) 0.0734(16) Uani 1 1 d . . . . .
H16 H 0.0138 0.5368 0.1039 0.088 Uiso 1 1 calc R . . . .
C15 C -0.0860(3) 0.4885(4) 0.0466(4) 0.0711(16) Uani 1 1 d . . . . .
H15 H -0.0801 0.4909 0.0015 0.085 Uiso 1 1 calc R . . . .
C14 C -0.1461(3) 0.4588(3) 0.0569(3) 0.0629(13) Uani 1 1 d . . . . .
H14 H -0.1837 0.4372 0.0185 0.076 Uiso 1 1 calc R . . . .
B1 B -0.1956(3) 0.2991(3) 0.0956(3) 0.0482(11) Uani 1 1 d . . . . .
Br2 Br 0.34067(3) 0.39555(3) 0.36657(3) 0.0598(3) Uani 1 1 d . . . . .
N2 N 0.2744(2) 0.4159(2) 0.4795(2) 0.0494(9) Uani 1 1 d D . . . .
H2 H 0.314(3) 0.444(3) 0.506(3) 0.059 Uiso 1 1 d DR . . . .
C19 C 0.2023(3) 0.3216(3) 0.3744(2) 0.0483(10) Uani 1 1 d . . . . .
C20 C 0.1310(3) 0.3471(3) 0.3528(3) 0.0523(11) Uani 1 1 d . . . . .
C21 C 0.0751(3) 0.2960(3) 0.3199(3) 0.0610(13) Uani 1 1 d . . . . .
H21 H 0.0247 0.3121 0.3047 0.073 Uiso 1 1 calc R . . . .
C22 C 0.0894(3) 0.2227(3) 0.3083(4) 0.0655(14) Uani 1 1 d . . . . .
H22 H 0.0492 0.1908 0.2859 0.079 Uiso 1 1 calc R . . . .
C23 C 0.1595(3) 0.1978(3) 0.3290(3) 0.0634(13) Uani 1 1 d . . . . .
H23 H 0.1702 0.1486 0.3209 0.076 Uiso 1 1 calc R . . . .
C24 C 0.2164(3) 0.2458(3) 0.3625(3) 0.0524(11) Uani 1 1 d . . . . .
C25 C 0.2903(3) 0.2163(3) 0.3862(3) 0.0521(11) Uani 1 1 d . . . . .
C30 C 0.3172(3) 0.1814(3) 0.3329(3) 0.0558(12) Uani 1 1 d . . . . .
H30 H 0.2864 0.1780 0.2854 0.067 Uiso 1 1 calc R . . . .
C29 C 0.3862(4) 0.1548(3) 0.3539(3) 0.0630(13) Uani 1 1 d . . . . .
H29 H 0.4065 0.1325 0.3214 0.076 Uiso 1 1 calc R . . . .
C28 C 0.4305(4) 0.1608(4) 0.4288(4) 0.0676(14) Uani 1 1 d . . . . .
H28 H 0.4797 0.1414 0.4429 0.081 Uiso 1 1 calc R . . . .
C27 C 0.4053(4) 0.1939(4) 0.4829(4) 0.0706(15) Uani 1 1 d . . . . .
H27 H 0.4359 0.1958 0.5307 0.085 Uiso 1 1 calc R . . . .
C26 C 0.3360(3) 0.2217(3) 0.4612(3) 0.0604(13) Uani 1 1 d . . . . .
H26 H 0.3163 0.2447 0.4937 0.072 Uiso 1 1 calc R . . . .
C31 C 0.1116(3) 0.4254(3) 0.3614(2) 0.0500(8) Uani 1 1 d . U . . .
C32 C 0.1481(3) 0.4853(3) 0.3421(3) 0.0533(9) Uani 1 1 d . U . . .
H32 H 0.1865 0.4759 0.3223 0.064 Uiso 1 1 calc R . . . .
C33 C 0.1299(3) 0.5578(3) 0.3511(3) 0.0575(10) Uani 1 1 d . U . . .
H33 H 0.1562 0.5965 0.3381 0.069 Uiso 1 1 calc R . . . .
C34 C 0.0740(3) 0.5731(3) 0.3786(3) 0.0634(11) Uani 1 1 d . U . . .
H34 H 0.0616 0.6221 0.3853 0.076 Uiso 1 1 calc R . . . .
C35 C 0.0357(3) 0.5152(3) 0.3965(3) 0.0645(12) Uani 1 1 d . U . . .
H35 H -0.0040 0.5250 0.4145 0.077 Uiso 1 1 calc R . . . .
C36 C 0.0554(3) 0.4421(3) 0.3880(3) 0.0614(11) Uani 1 1 d . U . . .
H36 H 0.0289 0.4036 0.4011 0.074 Uiso 1 1 calc R . . . .
B2 B 0.2661(3) 0.3755(3) 0.4137(3) 0.0493(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 B1 1.892(6) . ?
N1 N1 1.391(8) 2_455 ?
N1 H1 0.89(2) . ?
N1 B1 1.440(7) . ?
C1 C2 1.409(7) . ?
C1 C6 1.341(7) . ?
C1 B1 1.547(7) . ?
C2 C3 1.374(7) . ?
C2 C13 1.417(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.311(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.368(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.390(7) . ?
C6 C7 1.472(7) . ?
C7 C8 1.383(8) . ?
C7 C12 1.385(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.368(8) . ?
C9 H9 0.9300 . ?
C9 C10 1.371(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.353(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.367(9) . ?
C12 H12 0.9300 . ?
C13 C18 1.405(8) . ?
C13 C14 1.489(8) . ?
C18 H18 0.9300 . ?
C18 C17 1.311(9) . ?
C17 H17 0.9300 . ?
C17 C16 1.452(10) . ?
C16 H16 0.9300 . ?
C16 C15 1.414(10) . ?
C15 H15 0.9300 . ?
C15 C14 1.306(8) . ?
C14 H14 0.9300 . ?
Br2 B2 1.928(6) . ?
N2 N2 1.393(8) 2_556 ?
N2 H2 0.90(2) . ?
N2 B2 1.448(7) . ?
C19 C20 1.329(7) . ?
C19 C24 1.417(7) . ?
C19 B2 1.531(7) . ?
C20 C21 1.379(8) . ?
C20 C31 1.473(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.374(9) . ?
C22 H22 0.9300 . ?
C22 C23 1.308(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.355(8) . ?
C24 C25 1.401(8) . ?
C25 C30 1.439(7) . ?
C25 C26 1.451(8) . ?
C30 H30 0.9300 . ?
C30 C29 1.299(9) . ?
C29 H29 0.9300 . ?
C29 C28 1.444(10) . ?
C28 H28 0.9300 . ?
C28 C27 1.424(9) . ?
C27 H27 0.9300 . ?
C27 C26 1.311(9) . ?
C26 H26 0.9300 . ?
C31 C32 1.386(7) . ?
C31 C36 1.339(8) . ?
C32 H32 0.9300 . ?
C32 C33 1.368(8) . ?
C33 H33 0.9300 . ?
C33 C34 1.339(9) . ?
C34 H34 0.9300 . ?
C34 C35 1.365(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.385(9) . ?
C36 H36 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
N1 N1 H1 103(4) 2_455 . ?
N1 N1 B1 128.6(4) 2_455 . ?
B1 N1 H1 128(4) . . ?
C2 C1 B1 123.3(4) . . ?
C6 C1 C2 117.9(4) . . ?
C6 C1 B1 118.8(5) . . ?
C1 C2 C13 120.7(4) . . ?
C3 C2 C1 122.8(5) . . ?
C3 C2 C13 116.4(5) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.4(5) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 118.6 . . ?
C4 C5 C6 122.8(5) . . ?
C6 C5 H5 118.6 . . ?
C1 C6 C5 117.9(5) . . ?
C1 C6 C7 121.0(4) . . ?
C5 C6 C7 121.1(5) . . ?
C8 C7 C6 119.5(5) . . ?
C8 C7 C12 117.0(5) . . ?
C12 C7 C6 123.5(5) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.6(5) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.8(6) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.7(6) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.5(6) . . ?
C12 C11 H11 120.2 . . ?
C7 C12 H12 118.9 . . ?
C11 C12 C7 122.3(5) . . ?
C11 C12 H12 118.9 . . ?
C2 C13 C14 120.5(5) . . ?
C18 C13 C2 116.5(5) . . ?
C18 C13 C14 122.9(5) . . ?
C13 C18 H18 122.1 . . ?
C17 C18 C13 115.7(6) . . ?
C17 C18 H18 122.1 . . ?
C18 C17 H17 119.4 . . ?
C18 C17 C16 121.2(6) . . ?
C16 C17 H17 119.4 . . ?
C17 C16 H16 118.1 . . ?
C15 C16 C17 123.9(6) . . ?
C15 C16 H16 118.1 . . ?
C16 C15 H15 122.3 . . ?
C14 C15 C16 115.4(6) . . ?
C14 C15 H15 122.3 . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.7(6) . . ?
C15 C14 H14 119.6 . . ?
N1 B1 Br1 116.2(4) . . ?
N1 B1 C1 129.5(5) . . ?
C1 B1 Br1 114.3(4) . . ?
N2 N2 H2 102(4) 2_556 . ?
N2 N2 B2 128.0(4) 2_556 . ?
B2 N2 H2 129(4) . . ?
C20 C19 C24 119.5(5) . . ?
C20 C19 B2 118.0(5) . . ?
C24 C19 B2 122.4(4) . . ?
C19 C20 C21 116.1(5) . . ?
C19 C20 C31 123.0(5) . . ?
C21 C20 C31 120.9(5) . . ?
C20 C21 H21 118.0 . . ?
C22 C21 C20 124.0(6) . . ?
C22 C21 H21 118.0 . . ?
C21 C22 H22 120.1 . . ?
C23 C22 C21 119.9(5) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 120.9 . . ?
C22 C23 C24 118.2(6) . . ?
C24 C23 H23 120.9 . . ?
C23 C24 C19 122.3(5) . . ?
C23 C24 C25 116.4(5) . . ?
C25 C24 C19 121.3(4) . . ?
C24 C25 C30 116.8(5) . . ?
C24 C25 C26 120.1(5) . . ?
C30 C25 C26 123.1(5) . . ?
C25 C30 H30 121.3 . . ?
C29 C30 C25 117.5(5) . . ?
C29 C30 H30 121.3 . . ?
C30 C29 H29 120.8 . . ?
C30 C29 C28 118.5(5) . . ?
C28 C29 H29 120.8 . . ?
C29 C28 H28 117.3 . . ?
C27 C28 C29 125.4(6) . . ?
C27 C28 H28 117.3 . . ?
C28 C27 H27 122.1 . . ?
C26 C27 C28 115.8(6) . . ?
C26 C27 H27 122.1 . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.8(5) . . ?
C27 C26 H26 120.1 . . ?
C32 C31 C20 123.4(5) . . ?
C36 C31 C20 120.5(5) . . ?
C36 C31 C32 116.1(5) . . ?
C31 C32 H32 118.6 . . ?
C33 C32 C31 122.7(5) . . ?
C33 C32 H32 118.6 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 120.0(5) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 120.6 . . ?
C33 C34 C35 118.8(6) . . ?
C35 C34 H34 120.6 . . ?
C34 C35 H35 119.7 . . ?
C34 C35 C36 120.6(6) . . ?
C36 C35 H35 119.7 . . ?
C31 C36 C35 121.8(5) . . ?
C31 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
N2 B2 Br2 116.8(4) . . ?
N2 B2 C19 127.7(5) . . ?
C19 B2 Br2 115.4(4) . . ?

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 N1 B1 Br1 174.7(3) 2_455 . . . ?
N1 N1 B1 C1 -4.9(8) 2_455 . . . ?
C1 C2 C3 C4 -0.1(8) . . . . ?
C1 C2 C13 C18 -120.6(5) . . . . ?
C1 C2 C13 C14 60.5(7) . . . . ?
C1 C6 C7 C8 -119.2(6) . . . . ?
C1 C6 C7 C12 61.9(7) . . . . ?
C2 C1 C6 C5 0.8(7) . . . . ?
C2 C1 C6 C7 -179.5(5) . . . . ?
C2 C1 B1 Br1 64.9(6) . . . . ?
C2 C1 B1 N1 -115.5(6) . . . . ?
C2 C3 C4 C5 1.4(9) . . . . ?
C2 C13 C18 C17 -179.0(5) . . . . ?
C2 C13 C14 C15 176.9(6) . . . . ?
C3 C2 C13 C18 62.0(7) . . . . ?
C3 C2 C13 C14 -116.9(6) . . . . ?
C3 C4 C5 C6 -1.6(9) . . . . ?
C4 C5 C6 C1 0.4(9) . . . . ?
C4 C5 C6 C7 -179.2(5) . . . . ?
C5 C6 C7 C8 60.5(7) . . . . ?
C5 C6 C7 C12 -118.4(6) . . . . ?
C6 C1 C2 C3 -1.0(8) . . . . ?
C6 C1 C2 C13 -178.3(5) . . . . ?
C6 C1 B1 Br1 -116.4(5) . . . . ?
C6 C1 B1 N1 63.2(7) . . . . ?
C6 C7 C8 C9 178.3(5) . . . . ?
C6 C7 C12 C11 -179.5(5) . . . . ?
C7 C8 C9 C10 1.7(9) . . . . ?
C8 C7 C12 C11 1.6(7) . . . . ?
C8 C9 C10 C11 0.4(9) . . . . ?
C9 C10 C11 C12 -1.5(9) . . . . ?
C10 C11 C12 C7 0.5(9) . . . . ?
C12 C7 C8 C9 -2.7(7) . . . . ?
C13 C2 C3 C4 177.2(5) . . . . ?
C13 C18 C17 C16 1.0(9) . . . . ?
C18 C13 C14 C15 -1.9(9) . . . . ?
C18 C17 C16 C15 0.1(11) . . . . ?
C17 C16 C15 C14 -2.1(11) . . . . ?
C16 C15 C14 C13 2.8(10) . . . . ?
C14 C13 C18 C17 -0.2(8) . . . . ?
B1 C1 C2 C3 177.7(5) . . . . ?
B1 C1 C2 C13 0.4(8) . . . . ?
B1 C1 C6 C5 -177.9(5) . . . . ?
B1 C1 C6 C7 1.7(7) . . . . ?
N2 N2 B2 Br2 174.7(3) 2_556 . . . ?
N2 N2 B2 C19 -1.6(8) 2_556 . . . ?
C19 C20 C21 C22 -0.7(9) . . . . ?
C19 C20 C31 C32 48.4(7) . . . . ?
C19 C20 C31 C36 -132.5(6) . . . . ?
C19 C24 C25 C30 -124.1(5) . . . . ?
C19 C24 C25 C26 55.9(7) . . . . ?
C20 C19 C24 C23 0.6(8) . . . . ?
C20 C19 C24 C25 -178.3(5) . . . . ?
C20 C19 B2 Br2 -117.5(4) . . . . ?
C20 C19 B2 N2 58.9(7) . . . . ?
C20 C21 C22 C23 0.0(10) . . . . ?
C20 C31 C32 C33 -179.3(5) . . . . ?
C20 C31 C36 C35 -179.8(5) . . . . ?
C21 C20 C31 C32 -130.3(6) . . . . ?
C21 C20 C31 C36 48.7(7) . . . . ?
C21 C22 C23 C24 1.0(10) . . . . ?
C22 C23 C24 C19 -1.3(9) . . . . ?
C22 C23 C24 C25 177.7(5) . . . . ?
C23 C24 C25 C30 56.9(6) . . . . ?
C23 C24 C25 C26 -123.1(6) . . . . ?
C24 C19 C20 C21 0.4(7) . . . . ?
C24 C19 C20 C31 -178.4(4) . . . . ?
C24 C19 B2 Br2 64.3(6) . . . . ?
C24 C19 B2 N2 -119.3(6) . . . . ?
C24 C25 C30 C29 178.9(5) . . . . ?
C24 C25 C26 C27 -180.0(6) . . . . ?
C25 C30 C29 C28 1.1(8) . . . . ?
C30 C25 C26 C27 0.0(9) . . . . ?
C30 C29 C28 C27 -0.1(10) . . . . ?
C29 C28 C27 C26 -0.9(10) . . . . ?
C28 C27 C26 C25 0.9(9) . . . . ?
C26 C25 C30 C29 -1.1(8) . . . . ?
C31 C20 C21 C22 178.1(5) . . . . ?
C31 C32 C33 C34 -0.9(8) . . . . ?
C32 C31 C36 C35 -0.7(8) . . . . ?
C32 C33 C34 C35 -0.7(9) . . . . ?
C33 C34 C35 C36 1.5(9) . . . . ?
C34 C35 C36 C31 -0.8(10) . . . . ?
C36 C31 C32 C33 1.6(8) . . . . ?
B2 C19 C20 C21 -177.8(5) . . . . ?
B2 C19 C20 C31 3.4(7) . . . . ?
B2 C19 C24 C23 178.7(5) . . . . ?
B2 C19 C24 C25 -0.3(7) . . . . ?

_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 1.553
_oxdiff_exptl_absorpt_empirical_full_min 0.613
####################################################################### 
# 
# 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_klb-5_sq
_database_code_depnum_ccdc_archive 'CCDC 1977882'
loop_
_audit_author_name
_audit_author_address
'Lingbing Kong'
;Shandong University
China
;
_audit_update_record             
;
2020-05-25 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_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         'C36 H60 B2 Br2 N2'
_chemical_formula_sum            'C36 H60 B2 Br2 N2'
_chemical_formula_weight         702.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   32.9585(3)
_cell_length_b                   32.9585(3)
_cell_length_c                   9.9663(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9375.6(3)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    11419
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.9440
_cell_measurement_theta_min      4.6160
_shelx_estimated_absorpt_T_max   0.780
_shelx_estimated_absorpt_T_min   0.420
_exptl_absorpt_coefficient_mu    2.621
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3330
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20723
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.569
_diffrn_reflns_theta_max         66.569
_diffrn_reflns_theta_min         2.681
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_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     -8.00  21.00   1.00    5.00    --    0.00  57.00  73.00   29
  2  ω    -25.00  16.00   1.00    5.00    --    0.00  77.00 -30.00   41
  3  ω     21.00  69.00   1.00    5.00    --    0.00  77.00 -30.00   48
  4  ω     31.00  65.00   1.00    5.00    --    0.00  57.00  73.00   34
  5  ω    -64.00  -6.00   1.00    5.00    --    0.00 -57.00-120.00   58
  6  ω     32.00 124.00   1.00   20.00    --   54.47  77.00  90.00   92
  7  ω      5.00  74.00   1.00   20.00    --   54.47 -57.00 120.00   69
  8  ω     38.00 110.00   1.00   20.00    --   54.47-125.00  60.00   72
  9  ω     30.00 123.00   1.00   20.00    --   54.47  37.00  30.00   93
 10  ω     20.00  55.00   1.00   20.00    --   54.47 -57.00-180.00   35
 11  ω     68.00  99.00   1.00   20.00    --   54.47 -19.00 120.00   31
 12  ω     -2.00  24.00   1.00   20.00    --   54.47 -19.00 120.00   26
 13  ω     -2.00  67.00   1.00   20.00    --   54.47 -57.00-120.00   69
 14  ω    142.00 176.00   1.00   20.00    --  108.95  50.00   0.00   34
 15  ω     87.00 112.00   1.00   20.00    --  108.95  50.00   0.00   25
 16  ω     39.00  77.00   1.00   20.00    --  108.95-111.00-150.00   38
 17  ω     38.00 112.00   1.00   20.00    --  108.95-111.00  30.00   74
 18  ω     40.00 142.00   1.00   20.00    --  108.95 -25.00-180.00  102
 19  ω    104.00 154.00   1.00   20.00    --  108.95 111.00-120.00   50
 20  ω    119.00 145.00   1.00   20.00    --  108.95 178.00  60.00   26
 21  ω     46.00 131.00   1.00   20.00    --  108.95 -50.00 -30.00   85
 22  ω     63.00 137.00   1.00   20.00    --  108.95 -77.00  30.00   74
 23  ω     60.00  99.00   1.00   20.00    --  108.95 178.00  60.00   39
 24  ω     37.00 113.00   1.00   20.00    --  108.95-111.00-120.00   76
 25  ω     80.00 110.00   1.00   20.00    --  108.95-111.00 150.00   30
 26  ω     42.00 124.00   1.00   20.00    --  108.95 -25.00  60.00   82
 27  ω     40.00 152.00   1.00   20.00    --  108.95  12.00  90.00  112
 28  ω     42.00 131.00   1.00   20.00    --  108.95 -63.00-150.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3255
_reflns_number_total             3651
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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         0.651
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3651
_refine_ls_number_restraints     139
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0559
_refine_ls_restrained_S_all      1.090
_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)+(0.1017P)²+18.1644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1691
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16B-C15 = C17A-C15 = C17B-C15 = C18A-C15 = C18B-C15 = C16A-C15 = C12A-C11 =
 C12B-C11 = C13A-C11 = C14B-C11 = C14A-C11 = C13B-C11
 1.53 with sigma of 0.02
 Br1A-B1 \\sim Br1B-B1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C12A \\sim C12B \\sim C13A \\sim C13B \\sim C14A \\sim C14B: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Br1A \\sim Br1B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C12B) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C13B) \\sim Ueq,
Uanis(C14A) \\sim Ueq, Uanis(C14B) \\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18B) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C16B) \\sim Ueq,
Uanis(C17A) \\sim Ueq, Uanis(C17B) \\sim Ueq, Uanis(C18A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br1B) \\sim Ueq, Uanis(Br1A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.02
4. Others
 Sof(Br1B)=1-FVAR(1)
 Sof(Br1A)=FVAR(1)
 Sof(C12B)=Sof(H12d)=Sof(H12e)=Sof(H12f)=Sof(C13B)=Sof(H13d)=Sof(H13e)=
 Sof(H13f)=Sof(C14B)=Sof(H14d)=Sof(H14e)=Sof(H14f)=1-FVAR(2)
 Sof(C12A)=Sof(H12a)=Sof(H12b)=Sof(H12c)=Sof(C13A)=Sof(H13a)=Sof(H13b)=
 Sof(H13c)=Sof(C14A)=Sof(H14a)=Sof(H14b)=Sof(H14c)=FVAR(2)
 Sof(C16B)=Sof(H16d)=Sof(H16e)=Sof(H16f)=Sof(C17B)=Sof(H17d)=Sof(H17e)=
 Sof(H17f)=Sof(C18B)=Sof(H18d)=Sof(H18e)=Sof(H18f)=1-FVAR(3)
 Sof(C16A)=Sof(H16a)=Sof(H16b)=Sof(H16c)=Sof(C17A)=Sof(H17a)=Sof(H17b)=
 Sof(H17c)=Sof(C18A)=Sof(H18a)=Sof(H18b)=Sof(H18c)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C5(H5)
5.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C12A(H12a,H12b,H12c),
 C12B(H12d,H12e,H12f), C13A(H13a,H13b,H13c), C13B(H13d,H13e,H13f), C14A(H14a,
 H14b,H14c), C14B(H14d,H14e,H14f), C16A(H16a,H16b,H16c), C16B(H16d,H16e,H16f),
 C17A(H17a,H17b,H17c), C17B(H17d,H17e,H17f), C18A(H18a,H18b,H18c), C18B(H18d,
 H18e,H18f)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1A Br 0.91735(15) 0.67193(16) 0.7707(6) 0.0885(8) Uani 0.264(5) 1 d D U P A 5
Br1B Br 0.92971(5) 0.68676(7) 0.7145(2) 0.0890(5) Uani 0.736(5) 1 d D U P A 6
N1 N 0.83392(7) 0.64816(8) 0.6345(2) 0.0457(5) Uani 1 1 d . . . . .
