# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_MaMi066_NiHe_a
_database_code_depnum_ccdc_archive 'CCDC 2468860'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2025-07-01 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-22)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H39 B3 N6'
_chemical_formula_sum            'C19 H39 B3 N6'
_chemical_formula_weight         383.99

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.87710(10)
_cell_length_b                   19.8671(2)
_cell_length_c                   15.1839(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.3510(10)
_cell_angle_gamma                90
_cell_volume                     2356.68(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15593
_cell_measurement_theta_min      2.9780
_cell_measurement_theta_max      74.6960


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800).
;
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.085
_exptl_absorpt_coefficient_mu    0.492
_shelx_estimated_absorpt_T_min   0.820
_shelx_estimated_absorpt_T_max   0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64620
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 
ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -2 -1 0.0431
0 2 1 0.0422
0 -2 1 0.0341
0 -1 1 0.0230
0 1 -1 0.0930
-1 -2 -2 0.1387
1 2 2 0.1279
-1 0 0 0.1802
1 0 0 0.2196
-2 2 1 0.1815
1 -2 -1 0.1816
0 -1 2 0.0274
0 0 -1 0.0962
0 0 1 0.0303

_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 
   # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
 --------------------------------------------------------------------------
   1  ω     98.00 130.00   0.50    0.10    --   85.25  55.00 143.45   64
   2  ω    104.00 135.00   0.50    0.10    --   85.25  46.00  91.34   62
   3  ω    100.00 133.00   0.50    0.10    --   85.25  50.00  44.23   66
   4  ω     99.00 126.00   0.50    0.10    --   85.25  44.00 -12.96   54
   5  ω    104.00 133.00   0.50    0.10    --   85.25  41.00  10.88   58
   6  ω     98.00 126.00   0.50    0.10    --   85.25  43.00  37.60   56
   7  ω    100.00 131.00   0.50    0.10    --   85.25  37.00  70.15   62
   8  ω    104.00 134.00   0.50    0.10    --   85.25  31.00 -42.79   60
   9  ω    100.00 126.00   0.50    0.10    --   85.25  58.00-114.72   52
  10  ω    100.00 125.00   0.50    0.10    --   85.25  54.00-144.56   50
  11  ω    104.00 133.00   0.50    0.10    --   85.25  44.00-176.89   58
  12  ω     46.00 123.00   0.50    0.10    --   82.31  15.00 -90.00  154
  13  ω    107.00 132.00   0.50    0.10    --   85.25 115.00 -28.20   50
  14  ω    103.00 129.00   0.50    0.10    --   85.25 114.00 -70.78   52
  15  ω     46.00  71.00   0.50    0.10    --   85.25 -77.00 -79.17   50
  16  ω     44.00  69.00   0.50    0.10    --   85.25 -72.00   9.55   50
  17  ω     45.00  70.00   0.50    0.10    --   85.25 -75.00 109.85   50
  18  ω     46.00  71.00   0.50    0.10    --   85.25 -86.00  78.78   50
  19  ω     71.00  97.00   0.50    0.10    --   85.25-118.00 169.40   52
  20  ω     52.00  83.00   0.50    0.10    --   85.25-113.00  85.34   62
  21  ω     46.00  81.00   0.50    0.10    --   85.25 -98.00  24.07   70
  22  ω     37.00  70.00   0.50    0.10    --   85.25-118.00   5.70   66
  23  ω     45.00  70.00   0.50    0.10    --   82.31 -95.00   0.00   50
  24  ω     42.00  88.00   0.50    0.10    --   85.25 -96.00 -30.64   92
  25  ω     43.00  81.00   0.50    0.10    --   85.25-110.00 -62.16   76
  26  ω     39.00  68.00   0.50    0.10    --   85.25-135.00-124.29   58
  27  ω     40.00  90.00   0.50    0.10    --   82.31 -95.00-150.00  100
  28  ω     53.00  81.00   0.50    0.10    --   85.25-108.00 -90.72   56
  29  ω     16.00  66.00   0.50    0.10    --   58.61 -95.00 120.00  100
  30  ω     49.00  76.00   0.50    0.10    --   85.25 -92.00 115.20   54
  31  ω   -110.00 -31.00   0.50    0.10    --  -60.19 -15.00  60.00  158
  32  ω   -125.00 -91.00   0.50    0.10    --  -79.50 -60.00  68.58   68
  33  ω   -106.00 -71.00   0.50    0.10    --  -58.00 -51.00 -63.70   70
  34  ω   -128.00 -93.00   0.50    0.10    --  -79.50 -51.00-176.46   70
  35  ω   -128.00 -93.00   0.50    0.10    --  -79.50 -51.00 -74.93   70
  36  ω   -103.00 -68.00   0.50    0.10    --  -54.00 -50.00 -30.04   70
  37  ω   -105.00 -65.00   0.50    0.10    --  -54.00 -37.00 174.93   80
  38  ω    -98.00 -31.00   0.50    0.10    --  -79.50 121.00 -22.74  134

;
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            25080
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.683
_diffrn_reflns_theta_max         75.230
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4835
_reflns_number_gt                4085
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0705P)²+0.3273P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4835
_refine_ls_number_parameters     265
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1266
_refine_ls_wR_factor_gt          0.1230
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.54752(13) 0.71062(5) 0.67374(6) 0.0242(2) Uani 1 1 d . . . . .