H1 H 0.808471 0.628525 0.590200 0.055 Uiso 1 1 calc R . . . .
C1 C 0.86649(9) 0.59528(9) 0.5594(3) 0.0440(6) Uani 1 1 d . . . . .
C2 C 0.84634(10) 0.55124(10) 0.6257(3) 0.0499(6) Uani 1 1 d . . . . .
C3 C 0.84354(11) 0.51320(10) 0.5586(3) 0.0545(7) Uani 1 1 d . . . . .
H3 H 0.829460 0.483798 0.603275 0.065 Uiso 1 1 calc R . . . .
C4 C 0.86025(10) 0.51587(10) 0.4297(3) 0.0520(7) Uani 1 1 d . . . . .
C5 C 0.87968(10) 0.55869(10) 0.3665(3) 0.0505(6) Uani 1 1 d . . . . .
H5 H 0.891325 0.561142 0.277923 0.061 Uiso 1 1 calc R . . . .
C6 C 0.88317(9) 0.59860(9) 0.4256(3) 0.0451(6) Uani 1 1 d . . . . .
C7 C 0.90725(10) 0.64401(10) 0.3385(3) 0.0569(7) Uani 1 1 d . . . . .
C8 C 0.96027(14) 0.66708(16) 0.3559(5) 0.0921(13) Uani 1 1 d . . . . .
H8A H 0.970582 0.645151 0.328109 0.138 Uiso 1 1 calc GR . . . .
H8B H 0.968434 0.675532 0.450280 0.138 Uiso 1 1 calc GR . . . .
H8C H 0.975802 0.695371 0.300331 0.138 Uiso 1 1 calc GR . . . .
C9 C 0.89123(18) 0.67936(15) 0.3625(5) 0.0898(13) Uani 1 1 d . . . . .
H9A H 0.856926 0.663345 0.360463 0.135 Uiso 1 1 calc GR . . . .
H9B H 0.903985 0.703365 0.292296 0.135 Uiso 1 1 calc GR . . . .
H9C H 0.902439 0.694162 0.450371 0.135 Uiso 1 1 calc GR . . . .
C10 C 0.89769(18) 0.63235(16) 0.1859(4) 0.0897(12) Uani 1 1 d . . . . .
H10A H 0.864015 0.611705 0.171382 0.135 Uiso 1 1 calc GR . . . .
H10B H 0.914602 0.616623 0.155443 0.135 Uiso 1 1 calc GR . . . .
H10C H 0.908453 0.661415 0.135019 0.135 Uiso 1 1 calc GR . . . .
C11 C 0.85752(13) 0.47281(11) 0.3608(4) 0.0676(9) Uani 1 1 d D . . . .
C12A C 0.8616(5) 0.4397(4) 0.4706(12) 0.1076(17) Uani 0.446(5) 1 d D U P B 3
H12A H 0.864808 0.415014 0.425499 0.161 Uiso 0.446(5) 1 calc GR . P B 3
H12B H 0.833303 0.425365 0.526449 0.161 Uiso 0.446(5) 1 calc GR . P B 3
H12C H 0.889067 0.458283 0.527248 0.161 Uiso 0.446(5) 1 calc GR . P B 3
C12B C 0.8291(4) 0.4284(3) 0.4313(11) 0.1179(18) Uani 0.554(5) 1 d D U P B 4
H12D H 0.795891 0.419027 0.423947 0.177 Uiso 0.554(5) 1 calc GR . P B 4
H12E H 0.838139 0.432136 0.526132 0.177 Uiso 0.554(5) 1 calc GR . P B 4
H12F H 0.834193 0.404145 0.391027 0.177 Uiso 0.554(5) 1 calc GR . P B 4
C13A C 0.8077(4) 0.4408(4) 0.3123(14) 0.1153(18) Uani 0.446(5) 1 d D U P B 3
H13A H 0.800555 0.456241 0.239506 0.173 Uiso 0.446(5) 1 calc GR . P B 3
H13B H 0.785851 0.434265 0.386720 0.173 Uiso 0.446(5) 1 calc GR . P B 3
H13C H 0.804684 0.411418 0.279524 0.173 Uiso 0.446(5) 1 calc GR . P B 3
C13B C 0.8464(4) 0.4725(3) 0.2107(10) 0.1134(17) Uani 0.554(5) 1 d D U P B 4
H13D H 0.869260 0.502470 0.170238 0.170 Uiso 0.554(5) 1 calc GR . P B 4
H13E H 0.814833 0.468058 0.200565 0.170 Uiso 0.554(5) 1 calc GR . P B 4
H13F H 0.848003 0.446931 0.165839 0.170 Uiso 0.554(5) 1 calc GR . P B 4
C14A C 0.8945(5) 0.4831(4) 0.2619(14) 0.1121(18) Uani 0.446(5) 1 d D U P B 3
H14A H 0.889877 0.498036 0.183013 0.168 Uiso 0.446(5) 1 calc GR . P B 3
H14B H 0.893221 0.453859 0.235004 0.168 Uiso 0.446(5) 1 calc GR . P B 3
H14C H 0.925187 0.504233 0.301849 0.168 Uiso 0.446(5) 1 calc GR . P B 3
C14B C 0.9085(3) 0.4821(3) 0.3530(12) 0.1061(17) Uani 0.554(5) 1 d D U P B 4
H14D H 0.919280 0.480115 0.443211 0.159 Uiso 0.554(5) 1 calc GR . P B 4
H14E H 0.928984 0.513361 0.315952 0.159 Uiso 0.554(5) 1 calc GR . P B 4
H14F H 0.909441 0.458519 0.295059 0.159 Uiso 0.554(5) 1 calc GR . P B 4
C15 C 0.82716(13) 0.54104(13) 0.7724(3) 0.0668(9) Uani 1 1 d D . . . .
C16A C 0.8345(6) 0.5043(5) 0.8344(10) 0.110(4) Uani 0.508(8) 1 d D U P C 5
H16A H 0.867764 0.513670 0.828803 0.166 Uiso 0.508(8) 1 calc GR . P C 5
H16B H 0.815796 0.474656 0.786661 0.166 Uiso 0.508(8) 1 calc GR . P C 5
H16C H 0.824906 0.500414 0.928741 0.166 Uiso 0.508(8) 1 calc GR . P C 5
C16B C 0.8637(4) 0.5415(5) 0.8635(10) 0.100(3) Uani 0.492(8) 1 d D U P C 6
H16D H 0.849167 0.526167 0.948421 0.150 Uiso 0.492(8) 1 calc GR . P C 6
H16E H 0.888081 0.573999 0.880904 0.150 Uiso 0.492(8) 1 calc GR . P C 6
H16F H 0.877807 0.524754 0.820557 0.150 Uiso 0.492(8) 1 calc GR . P C 6
C17A C 0.8581(4) 0.5860(3) 0.8663(7) 0.092(3) Uani 0.508(8) 1 d D U P C 5
H17A H 0.891135 0.594724 0.860562 0.139 Uiso 0.508(8) 1 calc GR . P C 5
H17B H 0.847440 0.578383 0.959517 0.139 Uiso 0.508(8) 1 calc GR . P C 5
H17C H 0.854429 0.612317 0.836024 0.139 Uiso 0.508(8) 1 calc GR . P C 5
C17B C 0.8063(4) 0.5689(4) 0.8344(9) 0.091(3) Uani 0.492(8) 1 d D U P C 6
H17D H 0.789795 0.553608 0.917440 0.136 Uiso 0.492(8) 1 calc GR . P C 6
H17E H 0.784247 0.570246 0.771118 0.136 Uiso 0.492(8) 1 calc GR . P C 6
H17F H 0.831474 0.600783 0.854581 0.136 Uiso 0.492(8) 1 calc GR . P C 6
C18A C 0.7800(3) 0.5346(4) 0.7697(9) 0.091(3) Uani 0.508(8) 1 d D U P C 5
H18A H 0.781674 0.564105 0.744425 0.136 Uiso 0.508(8) 1 calc GR . P C 5
H18B H 0.765806 0.525005 0.858863 0.136 Uiso 0.508(8) 1 calc GR . P C 5
H18C H 0.760922 0.510299 0.704126 0.136 Uiso 0.508(8) 1 calc GR . P C 5
C18B C 0.7838(4) 0.4885(3) 0.7855(10) 0.106(4) Uani 0.492(8) 1 d D U P C 6
H18D H 0.794056 0.466177 0.762149 0.159 Uiso 0.492(8) 1 calc GR . P C 6
H18E H 0.758664 0.484377 0.724479 0.159 Uiso 0.492(8) 1 calc GR . P C 6
H18F H 0.772092 0.482913 0.878017 0.159 Uiso 0.492(8) 1 calc GR . P C 6
B1 B 0.86995(11) 0.63874(11) 0.6322(3) 0.0500(7) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1A B1 1.958(4) . ?
Br1B B1 1.985(3) . ?
N1 N1 1.396(4) 13_666 ?
N1 B1 1.370(4) . ?
C1 C2 1.422(4) . ?
C1 C6 1.425(4) . ?
C1 B1 1.558(4) . ?
C2 C3 1.382(4) . ?
C2 C15 1.561(4) . ?
C3 C4 1.383(4) . ?
C4 C5 1.376(4) . ?
C4 C11 1.538(4) . ?
C5 C6 1.393(4) . ?
C6 C7 1.561(4) . ?
C7 C8 1.527(5) . ?
C7 C9 1.519(5) . ?
C7 C10 1.562(5) . ?
C11 C12A 1.598(11) . ?
C11 C12B 1.465(10) . ?
C11 C13A 1.519(11) . ?
C11 C13B 1.539(10) . ?
C11 C14A 1.470(12) . ?
C11 C14B 1.553(9) . ?
C15 C16A 1.483(9) . ?
C15 C16B 1.503(9) . ?
C15 C17A 1.614(9) . ?
C15 C17B 1.527(8) . ?
C15 C18A 1.459(9) . ?
C15 C18B 1.608(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B1 N1 N1 127.7(3) . 13_666 ?
C2 C1 C6 118.6(2) . . ?
C2 C1 B1 120.3(2) . . ?
C6 C1 B1 121.1(2) . . ?
C1 C2 C15 126.0(2) . . ?
C3 C2 C1 119.1(2) . . ?
C3 C2 C15 114.9(3) . . ?
C2 C3 C4 123.2(3) . . ?
C3 C4 C11 121.2(3) . . ?
C5 C4 C3 117.2(2) . . ?
C5 C4 C11 121.6(3) . . ?
C4 C5 C6 123.4(3) . . ?
C1 C6 C7 125.8(2) . . ?
C5 C6 C1 118.5(2) . . ?
C5 C6 C7 115.7(2) . . ?
C6 C7 C10 111.2(3) . . ?
C8 C7 C6 108.7(3) . . ?
C8 C7 C10 105.8(3) . . ?
C9 C7 C6 116.3(3) . . ?
C9 C7 C8 110.5(3) . . ?
C9 C7 C10 103.7(3) . . ?
C4 C11 C12A 109.8(4) . . ?
C4 C11 C13B 110.1(4) . . ?
C4 C11 C14B 106.4(4) . . ?
C12B C11 C4 114.9(4) . . ?
C12B C11 C13B 115.4(6) . . ?
C12B C11 C14B 108.0(7) . . ?
C13A C11 C4 109.0(4) . . ?
C13A C11 C12A 100.0(8) . . ?
C13B C11 C14B 100.6(6) . . ?
C14A C11 C4 115.3(5) . . ?
C14A C11 C12A 105.9(8) . . ?
C14A C11 C13A 115.5(8) . . ?
C2 C15 C17A 110.1(4) . . ?
C2 C15 C18B 110.8(4) . . ?
C16A C15 C2 110.6(5) . . ?
C16A C15 C17A 102.8(7) . . ?
C16B C15 C2 109.1(5) . . ?
C16B C15 C17B 110.4(7) . . ?
C16B C15 C18B 103.8(7) . . ?
C17B C15 C2 120.4(4) . . ?
C17B C15 C18B 100.9(6) . . ?
C18A C15 C2 107.5(4) . . ?
C18A C15 C16A 119.0(8) . . ?
C18A C15 C17A 106.3(6) . . ?
N1 B1 Br1A 113.7(2) . . ?
N1 B1 Br1B 116.1(2) . . ?
N1 B1 C1 122.9(2) . . ?
C1 B1 Br1A 120.9(2) . . ?
C1 B1 Br1B 120.9(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# 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_klb-2
_database_code_depnum_ccdc_archive 'CCDC 1977879'
loop_
_audit_author_name
_audit_author_address
'Lingbing Kong'
;Shandong University
China
;
_audit_update_record             
;
2020-05-25 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_audit_creation_date             2020-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H26 B Br N'
_chemical_formula_sum            'C24 H26 B Br N'
_chemical_formula_weight         419.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         CBN
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   13.4204(6)
_cell_length_b                   13.4075(4)
_cell_length_c                   13.5682(5)
_cell_angle_alpha                90
_cell_angle_beta                 118.076(5)
_cell_angle_gamma                90
_cell_volume                     2154.09(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5356
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      76.1910
_cell_measurement_theta_min      3.7450
_shelx_estimated_absorpt_T_max   0.621
_shelx_estimated_absorpt_T_min   0.505
_exptl_absorpt_coefficient_mu    2.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11490
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         3.820
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00 -62.00   1.00    0.10    --  -48.45-155.00 175.00   26
  2  ω   -119.00 -74.00   1.00    0.10    --  -48.45-120.00 -28.00   45
  3  ω    -87.00 -35.00   1.00    0.10    --  -48.45 120.00  56.00   52
  4  ω     28.00  93.00   1.00    0.10    --   48.45-120.00 -28.00   65
  5  ω     57.00  82.00   1.00    0.10    --   48.45-155.00 175.00   25
  6  ω   -141.00-116.00   1.00    0.43    --  -86.25-120.00 -28.00   25
  7  ω     82.00 137.00   1.00    0.43    --  107.75-155.00 175.00   55
  8  ω     97.00 153.00   1.00    0.43    --  107.75 120.00  56.00   56
  9  ω     69.00 113.00   1.00    0.43    --  107.75-120.00 -28.00   44
 10  ω   -120.00 -26.00   1.00    0.10    --  -48.45 -77.00 -30.00   94
 11  ω     35.00 122.00   1.00    0.43    --  107.75 -57.00 -60.00   87
 12  ω     35.00 120.00   1.00    0.43    --  107.75 -37.00 -60.00   85
 13  ω     93.00 178.00   1.00    0.43    --  107.75  57.00-120.00   85
 14  ω     93.00 172.00   1.00    0.43    --  107.75  57.00 150.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0299628000
_diffrn_orient_matrix_UB_12      -0.1107222000
_diffrn_orient_matrix_UB_13      -0.0016983000
_diffrn_orient_matrix_UB_21      -0.1258072000
_diffrn_orient_matrix_UB_22      -0.0278520000
_diffrn_orient_matrix_UB_23      -0.0497788000
_diffrn_orient_matrix_UB_31      -0.0140092000
_diffrn_orient_matrix_UB_32      0.0134804000
_diffrn_orient_matrix_UB_33      -0.1185935000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3104
_reflns_number_total             3751
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3751
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.044
_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)+(0.0553P)²+1.7784P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1161
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C3(H3), C20(H20), C9(H9), C18(H18), C4(H4)
3.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C13(H13a,H13b,H13c), C22(H22a,H22b,H22c), C15(H15a,H15b,
 H15c), C24(H24a,H24b,H24c), C23(H23a,H23b,H23c)
;
_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
Br1 Br 0.49763(3) 0.31920(2) 0.62183(3) 0.04048(15) Uani 1 1 d . . . . .
N1 N 0.5006(2) 0.51859(18) 0.54844(19) 0.0283(5) Uani 1 1 d D . . . .
C1 C 0.4985(2) 0.51670(19) 0.7365(2) 0.0233(5) Uani 1 1 d . . . . .
C7 C 0.7113(2) 0.5105(2) 0.8397(2) 0.0252(6) Uani 1 1 d . . . . .
C6 C 0.5998(2) 0.5411(2) 0.8317(2) 0.0256(5) Uani 1 1 d . . . . .
C2 C 0.3950(2) 0.5393(2) 0.7347(2) 0.0262(5) Uani 1 1 d . . . . .
C8 C 0.7675(2) 0.5710(2) 0.7977(2) 0.0284(6) Uani 1 1 d . . . . .
C12 C 0.7612(2) 0.4207(2) 0.8944(2) 0.0288(6) Uani 1 1 d . . . . .
C16 C 0.2868(2) 0.5036(2) 0.6391(2) 0.0269(6) Uani 1 1 d . . . . .
C21 C 0.2311(2) 0.5573(2) 0.5400(2) 0.0289(6) Uani 1 1 d . . . . .
C5 C 0.5971(2) 0.5906(2) 0.9206(2) 0.0306(6) Uani 1 1 d . . . . .
H5 H 0.6658 0.6077 0.9846 0.037 Uiso 1 1 calc R . . . .
C11 C 0.8652(2) 0.3930(2) 0.9038(2) 0.0304(6) Uani 1 1 d . . . . .
H11 H 0.8983 0.3318 0.9397 0.036 Uiso 1 1 calc R . . . .
C3 C 0.3943(2) 0.5888(2) 0.8244(2) 0.0327(6) Uani 1 1 d . . . . .
H3 H 0.3246 0.6048 0.8228 0.039 Uiso 1 1 calc R . . . .
C20 C 0.1320(2) 0.5183(2) 0.4533(2) 0.0332(6) Uani 1 1 d . . . . .
H20 H 0.0949 0.5546 0.3853 0.040 Uiso 1 1 calc R . . . .
C17 C 0.2409(2) 0.4126(2) 0.6509(2) 0.0321(6) Uani 1 1 d . . . . .
C9 C 0.8722(2) 0.5401(2) 0.8097(2) 0.0319(6) Uani 1 1 d . . . . .
H9 H 0.9102 0.5810 0.7808 0.038 Uiso 1 1 calc R . . . .
C18 C 0.1421(3) 0.3773(2) 0.5631(3) 0.0362(7) Uani 1 1 d . . . . .
H18 H 0.1116 0.3159 0.5714 0.043 Uiso 1 1 calc R . . . .
C19 C 0.0863(2) 0.4292(2) 0.4629(2) 0.0345(7) Uani 1 1 d . . . . .
C10 C 0.9220(2) 0.4518(2) 0.8624(2) 0.0329(6) Uani 1 1 d . . . . .
C4 C 0.4954(3) 0.6149(2) 0.9162(2) 0.0351(7) Uani 1 1 d . . . . .
H4 H 0.4945 0.6498 0.9767 0.042 Uiso 1 1 calc R . . . .
C14 C 0.7041(3) 0.3545(2) 0.9431(3) 0.0384(7) Uani 1 1 d . . . . .
H14A H 0.6960 0.3910 1.0016 0.058 Uiso 1 1 calc GR . . . .
H14B H 0.7501 0.2947 0.9754 0.058 Uiso 1 1 calc GR . . . .
H14C H 0.6294 0.3350 0.8841 0.058 Uiso 1 1 calc GR . . . .
C13 C 0.7184(3) 0.6689(2) 0.7403(3) 0.0374(7) Uani 1 1 d . . . . .
H13A H 0.6487 0.6828 0.7443 0.056 Uiso 1 1 calc GR . . . .
H13B H 0.7016 0.6648 0.6618 0.056 Uiso 1 1 calc GR . . . .
H13C H 0.7730 0.7225 0.7774 0.056 Uiso 1 1 calc GR . . . .
C22 C 0.2729(3) 0.6576(2) 0.5249(3) 0.0403(7) Uani 1 1 d . . . . .
H22A H 0.3325 0.6812 0.5970 0.060 Uiso 1 1 calc GR . . . .
H22B H 0.2102 0.7053 0.4959 0.060 Uiso 1 1 calc GR . . . .
H22C H 0.3031 0.6515 0.4720 0.060 Uiso 1 1 calc GR . . . .
C15 C 1.0345(3) 0.4186(3) 0.8749(3) 0.0433(8) Uani 1 1 d . . . . .
H15A H 1.0822 0.3952 0.9514 0.065 Uiso 1 1 calc GR . . . .
H15B H 1.0715 0.4747 0.8591 0.065 Uiso 1 1 calc GR . . . .
H15C H 1.0232 0.3642 0.8224 0.065 Uiso 1 1 calc GR . . . .
B1 B 0.4993(2) 0.4642(2) 0.6341(2) 0.0269(6) Uani 1 1 d . . . . .
C24 C -0.0210(3) 0.3879(3) 0.3690(3) 0.0452(8) Uani 1 1 d . . . . .
H24A H -0.0692 0.4430 0.3248 0.068 Uiso 1 1 calc GR . . . .
H24B H -0.0610 0.3484 0.4001 0.068 Uiso 1 1 calc GR . . . .
H24C H -0.0024 0.3455 0.3211 0.068 Uiso 1 1 calc GR . . . .
C23 C 0.2977(3) 0.3527(3) 0.7578(3) 0.0461(8) Uani 1 1 d . . . . .
H23A H 0.3749 0.3363 0.7736 0.069 Uiso 1 1 calc GR . . . .
H23B H 0.2552 0.2910 0.7494 0.069 Uiso 1 1 calc GR . . . .
H23C H 0.2996 0.3920 0.8196 0.069 Uiso 1 1 calc GR . . . .
H1 H 0.501(3) 0.5852(14) 0.554(3) 0.055 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 B1 1.951(3) . ?
N1 N1 1.399(4) 3_666 ?
N1 B1 1.379(4) . ?
N1 H1 0.895(19) . ?
C1 C6 1.404(4) . ?
C1 C2 1.410(4) . ?
C1 B1 1.562(4) . ?
C7 C6 1.505(4) . ?
C7 C8 1.399(4) . ?
C7 C12 1.407(4) . ?
C6 C5 1.392(4) . ?
C2 C16 1.499(4) . ?
C2 C3 1.390(4) . ?
C8 C9 1.400(4) . ?
C8 C13 1.509(4) . ?
C12 C11 1.391(4) . ?
C12 C14 1.512(4) . ?
C16 C21 1.393(4) . ?
C16 C17 1.409(4) . ?
C21 C20 1.398(4) . ?
C21 C22 1.508(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.377(4) . ?
C11 H11 0.9500 . ?
C11 C10 1.386(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(4) . ?
C20 H20 0.9500 . ?
C20 C19 1.378(5) . ?
C17 C18 1.384(4) . ?
C17 C23 1.512(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.391(4) . ?
C19 C24 1.508(4) . ?
C10 C15 1.506(4) . ?
C4 H4 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 N1 H1 115(3) 3_666 . ?
B1 N1 N1 127.2(3) . 3_666 ?
B1 N1 H1 118(2) . . ?
C6 C1 C2 119.1(2) . . ?
C6 C1 B1 120.9(2) . . ?
C2 C1 B1 120.0(2) . . ?
C8 C7 C6 121.3(2) . . ?
C8 C7 C12 119.8(3) . . ?
C12 C7 C6 118.8(2) . . ?
C1 C6 C7 120.2(2) . . ?
C5 C6 C1 119.9(2) . . ?
C5 C6 C7 119.8(2) . . ?
C1 C2 C16 119.5(2) . . ?
C3 C2 C1 119.9(2) . . ?
C3 C2 C16 120.5(2) . . ?
C7 C8 C9 119.0(3) . . ?
C7 C8 C13 121.8(3) . . ?
C9 C8 C13 119.2(3) . . ?
C7 C12 C14 121.3(3) . . ?