N2 N 0.64301(13) 0.69038(5) 0.83270(6) 0.0248(2) Uani 1 1 d . . . . .
N3 N 0.19882(13) 0.65478(5) 0.74013(6) 0.0252(2) Uani 1 1 d . . . . .
N5 N 0.34749(14) 0.46848(5) 0.65534(7) 0.0295(2) Uani 1 1 d . . . . .
N6 N 0.64289(13) 0.50970(5) 0.70240(7) 0.0288(2) Uani 1 1 d . . . . .
N7 N 0.32235(14) 0.52977(5) 0.86546(7) 0.0293(2) Uani 1 1 d . . . . .
C1 C 0.48334(17) 0.68126(7) 0.58857(8) 0.0302(3) Uani 1 1 d . . . . .
H1A H 0.394498 0.710452 0.557820 0.045 Uiso 1 1 calc R U . . .
H1B H 0.434753 0.636793 0.597786 0.045 Uiso 1 1 calc R U . . .
H1C H 0.577383 0.676703 0.552516 0.045 Uiso 1 1 calc R U . . .
C2 C 0.61517(18) 0.77805(6) 0.66493(8) 0.0313(3) Uani 1 1 d . . . . .
H2A H 0.722077 0.775450 0.638436 0.047 Uiso 1 1 calc R U . . .
H2B H 0.637391 0.799051 0.723679 0.047 Uiso 1 1 calc R U . . .
H2C H 0.531623 0.805101 0.626745 0.047 Uiso 1 1 calc R U . . .
C3 C 0.81803(16) 0.71217(7) 0.82926(8) 0.0300(3) Uani 1 1 d . . . . .
H3A H 0.839685 0.714810 0.767217 0.045 Uiso 1 1 calc R U . . .
H3B H 0.897180 0.679805 0.861230 0.045 Uiso 1 1 calc R U . . .
H3C H 0.835323 0.756596 0.857006 0.045 Uiso 1 1 calc R U . . .
C4 C 0.61308(17) 0.67323(7) 0.92241(8) 0.0302(3) Uani 1 1 d . . . . .
H4A H 0.495397 0.657035 0.921689 0.045 Uiso 1 1 calc R U . . .
H4B H 0.630441 0.713204 0.960310 0.045 Uiso 1 1 calc R U . . .
H4C H 0.693220 0.637872 0.945774 0.045 Uiso 1 1 calc R U . . .
C5 C 0.35544(15) 0.63490(6) 0.76429(7) 0.0231(2) Uani 1 1 d . . . . .
C6 C 0.22569(18) 0.56566(7) 0.92659(9) 0.0350(3) Uani 1 1 d . . . . .
H6A H 0.209581 0.612567 0.907361 0.052 Uiso 1 1 calc R U . . .
H6B H 0.288822 0.564325 0.986526 0.052 Uiso 1 1 calc R U . . .
H6C H 0.113778 0.544179 0.926924 0.052 Uiso 1 1 calc R U . . .
C7 C 0.3434(2) 0.45882(7) 0.88883(10) 0.0397(3) Uani 1 1 d . . . . .
H7A H 0.230898 0.437124 0.884014 0.059 Uiso 1 1 calc R U . . .
H7B H 0.400182 0.454792 0.949912 0.059 Uiso 1 1 calc R U . . .