C11 C12 C7 119.0(3) . . ?
C11 C12 C14 119.7(3) . . ?
C21 C16 C2 122.1(3) . . ?
C21 C16 C17 119.5(3) . . ?
C17 C16 C2 118.4(2) . . ?
C16 C21 C20 119.0(3) . . ?
C16 C21 C22 121.9(3) . . ?
C20 C21 C22 119.1(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 H5 119.8 . . ?
C12 C11 H11 119.0 . . ?
C10 C11 C12 122.0(3) . . ?
C10 C11 H11 119.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H3 120.0 . . ?
C21 C20 H20 118.8 . . ?
C19 C20 C21 122.3(3) . . ?
C19 C20 H20 118.8 . . ?
C16 C17 C23 121.2(3) . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 C23 119.4(3) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 C8 121.9(3) . . ?
C10 C9 H9 119.1 . . ?
C17 C18 H18 119.1 . . ?
C17 C18 C19 121.9(3) . . ?
C19 C18 H18 119.1 . . ?
C20 C19 C18 117.9(3) . . ?
C20 C19 C24 121.9(3) . . ?
C18 C19 C24 120.2(3) . . ?
C11 C10 C15 120.0(3) . . ?
C9 C10 C11 118.3(3) . . ?
C9 C10 C15 121.7(3) . . ?
C5 C4 C3 120.6(3) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 B1 Br1 117.3(2) . . ?
N1 B1 C1 121.3(3) . . ?
C1 B1 Br1 121.4(2) . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C17 C23 H23A 109.5 . . ?
C17 C23 H23B 109.5 . . ?
C17 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.676
_oxdiff_exptl_absorpt_empirical_full_min 0.660
####################################################################### 
# 
# 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_klb-6
_database_code_depnum_ccdc_archive 'CCDC 1977883'
loop_
_audit_author_name
_audit_author_address
'Lingbing Kong'
;Shandong University
China
;
_audit_update_record             
;
2020-05-25 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_audit_creation_date             2020-05-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C47 H78 B2 N4, 1.5(C7 H8)'
_chemical_formula_sum            'C57.50 H90 B2 N4'
_chemical_formula_weight         858.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         CBN
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.7577(4)
_cell_length_b                   13.9324(4)
_cell_length_c                   18.6526(5)
_cell_angle_alpha                102.637(2)
_cell_angle_beta                 99.834(2)
_cell_angle_gamma                105.896(3)
_cell_volume                     2779.50(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10907
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.0120
_cell_measurement_theta_min      3.3950
_shelx_estimated_absorpt_T_max   0.881
_shelx_estimated_absorpt_T_min   0.813
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26375
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         2.504
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00  66.00   1.00    5.00    --  106.49 -57.00  30.00   31
  2  ω     43.00 106.00   1.00    5.00    --  106.49 -99.00 -30.00   63
  3  ω     50.00 106.00   1.00    5.00    --  106.49 -99.00-120.00   56
  4  ω     80.00 109.00   1.00    5.00    --  106.49-125.00-180.00   29
  5  ω     73.00 104.00   1.00    5.00    --  106.49-102.00-146.00   31
  6  ω     35.00 103.00   1.00    5.00    --  106.49 -99.00-180.00   68
  7  ω     38.00  77.00   1.00    5.00    --  106.49-125.00-180.00   39
  8  ω     14.00  56.00   1.00    0.50    --   48.45-102.00-146.00   42
  9  ω    -24.00  23.00   1.00    0.50    --   48.45 -19.00 -60.00   47
 10  ω     93.00 139.00   1.00    5.00    --  106.49  38.00-120.00   46
 11  ω    141.00 176.00   1.00    5.00    --  106.49  38.00-120.00   35
 12  ω    106.00 168.00   1.00    5.00    --  106.49 102.00 -43.00   62
 13  ω     94.00 178.00   1.00    5.00    --  106.49  38.00  30.00   84
 14  ω     97.00 171.00   1.00    5.00    --  106.49  19.00 -30.00   74
 15  ω     96.00 178.00   1.00    5.00    --  106.49  19.00 -60.00   82
 16  ω     34.00 103.00   1.00    5.00    --  106.49 -99.00 120.00   69
 17  ω     34.00 106.00   1.00    5.00    --  106.49 -99.00  30.00   72
 18  ω     40.00 103.00   1.00    5.00    --  106.49 -77.00  30.00   63
 19  ω    -43.00  25.00   1.00    0.50    --  -48.45  38.00-120.00   68
 20  ω    -66.00 -14.00   1.00    5.00    --  -86.25  57.00 -60.00   52
 21  ω    -79.00   8.00   1.00    0.50    --  -48.45 102.00 -43.00   87
 22  ω   -117.00 -74.00   1.00    0.50    --  -48.45-125.00  30.00   43
 23  ω   -119.00 -35.00   1.00    0.50    --  -48.45 -77.00 120.00   84
 24  ω    -43.00 -15.00   1.00    5.00    --  -86.25  38.00 150.00   28
 25  ω    -42.00 -16.00   1.00    5.00    --  -86.25  38.00 120.00   26
 26  ω    -81.00 -33.00   1.00    5.00    --  -86.25 102.00 -43.00   48
 27  ω   -138.00 -85.00   1.00    5.00    --  -86.25-102.00-146.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1302567000
_diffrn_orient_matrix_UB_12      0.0701727000
_diffrn_orient_matrix_UB_13      0.0070595000
_diffrn_orient_matrix_UB_21      0.0095847000
_diffrn_orient_matrix_UB_22      0.0535145000
_diffrn_orient_matrix_UB_23      0.0833643000
_diffrn_orient_matrix_UB_31      0.0519161000
_diffrn_orient_matrix_UB_32      -0.0809728000
_diffrn_orient_matrix_UB_33      0.0250170000
_diffrn_oxdiff_digest_frames     
;
013c0db2bc851586cca7c1b59c25d34f62000266b7e
;
_diffrn_oxdiff_digest_hkl        
;
0180f37593be9cfd47ff2d316b20c2ad4b1483
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7728
_reflns_number_total             9658
_reflns_odcompleteness_completeness 98.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         9658
_refine_ls_number_restraints     475
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0595
_refine_ls_restrained_S_all      1.057
_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)+(0.0421P)²+1.7653P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1519
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C60-C61
 1.53 with sigma of 0.02
 C49A-C48A \\sim C48A-C53A \\sim C52B-C53A \\sim C51A-C52B \\sim C51A-C50A
\\sim C50A-C49A
 with sigma of 0.02
 C23-C21 \\sim C24B-C21 \\sim C24A-C21 \\sim C22-C21
 with sigma of 0.02
 C60-C59 \\sim C55-C56 \\sim C57-C58
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C24A \\sim C24B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C48A \\sim C48B \\sim C49A \\sim C49B \\sim C50A \\sim C50B \\sim C51A \\sim
C51B \\sim C52A \\sim C52B \\sim C53A \\sim C53B \\sim C54A \\sim C54B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24B) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C51B) \\sim Ueq, Uanis(C48A) \\sim Ueq, Uanis(C49A) \\sim Ueq,
Uanis(C53A) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C52B) \\sim Ueq,
Uanis(C54A) \\sim Ueq, Uanis(C53B) \\sim Ueq, Uanis(C48B) \\sim Ueq,
Uanis(C50B) \\sim Ueq, Uanis(C49B) \\sim Ueq, Uanis(C51A) \\sim Ueq,
Uanis(C54B) \\sim Ueq, Uanis(C52A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C61) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C55, C56, C57, C58, C59, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
 Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=
 Sof(H51A)=Sof(C52B)=Sof(H52B)=Sof(C53A)=Sof(C54A)=Sof(H54A)=Sof(H54B)=
 Sof(H54C)=1-FVAR(2)
 Sof(C48B)=Sof(H48B)=Sof(C49B)=Sof(H49B)=Sof(C50B)=Sof(H50B)=Sof(C51B)=
 Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(C53B)=Sof(C54B)=Sof(H54D)=Sof(H54E)=
 Sof(H54F)=FVAR(2)
 Fixed Sof: C55(0.5) H55(0.5) C56(0.5) H56(0.5) C57(0.5) H57(0.5) C58(0.5)
 H58(0.5) C59(0.5) H59(0.5) C60(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
6.a Ternary CH refined with riding coordinates:
 C40(H40), C43(H43)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C48A(H48A), C48B(H48B), C49A(H49A),
 C49B(H49B), C50A(H50A), C50B(H50B), C51A(H51A), C51B(H51B), C52A(H52A),
 C52B(H52B), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C54A(H54A,H54B,
 H54C), C54B(H54D,H54E,H54F), C61(H61A,H61B,H61C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.63696(15) 0.40999(13) 0.25664(9) 0.0337(4) Uani 1 1 d . . . . .
N2 N 0.60890(14) 0.47140(13) 0.31303(9) 0.0316(4) Uani 1 1 d . . . . .
N3 N 0.69960(15) 0.72210(14) 0.46524(9) 0.0352(4) Uani 1 1 d . . . . .
N4 N 0.51615(13) 0.61400(12) 0.41875(8) 0.0286(3) Uani 1 1 d . . . . .
C1 C 0.67565(19) 0.25090(16) 0.15570(12) 0.0356(4) Uani 1 1 d . . . . .
C2 C 0.70697(18) 0.25995(16) 0.08663(11) 0.0334(4) Uani 1 1 d . . . . .
C3 C 0.72983(18) 0.17684(16) 0.04129(11) 0.0339(4) Uani 1 1 d . . . . .
H3 H 0.7513 0.1836 -0.0035 0.041 Uiso 1 1 calc R . . . .
C4 C 0.72196(18) 0.08480(16) 0.05996(12) 0.0353(4) Uani 1 1 d . . . . .
C5 C 0.6886(2) 0.07689(17) 0.12690(13) 0.0420(5) Uani 1 1 d . . . . .
H5 H 0.6819 0.0154 0.1402 0.050 Uiso 1 1 calc R . . . .
C6 C 0.6647(2) 0.15629(18) 0.17484(13) 0.0422(5) Uani 1 1 d . . . . .
C7 C 0.78051(17) 0.63442(16) 0.30429(10) 0.0309(4) Uani 1 1 d . . . . .
C8 C 0.89801(18) 0.62399(18) 0.32008(12) 0.0384(5) Uani 1 1 d . . . . .
C9 C 0.98713(19) 0.67143(19) 0.28615(12) 0.0423(5) Uani 1 1 d . . . . .
H9 H 1.0627 0.6616 0.2961 0.051 Uiso 1 1 calc R . . . .
C10 C 0.96842(19) 0.73165(17) 0.23903(12) 0.0390(5) Uani 1 1 d . . . . .
C11 C 0.85318(19) 0.74125(16) 0.22341(11) 0.0350(4) Uani 1 1 d . . . . .
H11 H 0.8385 0.7821 0.1919 0.042 Uiso 1 1 calc R . . . .
C12 C 0.75850(18) 0.69351(15) 0.25209(10) 0.0304(4) Uani 1 1 d . . . . .
C13 C 0.7138(2) 0.35874(16) 0.05992(11) 0.0376(5) Uani 1 1 d . . . . .
C14 C 0.5886(2) 0.37425(18) 0.04933(13) 0.0435(5) Uani 1 1 d . . . . .
H14A H 0.5664 0.3844 0.0970 0.065 Uiso 1 1 calc GR . . . .
H14B H 0.5289 0.3139 0.0132 0.065 Uiso 1 1 calc GR . . . .
H14C H 0.5921 0.4342 0.0312 0.065 Uiso 1 1 calc GR . . . .
C15 C 0.8103(2) 0.45467(18) 0.11684(13) 0.0462(5) Uani 1 1 d . . . . .
H15A H 0.8885 0.4446 0.1225 0.069 Uiso 1 1 calc GR . . . .
H15B H 0.7896 0.4650 0.1649 0.069 Uiso 1 1 calc GR . . . .
H15C H 0.8132 0.5146 0.0988 0.069 Uiso 1 1 calc GR . . . .
C16 C 0.7477(3) 0.35004(19) -0.01681(14) 0.0529(6) Uani 1 1 d . . . . .
H16A H 0.6898 0.2897 -0.0540 0.079 Uiso 1 1 calc GR . . . .
H16B H 0.8279 0.3440 -0.0118 0.079 Uiso 1 1 calc GR . . . .
H16C H 0.7466 0.4110 -0.0325 0.079 Uiso 1 1 calc GR . . . .
C17 C 0.7448(2) -0.00796(16) 0.00980(13) 0.0416(5) Uani 1 1 d . . . . .
C18 C 0.6276(3) -0.1008(2) -0.01512(16) 0.0604(7) Uani 1 1 d . . . . .
H18A H 0.5638 -0.0840 -0.0440 0.091 Uiso 1 1 calc GR . . . .
H18B H 0.6043 -0.1172 0.0288 0.091 Uiso 1 1 calc GR . . . .
H18C H 0.6411 -0.1597 -0.0458 0.091 Uiso 1 1 calc GR . . . .
C19 C 0.7842(3) 0.0151(2) -0.05964(16) 0.0625(8) Uani 1 1 d . . . . .
H19A H 0.8594 0.0719 -0.0440 0.094 Uiso 1 1 calc GR . . . .
H19B H 0.7224 0.0332 -0.0893 0.094 Uiso 1 1 calc GR . . . .
H19C H 0.7957 -0.0454 -0.0896 0.094 Uiso 1 1 calc GR . . . .
C20 C 0.8459(3) -0.0368(2) 0.05505(18) 0.0660(8) Uani 1 1 d . . . . .
H20A H 0.8220 -0.0546 0.0984 0.099 Uiso 1 1 calc GR . . . .
H20B H 0.9199 0.0214 0.0716 0.099 Uiso 1 1 calc GR . . . .
H20C H 0.8591 -0.0951 0.0235 0.099 Uiso 1 1 calc GR . . . .
C21 C 0.6277(3) 0.1388(2) 0.24823(15) 0.0591(7) Uani 1 1 d D . . . .
C22 C 0.5054(3) 0.1578(2) 0.25186(16) 0.0641(8) Uani 1 1 d D . . . .
H22A H 0.4453 0.1173 0.2057 0.096 Uiso 1 1 calc GR . . . .
H22B H 0.5159 0.2302 0.2583 0.096 Uiso 1 1 calc GR . . . .
H22C H 0.4790 0.1378 0.2939 0.096 Uiso 1 1 calc GR . . . .
C23 C 0.7284(3) 0.2113(3) 0.31785(15) 0.0706(9) Uani 1 1 d D . . . .
H23A H 0.7364 0.2823 0.3197 0.106 Uiso 1 1 calc GR . . . .
H23B H 0.8043 0.1996 0.3145 0.106 Uiso 1 1 calc GR . . . .
H23C H 0.7076 0.1974 0.3630 0.106 Uiso 1 1 calc GR . . . .
C24A C 0.639(3) 0.0359(15) 0.2621(14) 0.071(4) Uani 0.42(5) 1 d D U P A 1
H24A H 0.5896 -0.0211 0.2190 0.107 Uiso 0.42(5) 1 calc GR . P A 1
H24B H 0.6107 0.0267 0.3064 0.107 Uiso 0.42(5) 1 calc GR . P A 1
H24C H 0.7223 0.0384 0.2696 0.107 Uiso 0.42(5) 1 calc GR . P A 1
C24B C 0.590(2) 0.0198(9) 0.2435(12) 0.067(3) Uani 0.58(5) 1 d D U P A 2
H24D H 0.5254 -0.0187 0.1989 0.101 Uiso 0.58(5) 1 calc GR . P A 2
H24E H 0.5622 0.0093 0.2876 0.101 Uiso 0.58(5) 1 calc GR . P A 2
H24F H 0.6590 -0.0038 0.2412 0.101 Uiso 0.58(5) 1 calc GR . P A 2
C25 C 0.63212(18) 0.70494(16) 0.22270(10) 0.0321(4) Uani 1 1 d . . . . .
C26 C 0.6324(2) 0.76041(19) 0.15948(12) 0.0443(5) Uani 1 1 d . . . . .
H26A H 0.6558 0.7226 0.1182 0.066 Uiso 1 1 calc GR . . . .
H26B H 0.6894 0.8297 0.1791 0.066 Uiso 1 1 calc GR . . . .
H26C H 0.5522 0.7635 0.1418 0.066 Uiso 1 1 calc GR . . . .
C27 C 0.5950(2) 0.77172(17) 0.28544(11) 0.0373(5) Uani 1 1 d . . . . .
H27A H 0.6550 0.8396 0.3044 0.056 Uiso 1 1 calc GR . . . .
H27B H 0.5893 0.7397 0.3259 0.056 Uiso 1 1 calc GR . . . .
H27C H 0.5172 0.7777 0.2653 0.056 Uiso 1 1 calc GR . . . .
C28 C 0.5337(2) 0.59875(17) 0.18778(12) 0.0426(5) Uani 1 1 d . . . . .
H28A H 0.5277 0.5611 0.2251 0.064 Uiso 1 1 calc GR . . . .
H28B H 0.5547 0.5603 0.1456 0.064 Uiso 1 1 calc GR . . . .
H28C H 0.4567 0.6081 0.1706 0.064 Uiso 1 1 calc GR . . . .
C29 C 1.0668(2) 0.7853(2) 0.20291(14) 0.0505(6) Uani 1 1 d . . . . .
C30 C 1.0940(3) 0.9028(2) 0.23050(18) 0.0775(9) Uani 1 1 d . . . . .
H30A H 1.1241 0.9258 0.2846 0.116 Uiso 1 1 calc GR . . . .
H30B H 1.0207 0.9192 0.2166 0.116 Uiso 1 1 calc GR . . . .
H30C H 1.1545 0.9370 0.2076 0.116 Uiso 1 1 calc GR . . . .
C31 C 1.0184(3) 0.7496(2) 0.11674(15) 0.0594(7) Uani 1 1 d . . . . .
H31A H 0.9472 0.7691 0.1032 0.089 Uiso 1 1 calc GR . . . .
H31B H 0.9976 0.6754 0.0991 0.089 Uiso 1 1 calc GR . . . .
H31C H 1.0801 0.7818 0.0938 0.089 Uiso 1 1 calc GR . . . .
C32 C 1.1828(3) 0.7567(3) 0.2206(2) 0.0888(12) Uani 1 1 d . . . . .
H32A H 1.1627 0.6825 0.2057 0.133 Uiso 1 1 calc GR . . . .
H32B H 1.2200 0.7834 0.2740 0.133 Uiso 1 1 calc GR . . . .
H32C H 1.2386 0.7863 0.1931 0.133 Uiso 1 1 calc GR . . . .
C33 C 0.94661(19) 0.5632(2) 0.37261(15) 0.0547(7) Uani 1 1 d . . . . .
C34 C 0.9761(2) 0.4737(2) 0.32360(19) 0.0692(9) Uani 1 1 d . . . . .
H34A H 1.0332 0.5011 0.2961 0.104 Uiso 1 1 calc GR . . . .
H34B H 0.9026 0.4257 0.2885 0.104 Uiso 1 1 calc GR . . . .
H34C H 1.0111 0.4384 0.3555 0.104 Uiso 1 1 calc GR . . . .
C35 C 1.0637(2) 0.6382(3) 0.43129(17) 0.0729(10) Uani 1 1 d . . . . .
H35A H 1.0451 0.6944 0.4616 0.109 Uiso 1 1 calc GR . . . .
H35B H 1.1235 0.6655 0.4054 0.109 Uiso 1 1 calc GR . . . .
H35C H 1.0954 0.6015 0.4634 0.109 Uiso 1 1 calc GR . . . .
C36 C 0.8614(2) 0.5148(3) 0.41906(16) 0.0663(9) Uani 1 1 d . . . . .
H36A H 0.7895 0.4627 0.3852 0.099 Uiso 1 1 calc GR . . . .
H36B H 0.8387 0.5681 0.4496 0.099 Uiso 1 1 calc GR . . . .
H36C H 0.9031 0.4835 0.4513 0.099 Uiso 1 1 calc GR . . . .
C37 C 0.63078(16) 0.63628(15) 0.40764(10) 0.0290(4) Uani 1 1 d . . . . .
C38 C 0.6279(2) 0.75361(17) 0.51121(11) 0.0383(5) Uani 1 1 d . . . . .
C39 C 0.51385(19) 0.68596(16) 0.48272(11) 0.0347(4) Uani 1 1 d . . . . .
C40 C 0.8332(2) 0.7708(2) 0.47684(12) 0.0517(6) Uani 1 1 d . . . . .
H40 H 0.8595 0.7237 0.4410 0.062 Uiso 1 1 calc R . . . .
C41 C 0.8629(3) 0.8735(2) 0.45711(16) 0.0752(9) Uani 1 1 d . . . . .
H41A H 0.8381 0.9221 0.4908 0.113 Uiso 1 1 calc GR . . . .
H41B H 0.8201 0.8628 0.4058 0.113 Uiso 1 1 calc GR . . . .
H41C H 0.9491 0.9007 0.4622 0.113 Uiso 1 1 calc GR . . . .
C42 C 0.9030(2) 0.7790(3) 0.55656(14) 0.0746(9) Uani 1 1 d . . . . .
H42A H 0.8725 0.7145 0.5684 0.112 Uiso 1 1 calc GR . . . .
H42B H 0.8920 0.8340 0.5929 0.112 Uiso 1 1 calc GR . . . .
H42C H 0.9883 0.7935 0.5583 0.112 Uiso 1 1 calc GR . . . .
C43 C 0.40791(17) 0.53014(16) 0.36507(11) 0.0326(4) Uani 1 1 d . . . . .
H43 H 0.4384 0.4915 0.3265 0.039 Uiso 1 1 calc R . . . .
C44 C 0.32197(19) 0.57543(19) 0.32398(13) 0.0440(5) Uani 1 1 d . . . . .
H44A H 0.3671 0.6255 0.3025 0.066 Uiso 1 1 calc GR . . . .
H44B H 0.2842 0.6087 0.3592 0.066 Uiso 1 1 calc GR . . . .
H44C H 0.2602 0.5207 0.2843 0.066 Uiso 1 1 calc GR . . . .
C45 C 0.3455(2) 0.4532(2) 0.40400(15) 0.0535(6) Uani 1 1 d . . . . .
H45A H 0.3090 0.4868 0.4398 0.080 Uiso 1 1 calc GR . . . .
H45B H 0.4046 0.4287 0.4300 0.080 Uiso 1 1 calc GR . . . .
H45C H 0.2835 0.3955 0.3668 0.080 Uiso 1 1 calc GR . . . .
C46 C 0.4066(2) 0.6823(2) 0.51646(13) 0.0488(6) Uani 1 1 d . . . . .
H46A H 0.3993 0.6334 0.5459 0.073 Uiso 1 1 calc GR . . . .
H46B H 0.3337 0.6611 0.4766 0.073 Uiso 1 1 calc GR . . . .
H46C H 0.4178 0.7500 0.5485 0.073 Uiso 1 1 calc GR . . . .
C47 C 0.6713(3) 0.8443(2) 0.58068(13) 0.0553(6) Uani 1 1 d . . . . .
H47A H 0.7328 0.9000 0.5731 0.083 Uiso 1 1 calc GR . . . .
H47B H 0.7050 0.8239 0.6233 0.083 Uiso 1 1 calc GR . . . .
H47C H 0.6040 0.8672 0.5903 0.083 Uiso 1 1 calc GR . . . .
B1 B 0.6529(2) 0.3404(2) 0.20961(13) 0.0363(5) Uani 1 1 d . . . . .
B2 B 0.67342(19) 0.57533(18) 0.33835(11) 0.0294(5) Uani 1 1 d . . . . .