H7C H 0.413401 0.436856 0.848264 0.059 Uiso 1 1 calc R U . . .
C8 C 0.16348(17) 0.47747(7) 0.65050(10) 0.0374(3) Uani 1 1 d . . . . .
H8A H 0.113192 0.480325 0.588148 0.056 Uiso 1 1 calc R U . . .
H8B H 0.139251 0.519040 0.681325 0.056 Uiso 1 1 calc R U . . .
H8C H 0.113868 0.439112 0.678749 0.056 Uiso 1 1 calc R U . . .
C9 C 0.38897(18) 0.40767(7) 0.60921(9) 0.0345(3) Uani 1 1 d . . . . .
H9A H 0.367129 0.415064 0.544944 0.052 Uiso 1 1 calc R U . . .
H9B H 0.317723 0.370425 0.625634 0.052 Uiso 1 1 calc R U . . .
H9C H 0.509994 0.396539 0.625965 0.052 Uiso 1 1 calc R U . . .
C10 C 0.77267(17) 0.53425(7) 0.77182(9) 0.0343(3) Uani 1 1 d . . . . .
H10A H 0.858552 0.499066 0.787225 0.051 Uiso 1 1 calc R U . . .
H10B H 0.718794 0.546018 0.824463 0.051 Uiso 1 1 calc R U . . .
H10C H 0.828040 0.574183 0.750530 0.051 Uiso 1 1 calc R U . . .
C11 C 0.71215(17) 0.49607(7) 0.61986(9) 0.0336(3) Uani 1 1 d . . . . .
H11A H 0.618018 0.491561 0.571358 0.050 Uiso 1 1 calc R U . . .
H11B H 0.778342 0.454189 0.625737 0.050 Uiso 1 1 calc R U . . .
H11C H 0.786730 0.533294 0.606881 0.050 Uiso 1 1 calc R U . . .
C12 C 0.16611(15) 0.72054(6) 0.70447(8) 0.0250(3) Uani 1 1 d . . . . .
C13 C 0.08527(16) 0.72479(7) 0.61639(8) 0.0285(3) Uani 1 1 d . . . . .
C14 C 0.05466(17) 0.78796(7) 0.57835(9) 0.0328(3) Uani 1 1 d . . . . .
H14 H 0.005151 0.791228 0.518077 0.039 Uiso 1 1 calc R U . . .
C15 C 0.09493(18) 0.84625(7) 0.62658(9) 0.0349(3) Uani 1 1 d . . . . .
H15 H 0.076761 0.889062 0.599123 0.042 Uiso 1 1 calc R U . . .
C16 C 0.16192(17) 0.84148(7) 0.71520(9) 0.0314(3) Uani 1 1 d . . . . .
H16 H 0.184781 0.881435 0.749017 0.038 Uiso 1 1 calc R U . . .
C17 C 0.19643(16) 0.77923(6) 0.75573(8) 0.0263(3) Uani 1 1 d . . . . .
C18 C 0.03036(19) 0.66179(7) 0.56498(9) 0.0366(3) Uani 1 1 d . . . . .
H18A H -0.028761 0.674114 0.506461 0.055 Uiso 1 1 calc R U . . .
H18B H -0.047185 0.635762 0.597437 0.055 Uiso 1 1 calc R U . . .
H18C H 0.131358 0.634572 0.557643 0.055 Uiso 1 1 calc R U . . .
C19 C 0.25964(18) 0.77662(6) 0.85375(8) 0.0300(3) Uani 1 1 d . . . . .
H19A H 0.385059 0.775663 0.862451 0.045 Uiso 1 1 calc R U . . .
H19B H 0.215504 0.735990 0.879539 0.045 Uiso 1 1 calc R U . . .
H19C H 0.219420 0.816491 0.882947 0.045 Uiso 1 1 calc R U . . .
B1 B 0.52150(17) 0.68097(7) 0.75624(9) 0.0228(3) Uani 1 1 d . . . . .
B2 B 0.38016(17) 0.55745(7) 0.79009(9) 0.0257(3) Uani 1 1 d . . . . .
B3 B 0.46539(19) 0.50815(7) 0.71282(9) 0.0272(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 B1 1.4227(16) . ?
N1 C1 1.4494(15) . ?
N1 C2 1.4543(15) . ?
N2 B1 1.4193(16) . ?
N2 C3 1.4523(16) . ?