C48A C 0.2394(5) 0.2758(4) 0.2012(3) 0.0604(12) Uani 0.748(5) 1 d D U P B 4
H48A H 0.2760 0.2486 0.2365 0.073 Uiso 0.748(5) 1 calc R . P B 4
C48B C 0.2805(18) 0.2983(14) 0.1766(10) 0.062(3) Uani 0.252(5) 1 d . U P B 3
H48B H 0.3641 0.3184 0.1806 0.074 Uiso 0.252(5) 1 calc R . P B 3
C49A C 0.3087(4) 0.3310(4) 0.1630(3) 0.0675(14) Uani 0.748(5) 1 d D U P B 4
H49A H 0.3920 0.3409 0.1726 0.081 Uiso 0.748(5) 1 calc R . P B 4
C49B C 0.2324(17) 0.2455(14) 0.2224(9) 0.070(3) Uani 0.252(5) 1 d . U P B 3
H49B H 0.2832 0.2223 0.2533 0.084 Uiso 0.252(5) 1 calc R . P B 3
C50A C 0.2576(5) 0.3720(4) 0.1111(3) 0.0815(13) Uani 0.748(5) 1 d D U P B 4
H50A H 0.3053 0.4084 0.0846 0.098 Uiso 0.748(5) 1 calc R . P B 4
C50B C 0.1235(15) 0.2256(12) 0.2260(9) 0.077(3) Uani 0.252(5) 1 d . U P B 3
H50B H 0.0965 0.1922 0.2610 0.093 Uiso 0.252(5) 1 calc R . P B 3
C51A C 0.1362(5) 0.3592(4) 0.0982(3) 0.0875(14) Uani 0.748(5) 1 d D U P B 4
H51A H 0.1007 0.3876 0.0633 0.105 Uiso 0.748(5) 1 calc R . P B 4
C51B C 0.0396(16) 0.2549(12) 0.1753(9) 0.079(3) Uani 0.252(5) 1 d . U P B 3
H51B H -0.0397 0.2469 0.1799 0.095 Uiso 0.252(5) 1 calc R . P B 3
C52A C 0.084(2) 0.297(2) 0.1180(12) 0.071(3) Uani 0.252(5) 1 d . U P B 3
H52A H 0.0301 0.3048 0.0788 0.085 Uiso 0.252(5) 1 calc R . P B 3
C52B C 0.0652(6) 0.3032(6) 0.1378(3) 0.0699(16) Uani 0.748(5) 1 d D U P B 4
H52B H -0.0175 0.2957 0.1294 0.084 Uiso 0.748(5) 1 calc R . P B 4
C53A C 0.1144(4) 0.2597(3) 0.1880(2) 0.0616(10) Uani 0.748(5) 1 d D U P B 4
C53B C 0.2018(13) 0.3230(11) 0.1219(7) 0.065(2) Uani 0.252(5) 1 d . U P B 3
C54A C 0.0391(5) 0.2012(5) 0.2298(3) 0.0955(16) Uani 0.748(5) 1 d . U P B 4
H54A H 0.0676 0.1450 0.2373 0.143 Uiso 0.748(5) 1 calc GR . P B 4
H54B H -0.0444 0.1738 0.2012 0.143 Uiso 0.748(5) 1 calc GR . P B 4
H54C H 0.0451 0.2467 0.2781 0.143 Uiso 0.748(5) 1 calc GR . P B 4
C54B C 0.2497(13) 0.3667(12) 0.0584(10) 0.086(4) Uani 0.252(5) 1 d . U P B 3
H54D H 0.3278 0.4195 0.0801 0.128 Uiso 0.252(5) 1 calc GR . P B 3
H54E H 0.1931 0.3960 0.0354 0.128 Uiso 0.252(5) 1 calc GR . P B 3
H54F H 0.2575 0.3114 0.0206 0.128 Uiso 0.252(5) 1 calc GR . P B 3
C55 C 0.4676(11) 1.0383(8) 0.5528(6) 0.080(3) Uani 0.5 1 d D U P C -1
H55 H 0.4235 1.0567 0.5874 0.095 Uiso 0.5 1 calc R . P C -1
C56 C 0.5905(12) 1.1015(8) 0.5713(7) 0.110(3) Uani 0.5 1 d D U P C -1
H56 H 0.6296 1.1548 0.6158 0.132 Uiso 0.5 1 calc R . P C -1
C57 C 0.6465(14) 1.0712(11) 0.5109(8) 0.116(3) Uani 0.5 1 d D U P C -1
H57 H 0.7260 1.1099 0.5133 0.139 Uiso 0.5 1 calc R . P C -1
C58 C 0.5855(10) 0.9879(9) 0.4513(6) 0.079(2) Uani 0.5 1 d D U P C -1
H58 H 0.6264 0.9693 0.4149 0.095 Uiso 0.5 1 calc R . P C -1
C59 C 0.4657(12) 0.9280(11) 0.4409(7) 0.093(3) Uani 0.5 1 d D U P C -1
H59 H 0.4269 0.8700 0.3994 0.111 Uiso 0.5 1 calc R . P C -1
C60 C 0.4060(10) 0.9585(8) 0.4953(7) 0.101(3) Uani 0.5 1 d D U P C -1
C61 C 0.2754(11) 0.8910(8) 0.4652(9) 0.174(5) Uani 0.5 1 d D U P C -1
H61A H 0.2396 0.9081 0.4214 0.261 Uiso 0.5 1 calc GR . P C -1
H61B H 0.2316 0.9022 0.5035 0.261 Uiso 0.5 1 calc GR . P C -1
H61C H 0.2712 0.8194 0.4512 0.261 Uiso 0.5 1 calc GR . P C -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 N2 1.351(2) . ?
N1 B1 1.236(3) . ?
N2 B2 1.368(3) . ?
N3 C37 1.360(3) . ?
N3 C38 1.387(3) . ?
N3 C40 1.487(3) . ?
N4 C37 1.360(2) . ?
N4 C39 1.390(2) . ?
N4 C43 1.492(2) . ?
C1 C2 1.421(3) . ?
C1 C6 1.418(3) . ?
C1 B1 1.538(3) . ?
C2 C3 1.396(3) . ?
C2 C13 1.550(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(3) . ?
C4 C5 1.389(3) . ?
C4 C17 1.537(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.388(3) . ?
C6 C21 1.554(3) . ?
C7 C8 1.416(3) . ?
C7 C12 1.440(3) . ?
C7 B2 1.613(3) . ?
C8 C9 1.402(3) . ?
C8 C33 1.563(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.372(3) . ?
C10 C11 1.386(3) . ?
C10 C29 1.537(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.386(3) . ?
C12 C25 1.557(3) . ?
C13 C14 1.532(3) . ?
C13 C15 1.529(3) . ?
C13 C16 1.538(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.526(3) . ?
C17 C19 1.517(3) . ?
C17 C20 1.534(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.541(4) . ?
C21 C23 1.535(4) . ?
C21 C24A 1.546(12) . ?
C21 C24B 1.573(9) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?
C25 C26 1.545(3) . ?
C25 C27 1.532(3) . ?
C25 C28 1.528(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.528(4) . ?
C29 C31 1.529(4) . ?
C29 C32 1.526(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.535(4) . ?
C33 C35 1.544(4) . ?
C33 C36 1.546(3) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 B2 1.618(3) . ?
C38 C39 1.347(3) . ?
C38 C47 1.497(3) . ?
C39 C46 1.497(3) . ?
C40 H40 0.9800 . ?
C40 C41 1.519(4) . ?
C40 C42 1.535(3) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43 0.9800 . ?
C43 C44 1.517(3) . ?
C43 C45 1.518(3) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48A H48A 0.9300 . ?
C48A C49A 1.362(6) . ?
C48A C53A 1.395(6) . ?
C48B H48B 0.9300 . ?
C48B C49B 1.34(2) . ?
C48B C53B 1.42(2) . ?
C49A H49A 0.9300 . ?
C49A C50A 1.363(7) . ?
C49B H49B 0.9300 . ?
C49B C50B 1.25(2) . ?
C50A H50A 0.9300 . ?
C50A C51A 1.361(6) . ?
C50B H50B 0.9300 . ?
C50B C51B 1.45(2) . ?
C51A H51A 0.9300 . ?
C51A C52B 1.398(8) . ?
C51B H51B 0.9300 . ?
C51B C52A 1.43(3) . ?
C52A H52A 0.9300 . ?
C52A C53B 1.32(3) . ?
C52B H52B 0.9300 . ?
C52B C53A 1.355(8) . ?
C53A C54A 1.474(7) . ?
C53B C54B 1.56(2) . ?
C54A H54A 0.9600 . ?
C54A H54B 0.9600 . ?
C54A H54C 0.9600 . ?
C54B H54D 0.9600 . ?
C54B H54E 0.9600 . ?
C54B H54F 0.9600 . ?
C55 H55 0.9300 . ?
C55 C56 1.408(12) . ?
C55 C60 1.298(14) . ?
C56 H56 0.9300 . ?
C56 C57 1.442(19) . ?
C57 H57 0.9300 . ?
C57 C58 1.344(14) . ?
C58 H58 0.9300 . ?
C58 C59 1.382(15) . ?
C59 H59 0.9300 . ?
C59 C60 1.385(14) . ?
C60 C61 1.497(12) . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?

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
B1 N1 N2 169.24(19) . . ?
N1 N2 B2 119.38(16) . . ?
C37 N3 C38 110.20(16) . . ?
C37 N3 C40 123.48(18) . . ?
C38 N3 C40 126.29(18) . . ?
C37 N4 C39 110.15(16) . . ?
C37 N4 C43 123.86(15) . . ?
C39 N4 C43 125.75(15) . . ?
C2 C1 B1 121.81(18) . . ?
C6 C1 C2 118.73(19) . . ?
C6 C1 B1 119.46(17) . . ?
C1 C2 C13 121.62(18) . . ?
C3 C2 C1 118.93(17) . . ?
C3 C2 C13 119.45(16) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 C2 123.01(18) . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C5 117.03(19) . . ?
C3 C4 C17 123.47(17) . . ?
C5 C4 C17 119.48(18) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 C4 123.17(19) . . ?
C6 C5 H5 118.4 . . ?
C1 C6 C21 122.08(19) . . ?
C5 C6 C1 119.10(18) . . ?
C5 C6 C21 118.82(18) . . ?
C8 C7 C12 117.02(16) . . ?
C8 C7 B2 121.25(16) . . ?
C12 C7 B2 121.57(16) . . ?
C7 C8 C33 128.24(17) . . ?
C9 C8 C7 119.94(17) . . ?
C9 C8 C33 111.82(17) . . ?
C8 C9 H9 118.4 . . ?
C10 C9 C8 123.30(19) . . ?
C10 C9 H9 118.4 . . ?
C9 C10 C11 116.58(18) . . ?
C9 C10 C29 123.36(19) . . ?
C11 C10 C29 120.05(18) . . ?
C10 C11 H11 118.1 . . ?
C10 C11 C12 123.77(17) . . ?
C12 C11 H11 118.1 . . ?
C7 C12 C25 124.10(16) . . ?
C11 C12 C7 119.27(17) . . ?
C11 C12 C25 116.60(16) . . ?
C14 C13 C2 109.37(17) . . ?
C14 C13 C16 106.92(18) . . ?
C15 C13 C2 111.10(17) . . ?
C15 C13 C14 110.12(18) . . ?
C15 C13 C16 106.98(18) . . ?
C16 C13 C2 112.24(17) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C4 108.66(18) . . ?
C18 C17 C20 108.7(2) . . ?
C19 C17 C4 112.56(17) . . ?
C19 C17 C18 109.4(2) . . ?
C19 C17 C20 107.5(2) . . ?
C20 C17 C4 110.0(2) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C6 C21 C24B 110.1(6) . . ?
C22 C21 C6 110.9(2) . . ?
C22 C21 C24A 116.2(12) . . ?
C22 C21 C24B 99.8(8) . . ?
C23 C21 C6 109.7(2) . . ?
C23 C21 C22 110.3(2) . . ?
C23 C21 C24A 96.3(12) . . ?
C23 C21 C24B 115.7(10) . . ?
C24A C21 C6 112.5(8) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24A H24A 109.5 . . ?
C21 C24A H24B 109.5 . . ?
C21 C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C21 C24B H24D 109.5 . . ?
C21 C24B H24E 109.5 . . ?
C21 C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C26 C25 C12 112.32(16) . . ?
C27 C25 C12 111.66(16) . . ?
C27 C25 C26 105.13(16) . . ?
C28 C25 C12 111.23(16) . . ?
C28 C25 C26 105.66(17) . . ?
C28 C25 C27 110.52(17) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C10 108.8(2) . . ?
C30 C29 C31 108.9(2) . . ?
C31 C29 C10 109.1(2) . . ?
C32 C29 C10 112.14(19) . . ?
C32 C29 C30 110.9(3) . . ?
C32 C29 C31 107.0(2) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C8 108.5(2) . . ?
C34 C33 C35 109.7(2) . . ?
C34 C33 C36 106.7(2) . . ?
C35 C33 C8 108.6(2) . . ?
C35 C33 C36 105.8(2) . . ?
C36 C33 C8 117.31(18) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N3 C37 N4 105.41(16) . . ?
N3 C37 B2 127.84(16) . . ?
N4 C37 B2 126.71(17) . . ?
N3 C38 C47 125.8(2) . . ?
C39 C38 N3 107.19(17) . . ?
C39 C38 C47 126.9(2) . . ?
N4 C39 C46 125.73(19) . . ?
C38 C39 N4 107.04(17) . . ?
C38 C39 C46 127.04(19) . . ?
N3 C40 H40 106.7 . . ?
N3 C40 C41 111.6(2) . . ?
N3 C40 C42 111.37(18) . . ?
C41 C40 H40 106.7 . . ?
C41 C40 C42 113.4(2) . . ?
C42 C40 H40 106.7 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 H43 106.8 . . ?
N4 C43 C44 111.12(17) . . ?
N4 C43 C45 111.59(16) . . ?
C44 C43 H43 106.8 . . ?
C44 C43 C45 113.31(18) . . ?
C45 C43 H43 106.8 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C39 C46 H46A 109.5 . . ?
C39 C46 H46B 109.5 . . ?
C39 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C38 C47 H47A 109.5 . . ?
C38 C47 H47B 109.5 . . ?
C38 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N1 B1 C1 176.0(2) . . ?
N2 B2 C7 125.26(18) . . ?
N2 B2 C37 112.80(16) . . ?
C7 B2 C37 121.94(18) . . ?
C49A C48A H48A 119.6 . . ?
C49A C48A C53A 120.8(5) . . ?
C53A C48A H48A 119.6 . . ?
C49B C48B H48B 120.5 . . ?
C49B C48B C53B 119.0(18) . . ?
C53B C48B H48B 120.5 . . ?
C48A C49A H49A 119.6 . . ?
C48A C49A C50A 120.9(5) . . ?
C50A C49A H49A 119.6 . . ?
C48B C49B H49B 118.0 . . ?
C50B C49B C48B 124.1(19) . . ?
C50B C49B H49B 118.0 . . ?
C49A C50A H50A 120.3 . . ?
C51A C50A C49A 119.5(5) . . ?
C51A C50A H50A 120.3 . . ?
C49B C50B H50B 120.2 . . ?
C49B C50B C51B 119.6(19) . . ?
C51B C50B H50B 120.2 . . ?
C50A C51A H51A 120.2 . . ?
C50A C51A C52B 119.7(5) . . ?
C52B C51A H51A 120.2 . . ?
C50B C51B H51B 121.3 . . ?
C52A C51B C50B 117.4(19) . . ?
C52A C51B H51B 121.3 . . ?
C51B C52A H52A 120.6 . . ?
C53B C52A C51B 119(2) . . ?
C53B C52A H52A 120.6 . . ?
C51A C52B H52B 119.3 . . ?
C53A C52B C51A 121.3(5) . . ?
C53A C52B H52B 119.3 . . ?
C48A C53A C54A 121.1(5) . . ?
C52B C53A C48A 117.8(5) . . ?
C52B C53A C54A 121.0(5) . . ?
C48B C53B C54B 120.7(14) . . ?
C52A C53B C48B 120.0(18) . . ?
C52A C53B C54B 118.7(15) . . ?
C53A C54A H54A 109.5 . . ?
C53A C54A H54B 109.5 . . ?
C53A C54A H54C 109.5 . . ?
H54A C54A H54B 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C53B C54B H54D 109.5 . . ?
C53B C54B H54E 109.5 . . ?
C53B C54B H54F 109.5 . . ?
H54D C54B H54E 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C56 C55 H55 114.8 . . ?
C60 C55 H55 114.8 . . ?
C60 C55 C56 130.3(12) . . ?
C55 C56 H56 125.1 . . ?
C55 C56 C57 109.8(11) . . ?
C57 C56 H56 125.1 . . ?
C56 C57 H57 119.6 . . ?
C58 C57 C56 120.9(12) . . ?
C58 C57 H57 119.6 . . ?
C57 C58 H58 118.0 . . ?
C57 C58 C59 124.1(12) . . ?
C59 C58 H58 118.0 . . ?
C58 C59 H59 121.6 . . ?
C58 C59 C60 116.8(11) . . ?
C60 C59 H59 121.6 . . ?
C55 C60 C59 117.8(10) . . ?
C55 C60 C61 136.0(12) . . ?
C59 C60 C61 105.8(11) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?

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 N2 B2 C7 2.3(3) . . . . ?
N1 N2 B2 C37 -178.14(15) . . . . ?
N3 C37 B2 N2 149.95(18) . . . . ?
N3 C37 B2 C7 -30.4(3) . . . . ?
N3 C38 C39 N4 -0.7(2) . . . . ?
N3 C38 C39 C46 174.4(2) . . . . ?
N4 C37 B2 N2 -32.7(3) . . . . ?
N4 C37 B2 C7 146.94(18) . . . . ?
C1 C2 C3 C4 0.8(3) . . . . ?
C1 C2 C13 C14 -60.7(3) . . . . ?
C1 C2 C13 C15 61.0(3) . . . . ?
C1 C2 C13 C16 -179.2(2) . . . . ?
C1 C6 C21 C22 55.6(3) . . . . ?
C1 C6 C21 C23 -66.5(3) . . . . ?
C1 C6 C21 C24A -172.3(14) . . . . ?
C1 C6 C21 C24B 165.2(10) . . . . ?
C2 C1 C6 C5 2.0(3) . . . . ?
C2 C1 C6 C21 -178.5(2) . . . . ?
C2 C3 C4 C5 0.6(3) . . . . ?
C2 C3 C4 C17 178.9(2) . . . . ?
C3 C2 C13 C14 118.1(2) . . . . ?
C3 C2 C13 C15 -120.2(2) . . . . ?
C3 C2 C13 C16 -0.4(3) . . . . ?
C3 C4 C5 C6 -0.7(3) . . . . ?
C3 C4 C17 C18 -117.8(2) . . . . ?
C3 C4 C17 C19 3.5(3) . . . . ?
C3 C4 C17 C20 123.4(2) . . . . ?
C4 C5 C6 C1 -0.6(4) . . . . ?
C4 C5 C6 C21 179.8(2) . . . . ?
C5 C4 C17 C18 60.5(3) . . . . ?
C5 C4 C17 C19 -178.2(2) . . . . ?
C5 C4 C17 C20 -58.3(3) . . . . ?
C5 C6 C21 C22 -124.8(2) . . . . ?
C5 C6 C21 C23 113.1(3) . . . . ?
C5 C6 C21 C24A 7.2(14) . . . . ?
C5 C6 C21 C24B -15.3(11) . . . . ?
C6 C1 C2 C3 -2.1(3) . . . . ?
C6 C1 C2 C13 176.7(2) . . . . ?
C7 C8 C9 C10 2.1(4) . . . . ?
C7 C8 C33 C34 115.5(3) . . . . ?
C7 C8 C33 C35 -125.3(3) . . . . ?
C7 C8 C33 C36 -5.5(4) . . . . ?
C7 C12 C25 C26 -172.39(19) . . . . ?
C7 C12 C25 C27 69.8(2) . . . . ?
C7 C12 C25 C28 -54.2(2) . . . . ?
C8 C7 C12 C11 -3.4(3) . . . . ?
C8 C7 C12 C25 174.41(19) . . . . ?
C8 C7 B2 N2 -75.1(3) . . . . ?
C8 C7 B2 C37 105.4(2) . . . . ?
C8 C9 C10 C11 -2.3(4) . . . . ?
C8 C9 C10 C29 178.9(2) . . . . ?
C9 C8 C33 C34 -64.1(3) . . . . ?
C9 C8 C33 C35 55.1(3) . . . . ?
C9 C8 C33 C36 174.9(3) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
C9 C10 C29 C30 -118.5(3) . . . . ?
C9 C10 C29 C31 122.8(3) . . . . ?
C9 C10 C29 C32 4.5(4) . . . . ?
C10 C11 C12 C7 3.3(3) . . . . ?
C10 C11 C12 C25 -174.67(19) . . . . ?
C11 C10 C29 C30 62.7(3) . . . . ?
C11 C10 C29 C31 -55.9(3) . . . . ?
C11 C10 C29 C32 -174.2(3) . . . . ?
C11 C12 C25 C26 5.5(3) . . . . ?
C11 C12 C25 C27 -112.3(2) . . . . ?
C11 C12 C25 C28 123.7(2) . . . . ?
C12 C7 C8 C9 0.9(3) . . . . ?
C12 C7 C8 C33 -178.7(2) . . . . ?
C12 C7 B2 N2 100.2(2) . . . . ?
C12 C7 B2 C37 -79.4(2) . . . . ?
C13 C2 C3 C4 -178.00(19) . . . . ?
C17 C4 C5 C6 -179.1(2) . . . . ?
C29 C10 C11 C12 178.4(2) . . . . ?
C33 C8 C9 C10 -178.3(2) . . . . ?
C37 N3 C38 C39 0.9(2) . . . . ?
C37 N3 C38 C47 179.3(2) . . . . ?
C37 N3 C40 C41 108.0(2) . . . . ?
C37 N3 C40 C42 -124.2(2) . . . . ?
C37 N4 C39 C38 0.3(2) . . . . ?
C37 N4 C39 C46 -175.0(2) . . . . ?
C37 N4 C43 C44 -108.9(2) . . . . ?
C37 N4 C43 C45 123.6(2) . . . . ?
C38 N3 C37 N4 -0.7(2) . . . . ?
C38 N3 C37 B2 177.09(17) . . . . ?
C38 N3 C40 C41 -74.2(3) . . . . ?
C38 N3 C40 C42 53.5(3) . . . . ?
C39 N4 C37 N3 0.3(2) . . . . ?
C39 N4 C37 B2 -177.59(17) . . . . ?
C39 N4 C43 C44 64.9(2) . . . . ?
C39 N4 C43 C45 -62.6(2) . . . . ?
C40 N3 C37 N4 177.36(18) . . . . ?
C40 N3 C37 B2 -4.8(3) . . . . ?
C40 N3 C38 C39 -177.10(19) . . . . ?
C40 N3 C38 C47 1.3(3) . . . . ?
C43 N4 C37 N3 174.94(16) . . . . ?
C43 N4 C37 B2 -2.9(3) . . . . ?
C43 N4 C39 C38 -174.25(17) . . . . ?
C43 N4 C39 C46 10.5(3) . . . . ?
C47 C38 C39 N4 -179.1(2) . . . . ?
C47 C38 C39 C46 -3.9(4) . . . . ?
B1 N1 N2 B2 159.2(10) . . . . ?
B1 C1 C2 C3 178.20(19) . . . . ?
B1 C1 C2 C13 -3.0(3) . . . . ?