N2 C4 1.4524(15) . ?
N3 C5 1.3026(16) . ?
N3 C12 1.4250(15) . ?
N5 B3 1.4276(18) . ?
N5 C8 1.4529(17) . ?
N5 C9 1.4546(15) . ?
N6 B3 1.4274(18) . ?
N6 C11 1.4549(16) . ?
N6 C10 1.4554(16) . ?
N7 B2 1.3976(17) . ?
N7 C7 1.4577(16) . ?
N7 C6 1.4596(16) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 B2 1.5936(18) . ?
C5 B1 1.6139(18) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C17 1.4053(17) . ?
C12 C13 1.4083(17) . ?
C13 C14 1.3897(18) . ?
C13 C18 1.5089(18) . ?
C14 C15 1.385(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.3844(19) . ?
C15 H15 0.9500 . ?
C16 C17 1.3925(17) . ?
C16 H16 0.9500 . ?
C17 C19 1.5088(17) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
B2 B3 1.729(2) . ?

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 C1 123.09(10) . . ?
B1 N1 C2 123.93(10) . . ?
C1 N1 C2 112.25(10) . . ?
B1 N2 C3 123.63(10) . . ?
B1 N2 C4 124.25(10) . . ?
C3 N2 C4 111.86(10) . . ?
C5 N3 C12 120.24(10) . . ?
B3 N5 C8 122.00(11) . . ?
B3 N5 C9 125.76(11) . . ?
C8 N5 C9 111.21(10) . . ?
B3 N6 C11 124.89(11) . . ?
B3 N6 C10 122.28(11) . . ?
C11 N6 C10 112.35(10) . . ?
B2 N7 C7 122.75(11) . . ?
B2 N7 C6 125.42(11) . . ?
C7 N7 C6 111.72(10) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 B2 116.33(11) . . ?
N3 C5 B1 123.67(10) . . ?
B2 C5 B1 119.43(10) . . ?
N7 C6 H6A 109.5 . . ?
N7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N7 C7 H7A 109.5 . . ?
N7 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N7 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C8 H8A 109.5 . . ?
N5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N5 C9 H9A 109.5 . . ?
N5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N6 C10 H10A 109.5 . . ?
N6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N6 C11 H11A 109.5 . . ?
N6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C17 C12 C13 120.02(11) . . ?
C17 C12 N3 122.73(11) . . ?
C13 C12 N3 116.97(11) . . ?
C14 C13 C12 118.83(12) . . ?
C14 C13 C18 120.73(12) . . ?
C12 C13 C18 120.43(11) . . ?
C15 C14 C13 121.30(12) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C16 C15 C14 119.32(12) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 121.26(12) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C16 C17 C12 118.84(11) . . ?
C16 C17 C19 119.19(11) . . ?
C12 C17 C19 121.94(11) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 B1 N1 120.51(11) . . ?
N2 B1 C5 118.76(10) . . ?
N1 B1 C5 120.73(11) . . ?
N7 B2 C5 122.61(11) . . ?
N7 B2 B3 121.89(11) . . ?
C5 B2 B3 115.22(10) . . ?
N6 B3 N5 120.93(11) . . ?
N6 B3 B2 122.28(11) . . ?
N5 B3 B2 116.68(11) . . ?

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
C12 N3 C5 B2 -171.47(10) . . . . ?
C12 N3 C5 B1 -0.19(16) . . . . ?
C5 N3 C12 C17 -68.66(15) . . . . ?
C5 N3 C12 C13 117.38(12) . . . . ?
C17 C12 C13 C14 7.37(18) . . . . ?
N3 C12 C13 C14 -178.50(11) . . . . ?
C17 C12 C13 C18 -171.61(11) . . . . ?
N3 C12 C13 C18 2.52(17) . . . . ?
C12 C13 C14 C15 -2.97(19) . . . . ?
C18 C13 C14 C15 176.01(12) . . . . ?
C13 C14 C15 C16 -2.1(2) . . . . ?
C14 C15 C16 C17 2.8(2) . . . . ?
C15 C16 C17 C12 1.58(19) . . . . ?
C15 C16 C17 C19 -176.45(12) . . . . ?
C13 C12 C17 C16 -6.69(18) . . . . ?
N3 C12 C17 C16 179.53(11) . . . . ?
C13 C12 C17 C19 171.28(11) . . . . ?