B1 C1 C6 C5 -178.3(2) . . . . ?
B1 C1 C6 C21 1.2(3) . . . . ?
B2 C7 C8 C9 176.3(2) . . . . ?
B2 C7 C8 C33 -3.3(4) . . . . ?
B2 C7 C12 C11 -178.82(19) . . . . ?
B2 C7 C12 C25 -1.0(3) . . . . ?
C48A C49A C50A C51A 1.2(8) . . . . ?
C48B C49B C50B C51B 4(3) . . . . ?
C49A C48A C53A C52B -1.8(7) . . . . ?
C49A C48A C53A C54A -179.2(5) . . . . ?
C49A C50A C51A C52B -0.8(8) . . . . ?
C49B C48B C53B C52A 2(3) . . . . ?
C49B C48B C53B C54B -169.2(15) . . . . ?
C49B C50B C51B C52A 6(2) . . . . ?
C50A C51A C52B C53A -1.0(9) . . . . ?
C50B C51B C52A C53B -12(3) . . . . ?
C51A C52B C53A C48A 2.3(8) . . . . ?
C51A C52B C53A C54A 179.7(5) . . . . ?
C51B C52A C53B C48B 8(3) . . . . ?
C51B C52A C53B C54B 178.9(15) . . . . ?
C53A C48A C49A C50A 0.1(7) . . . . ?
C53B C48B C49B C50B -8(3) . . . . ?
C55 C56 C57 C58 -5.3(16) . . . . ?
C56 C55 C60 C59 -1.1(19) . . . . ?
C56 C55 C60 C61 -173.4(13) . . . . ?
C56 C57 C58 C59 2.9(17) . . . . ?
C57 C58 C59 C60 1.3(16) . . . . ?
C58 C59 C60 C55 -2.2(17) . . . . ?
C58 C59 C60 C61 172.3(9) . . . . ?
C60 C55 C56 C57 4.7(17) . . . . ?

_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 1.335
_oxdiff_exptl_absorpt_empirical_full_min 0.444
####################################################################### 
# 
# 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_klb-4
_database_code_depnum_ccdc_archive 'CCDC 1977881'
loop_
_audit_author_name
_audit_author_address
'Lingbing Kong'
;Shandong University
China
;
_audit_update_record             
;
2020-05-25 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_audit_creation_date             2020-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C59 H70 B2 N4, C7 H8'
_chemical_formula_sum            'C66 H78 B2 N4'
_chemical_formula_weight         948.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         CBNBr
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.75034(11)
_cell_length_b                   23.8044(3)
_cell_length_c                   19.95734(18)
_cell_angle_alpha                90
_cell_angle_beta                 98.1553(9)
_cell_angle_gamma                90
_cell_volume                     5525.81(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14527
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.0010
_cell_measurement_theta_min      2.8590
_shelx_estimated_absorpt_T_max   0.908
_shelx_estimated_absorpt_T_min   0.792
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.19a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31156
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         2.907
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  24.00   1.00    0.11    --  -48.45  58.00 133.00   87
  2  ω    -10.00  43.00   1.00    0.11    --   48.45 -58.00  -7.00   53
  3  ω     83.00 110.00   1.00    0.11    --   48.45  58.00 133.00   27
  4  ω    -94.00 -62.00   1.00    0.90    --  -86.25  58.00 133.00   32
  5  ω   -139.00-114.00   1.00    0.90    --  -86.25 -58.00  -7.00   25
  6  ω    -50.00 -23.00   1.00    0.90    --  -86.25  58.00 133.00   27
  7  ω     91.00 178.00   1.00    0.90    --  106.49  58.00 133.00   87
  8  ω     36.00 122.00   1.00    0.90    --  106.49 -58.00  -7.00   86
  9  ω   -120.00 -78.00   1.00    0.11    --  -48.45-125.00 150.00   42
 10  ω   -119.00 -34.00   1.00    0.11    --  -48.45 -58.00  -7.00   85
 11  ω     34.00  92.00   1.00    0.90    --  106.49 -94.00 -60.00   58
 12  ω     34.00 108.00   1.00    0.90    --  106.49 -94.00 -30.00   74
 13  ω     93.00 178.00   1.00    0.90    --  106.49  15.00 -90.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0864826000
_diffrn_orient_matrix_UB_12      -0.0203941000
_diffrn_orient_matrix_UB_13      -0.0603788000
_diffrn_orient_matrix_UB_21      -0.0552750000
_diffrn_orient_matrix_UB_22      -0.0394808000
_diffrn_orient_matrix_UB_23      0.0474448000
_diffrn_orient_matrix_UB_31      -0.0836086000
_diffrn_orient_matrix_UB_32      0.0471071000
_diffrn_orient_matrix_UB_33      0.0136757000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8200
_reflns_number_total             9650
_reflns_odcompleteness_completeness 95.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.19a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         9650
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0440
_refine_ls_restrained_S_all      1.019
_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)+(0.0588P)²+2.0949P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1211
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C35(H35), C52(H52), C55(H55)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C28(H28), C29(H29), C33(H33), C20(H20), C44(H44), C3(H3), C5(H5),
 C18(H18), C9(H9), C4(H4), C11(H11), C42(H42), C61(H61), C65(H65), C64(H64),
 C63(H63), C62(H62)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C22(H22A,H22B,H22C), C39(H39A,H39B,H39C), C53(H53A,H53B,
 H53C), C24(H24A,H24B,H24C), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C13(H13A,H13B,H13C),
 C59(H59A,H59B,H59C), C38(H38A,H38B,H38C), C23(H23A,H23B,H23C), C15(H15A,H15B,
 H15C), C14(H14A,H14B,H14C), C57(H57A,H57B,H57C), C48(H48A,H48B,H48C), C66(H66A,
 H66B,H66C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N 0.60317(9) 0.68893(5) 0.65884(6) 0.0208(2) Uani 1 1 d . . . . .
N1 N 0.56262(10) 0.74379(5) 0.64341(6) 0.0230(3) Uani 1 1 d . . . . .
N3 N 0.33304(10) 0.67493(5) 0.70390(6) 0.0244(3) Uani 1 1 d . . . . .
N4 N 0.34077(10) 0.64268(5) 0.60356(6) 0.0257(3) Uani 1 1 d . . . . .
C30 C 0.68680(12) 0.57678(6) 0.64171(7) 0.0246(3) Uani 1 1 d . . . . .
C49 C 0.40368(12) 0.65229(6) 0.66423(7) 0.0218(3) Uani 1 1 d . . . . .
C26 C 0.56823(12) 0.53781(6) 0.72010(7) 0.0246(3) Uani 1 1 d . . . . .
C25 C 0.59870(11) 0.58426(6) 0.68292(7) 0.0226(3) Uani 1 1 d . . . . .
C35 C 0.75986(12) 0.73523(6) 0.61304(7) 0.0232(3) Uani 1 1 d . . . . .
H35 H 0.8254 0.7524 0.6416 0.028 Uiso 1 1 calc R . . . .
C31 C 0.72507(12) 0.62701(6) 0.60677(7) 0.0240(3) Uani 1 1 d . . . . .
C40 C 0.48932(12) 0.54014(6) 0.77326(7) 0.0254(3) Uani 1 1 d . . . . .
C36 C 0.72796(11) 0.68069(6) 0.64824(7) 0.0219(3) Uani 1 1 d . . . . .
C1 C 0.63565(12) 0.84030(6) 0.60338(7) 0.0243(3) Uani 1 1 d . . . . .
C2 C 0.72051(13) 0.87830(6) 0.63463(7) 0.0266(3) Uani 1 1 d . . . . .
C16 C 0.82283(13) 0.86002(6) 0.68360(7) 0.0257(3) Uani 1 1 d . . . . .
C6 C 0.54096(13) 0.86460(6) 0.56161(7) 0.0278(3) Uani 1 1 d . . . . .
C21 C 0.80774(13) 0.83883(6) 0.74770(8) 0.0272(3) Uani 1 1 d . . . . .
C27 C 0.61897(13) 0.48543(6) 0.71275(8) 0.0290(3) Uani 1 1 d . . . . .
H27 H 0.5964 0.4547 0.7364 0.035 Uiso 1 1 calc R . . . .
C28 C 0.70192(13) 0.47860(6) 0.67097(8) 0.0311(3) Uani 1 1 d . . . . .
H28 H 0.7340 0.4434 0.6659 0.037 Uiso 1 1 calc R . . . .
C7 C 0.44015(13) 0.83267(6) 0.52529(8) 0.0283(3) Uani 1 1 d . . . . .
C50 C 0.22349(12) 0.68134(7) 0.66732(8) 0.0309(3) Uani 1 1 d . . . . .
C34 C 0.79165(13) 0.72817(6) 0.54367(8) 0.0279(3) Uani 1 1 d . . . . .
C29 C 0.73704(13) 0.52450(6) 0.63659(8) 0.0291(3) Uani 1 1 d . . . . .
H29 H 0.7950 0.5202 0.6097 0.035 Uiso 1 1 calc R . . . .
C52 C 0.37435(13) 0.69126(7) 0.77493(7) 0.0285(3) Uani 1 1 d . . . . .
H52 H 0.4501 0.6739 0.7870 0.034 Uiso 1 1 calc R . . . .
C45 C 0.53182(13) 0.56019(6) 0.83818(8) 0.0298(3) Uani 1 1 d . . . . .
C17 C 0.93561(13) 0.86964(6) 0.66933(8) 0.0294(3) Uani 1 1 d . . . . .
C37 C 0.80159(12) 0.67545(6) 0.71756(8) 0.0274(3) Uani 1 1 d . . . . .
H37A H 0.7948 0.7092 0.7431 0.041 Uiso 1 1 calc GR . . . .
H37B H 0.8805 0.6700 0.7117 0.041 Uiso 1 1 calc GR . . . .
H37C H 0.7757 0.6440 0.7414 0.041 Uiso 1 1 calc GR . . . .
C32 C 0.74223(14) 0.62767(6) 0.54140(8) 0.0308(3) Uani 1 1 d . . . . .
C33 C 0.78042(14) 0.67897(7) 0.51136(8) 0.0328(3) Uani 1 1 d . . . . .
H33 H 0.7979 0.6773 0.4674 0.039 Uiso 1 1 calc R . . . .
C41 C 0.38100(13) 0.51447(7) 0.76184(8) 0.0301(3) Uani 1 1 d . . . . .
C20 C 0.90406(14) 0.82657(6) 0.79450(8) 0.0326(3) Uani 1 1 d . . . . .
H20 H 0.8934 0.8121 0.8364 0.039 Uiso 1 1 calc R . . . .
C8 C 0.43716(14) 0.81739(7) 0.45711(8) 0.0332(3) Uani 1 1 d . . . . .
C55 C 0.39482(14) 0.62115(7) 0.54541(8) 0.0324(3) Uani 1 1 d . . . . .
H55 H 0.4708 0.6068 0.5643 0.039 Uiso 1 1 calc R . . . .
C12 C 0.34123(13) 0.82579(7) 0.55637(8) 0.0322(3) Uani 1 1 d . . . . .
C44 C 0.46487(15) 0.55426(7) 0.89014(8) 0.0362(4) Uani 1 1 d . . . . .
H44 H 0.4929 0.5680 0.9330 0.043 Uiso 1 1 calc R . . . .
C51 C 0.22851(13) 0.66084(7) 0.60463(8) 0.0312(3) Uani 1 1 d . . . . .
C3 C 0.71004(15) 0.93604(7) 0.62395(8) 0.0345(4) Uani 1 1 d . . . . .
H3 H 0.7666 0.9599 0.6452 0.041 Uiso 1 1 calc R . . . .
C5 C 0.53364(15) 0.92270(7) 0.55168(9) 0.0365(4) Uani 1 1 d . . . . .
H5 H 0.4708 0.9375 0.5237 0.044 Uiso 1 1 calc R . . . .
C18 C 1.02855(14) 0.85690(7) 0.71805(9) 0.0347(4) Uani 1 1 d . . . . .
H18 H 1.1025 0.8632 0.7082 0.042 Uiso 1 1 calc R . . . .
C10 C 0.23591(14) 0.79127(7) 0.45085(9) 0.0370(4) Uani 1 1 d . . . . .
C19 C 1.01503(14) 0.83514(7) 0.78102(9) 0.0356(4) Uani 1 1 d . . . . .
C9 C 0.33491(15) 0.79728(7) 0.42122(8) 0.0367(4) Uani 1 1 d . . . . .
H9 H 0.3331 0.7876 0.3759 0.044 Uiso 1 1 calc R . . . .
C4 C 0.61730(16) 0.95844(7) 0.58241(9) 0.0400(4) Uani 1 1 d . . . . .
H4 H 0.6114 0.9970 0.5753 0.048 Uiso 1 1 calc R . . . .
C11 C 0.24125(14) 0.80482(7) 0.51871(9) 0.0377(4) Uani 1 1 d . . . . .
H11 H 0.1763 0.7998 0.5398 0.045 Uiso 1 1 calc R . . . .
C42 C 0.31746(14) 0.50903(7) 0.81559(9) 0.0364(4) Uani 1 1 d . . . . .
H42 H 0.2458 0.4918 0.8080 0.044 Uiso 1 1 calc R . . . .
C22 C 0.69071(14) 0.83202(7) 0.76858(8) 0.0352(4) Uani 1 1 d . . . . .
H22A H 0.6425 0.8627 0.7510 0.053 Uiso 1 1 calc GR . . . .
H22B H 0.6974 0.8317 0.8171 0.053 Uiso 1 1 calc GR . . . .
H22C H 0.6574 0.7973 0.7510 0.053 Uiso 1 1 calc GR . . . .
C39 C 0.84108(15) 0.77843(7) 0.51290(9) 0.0378(4) Uani 1 1 d . . . . .
H39A H 0.7880 0.8092 0.5115 0.057 Uiso 1 1 calc GR . . . .
H39B H 0.8546 0.7695 0.4678 0.057 Uiso 1 1 calc GR . . . .
H39C H 0.9124 0.7887 0.5398 0.057 Uiso 1 1 calc GR . . . .
C53 C 0.39242(15) 0.75418(7) 0.78009(9) 0.0364(4) Uani 1 1 d . . . . .
H53A H 0.4473 0.7654 0.7513 0.055 Uiso 1 1 calc GR . . . .
H53B H 0.4207 0.7641 0.8261 0.055 Uiso 1 1 calc GR . . . .
H53C H 0.3207 0.7730 0.7661 0.055 Uiso 1 1 calc GR . . . .
C43 C 0.35808(15) 0.52862(7) 0.87997(9) 0.0386(4) Uani 1 1 d . . . . .
C24 C 0.95996(16) 0.89672(7) 0.60462(9) 0.0393(4) Uani 1 1 d . . . . .
H24A H 0.8967 0.8900 0.5695 0.059 Uiso 1 1 calc GR . . . .
H24B H 1.0289 0.8810 0.5917 0.059 Uiso 1 1 calc GR . . . .
H24C H 0.9698 0.9364 0.6115 0.059 Uiso 1 1 calc GR . . . .
C47 C 0.33408(15) 0.49136(8) 0.69321(9) 0.0412(4) Uani 1 1 d . . . . .
H47A H 0.3220 0.5216 0.6611 0.062 Uiso 1 1 calc GR . . . .
H47B H 0.2624 0.4727 0.6957 0.062 Uiso 1 1 calc GR . . . .
H47C H 0.3880 0.4651 0.6791 0.062 Uiso 1 1 calc GR . . . .
C46 C 0.65031(15) 0.58539(7) 0.85311(9) 0.0382(4) Uani 1 1 d . . . . .
H46A H 0.7054 0.5600 0.8385 0.057 Uiso 1 1 calc GR . . . .
H46B H 0.6689 0.5918 0.9009 0.057 Uiso 1 1 calc GR . . . .
H46C H 0.6522 0.6204 0.8294 0.057 Uiso 1 1 calc GR . . . .
C54 C 0.29786(16) 0.66802(8) 0.82366(9) 0.0392(4) Uani 1 1 d . . . . .
H54A H 0.2296 0.6905 0.8214 0.059 Uiso 1 1 calc GR . . . .
H54B H 0.3386 0.6689 0.8689 0.059 Uiso 1 1 calc GR . . . .
H54C H 0.2771 0.6300 0.8115 0.059 Uiso 1 1 calc GR . . . .
C56 C 0.41482(18) 0.66839(8) 0.49811(9) 0.0449(4) Uani 1 1 d . . . . .
H56A H 0.3422 0.6818 0.4757 0.067 Uiso 1 1 calc GR . . . .
H56B H 0.4602 0.6550 0.4650 0.067 Uiso 1 1 calc GR . . . .
H56C H 0.4548 0.6984 0.5235 0.067 Uiso 1 1 calc GR . . . .
B2 B 0.53937(13) 0.64367(7) 0.67623(8) 0.0212(3) Uani 1 1 d . . . . .
C58 C 0.12322(14) 0.70718(9) 0.69406(10) 0.0475(5) Uani 1 1 d . . . . .
H58A H 0.0990 0.6831 0.7280 0.071 Uiso 1 1 calc GR . . . .
H58B H 0.0611 0.7120 0.6577 0.071 Uiso 1 1 calc GR . . . .
H58C H 0.1451 0.7431 0.7137 0.071 Uiso 1 1 calc GR . . . .
C13 C 0.34159(16) 0.84225(9) 0.62900(9) 0.0461(4) Uani 1 1 d . . . . .
H13A H 0.4082 0.8267 0.6561 0.069 Uiso 1 1 calc GR . . . .
H13B H 0.2735 0.8281 0.6446 0.069 Uiso 1 1 calc GR . . . .
H13C H 0.3434 0.8824 0.6328 0.069 Uiso 1 1 calc GR . . . .
C59 C 0.13441(16) 0.65781(9) 0.54585(10) 0.0478(5) Uani 1 1 d . . . . .
H59A H 0.1611 0.6731 0.5064 0.072 Uiso 1 1 calc GR . . . .
H59B H 0.0694 0.6790 0.5558 0.072 Uiso 1 1 calc GR . . . .
H59C H 0.1123 0.6193 0.5375 0.072 Uiso 1 1 calc GR . . . .
B1 B 0.64648(14) 0.77441(7) 0.61802(8) 0.0229(3) Uani 1 1 d . . . . .
C38 C 0.7216(2) 0.57770(8) 0.49479(9) 0.0485(5) Uani 1 1 d . . . . .
H38A H 0.7925 0.5578 0.4942 0.073 Uiso 1 1 calc GR . . . .
H38B H 0.6930 0.5903 0.4499 0.073 Uiso 1 1 calc GR . . . .
H38C H 0.6663 0.5532 0.5106 0.073 Uiso 1 1 calc GR . . . .
C23 C 1.11662(17) 0.82329(9) 0.83428(10) 0.0518(5) Uani 1 1 d . . . . .
H23A H 1.0985 0.8341 0.8779 0.078 Uiso 1 1 calc GR . . . .
H23B H 1.1819 0.8443 0.8244 0.078 Uiso 1 1 calc GR . . . .
H23C H 1.1341 0.7839 0.8345 0.078 Uiso 1 1 calc GR . . . .
C15 C 0.54162(17) 0.82337(10) 0.42221(10) 0.0510(5) Uani 1 1 d . . . . .
H15A H 0.5711 0.8609 0.4284 0.077 Uiso 1 1 calc GR . . . .
H15B H 0.5211 0.8159 0.3747 0.077 Uiso 1 1 calc GR . . . .
H15C H 0.5993 0.7971 0.4412 0.077 Uiso 1 1 calc GR . . . .
C14 C 0.12500(17) 0.77167(9) 0.40997(11) 0.0520(5) Uani 1 1 d . . . . .
H14A H 0.1299 0.7757 0.3626 0.078 Uiso 1 1 calc GR . . . .
H14B H 0.0624 0.7939 0.4214 0.078 Uiso 1 1 calc GR . . . .
H14C H 0.1123 0.7329 0.4199 0.078 Uiso 1 1 calc GR . . . .
C60 C 1.01821(16) 0.51313(10) 0.71901(12) 0.0551(5) Uani 1 1 d . . . . .
C57 C 0.3294(2) 0.57225(9) 0.50998(11) 0.0604(6) Uani 1 1 d . . . . .
H57A H 0.3078 0.5466 0.5431 0.091 Uiso 1 1 calc GR . . . .
H57B H 0.3772 0.5532 0.4821 0.091 Uiso 1 1 calc GR . . . .
H57C H 0.2615 0.5859 0.4823 0.091 Uiso 1 1 calc GR . . . .
C48 C 0.2877(2) 0.52159(11) 0.93739(11) 0.0629(6) Uani 1 1 d . . . . .
H48A H 0.3372 0.5103 0.9776 0.094 Uiso 1 1 calc GR . . . .
H48B H 0.2300 0.4934 0.9255 0.094 Uiso 1 1 calc GR . . . .
H48C H 0.2515 0.5566 0.9454 0.094 Uiso 1 1 calc GR . . . .
C61 C 1.01598(18) 0.45582(10) 0.72582(14) 0.0628(6) Uani 1 1 d . . . . .
H61 H 1.0077 0.4401 0.7675 0.075 Uiso 1 1 calc R . . . .
C65 C 1.03255(19) 0.53557(12) 0.65708(13) 0.0662(6) Uani 1 1 d . . . . .
H65 H 1.0354 0.5744 0.6520 0.079 Uiso 1 1 calc R . . . .
C66 C 1.0039(2) 0.55085(11) 0.77853(14) 0.0718(7) Uani 1 1 d . . . . .
H66A H 0.9240 0.5596 0.7778 0.108 Uiso 1 1 calc GR . . . .
H66B H 1.0466 0.5849 0.7755 0.108 Uiso 1 1 calc GR . . . .
H66C H 1.0321 0.5319 0.8200 0.108 Uiso 1 1 calc GR . . . .
C64 C 1.0426(2) 0.50152(14) 0.60299(14) 0.0744(7) Uani 1 1 d . . . . .
H64 H 1.0527 0.5175 0.5617 0.089 Uiso 1 1 calc R . . . .
C63 C 1.0380(2) 0.44415(15) 0.60888(16) 0.0849(9) Uani 1 1 d . . . . .
H63 H 1.0428 0.4212 0.5716 0.102 Uiso 1 1 calc R . . . .
C62 C 1.0260(2) 0.42096(13) 0.67096(18) 0.0826(8) Uani 1 1 d . . . . .
H62 H 1.0247 0.3821 0.6761 0.099 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
N2 N1 1.4091(16) . ?
N2 C36 1.5235(17) . ?
N2 B2 1.384(2) . ?
N1 B1 1.379(2) . ?
N3 C49 1.3390(18) . ?
N3 C50 1.3951(19) . ?
N3 C52 1.4837(19) . ?
N4 C49 1.3458(19) . ?
N4 C55 1.4906(19) . ?
N4 C51 1.391(2) . ?
C30 C25 1.422(2) . ?
C30 C31 1.486(2) . ?
C30 C29 1.387(2) . ?
C49 B2 1.592(2) . ?
C26 C25 1.406(2) . ?
C26 C40 1.506(2) . ?
C26 C27 1.399(2) . ?
C25 B2 1.574(2) . ?
C35 H35 0.9800 . ?
C35 C36 1.5472(19) . ?
C35 C34 1.494(2) . ?
C35 B1 1.641(2) . ?
C31 C36 1.5202(19) . ?
C31 C32 1.348(2) . ?
C40 C45 1.404(2) . ?
C40 C41 1.401(2) . ?
C36 C37 1.529(2) . ?
C1 C2 1.423(2) . ?
C1 C6 1.416(2) . ?
C1 B1 1.597(2) . ?
C2 C16 1.502(2) . ?
C2 C3 1.394(2) . ?
C16 C21 1.409(2) . ?
C16 C17 1.413(2) . ?
C6 C7 1.504(2) . ?
C6 C5 1.398(2) . ?
C21 C20 1.392(2) . ?
C21 C22 1.501(2) . ?
C27 H27 0.9300 . ?
C27 C28 1.379(2) . ?
C28 H28 0.9300 . ?
C28 C29 1.384(2) . ?
C7 C8 1.404(2) . ?
C7 C12 1.403(2) . ?
C50 C51 1.352(2) . ?
C50 C58 1.493(2) . ?
C34 C33 1.334(2) . ?
C34 C39 1.499(2) . ?
C29 H29 0.9300 . ?
C52 H52 0.9800 . ?
C52 C53 1.514(2) . ?
C52 C54 1.519(2) . ?
C45 C44 1.395(2) . ?
C45 C46 1.507(2) . ?
C17 C18 1.389(2) . ?
C17 C24 1.507(2) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C32 C33 1.459(2) . ?
C32 C38 1.508(2) . ?
C33 H33 0.9300 . ?
C41 C42 1.397(2) . ?
C41 C47 1.506(2) . ?
C20 H20 0.9300 . ?
C20 C19 1.383(2) . ?
C8 C9 1.393(2) . ?
C8 C15 1.502(2) . ?
C55 H55 0.9800 . ?
C55 C56 1.508(2) . ?
C55 C57 1.514(3) . ?
C12 C11 1.394(2) . ?
C12 C13 1.501(2) . ?
C44 H44 0.9300 . ?
C44 C43 1.384(3) . ?
C51 C59 1.495(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(2) . ?
C5 H5 0.9300 . ?
C5 C4 1.377(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.389(3) . ?
C10 C9 1.385(3) . ?
C10 C11 1.385(3) . ?
C10 C14 1.510(2) . ?
C19 C23 1.508(2) . ?
C9 H9 0.9300 . ?
C4 H4 0.9300 . ?
C11 H11 0.9300 . ?
C42 H42 0.9300 . ?
C42 C43 1.386(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C43 C48 1.514(2) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C60 C61 1.372(3) . ?
C60 C65 1.378(3) . ?
C60 C66 1.517(4) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C61 H61 0.9300 . ?
C61 C62 1.392(4) . ?
C65 H65 0.9300 . ?
C65 C64 1.368(4) . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C64 H64 0.9300 . ?
C64 C63 1.372(4) . ?
C63 H63 0.9300 . ?
C63 C62 1.382(4) . ?
C62 H62 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
N1 N2 C36 113.03(10) . . ?
B2 N2 N1 126.69(11) . . ?
B2 N2 C36 120.05(11) . . ?
B1 N1 N2 109.46(11) . . ?
C49 N3 C50 109.76(12) . . ?
C49 N3 C52 121.61(12) . . ?
C50 N3 C52 128.60(12) . . ?
C49 N4 C55 121.23(12) . . ?
C49 N4 C51 109.54(12) . . ?
C51 N4 C55 128.94(13) . . ?
C25 C30 C31 117.67(12) . . ?
C29 C30 C25 120.49(13) . . ?
C29 C30 C31 121.81(13) . . ?
N3 C49 N4 107.03(12) . . ?
N3 C49 B2 130.90(12) . . ?
N4 C49 B2 121.62(12) . . ?
C25 C26 C40 124.85(13) . . ?
C27 C26 C25 120.10(13) . . ?
C27 C26 C40 114.88(13) . . ?
C30 C25 B2 114.43(12) . . ?
C26 C25 C30 117.88(13) . . ?
C26 C25 B2 127.48(13) . . ?
C36 C35 H35 107.8 . . ?
C36 C35 B1 101.44(11) . . ?
C34 C35 H35 107.8 . . ?
C34 C35 C36 115.79(12) . . ?
C34 C35 B1 115.59(12) . . ?
B1 C35 H35 107.8 . . ?
C30 C31 C36 113.95(12) . . ?
C32 C31 C30 124.08(13) . . ?
C32 C31 C36 121.48(13) . . ?
C45 C40 C26 119.25(13) . . ?
C41 C40 C26 120.36(13) . . ?
C41 C40 C45 119.61(14) . . ?
N2 C36 C35 104.77(10) . . ?
N2 C36 C37 108.49(11) . . ?
C31 C36 N2 103.65(10) . . ?
C31 C36 C35 116.50(12) . . ?
C31 C36 C37 112.96(12) . . ?
C37 C36 C35 109.69(11) . . ?
C2 C1 B1 120.76(12) . . ?
C6 C1 C2 116.21(13) . . ?
C6 C1 B1 122.99(13) . . ?
C1 C2 C16 123.19(13) . . ?
C3 C2 C1 121.25(14) . . ?
C3 C2 C16 115.49(13) . . ?
C21 C16 C2 120.14(13) . . ?
C21 C16 C17 118.90(14) . . ?
C17 C16 C2 120.58(13) . . ?
C1 C6 C7 125.22(13) . . ?
C5 C6 C1 121.00(14) . . ?
C5 C6 C7 113.77(13) . . ?
C16 C21 C22 121.92(14) . . ?
C20 C21 C16 119.27(14) . . ?
C20 C21 C22 118.72(14) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 C26 121.12(14) . . ?
C28 C27 H27 119.4 . . ?
C27 C28 H28 120.2 . . ?
C27 C28 C29 119.51(14) . . ?
C29 C28 H28 120.2 . . ?
C8 C7 C6 120.51(14) . . ?
C12 C7 C6 119.41(14) . . ?
C12 C7 C8 119.34(14) . . ?
N3 C50 C58 125.05(15) . . ?
C51 C50 N3 106.65(13) . . ?
C51 C50 C58 128.29(15) . . ?
C35 C34 C39 116.90(13) . . ?
C33 C34 C35 121.72(14) . . ?
C33 C34 C39 121.34(14) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 C30 120.78(14) . . ?
C28 C29 H29 119.6 . . ?
N3 C52 H52 106.7 . . ?
N3 C52 C53 110.36(13) . . ?
N3 C52 C54 111.91(13) . . ?
C53 C52 H52 106.7 . . ?
C53 C52 C54 113.99(13) . . ?
C54 C52 H52 106.7 . . ?
C40 C45 C46 121.03(14) . . ?
C44 C45 C40 119.16(15) . . ?
C44 C45 C46 119.74(15) . . ?
C16 C17 C24 122.66(14) . . ?
C18 C17 C16 119.36(15) . . ?
C18 C17 C24 117.87(15) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C31 C32 C33 120.28(14) . . ?
C31 C32 C38 123.69(15) . . ?
C33 C32 C38 116.01(14) . . ?
C34 C33 C32 123.46(14) . . ?
C34 C33 H33 118.3 . . ?
C32 C33 H33 118.3 . . ?
C40 C41 C47 120.93(14) . . ?
C42 C41 C40 119.19(15) . . ?
C42 C41 C47 119.86(15) . . ?
C21 C20 H20 118.7 . . ?
C19 C20 C21 122.51(15) . . ?
C19 C20 H20 118.7 . . ?
C7 C8 C15 121.02(15) . . ?
C9 C8 C7 119.23(15) . . ?
C9 C8 C15 119.74(15) . . ?
N4 C55 H55 106.6 . . ?
N4 C55 C56 110.64(13) . . ?
N4 C55 C57 112.56(15) . . ?
C56 C55 H55 106.6 . . ?
C56 C55 C57 113.26(15) . . ?
C57 C55 H55 106.6 . . ?
C7 C12 C13 120.51(15) . . ?
C11 C12 C7 119.42(15) . . ?
C11 C12 C13 120.05(15) . . ?
C45 C44 H44 119.0 . . ?
C43 C44 C45 122.05(15) . . ?
C43 C44 H44 119.0 . . ?
N4 C51 C59 124.76(15) . . ?
C50 C51 N4 107.00(13) . . ?
C50 C51 C59 128.24(15) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 C2 121.21(15) . . ?
C4 C3 H3 119.4 . . ?
C6 C5 H5 119.3 . . ?
C4 C5 C6 121.50(15) . . ?
C4 C5 H5 119.3 . . ?
C17 C18 H18 118.8 . . ?
C17 C18 C19 122.36(15) . . ?
C19 C18 H18 118.8 . . ?
C9 C10 C14 120.93(17) . . ?
C11 C10 C9 117.98(15) . . ?
C11 C10 C14 121.08(17) . . ?
C20 C19 C18 117.58(15) . . ?
C20 C19 C23 120.59(17) . . ?
C18 C19 C23 121.78(17) . . ?
C8 C9 H9 119.0 . . ?
C10 C9 C8 122.09(15) . . ?
C10 C9 H9 119.0 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.83(15) . . ?
C5 C4 H4 120.6 . . ?
C12 C11 H11 119.1 . . ?
C10 C11 C12 121.89(16) . . ?
C10 C11 H11 119.1 . . ?
C41 C42 H42 119.0 . . ?
C43 C42 C41 121.94(16) . . ?
C43 C42 H42 119.0 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C44 C43 C42 118.04(15) . . ?
C44 C43 C48 121.23(17) . . ?
C42 C43 C48 120.73(18) . . ?
C17 C24 H24A 109.5 . . ?
C17 C24 H24B 109.5 . . ?
C17 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C41 C47 H47A 109.5 . . ?
C41 C47 H47B 109.5 . . ?
C41 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N2 B2 C49 115.37(12) . . ?
N2 B2 C25 118.12(12) . . ?
C25 B2 C49 123.42(12) . . ?
C50 C58 H58A 109.5 . . ?
C50 C58 H58B 109.5 . . ?
C50 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C51 C59 H59A 109.5 . . ?
C51 C59 H59B 109.5 . . ?
C51 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N1 B1 C35 110.52(12) . . ?
N1 B1 C1 122.95(13) . . ?
C1 B1 C35 126.26(12) . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C8 C15 H15A 109.5 . . ?
C8 C15 H15B 109.5 . . ?
C8 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C61 C60 C65 118.7(2) . . ?
C61 C60 C66 120.3(2) . . ?
C65 C60 C66 120.9(2) . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C60 C61 H61 119.7 . . ?
C60 C61 C62 120.7(3) . . ?
C62 C61 H61 119.7 . . ?
C60 C65 H65 119.6 . . ?
C64 C65 C60 120.9(3) . . ?
C64 C65 H65 119.6 . . ?
C60 C66 H66A 109.5 . . ?
C60 C66 H66B 109.5 . . ?
C60 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 C64 H64 119.6 . . ?
C65 C64 C63 120.9(3) . . ?
C63 C64 H64 119.6 . . ?
C64 C63 H63 120.5 . . ?
C64 C63 C62 119.0(3) . . ?
C62 C63 H63 120.5 . . ?
C61 C62 H62 120.1 . . ?
C63 C62 C61 119.9(3) . . ?
C63 C62 H62 120.1 . . ?

_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 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.654
####################################################################### 
# 
# 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_klb-3
_database_code_depnum_ccdc_archive 'CCDC 1977880'
loop_
_audit_author_name
_audit_author_address
'Lingbing Kong'
;Shandong University
China
;
_audit_update_record             
;
2020-05-25 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C47 H46 B2 N4'
_chemical_formula_sum            'C47 H46 B2 N4'
_chemical_formula_weight         688.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         CNB
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
B B 0.0013 0.0007 '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'

_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                   11.2493(3)
_cell_length_b                   26.0979(7)
_cell_length_c                   13.6593(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.818(3)
_cell_angle_gamma                90
_cell_volume                     3772.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6707
_cell_measurement_temperature    172.98(10)
_cell_measurement_theta_max      76.3480
_cell_measurement_theta_min      3.3480
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.966
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21327
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.559
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00 102.00   1.00    3.50    --   48.45  81.00 131.00   63
  2  ω     82.00 165.00   1.00   27.00    --  106.49  81.00 131.00   83
  3  ω     92.00 178.00   1.00   27.00    --  106.49  57.00  60.00   86
  4  ω     41.00 131.00   1.00   27.00    --  106.49 -81.00   9.00   90
  5  ω     31.00  96.00   1.00    3.50    --   48.45-125.00-120.00   65
  6  ω     34.00  90.00   1.00   27.00    --  106.49 -99.00 -30.00   56
  7  ω     34.00 117.00   1.00   27.00    --  106.49-125.00-120.00   83
  8  ω     34.00  98.00   1.00   27.00    --  106.49 -99.00 -60.00   64
  9  ω     -7.00  19.00   1.00    3.50    --   48.45 -81.00   9.00   26
 10  ω    -73.00 -10.00   1.00    3.50    --  -48.45  81.00 131.00   63
 11  ω    -63.00 -35.00   1.00   27.00    --  -86.25  81.00 131.00   28
 12  ω   -120.00 -24.00   1.00    3.50    --  -48.45 -81.00   9.00   96
 13  ω   -119.00 -88.00   1.00    3.50    --  -48.45-125.00-180.00   31
 14  ω   -159.00-133.00   1.00   27.00    --  -86.25 -81.00   9.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0875659000
_diffrn_orient_matrix_UB_12      -0.0169792000
_diffrn_orient_matrix_UB_13      -0.0596347000
_diffrn_orient_matrix_UB_21      -0.0817546000
_diffrn_orient_matrix_UB_22      -0.0481518000
_diffrn_orient_matrix_UB_23      -0.0384948000
_diffrn_orient_matrix_UB_31      -0.0827863000
_diffrn_orient_matrix_UB_32      0.0295623000
_diffrn_orient_matrix_UB_33      -0.0966636000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4878
_reflns_number_total             6608
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         6608
_refine_ls_number_restraints     204
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0451
_refine_ls_restrained_S_all      1.018
_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)+(0.0563P)²+1.1220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1224
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33A-C32A \\sim C33B-C32B \\sim C34B-C33B \\sim C34A-C33A \\sim C35A-C34A
\\sim C35B-C34B \\sim C36A-
 C35A \\sim C36B-C35B \\sim C36B-C31B \\sim C36A-C31A \\sim C32B-C31B \\sim
C32A-C31A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C31B \\sim C32B \\sim C33B \\sim C34B \\sim C35B \\sim C36B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31B) \\sim Ueq, Uanis(C32B) \\sim Ueq, Uanis(C33B) \\sim Ueq,
Uanis(C34B) \\sim Ueq, Uanis(C36A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C31A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33A) \\sim Ueq,
Uanis(C34A) \\sim Ueq, Uanis(C35B) \\sim Ueq, Uanis(C36B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=Sof(H33B)=Sof(C34B)=Sof(H34B)=
 Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=1-FVAR(1)
 Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C29(H29), C30(H30)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C26(H26), C27(H27), C28(H28), C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B),
 C36B(H36B), C38(H38), C39(H39), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A),
  C36A(H36A)
5.c Fitted hexagon refined as free rotating group:
 C31B(C32B,C33B,C34B,C35B,C36B)
5.d Idealised Me refined as rotating group:
 C41(H41a,H41b,H41c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C45(H45a,H45b,
 H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.32810(19) 0.13486(8) 0.81722(17) 0.0312(5) Uani 1 1 d . . . . .
B2 B 0.13187(18) 0.02179(8) 0.76485(15) 0.0251(4) Uani 1 1 d . . . . .
C1 C 0.45607(17) 0.16598(7) 0.86961(16) 0.0323(4) Uani 1 1 d . . . . .
C2 C 0.48840(17) 0.18878(7) 0.96953(16) 0.0356(4) Uani 1 1 d . . . . .
C3 C 0.60332(19) 0.21425(8) 1.01386(18) 0.0403(5) Uani 1 1 d . . . . .
H3 H 0.6237 0.2280 1.0803 0.048 Uiso 1 1 calc R . . . .
C4 C 0.68713(19) 0.21931(8) 0.96052(19) 0.0442(5) Uani 1 1 d . . . . .
H4 H 0.7649 0.2351 0.9917 0.053 Uiso 1 1 calc R . . . .
C5 C 0.65426(18) 0.20065(8) 0.86050(19) 0.0412(5) Uani 1 1 d . . . . .
H5 H 0.7089 0.2053 0.8232 0.049 Uiso 1 1 calc R . . . .
C6 C 0.53976(17) 0.17471(7) 0.81394(17) 0.0351(4) Uani 1 1 d . . . . .
C7 C 0.50543(18) 0.16093(8) 0.70137(17) 0.0361(4) Uani 1 1 d . . . . .
C8 C 0.5165(2) 0.19782(9) 0.6312(2) 0.0494(6) Uani 1 1 d . . . . .
H8 H 0.5457 0.2304 0.6553 0.059 Uiso 1 1 calc R . . . .
C9 C 0.4851(3) 0.18699(10) 0.5266(2) 0.0614(7) Uani 1 1 d . . . . .
H9 H 0.4937 0.2122 0.4813 0.074 Uiso 1 1 calc R . . . .
C10 C 0.4413(2) 0.13914(10) 0.48848(19) 0.0519(6) Uani 1 1 d . . . . .
H10 H 0.4194 0.1320 0.4179 0.062 Uiso 1 1 calc R . . . .
C11 C 0.4305(2) 0.10208(9) 0.55704(17) 0.0438(5) Uani 1 1 d . . . . .
H11 H 0.4014 0.0696 0.5323 0.053 Uiso 1 1 calc R . . . .
C12 C 0.46246(18) 0.11258(8) 0.66235(16) 0.0377(5) Uani 1 1 d . . . . .
H12 H 0.4551 0.0870 0.7074 0.045 Uiso 1 1 calc R . . . .
C13 C 0.40239(18) 0.18828(8) 1.03256(16) 0.0375(5) Uani 1 1 d . . . . .
C14 C 0.34546(19) 0.14407(8) 1.05179(17) 0.0418(5) Uani 1 1 d . . . . .
H14 H 0.3565 0.1134 1.0214 0.050 Uiso 1 1 calc R . . . .
C15 C 0.2722(2) 0.14493(10) 1.1158(2) 0.0523(6) Uani 1 1 d . . . . .
H15 H 0.2360 0.1148 1.1286 0.063 Uiso 1 1 calc R . . . .
C16 C 0.2527(2) 0.19028(11) 1.1605(2) 0.0623(7) Uani 1 1 d . . . . .
H16 H 0.2041 0.1908 1.2037 0.075 Uiso 1 1 calc R . . . .
C17 C 0.3063(3) 0.23470(11) 1.1401(2) 0.0691(8) Uani 1 1 d . . . . .
H17 H 0.2921 0.2655 1.1685 0.083 Uiso 1 1 calc R . . . .
C18 C 0.3812(2) 0.23394(9) 1.0777(2) 0.0542(6) Uani 1 1 d . . . . .
H18 H 0.4178 0.2642 1.0656 0.065 Uiso 1 1 calc R . . . .
C19 C -0.01869(15) 0.01844(7) 0.72060(12) 0.0251(4) Uani 1 1 d . . . . .
C20 C -0.09471(16) -0.02626(7) 0.69724(13) 0.0287(4) Uani 1 1 d . . . . .
C21 C -0.22669(17) -0.02210(8) 0.66760(14) 0.0340(4) Uani 1 1 d . . . . .
H21 H -0.2753 -0.0518 0.6545 0.041 Uiso 1 1 calc R . . . .
C22 C -0.28611(17) 0.02466(8) 0.65744(14) 0.0355(5) Uani 1 1 d . . . . .
H22 H -0.3738 0.0264 0.6366 0.043 Uiso 1 1 calc R . . . .
C23 C -0.21469(17) 0.06899(8) 0.67844(13) 0.0313(4) Uani 1 1 d . . . . .
H23 H -0.2545 0.1007 0.6708 0.038 Uiso 1 1 calc R . . . .
C24 C -0.08292(16) 0.06643(7) 0.71107(12) 0.0266(4) Uani 1 1 d . . . . .
C25 C -0.00790(16) 0.11368(7) 0.73919(14) 0.0311(4) Uani 1 1 d . . . . .
C26 C -0.0349(2) 0.15181(9) 0.79511(17) 0.0433(5) Uani 1 1 d . . . . .
H26 H -0.1072 0.1494 0.8133 0.052 Uiso 1 1 calc R . . . .
C27 C 0.0457(2) 0.19651(9) 0.8276(2) 0.0550(6) Uani 1 1 d . . . . .
H27 H 0.0235 0.2222 0.8654 0.066 Uiso 1 1 calc R . . . .
C28 C 0.1515(2) 0.20145(8) 0.80419(19) 0.0488(6) Uani 1 1 d . . . . .
H28 H 0.1991 0.2312 0.8247 0.059 Uiso 1 1 calc R . . . .
C29 C 0.19625(18) 0.16188(8) 0.74725(17) 0.0382(5) Uani 1 1 d . . . . .
H29 H 0.2075 0.1775 0.6857 0.046 Uiso 1 1 calc R . . . .
C30 C 0.11022(17) 0.11442(7) 0.71334(14) 0.0302(4) Uani 1 1 d . . . . .
H30 H 0.0883 0.1099 0.6381 0.036 Uiso 1 1 calc R . . . .
C31B C -0.0491(6) -0.08041(15) 0.6938(4) 0.0280(14) Uani 0.70(2) 1 d D U P A 2
C32B C 0.0211(5) -0.1061(2) 0.7840(4) 0.0332(14) Uani 0.70(2) 1 d DG U P A 2
H32B H 0.0464 -0.0891 0.8476 0.040 Uiso 0.70(2) 1 calc R . P A 2
C33B C 0.0536(4) -0.1572(2) 0.7792(6) 0.0395(14) Uani 0.70(2) 1 d DG U P A 2
H33B H 0.1006 -0.1743 0.8396 0.047 Uiso 0.70(2) 1 calc R . P A 2
C34B C 0.0158(4) -0.18260(13) 0.6842(7) 0.0385(13) Uani 0.70(2) 1 d DG U P A 2
H34B H 0.0376 -0.2168 0.6810 0.046 Uiso 0.70(2) 1 calc R . P A 2
C35B C -0.0544(5) -0.15694(15) 0.5940(5) 0.0387(12) Uani 0.70(2) 1 d DG U P A 2
H35B H -0.0797 -0.1740 0.5304 0.046 Uiso 0.70(2) 1 calc R . P A 2
C36B C -0.0869(6) -0.10585(16) 0.5987(4) 0.0311(12) Uani 0.70(2) 1 d DG U P A 2
H36B H -0.1339 -0.0887 0.5384 0.037 Uiso 0.70(2) 1 calc R . P A 2
C37 C 0.22535(15) -0.02519(6) 0.81191(12) 0.0223(4) Uani 1 1 d . . . . .
C38 C 0.35410(18) -0.09225(7) 0.82716(14) 0.0333(4) Uani 1 1 d . . . . .
H38 H 0.4008 -0.1181 0.8105 0.040 Uiso 1 1 calc R . . . .
C39 C 0.34758(18) -0.08258(7) 0.92163(15) 0.0334(4) Uani 1 1 d . . . . .
H39 H 0.3890 -0.1006 0.9824 0.040 Uiso 1 1 calc R . . . .
C40 C 0.24930(17) -0.01978(8) 1.00807(13) 0.0306(4) Uani 1 1 d . . . . .
C41 C 0.15062(18) 0.02233(8) 0.98179(15) 0.0355(4) Uani 1 1 d . . . . .
H41A H 0.1791 0.0505 0.9504 0.053 Uiso 1 1 calc GR . . . .
H41B H 0.1377 0.0337 1.0443 0.053 Uiso 1 1 calc GR . . . .
H41C H 0.0726 0.0094 0.9341 0.053 Uiso 1 1 calc GR . . . .