N3 C12 C17 C19 -2.50(18) . . . . ?
C3 N2 B1 N1 -18.44(18) . . . . ?
C4 N2 B1 N1 167.88(11) . . . . ?
C3 N2 B1 C5 160.40(11) . . . . ?
C4 N2 B1 C5 -13.28(17) . . . . ?
C1 N1 B1 N2 150.36(12) . . . . ?
C2 N1 B1 N2 -40.19(17) . . . . ?
C1 N1 B1 C5 -28.46(17) . . . . ?
C2 N1 B1 C5 141.00(12) . . . . ?
N3 C5 B1 N2 126.99(12) . . . . ?
B2 C5 B1 N2 -61.98(15) . . . . ?
N3 C5 B1 N1 -54.17(16) . . . . ?
B2 C5 B1 N1 116.86(12) . . . . ?
C7 N7 B2 C5 179.45(12) . . . . ?
C6 N7 B2 C5 3.59(19) . . . . ?
C7 N7 B2 B3 5.72(19) . . . . ?
C6 N7 B2 B3 -170.14(12) . . . . ?
N3 C5 B2 N7 -67.81(15) . . . . ?
B1 C5 B2 N7 120.52(13) . . . . ?
N3 C5 B2 B3 106.31(12) . . . . ?
B1 C5 B2 B3 -65.36(14) . . . . ?
C11 N6 B3 N5 25.11(19) . . . . ?
C10 N6 B3 N5 -163.40(12) . . . . ?
C11 N6 B3 B2 -150.85(12) . . . . ?
C10 N6 B3 B2 20.65(18) . . . . ?
C8 N5 B3 N6 -165.53(12) . . . . ?
C9 N5 B3 N6 27.15(19) . . . . ?
C8 N5 B3 B2 10.65(18) . . . . ?
C9 N5 B3 B2 -156.67(12) . . . . ?
N7 B2 B3 N6 -109.83(14) . . . . ?
C5 B2 B3 N6 76.00(15) . . . . ?
N7 B2 B3 N5 74.05(16) . . . . ?
C5 B2 B3 N5 -100.12(13) . . . . ?

_refine_diff_density_max         0.223
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.044


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive
####################################################################### 
# 
# 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_MaMi072_NiHe_a
_database_code_depnum_ccdc_archive 'CCDC 2468864'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2025-07-01 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_MaMi072_NiHe_a      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report
RESPONSE: reflections affected by beamstop
;
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-22)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        2
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H45 B4 N7'
_chemical_formula_sum            'C21 H45 B4 N7'
_chemical_formula_weight         438.88

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.82380(10)
_cell_length_b                   35.3927(2)
_cell_length_c                   8.66360(10)
_cell_angle_alpha                90
_cell_angle_beta                 115.4750(10)
_cell_angle_gamma                90
_cell_volume                     2719.38(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    39005
_cell_measurement_theta_min      4.9620
_cell_measurement_theta_max      73.8100


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.078
_exptl_absorpt_coefficient_mu    0.485
_shelx_estimated_absorpt_T_min   0.909
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 
ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -1 -2 0.0717
1 -1 -1 0.0589
-1 2 1 0.0879
0 1 0 0.0796
-1 0 0 0.0585
0 -2 0 0.0532
1 1 0 0.0250
1 -1 1 0.0358
-1 1 -1 0.0826
0 -2 -1 0.0923
0 2 1 0.0718
-2 -2 1 0.0637
-1 -1 0 0.0450

_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 
   # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
 --------------------------------------------------------------------------
   1  ω     40.00  72.00   0.50    0.20    --   36.00  76.00-178.18   64
   2  ω     45.00  77.00   0.50    0.20    --   36.00  63.00  -0.89   64
   3  ω     61.00  93.00   0.50    0.20    --   52.00  62.00  95.03   64
   4  ω     87.00 122.00   0.50    0.20    --   76.07  45.00 122.13   70
   5  ω     33.00 109.00   0.50    0.20    --   65.37  11.00 114.00  152
   6  ω     39.00 115.00   0.50    0.20    --   71.48  11.00 114.00  152
   7  ω     45.00 121.00   0.50    0.20    --   76.87  11.00 114.00  152
   8  ω     28.00 103.00   0.50    0.20    --   65.37   0.00  30.00  150
   9  ω     28.00 103.00   0.50    0.20    --   65.37   0.00 -60.00  150
  10  ω    -71.00 -40.00   0.50    0.20    --  -32.00 -67.00  10.31   62
  11  ω    -81.00 -49.00   0.50    0.20    --  -44.00 -73.00 121.19   64
  12  ω    -73.00 -42.00   0.50    0.20    --  -36.00 -72.00  58.80   62
  13  ω    -69.00 -38.00   0.50    0.20    --  -32.00 -72.00 -52.18   62
  14  ω    -63.00 -32.00   0.50    0.20    --  -28.00 -76.00-117.82   62
  15  ω     28.00  74.00   0.50    0.20    --   65.37 -95.00   0.00   92
  16  ω     22.00  94.00   0.50    0.20    --   65.37-126.00   0.00  144
  17  ω     33.00 106.00   0.50    0.20    --   76.87-126.00  30.00  146
  18  ω     33.00 106.00   0.50    0.20    --   76.87-126.00 120.00  146
  19  ω     33.00 106.00   0.50    0.20    --   76.87-126.00  60.00  146
  20  ω     33.00 106.00   0.50    0.20    --   76.87-126.00 150.00  146
  21  ω     28.00 100.00   0.50    0.20    --   71.48-126.00-180.00  144
  22  ω     33.00 106.00   0.50    0.20    --   76.87-126.00-180.00  146
  23  ω     33.00 106.00   0.50    0.20    --   76.87-126.00-150.00  146
  24  ω     33.00 106.00   0.50    0.20    --   76.87-126.00 -90.00  146
  25  ω     28.00  74.00   0.50    0.20    --   65.37 -95.00 150.00   92
  26  ω     34.00  80.00   0.50    0.20    --   71.48 -95.00  90.00   92
  27  ω     28.00  74.00   0.50    0.20    --   65.37 -95.00  60.00   92
  28  ω     14.00  42.00   0.50    0.20    --   16.00  86.00  96.32   56
  29  ω     14.00  41.00   0.50    0.20    --   20.00  92.00 169.09   54
  30  ω   -102.00 -30.00   0.50    0.20    --  -73.64 126.00 150.00  144
  31  ω   -105.00 -32.00   0.50    0.20    --  -75.90 126.00   0.00  146
  32  ω    -42.00 -15.00   0.50    0.20    --  -12.00 128.00 120.81   54
  33  ω     -4.00  22.00   0.50    0.20    --    8.00 100.00 -23.07   52
  34  ω    -94.00 -22.00   0.50    0.20    --  -65.34 126.00-150.00  144
  35  ω   -105.00 -32.00   0.50    0.20    --  -75.90 126.00-180.00  146
  36  ω   -105.00 -32.00   0.50    0.20    --  -75.90 126.00-120.00  146
  37  ω   -117.00 -41.00   0.50    0.20    --  -73.64 -11.00 -58.00  152
  38  ω   -100.00 -68.00   0.50    0.20    --  -64.00 -75.00  59.46   64
  39  ω   -100.00 -69.00   0.50    0.20    --  -64.00 -74.00 -43.91   62
  40  ω   -103.00 -72.00   0.50    0.20    --  -64.00 -67.00  12.61   62
  41  ω   -100.00 -68.00   0.50    0.20    --  -64.00 -75.00 -72.22   64
  42  ω    -88.00 -57.00   0.50    0.20    --  -52.00 -74.00-122.00   62
  43  ω    -94.00 -63.00   0.50    0.20    --  -56.00 -71.00-152.71   62
  44  ω   -117.00 -86.00   0.50    0.20    --  -77.32 -65.00-153.33   62
  45  ω   -117.00 -86.00   0.50    0.20    --  -77.32 -65.00-117.12   62
  46  ω   -122.00 -88.00   0.50    0.20    --  -77.32 -47.00-101.97   68
  47  ω   -118.00 -83.00   0.50    0.20    --  -72.00 -44.00 -60.78   70
  48  ω   -109.00 -33.00   0.50    0.20    --  -65.34 -11.00 -58.00  152
  49  ω   -119.00 -43.00   0.50    0.20    --  -75.90 -11.00 -58.00  152
  50  ω   -109.00 -75.00   0.50    0.20    --  -64.00 -46.00 106.71   68
  51  ω   -120.00 -88.00   0.50    0.20    --  -77.32 -55.00 162.89   64
  52  ω   -113.00 -81.00   0.50    0.20    --  -72.00 -62.00 178.89   64

;
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            63499
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.497
_diffrn_reflns_theta_max         74.271
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5454
_reflns_number_gt                5010
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²+0.7303P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5454
_refine_ls_number_parameters     303
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0926
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.80024(9) 0.43707(2) 0.29589(11) 0.02368(18) Uani 1 1 d . . . . .