C42 C 0.2067(2) -0.06320(9) 1.06369(16) 0.0486(6) Uani 1 1 d . . . . .
H42A H 0.1303 -0.0780 1.0174 0.073 Uiso 1 1 calc GR . . . .
H42B H 0.1918 -0.0499 1.1240 0.073 Uiso 1 1 calc GR . . . .
H42C H 0.2714 -0.0889 1.0846 0.073 Uiso 1 1 calc GR . . . .
C43 C 0.37759(19) 0.00144(9) 1.07605(16) 0.0415(5) Uani 1 1 d . . . . .
H43A H 0.4378 -0.0260 1.0966 0.062 Uiso 1 1 calc GR . . . .
H43B H 0.3694 0.0173 1.1369 0.062 Uiso 1 1 calc GR . . . .
H43C H 0.4061 0.0264 1.0373 0.062 Uiso 1 1 calc GR . . . .
C44 C 0.27693(17) -0.05443(7) 0.64841(13) 0.0281(4) Uani 1 1 d . . . . .
C45 C 0.1733(2) -0.01956(9) 0.58122(15) 0.0403(5) Uani 1 1 d . . . . .
H45A H 0.0935 -0.0302 0.5853 0.060 Uiso 1 1 calc GR . . . .
H45B H 0.1706 -0.0215 0.5103 0.060 Uiso 1 1 calc GR . . . .
H45C H 0.1904 0.0151 0.6055 0.060 Uiso 1 1 calc GR . . . .
C46 C 0.40582(19) -0.03450(8) 0.65249(16) 0.0387(5) Uani 1 1 d . . . . .
H46A H 0.4199 -0.0012 0.6844 0.058 Uiso 1 1 calc GR . . . .
H46B H 0.4084 -0.0321 0.5831 0.058 Uiso 1 1 calc GR . . . .
H46C H 0.4704 -0.0576 0.6925 0.058 Uiso 1 1 calc GR . . . .
C47 C 0.2558(2) -0.10858(8) 0.60319(16) 0.0424(5) Uani 1 1 d . . . . .
H47A H 0.3257 -0.1300 0.6410 0.064 Uiso 1 1 calc GR . . . .
H47B H 0.2492 -0.1075 0.5313 0.064 Uiso 1 1 calc GR . . . .
H47C H 0.1792 -0.1223 0.6088 0.064 Uiso 1 1 calc GR . . . .
N1 N 0.31576(13) 0.08211(6) 0.82177(12) 0.0278(3) Uani 1 1 d . . . . .
N2 N 0.18721(13) 0.06900(6) 0.76784(11) 0.0263(3) Uani 1 1 d . . . . .
N3 N 0.27875(13) -0.05677(5) 0.75932(11) 0.0244(3) Uani 1 1 d . . . . .
N4 N 0.26886(13) -0.04138(5) 0.91252(11) 0.0249(3) Uani 1 1 d . . . . .
C31A C -0.0440(18) -0.0776(6) 0.7119(14) 0.038(3) Uani 0.30(2) 1 d D U P A 1
C32A C 0.0121(17) -0.1014(6) 0.8074(15) 0.046(3) Uani 0.30(2) 1 d D U P A 1
H32A H 0.0192 -0.0829 0.8672 0.055 Uiso 0.30(2) 1 calc R . P A 1
C33A C 0.0580(14) -0.1508(5) 0.8187(19) 0.054(3) Uani 0.30(2) 1 d D U P A 1
H33A H 0.1010 -0.1645 0.8841 0.065 Uiso 0.30(2) 1 calc R . P A 1
C34A C 0.0375(14) -0.1794(5) 0.7288(19) 0.047(3) Uani 0.30(2) 1 d D U P A 1
H34A H 0.0729 -0.2120 0.7345 0.056 Uiso 0.30(2) 1 calc R . P A 1
C35A C -0.0324(15) -0.1618(6) 0.6322(18) 0.051(3) Uani 0.30(2) 1 d D U P A 1
H35A H -0.0540 -0.1828 0.5738 0.061 Uiso 0.30(2) 1 calc R . P A 1
C36A C -0.0691(17) -0.1112(6) 0.6260(16) 0.048(3) Uani 0.30(2) 1 d D U P A 1
H36A H -0.1138 -0.0981 0.5604 0.058 Uiso 0.30(2) 1 calc R . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C1 1.596(3) . ?
B1 C29 1.628(3) . ?
B1 N1 1.387(3) . ?
B2 C19 1.596(2) . ?
B2 C37 1.601(3) . ?
B2 N2 1.375(3) . ?
C1 C2 1.419(3) . ?
C1 C6 1.415(3) . ?
C2 C3 1.396(3) . ?
C2 C13 1.497(3) . ?
C3 C4 1.379(3) . ?
C4 C5 1.378(3) . ?
C5 C6 1.402(3) . ?
C6 C7 1.497(3) . ?
C7 C8 1.394(3) . ?
C7 C12 1.391(3) . ?
C8 C9 1.380(4) . ?
C9 C10 1.378(4) . ?
C10 C11 1.380(3) . ?
C11 C12 1.387(3) . ?
C13 C14 1.387(3) . ?
C13 C18 1.399(3) . ?
C14 C15 1.390(3) . ?
C15 C16 1.383(3) . ?
C16 C17 1.378(4) . ?
C17 C18 1.387(4) . ?
C19 C20 1.418(3) . ?
C19 C24 1.429(3) . ?
C20 C21 1.404(3) . ?
C20 C31B 1.510(4) . ?
C20 C31A 1.444(14) . ?
C21 C22 1.376(3) . ?
C22 C23 1.382(3) . ?
C23 C24 1.397(2) . ?
C24 C25 1.470(3) . ?
C25 C26 1.350(3) . ?
C25 C30 1.486(3) . ?
C26 C27 1.452(3) . ?
C27 C28 1.339(4) . ?
C28 C29 1.480(3) . ?
C29 C30 1.543(3) . ?
C30 N2 1.508(2) . ?
C31B C32B 1.3900 . ?
C31B C36B 1.3900 . ?
C32B C33B 1.3900 . ?
C33B C34B 1.3900 . ?
C34B C35B 1.3900 . ?
C35B C36B 1.3900 . ?
C37 N3 1.360(2) . ?
C37 N4 1.360(2) . ?
C38 C39 1.341(3) . ?
C38 N3 1.379(2) . ?
C39 N4 1.372(2) . ?
C40 C41 1.516(3) . ?
C40 C42 1.529(3) . ?
C40 C43 1.531(3) . ?
C40 N4 1.505(2) . ?
C44 C45 1.518(3) . ?
C44 C46 1.524(3) . ?
C44 C47 1.528(3) . ?
C44 N3 1.509(2) . ?
N1 N2 1.4243(19) . ?
C31A C32A 1.387(11) . ?
C31A C36A 1.413(11) . ?
C32A C33A 1.380(11) . ?
C33A C34A 1.389(11) . ?
C34A C35A 1.366(11) . ?
C35A C36A 1.379(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 B1 C29 123.15(17) . . ?
N1 B1 C1 125.02(16) . . ?
N1 B1 C29 111.78(16) . . ?
C19 B2 C37 125.33(16) . . ?
N2 B2 C19 118.17(16) . . ?
N2 B2 C37 116.43(15) . . ?
C2 C1 B1 122.88(17) . . ?
C6 C1 B1 120.30(18) . . ?
C6 C1 C2 116.71(17) . . ?
C1 C2 C13 123.00(17) . . ?
C3 C2 C1 121.0(2) . . ?
C3 C2 C13 116.02(19) . . ?
C4 C3 C2 121.0(2) . . ?
C5 C4 C3 119.22(19) . . ?
C4 C5 C6 121.1(2) . . ?
C1 C6 C7 121.78(17) . . ?
C5 C6 C1 120.7(2) . . ?
C5 C6 C7 117.34(19) . . ?
C8 C7 C6 119.26(19) . . ?
C12 C7 C6 123.13(18) . . ?
C12 C7 C8 117.6(2) . . ?
C9 C8 C7 121.3(2) . . ?
C10 C9 C8 120.6(2) . . ?
C9 C10 C11 118.8(2) . . ?
C10 C11 C12 120.9(2) . . ?
C11 C12 C7 120.7(2) . . ?
C14 C13 C2 123.09(18) . . ?
C14 C13 C18 117.8(2) . . ?
C18 C13 C2 119.1(2) . . ?
C13 C14 C15 121.1(2) . . ?
C16 C15 C14 120.5(2) . . ?
C17 C16 C15 119.0(2) . . ?
C16 C17 C18 120.7(2) . . ?
C17 C18 C13 120.8(2) . . ?
C20 C19 B2 127.74(16) . . ?
C20 C19 C24 116.92(15) . . ?
C24 C19 B2 115.17(16) . . ?
C19 C20 C31B 126.3(3) . . ?
C19 C20 C31A 123.6(8) . . ?
C21 C20 C19 119.96(18) . . ?
C21 C20 C31B 113.6(3) . . ?
C21 C20 C31A 116.2(8) . . ?
C22 C21 C20 121.85(19) . . ?
C21 C22 C23 119.55(17) . . ?
C22 C23 C24 120.35(18) . . ?
C19 C24 C25 118.91(15) . . ?
C23 C24 C19 121.32(17) . . ?
C23 C24 C25 119.75(17) . . ?
C24 C25 C30 115.42(16) . . ?
C26 C25 C24 123.15(18) . . ?
C26 C25 C30 121.03(18) . . ?
C25 C26 C27 121.9(2) . . ?
C28 C27 C26 121.2(2) . . ?
C27 C28 C29 123.1(2) . . ?
C28 C29 B1 113.48(17) . . ?
C28 C29 C30 115.28(18) . . ?
C30 C29 B1 100.52(15) . . ?
C25 C30 C29 117.35(17) . . ?
C25 C30 N2 106.42(15) . . ?
N2 C30 C29 106.62(14) . . ?
C32B C31B C20 121.4(3) . . ?
C32B C31B C36B 120.0 . . ?
C36B C31B C20 118.5(3) . . ?
C31B C32B C33B 120.0 . . ?
C34B C33B C32B 120.0 . . ?
C35B C34B C33B 120.0 . . ?
C34B C35B C36B 120.0 . . ?
C35B C36B C31B 120.0 . . ?
N3 C37 B2 126.85(14) . . ?
N3 C37 N4 105.86(14) . . ?
N4 C37 B2 127.28(15) . . ?
C39 C38 N3 107.38(17) . . ?
C38 C39 N4 107.72(16) . . ?
C41 C40 C42 109.11(17) . . ?
C41 C40 C43 110.20(16) . . ?
C42 C40 C43 110.89(17) . . ?
N4 C40 C41 112.13(14) . . ?
N4 C40 C42 108.42(16) . . ?
N4 C40 C43 106.06(15) . . ?
C45 C44 C46 110.10(16) . . ?
C45 C44 C47 109.13(16) . . ?
C46 C44 C47 110.25(16) . . ?
N3 C44 C45 112.19(15) . . ?
N3 C44 C46 106.75(14) . . ?
N3 C44 C47 108.39(15) . . ?
B1 N1 N2 108.35(14) . . ?
B2 N2 C30 120.77(14) . . ?
B2 N2 N1 126.93(14) . . ?
N1 N2 C30 112.27(13) . . ?
C37 N3 C38 109.45(14) . . ?
C37 N3 C44 130.36(14) . . ?
C38 N3 C44 119.85(15) . . ?
C37 N4 C39 109.59(14) . . ?
C37 N4 C40 130.66(14) . . ?
C39 N4 C40 119.65(14) . . ?
C32A C31A C20 125.3(12) . . ?
C32A C31A C36A 113.8(11) . . ?
C36A C31A C20 120.1(12) . . ?
C33A C32A C31A 123.9(12) . . ?
C32A C33A C34A 117.3(11) . . ?
C35A C34A C33A 122.8(10) . . ?
C34A C35A C36A 116.4(10) . . ?
C35A C36A C31A 124.8(12) . . ?

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
B1 C1 C2 C3 177.89(17) . . . . ?
B1 C1 C2 C13 -3.5(3) . . . . ?
B1 C1 C6 C5 -178.04(17) . . . . ?
B1 C1 C6 C7 7.4(3) . . . . ?
B1 C29 C30 C25 123.43(17) . . . . ?
B1 C29 C30 N2 4.31(19) . . . . ?
B1 N1 N2 B2 -171.37(18) . . . . ?
B1 N1 N2 C30 6.7(2) . . . . ?
B2 C19 C20 C21 174.22(16) . . . . ?
B2 C19 C20 C31B -10.0(4) . . . . ?
B2 C19 C20 C31A 0.7(9) . . . . ?
B2 C19 C24 C23 -176.70(15) . . . . ?
B2 C19 C24 C25 1.5(2) . . . . ?
B2 C37 N3 C38 179.58(16) . . . . ?
B2 C37 N3 C44 6.4(3) . . . . ?
B2 C37 N4 C39 -179.60(16) . . . . ?
B2 C37 N4 C40 -3.4(3) . . . . ?
C1 B1 C29 C28 -59.3(3) . . . . ?
C1 B1 C29 C30 177.09(18) . . . . ?
C1 B1 N1 N2 178.77(18) . . . . ?
C1 C2 C3 C4 1.9(3) . . . . ?
C1 C2 C13 C14 50.4(3) . . . . ?
C1 C2 C13 C18 -132.0(2) . . . . ?
C1 C6 C7 C8 127.8(2) . . . . ?
C1 C6 C7 C12 -52.2(3) . . . . ?
C2 C1 C6 C5 5.7(3) . . . . ?
C2 C1 C6 C7 -168.89(17) . . . . ?
C2 C3 C4 C5 2.6(3) . . . . ?
C2 C13 C14 C15 176.2(2) . . . . ?
C2 C13 C18 C17 -177.4(2) . . . . ?
C3 C2 C13 C14 -131.0(2) . . . . ?
C3 C2 C13 C18 46.7(3) . . . . ?
C3 C4 C5 C6 -2.8(3) . . . . ?
C4 C5 C6 C1 -1.4(3) . . . . ?
C4 C5 C6 C7 173.39(18) . . . . ?
C5 C6 C7 C8 -47.0(3) . . . . ?
C5 C6 C7 C12 133.0(2) . . . . ?
C6 C1 C2 C3 -6.0(3) . . . . ?
C6 C1 C2 C13 172.63(17) . . . . ?
C6 C7 C8 C9 -179.5(2) . . . . ?
C6 C7 C12 C11 179.21(18) . . . . ?
C7 C8 C9 C10 0.2(4) . . . . ?
C8 C7 C12 C11 -0.8(3) . . . . ?
C8 C9 C10 C11 -0.6(4) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C10 C11 C12 C7 0.5(3) . . . . ?
C12 C7 C8 C9 0.5(3) . . . . ?
C13 C2 C3 C4 -176.76(18) . . . . ?
C13 C14 C15 C16 1.1(4) . . . . ?
C14 C13 C18 C17 0.4(4) . . . . ?
C14 C15 C16 C17 0.4(4) . . . . ?
C15 C16 C17 C18 -1.5(4) . . . . ?
C16 C17 C18 C13 1.1(4) . . . . ?
C18 C13 C14 C15 -1.5(3) . . . . ?
C19 B2 C37 N3 91.9(2) . . . . ?
C19 B2 C37 N4 -88.9(2) . . . . ?
C19 B2 N2 C30 -11.0(2) . . . . ?
C19 B2 N2 N1 166.90(15) . . . . ?
C19 C20 C21 C22 1.9(3) . . . . ?
C19 C20 C31B C32B 70.5(4) . . . . ?
C19 C20 C31B C36B -114.3(3) . . . . ?
C19 C20 C31A C32A 71.9(15) . . . . ?
C19 C20 C31A C36A -119.5(10) . . . . ?
C19 C24 C25 C26 -136.69(19) . . . . ?
C19 C24 C25 C30 36.0(2) . . . . ?
C20 C19 C24 C23 -1.1(2) . . . . ?
C20 C19 C24 C25 177.15(15) . . . . ?
C20 C21 C22 C23 -1.1(3) . . . . ?
C20 C31B C32B C33B 175.2(5) . . . . ?
C20 C31B C36B C35B -175.3(5) . . . . ?
C20 C31A C32A C33A 179.0(16) . . . . ?
C20 C31A C36A C35A -175.7(15) . . . . ?
C21 C20 C31B C32B -113.5(3) . . . . ?
C21 C20 C31B C36B 61.7(4) . . . . ?
C21 C20 C31A C32A -101.8(14) . . . . ?
C21 C20 C31A C36A 66.7(12) . . . . ?
C21 C22 C23 C24 -0.8(3) . . . . ?
C22 C23 C24 C19 1.9(3) . . . . ?
C22 C23 C24 C25 -176.31(17) . . . . ?
C23 C24 C25 C26 41.6(3) . . . . ?
C23 C24 C25 C30 -145.71(16) . . . . ?
C24 C19 C20 C21 -0.8(2) . . . . ?
C24 C19 C20 C31B 175.0(3) . . . . ?
C24 C19 C20 C31A -174.3(9) . . . . ?
C24 C25 C26 C27 175.83(19) . . . . ?
C24 C25 C30 C29 -176.43(15) . . . . ?
C24 C25 C30 N2 -57.20(19) . . . . ?
C25 C26 C27 C28 -0.8(4) . . . . ?
C25 C30 N2 B2 45.1(2) . . . . ?
C25 C30 N2 N1 -133.04(15) . . . . ?
C26 C25 C30 C29 -3.5(3) . . . . ?
C26 C25 C30 N2 115.68(19) . . . . ?
C26 C27 C28 C29 -1.9(4) . . . . ?
C27 C28 C29 B1 -113.6(2) . . . . ?
C27 C28 C29 C30 1.6(3) . . . . ?
C28 C29 C30 C25 1.0(2) . . . . ?
C28 C29 C30 N2 -118.09(18) . . . . ?
C29 B1 C1 C2 87.7(2) . . . . ?
C29 B1 C1 C6 -88.3(2) . . . . ?
C29 B1 N1 N2 -3.5(2) . . . . ?
C29 C30 N2 B2 171.12(16) . . . . ?
C29 C30 N2 N1 -7.0(2) . . . . ?
C30 C25 C26 C27 3.5(3) . . . . ?
C31B C20 C21 C22 -174.4(3) . . . . ?
C31B C32B C33B C34B 0.0 . . . . ?
C32B C31B C36B C35B 0.0 . . . . ?
C32B C33B C34B C35B 0.0 . . . . ?
C33B C34B C35B C36B 0.0 . . . . ?
C34B C35B C36B C31B 0.0 . . . . ?
C36B C31B C32B C33B 0.0 . . . . ?
C37 B2 C19 C20 -12.5(3) . . . . ?
C37 B2 C19 C24 162.53(16) . . . . ?
C37 B2 N2 C30 171.95(15) . . . . ?
C37 B2 N2 N1 -10.2(3) . . . . ?
C38 C39 N4 C37 0.2(2) . . . . ?
C38 C39 N4 C40 -176.51(16) . . . . ?
C39 C38 N3 C37 -0.1(2) . . . . ?
C39 C38 N3 C44 173.85(15) . . . . ?
C41 C40 N4 C37 9.2(3) . . . . ?
C41 C40 N4 C39 -174.84(16) . . . . ?
C42 C40 N4 C37 129.76(19) . . . . ?
C42 C40 N4 C39 -54.3(2) . . . . ?
C43 C40 N4 C37 -111.1(2) . . . . ?
C43 C40 N4 C39 64.8(2) . . . . ?
C45 C44 N3 C37 -17.0(2) . . . . ?
C45 C44 N3 C38 170.44(17) . . . . ?
C46 C44 N3 C37 103.7(2) . . . . ?
C46 C44 N3 C38 -68.9(2) . . . . ?
C47 C44 N3 C37 -137.58(18) . . . . ?
C47 C44 N3 C38 49.9(2) . . . . ?
N1 B1 C1 C2 -94.9(2) . . . . ?
N1 B1 C1 C6 89.1(2) . . . . ?
N1 B1 C29 C28 123.0(2) . . . . ?
N1 B1 C29 C30 -0.7(2) . . . . ?
N2 B2 C19 C20 170.68(16) . . . . ?
N2 B2 C19 C24 -14.3(2) . . . . ?
N2 B2 C37 N3 -91.2(2) . . . . ?
N2 B2 C37 N4 88.0(2) . . . . ?
N3 C37 N4 C39 -0.29(19) . . . . ?
N3 C37 N4 C40 175.96(16) . . . . ?
N3 C38 C39 N4 -0.1(2) . . . . ?
N4 C37 N3 C38 0.25(19) . . . . ?
N4 C37 N3 C44 -172.89(15) . . . . ?
C31A C20 C21 C22 175.9(8) . . . . ?
C31A C32A C33A C34A -5.2(16) . . . . ?
C32A C31A C36A C35A -5.8(14) . . . . ?
C32A C33A C34A C35A -4.5(17) . . . . ?
C33A C34A C35A C36A 8.0(18) . . . . ?
C34A C35A C36A C31A -2.6(15) . . . . ?
C36A C31A C32A C33A 9.8(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.717
####################################################################### 
# 
# 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_klb-7
_database_code_depnum_ccdc_archive 'CCDC 1977884'
loop_
_audit_author_name
_audit_author_address
'Lingbing Kong'
;Shandong University
China
;
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_audit_creation_date             2020-06-09
_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         '2(C19 H29 B N O2)'
_chemical_formula_sum            'C38 H58 B2 N2 O4'
_chemical_formula_weight         628.48
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.0716(10)
_cell_length_b                   9.8412(13)
_cell_length_c                   11.5149(12)
_cell_angle_alpha                76.803(10)
_cell_angle_beta                 82.173(9)
_cell_angle_gamma                68.411(11)
_cell_volume                     929.1(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2294
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      75.3730
_cell_measurement_theta_min      3.9370
_shelx_estimated_absorpt_T_max   0.853
_shelx_estimated_absorpt_T_min   0.810
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8347
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.405
_diffrn_reflns_theta_min         3.950
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00  21.00   1.00    0.55    --  -48.45  38.00  90.00   82
  2  ω    -84.00   1.00   1.00    0.55    --  -48.45 109.00 -24.00   85
  3  ω     28.00  69.00   1.00    0.55    --   48.45-109.00-119.00   41
  4  ω     14.00  61.00   1.00    0.55    --   48.45 -38.00-150.00   47
  5  ω     69.00 108.00   1.00    4.00    --  106.49-109.00-119.00   39
  6  ω     35.00 129.00   1.00    4.00    --  106.49 -77.00-180.00   94
  7  ω    153.00 178.00   1.00    4.00    --  106.49  57.00-120.00   25
  8  ω    101.00 145.00   1.00    4.00    --  106.49 109.00 -24.00   44
  9  ω     92.00 141.00   1.00    4.00    --  106.49  57.00-120.00   49
 10  ω     94.00 174.00   1.00    4.00    --  106.49  57.00  60.00   80
 11  ω    152.00 178.00   1.00    4.00    --  106.49  19.00 150.00   26
 12  ω     94.00 164.00   1.00    4.00    --  106.49 125.00  90.00   70
 13  ω     94.00 149.00   1.00    4.00    --  106.49  19.00 150.00   55
 14  ω     74.00 114.00   1.00    4.00    --  106.49-125.00  60.00   40
 15  ω     34.00  69.00   1.00    4.00    --  106.49-125.00  60.00   35
 16  ω     34.00 109.00   1.00    4.00    --  106.49 -99.00  60.00   75
 17  ω     43.00 104.00   1.00    4.00    --  106.49 -99.00 150.00   61
 18  ω    -20.00  11.00   1.00    0.55    --   48.45 -38.00-150.00   31
 19  ω   -109.00 -71.00   1.00    0.55    --  -48.45-125.00  60.00   38
 20  ω   -120.00 -89.00   1.00    4.00    --  -86.25 -99.00  30.00   31
 21  ω   -125.00 -85.00   1.00    4.00    --  -86.25 -99.00 -30.00   40
 22  ω   -120.00 -79.00   1.00    4.00    --  -86.25-109.00-119.00   41
 23  ω   -111.00 -77.00   1.00    0.55    --  -48.45-125.00 -90.00   34
 24  ω   -154.00-127.00   1.00    4.00    --  -86.25 -99.00  30.00   27
 25  ω   -153.00-128.00   1.00    4.00    --  -86.25 -99.00 -30.00   25
 26  ω    -83.00 -57.00   1.00    4.00    --  -86.25 109.00 -24.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0600897000
_diffrn_orient_matrix_UB_12      -0.1078883000
_diffrn_orient_matrix_UB_13      -0.0410600000
_diffrn_orient_matrix_UB_21      0.0098008000
_diffrn_orient_matrix_UB_22      -0.0928196000
_diffrn_orient_matrix_UB_23      0.1279131000
_diffrn_orient_matrix_UB_31      -0.1725094000
_diffrn_orient_matrix_UB_32      0.0958581000
_diffrn_orient_matrix_UB_33      0.0299832000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2685
_reflns_number_total             3616
_reflns_odcompleteness_completeness 98.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     1042
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0803
_refine_ls_restrained_S_all      1.018
_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)+(0.0473P)²+1.2321P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2121
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8A-C7 \\sim C8B-C7 \\sim C9B-C7 \\sim C9A-C7 \\sim C7-C10B \\sim C7-C10A
\\sim C17A-C15 \\sim C16B-C15
 with sigma of 0.02
 C16A-C15 \\sim C17B-C15 \\sim C18A-C15 \\sim C18B-C15 \\sim C13B-C11 \\sim
C13A-C11 \\sim C14A-C11
 with sigma of 0.02
 C14B-C11 \\sim C12A-C11 \\sim C12B-C11
 with sigma of 0.02
 C19-O2 \\sim C20-O4
 with sigma of 0.01
 C1-B1 \\sim C1-B1A
 with sigma of 0.01
3. Restrained planarity
 B1, O1, C19, N1, N2, C20, O2, O3, O4, B2, C1
 with sigma of 0.01
 B1A, O1A, C19A, N1A, N2A, C20A, O2A, O3A, O4A, B2A, C1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C7 \\sim C8A \\sim C9A \\sim C10A \\sim C8B \\sim C9B \\sim C10B \\sim C11
\\sim C12A \\sim C13A \\sim C14A \\sim C12B \\sim C13B \\sim C14B \\sim C15
\\sim C16A \\sim C17A \\sim C18A \\sim C16B \\sim C17B \\sim C18B: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
B1 \\sim O1 \\sim C19 \\sim N1 \\sim N2 \\sim C20 \\sim O2 \\sim O3 \\sim O4
\\sim B2 \\sim B1A \\sim O1A \\sim C19A \\sim N1A \\sim N2A \\sim C20A \\sim
O2A \\sim O3A \\sim O4A \\sim B2A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(B1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(N2) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(B1A) \\sim Ueq,
Uanis(O1A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(N2A)
\\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O3A) \\sim Ueq,
Uanis(O4A) \\sim Ueq, Uanis(B2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 B1, O1, C19, N1, N2, C20, O2, O3, O4, B2, B1A, O1A, C19A, N1A, N2A, C20A, O2A,
  O3A, O4A, B2A, C7, C8A, C9A, C10A, C8B, C9B, C10B, C11, C12A, C13A, C14A,
 C12B, C13B, C14B, C15, C16A, C17A, C18A, C16B, C17B, C18B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Same fragment restrains
{B1, O1, C19, N1, N2, C20, O2, O3, O4, B2} sigma for 1-2: 0.01, 1-3: 0.04
as
{B1A, O1A, C19A, N1A, N2A, C20A, O2A, O3A, O4A, B2A}
7. Others
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13B)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13A)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
 Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17B)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(3)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17A)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(3)
 Sof(B1A)=Sof(O1A)=Sof(C19A)=Sof(N1A)=Sof(N2A)=Sof(C20A)=Sof(O2A)=Sof(O3A)=
 Sof(O4A)=Sof(B2A)=0.5*(1-FVAR(5))
 Sof(B1)=Sof(O1)=Sof(C19)=Sof(N1)=Sof(N2)=Sof(C20)=Sof(O2)=Sof(O3)=Sof(O4)=
 Sof(B2)=0.5*FVAR(5)
8.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
8.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
8.c Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C8B(H8BA,H8BB,
 H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C12A(H12A,H12B,H12C),
 C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C12B(H12D,H12E,H12F), C13B(H13D,
 H13E,H13F), C14B(H14D,H14E,H14F), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C),
 C18A(H18A,H18B,H18C), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C18B(H18D,
 H18E,H18F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.5128(16) 0.138(3) 0.380(3) 0.027(3) Uani 0.316(2) 1 d D U P A -1
O1 O 0.4443(12) 0.067(2) 0.314(2) 0.029(3) Uani 0.316(2) 1 d D U P A -1
C19 C 0.4185(14) -0.054(2) 0.399(2) 0.028(2) Uani 0.316(2) 1 d D U P A -1
N1 N 0.4627(14) -0.057(2) 0.4980(15) 0.031(2) Uani 0.316(2) 1 d D U P A -1
N2 N 0.5205(13) 0.060(2) 0.4908(15) 0.032(2) Uani 0.316(2) 1 d D U P A -1
C20 C 0.5696(16) 0.045(3) 0.613(2) 0.031(3) Uani 0.316(2) 1 d D U P A -1
O2 O 0.3611(15) -0.126(2) 0.359(2) 0.031(3) Uani 0.316(2) 1 d D U P A -1
O3 O 0.5384(14) -0.068(2) 0.680(2) 0.029(3) Uani 0.316(2) 1 d D U P A -1
O4 O 0.6246(15) 0.135(3) 0.627(3) 0.040(4) Uani 0.316(2) 1 d D U P A -1
B2 B 0.476(2) -0.144(3) 0.628(3) 0.029(3) Uani 0.316(2) 1 d D U P A -1
B1A B 0.556(2) 0.157(3) 0.440(3) 0.028(3) Uani 0.184(2) 1 d D U P A -2
O1A O 0.6091(16) 0.137(2) 0.560(2) 0.036(3) Uani 0.184(2) 1 d D U P A -2
C19A C 0.5748(19) 0.011(3) 0.629(2) 0.034(3) Uani 0.184(2) 1 d D U P A -2
N1A N 0.5132(16) -0.037(2) 0.564(2) 0.030(2) Uani 0.184(2) 1 d D U P A -2
N2A N 0.4984(15) 0.049(2) 0.447(2) 0.032(2) Uani 0.184(2) 1 d D U P A -2
C20A C 0.424(2) -0.020(4) 0.380(3) 0.031(3) Uani 0.184(2) 1 d D U P A -2
O2A O 0.612(2) -0.021(3) 0.731(2) 0.044(5) Uani 0.184(2) 1 d D U P A -2
O3A O 0.4001(17) -0.132(2) 0.4544(18) 0.032(3) Uani 0.184(2) 1 d D U P A -2
O4A O 0.400(2) 0.037(3) 0.276(2) 0.039(4) Uani 0.184(2) 1 d D U P A -2
B2A B 0.445(2) -0.160(3) 0.566(3) 0.029(3) Uani 0.184(2) 1 d D U P A -2
C1 C 0.56418(19) 0.28601(14) 0.32032(15) 0.0357(7) Uani 1 1 d D . . . .
C2 C 0.44663(15) 0.42616(16) 0.31100(15) 0.0307(6) Uani 1 1 d G . . A .
C3 C 0.47189(17) 0.54785(13) 0.23420(15) 0.0319(6) Uani 1 1 d G . . A .
H3 H 0.393246 0.641621 0.227959 0.038 Uiso 1 1 calc R . . . .
C4 C 0.6147(2) 0.52941(14) 0.16672(15) 0.0337(6) Uani 1 1 d G . . A .
C5 C 0.73224(16) 0.38926(17) 0.17604(15) 0.0345(6) Uani 1 1 d G . . A .
H5 H 0.827785 0.376919 0.130889 0.041 Uiso 1 1 calc R . . . .
C6 C 0.70699(17) 0.26756(13) 0.25284(16) 0.0325(6) Uani 1 1 d G . . A .
C7 C 0.6424(4) 0.6640(3) 0.0771(3) 0.0454(8) Uani 1 1 d D U . . .
C8A C 0.779(3) 0.613(3) -0.015(2) 0.077(6) Uani 0.251(18) 1 d D U P A 1
H8AA H 0.877996 0.578778 0.021576 0.116 Uiso 0.251(18) 1 calc GR . P A 1
H8AB H 0.774696 0.695574 -0.079924 0.116 Uiso 0.251(18) 1 calc GR . P A 1
H8AC H 0.768444 0.534124 -0.045276 0.116 Uiso 0.251(18) 1 calc GR . P A 1
C9A C 0.685(4) 0.757(3) 0.145(2) 0.067(5) Uani 0.251(18) 1 d D U P A 1
H9AA H 0.710549 0.835460 0.089705 0.101 Uiso 0.251(18) 1 calc GR . P A 1
H9AB H 0.774389 0.695845 0.191336 0.101 Uiso 0.251(18) 1 calc GR . P A 1
H9AC H 0.595897 0.799987 0.197311 0.101 Uiso 0.251(18) 1 calc GR . P A 1
C10A C 0.498(2) 0.751(3) 0.006(2) 0.066(5) Uani 0.251(18) 1 d D U P A 1
H10A H 0.516966 0.830613 -0.051902 0.099 Uiso 0.251(18) 1 calc GR . P A 1
H10B H 0.408190 0.790596 0.058374 0.099 Uiso 0.251(18) 1 calc GR . P A 1
H10C H 0.475656 0.685738 -0.034982 0.099 Uiso 0.251(18) 1 calc GR . P A 1
C8B C 0.7096(13) 0.6224(9) -0.0427(5) 0.062(2) Uani 0.749(18) 1 d D U P A 2
H8BA H 0.810676 0.543257 -0.033117 0.093 Uiso 0.749(18) 1 calc GR . P A 2
H8BB H 0.722891 0.707475 -0.097078 0.093 Uiso 0.749(18) 1 calc GR . P A 2
H8BC H 0.638075 0.590014 -0.074071 0.093 Uiso 0.749(18) 1 calc GR . P A 2
C9B C 0.7590(16) 0.7066(14) 0.1305(8) 0.085(3) Uani 0.749(18) 1 d D U P A 2
H9BA H 0.714485 0.735599 0.205473 0.128 Uiso 0.749(18) 1 calc GR . P A 2
H9BB H 0.780283 0.788356 0.076783 0.128 Uiso 0.749(18) 1 calc GR . P A 2
H9BC H 0.856121 0.622988 0.143183 0.128 Uiso 0.749(18) 1 calc GR . P A 2
C10B C 0.4869(9) 0.7989(8) 0.0552(9) 0.083(3) Uani 0.749(18) 1 d D U P A 2
H10D H 0.505688 0.873642 -0.008590 0.125 Uiso 0.749(18) 1 calc GR . P A 2
H10E H 0.451005 0.839260 0.126632 0.125 Uiso 0.749(18) 1 calc GR . P A 2
H10F H 0.407328 0.767613 0.033945 0.125 Uiso 0.749(18) 1 calc GR . P A 2
C11 C 0.8537(3) 0.1189(3) 0.2587(3) 0.0429(7) Uani 1 1 d D U . . .
C12A C 0.9219(13) 0.0843(14) 0.3838(9) 0.088(4) Uani 0.424(7) 1 d D U P A 1
H12A H 0.845408 0.064186 0.445069 0.132 Uiso 0.424(7) 1 calc GR . P A 1
H12B H 0.944250 0.168469 0.394655 0.132 Uiso 0.424(7) 1 calc GR . P A 1
H12C H 1.017900 -0.001171 0.388647 0.132 Uiso 0.424(7) 1 calc GR . P A 1
C13A C 0.9934(12) 0.1289(11) 0.1734(12) 0.082(4) Uani 0.424(7) 1 d D U P A 1
H13A H 1.030921 0.201144 0.190717 0.123 Uiso 0.424(7) 1 calc GR . P A 1
H13B H 0.960823 0.158580 0.092814 0.123 Uiso 0.424(7) 1 calc GR . P A 1
H13C H 1.077075 0.033484 0.182627 0.123 Uiso 0.424(7) 1 calc GR . P A 1
C14A C 0.8104(11) -0.0065(10) 0.2424(14) 0.072(3) Uani 0.424(7) 1 d D U P A 1
H14A H 0.747221 0.024775 0.174212 0.108 Uiso 0.424(7) 1 calc GR . P A 1
H14B H 0.750749 -0.036770 0.312346 0.108 Uiso 0.424(7) 1 calc GR . P A 1
H14C H 0.905217 -0.088623 0.229915 0.108 Uiso 0.424(7) 1 calc GR . P A 1
C12B C 0.9955(8) 0.1414(8) 0.2933(10) 0.081(3) Uani 0.576(7) 1 d D U P A 2
H12D H 0.975442 0.163899 0.372045 0.121 Uiso 0.576(7) 1 calc GR . P A 2
H12E H 1.015179 0.222555 0.237451 0.121 Uiso 0.576(7) 1 calc GR . P A 2
H12F H 1.086694 0.052266 0.292442 0.121 Uiso 0.576(7) 1 calc GR . P A 2
C13B C 0.8921(11) 0.0822(9) 0.1297(7) 0.086(3) Uani 0.576(7) 1 d D U P A 2
H13D H 0.907698 0.165524 0.074281 0.129 Uiso 0.576(7) 1 calc GR . P A 2
H13E H 0.805195 0.062530 0.106666 0.129 Uiso 0.576(7) 1 calc GR . P A 2
H13F H 0.986868 -0.003907 0.129280 0.129 Uiso 0.576(7) 1 calc GR . P A 2
C14B C 0.8315(8) -0.0181(6) 0.3378(8) 0.063(2) Uani 0.576(7) 1 d D U P A 2
H14D H 0.813141 -0.005285 0.419347 0.095 Uiso 0.576(7) 1 calc GR . P A 2
H14E H 0.925264 -0.103340 0.330495 0.095 Uiso 0.576(7) 1 calc GR . P A 2
H14F H 0.742061 -0.032867 0.313858 0.095 Uiso 0.576(7) 1 calc GR . P A 2
C15 C 0.2829(3) 0.4623(3) 0.3848(3) 0.0364(7) Uani 1 1 d D U . . .
C16A C 0.148(2) 0.495(4) 0.305(2) 0.072(5) Uani 0.154(6) 1 d D U P A 1
H16A H 0.146438 0.402600 0.291234 0.109 Uiso 0.154(6) 1 calc GR . P A 1
H16B H 0.165317 0.555170 0.229526 0.109 Uiso 0.154(6) 1 calc GR . P A 1
H16C H 0.049036 0.546562 0.342641 0.109 Uiso 0.154(6) 1 calc GR . P A 1
C17A C 0.232(3) 0.610(2) 0.427(3) 0.056(5) Uani 0.154(6) 1 d D U P A 1
H17A H 0.299329 0.600703 0.487958 0.084 Uiso 0.154(6) 1 calc GR . P A 1
H17B H 0.124029 0.636110 0.457863 0.084 Uiso 0.154(6) 1 calc GR . P A 1
H17C H 0.241990 0.686385 0.360439 0.084 Uiso 0.154(6) 1 calc GR . P A 1
C18A C 0.251(3) 0.337(2) 0.476(2) 0.067(6) Uani 0.154(6) 1 d D U P A 1
H18A H 0.138862 0.363434 0.494540 0.101 Uiso 0.154(6) 1 calc GR . P A 1
H18B H 0.303591 0.321963 0.547517 0.101 Uiso 0.154(6) 1 calc GR . P A 1
H18C H 0.290673 0.247752 0.444280 0.101 Uiso 0.154(6) 1 calc GR . P A 1
C16B C 0.1666(5) 0.6155(5) 0.3337(6) 0.0763(18) Uani 0.846(6) 1 d D U P A 2
H16D H 0.158795 0.623079 0.250036 0.114 Uiso 0.846(6) 1 calc GR . P A 2
H16E H 0.203883 0.691089 0.344638 0.114 Uiso 0.846(6) 1 calc GR . P A 2
H16F H 0.064063 0.628916 0.374367 0.114 Uiso 0.846(6) 1 calc GR . P A 2
C17B C 0.3087(5) 0.4577(7) 0.5120(4) 0.0781(17) Uani 0.846(6) 1 d D U P A 2
H17D H 0.349537 0.534117 0.514570 0.117 Uiso 0.846(6) 1 calc GR . P A 2
H17E H 0.383397 0.362136 0.544212 0.117 Uiso 0.846(6) 1 calc GR . P A 2
H17F H 0.209659 0.473958 0.558456 0.117 Uiso 0.846(6) 1 calc GR . P A 2
C18B C 0.1997(5) 0.3554(6) 0.3802(5) 0.0657(14) Uani 0.846(6) 1 d D U P A 2
H18D H 0.247235 0.262694 0.433574 0.098 Uiso 0.846(6) 1 calc GR . P A 2
H18E H 0.209947 0.338131 0.300284 0.098 Uiso 0.846(6) 1 calc GR . P A 2
H18F H 0.089303 0.397571 0.403980 0.098 Uiso 0.846(6) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 O1 1.47(4) . ?
B1 N2 1.32(3) . ?
B1 C1 1.66(3) . ?
O1 C19 1.43(3) . ?
C19 N1 1.25(3) . ?
C19 O2 1.211(11) . ?
N1 N2 1.419(7) . ?
N1 B2 1.54(3) . ?
N2 C20 1.50(3) . ?
C20 O3 1.31(4) . ?
C20 O4 1.210(11) . ?
O3 B2 1.35(4) . ?
B1A O1A 1.47(4) . ?
B1A N2A 1.32(3) . ?
B1A C1 1.67(3) . ?
O1A C19A 1.43(3) . ?
C19A N1A 1.25(3) . ?
C19A O2A 1.210(12) . ?
N1A N2A 1.417(8) . ?
N1A B2A 1.54(4) . ?
N2A C20A 1.49(3) . ?
C20A O3A 1.30(4) . ?
C20A O4A 1.209(13) . ?
O3A B2A 1.34(4) . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 C15 1.569(3) . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C7 1.559(3) . ?
C5 C6 1.3900 . ?
C6 C11 1.570(3) . ?
C7 C8A 1.528(13) . ?
C7 C9A 1.507(14) . ?
C7 C10A 1.509(13) . ?
C7 C8B 1.513(6) . ?
C7 C9B 1.515(8) . ?
C7 C10B 1.543(7) . ?
C11 C12A 1.561(10) . ?
C11 C13A 1.513(8) . ?
C11 C14A 1.481(9) . ?
C11 C12B 1.501(7) . ?
C11 C13B 1.572(8) . ?
C11 C14B 1.508(6) . ?
C15 C16A 1.526(14) . ?
C15 C17A 1.525(13) . ?
C15 C18A 1.512(14) . ?
C15 C16B 1.525(5) . ?
C15 C17B 1.502(5) . ?
C15 C18B 1.517(5) . ?

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
O1 B1 C1 124(2) . . ?
N2 B1 O1 105(2) . . ?
N2 B1 C1 131(2) . . ?
C19 O1 B1 105(2) . . ?
N1 C19 O1 109.2(19) . . ?
O2 C19 O1 114(3) . . ?
O2 C19 N1 137(3) . . ?
C19 N1 N2 110.5(14) . . ?
C19 N1 B2 143(2) . . ?
N2 N1 B2 106.8(15) . . ?
B1 N2 N1 109.8(17) . . ?
B1 N2 C20 144(2) . . ?
N1 N2 C20 105.9(15) . . ?
O3 C20 N2 107(2) . . ?
O4 C20 N2 117(3) . . ?
O4 C20 O3 136(3) . . ?
C20 O3 B2 118(2) . . ?
O3 B2 N1 103(2) . . ?
O1A B1A C1 128(2) . . ?
N2A B1A O1A 106(2) . . ?
N2A B1A C1 126(3) . . ?
C19A O1A B1A 105(2) . . ?
N1A C19A O1A 109(2) . . ?
O2A C19A O1A 114(3) . . ?
O2A C19A N1A 137(3) . . ?
C19A N1A N2A 111.2(16) . . ?
C19A N1A B2A 142(2) . . ?
N2A N1A B2A 106.8(16) . . ?
B1A N2A N1A 109.0(18) . . ?
B1A N2A C20A 145(3) . . ?
N1A N2A C20A 105.5(16) . . ?
O3A C20A N2A 107(2) . . ?
O4A C20A N2A 117(3) . . ?
O4A C20A O3A 136(3) . . ?
C20A O3A B2A 117(2) . . ?
O3A B2A N1A 103(2) . . ?
C2 C1 B1 118.1(2) . . ?
C2 C1 B1A 118.3(3) . . ?
C2 C1 C6 120.0 . . ?
C6 C1 B1 119.5(3) . . ?
C6 C1 B1A 119.0(3) . . ?
C1 C2 C3 120.0 . . ?
C1 C2 C15 124.88(13) . . ?
C3 C2 C15 115.10(13) . . ?
C2 C3 C4 120.0 . . ?
C3 C4 C7 120.50(16) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C7 119.47(16) . . ?
C4 C5 C6 120.0 . . ?
C1 C6 C11 125.87(14) . . ?
C5 C6 C1 120.0 . . ?
C5 C6 C11 114.05(14) . . ?
C8A C7 C4 111.9(9) . . ?
C9A C7 C4 109.1(11) . . ?
C9A C7 C8A 107.8(16) . . ?
C9A C7 C10A 113.0(13) . . ?
C10A C7 C4 109.7(7) . . ?
C10A C7 C8A 105.2(13) . . ?
C8B C7 C4 110.9(4) . . ?
C8B C7 C9B 109.8(5) . . ?
C8B C7 C10B 107.3(4) . . ?
C9B C7 C4 107.3(4) . . ?
C9B C7 C10B 109.6(5) . . ?
C10B C7 C4 112.0(3) . . ?
C6 C11 C13B 107.7(3) . . ?
C12A C11 C6 106.6(4) . . ?
C13A C11 C6 115.0(4) . . ?
C13A C11 C12A 102.9(8) . . ?
C14A C11 C6 112.3(4) . . ?
C14A C11 C12A 110.5(8) . . ?
C14A C11 C13A 109.1(7) . . ?
C12B C11 C6 109.4(4) . . ?
C12B C11 C13B 107.6(6) . . ?
C12B C11 C14B 110.1(5) . . ?
C14B C11 C6 116.4(3) . . ?
C14B C11 C13B 105.1(5) . . ?
C16A C15 C2 110.5(10) . . ?
C17A C15 C2 112.7(7) . . ?
C17A C15 C16A 100.5(16) . . ?
C18A C15 C2 118.2(8) . . ?
C18A C15 C16A 97.4(17) . . ?
C18A C15 C17A 114.8(15) . . ?
C16B C15 C2 111.6(2) . . ?
C17B C15 C2 109.3(3) . . ?
C17B C15 C16B 109.1(4) . . ?
C17B C15 C18B 110.2(4) . . ?
C18B C15 C2 112.0(2) . . ?
C18B C15 C16B 104.5(4) . . ?

_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 1.644
_oxdiff_exptl_absorpt_empirical_full_min 0.324