N2 N 0.77233(9) 0.37409(2) 0.15856(10) 0.02174(18) Uani 1 1 d . . . . .
N3 N 0.42358(9) 0.40517(2) 0.15904(10) 0.02223(18) Uani 1 1 d . . . . .
N4 N 0.64224(8) 0.37899(2) 0.59634(10) 0.01952(17) Uani 1 1 d . . . . .
N5 N 0.62277(9) 0.29516(2) 0.46215(11) 0.02339(18) Uani 1 1 d . . . . .
N6 N 0.27978(9) 0.32277(2) 0.49552(11) 0.02372(18) Uani 1 1 d . . . . .
N8 N 0.23488(9) 0.30121(3) 0.20264(12) 0.0276(2) Uani 1 1 d . . . . .
C1 C 0.95689(13) 0.44417(3) 0.33279(16) 0.0352(3) Uani 1 1 d . . . . .
H1A H 1.007407 0.420155 0.335182 0.053 Uiso 1 1 calc R U . . .
H1B H 1.007284 0.456649 0.444183 0.053 Uiso 1 1 calc R U . . .
H1C H 0.961666 0.460506 0.243911 0.053 Uiso 1 1 calc R U . . .
C2 C 0.72773(12) 0.47056(3) 0.32340(14) 0.0288(2) Uani 1 1 d . . . . .
H2A H 0.628356 0.463772 0.315901 0.043 Uiso 1 1 calc R U . . .
H2B H 0.715944 0.489478 0.235925 0.043 Uiso 1 1 calc R U . . .
H2C H 0.790022 0.481006 0.436897 0.043 Uiso 1 1 calc R U . . .
C3 C 0.85717(13) 0.38227(3) 0.05935(14) 0.0301(2) Uani 1 1 d . . . . .
H3A H 0.864516 0.409682 0.048972 0.045 Uiso 1 1 calc R U . . .
H3B H 0.805295 0.371106 -0.054813 0.045 Uiso 1 1 calc R U . . .
H3C H 0.958638 0.371498 0.117331 0.045 Uiso 1 1 calc R U . . .
C4 C 0.70795(11) 0.33636(3) 0.12196(13) 0.0260(2) Uani 1 1 d . . . . .
H4A H 0.646316 0.332160 0.184196 0.039 Uiso 1 1 calc R U . . .
H4B H 0.789279 0.317636 0.158090 0.039 Uiso 1 1 calc R U . . .
H4C H 0.644848 0.333844 -0.001105 0.039 Uiso 1 1 calc R U . . .
C5 C 0.40199(12) 0.42571(3) 0.00408(13) 0.0298(2) Uani 1 1 d . . . . .
H5A H 0.499362 0.428752 -0.000451 0.045 Uiso 1 1 calc R U . . .
H5B H 0.358972 0.450644 0.005032 0.045 Uiso 1 1 calc R U . . .
H5C H 0.333151 0.411528 -0.096368 0.045 Uiso 1 1 calc R U . . .
C6 C 0.28071(11) 0.39982(3) 0.17055(13) 0.0261(2) Uani 1 1 d . . . . .
H6A H 0.299366 0.387226 0.278561 0.039 Uiso 1 1 calc R U . . .
H6B H 0.213366 0.384197 0.074698 0.039 Uiso 1 1 calc R U . . .
H6C H 0.233587 0.424451 0.166104 0.039 Uiso 1 1 calc R U . . .
C7 C 0.57954(9) 0.36776(3) 0.43829(12) 0.01824(19) Uani 1 1 d . . . . .
C8 C 0.78552(11) 0.29890(3) 0.52194(15) 0.0302(2) Uani 1 1 d . . . . .
H8A H 0.810263 0.325189 0.509011 0.045 Uiso 1 1 calc R U . . .
H8B H 0.819158 0.282405 0.454277 0.045 Uiso 1 1 calc R U . . .
H8C H 0.836445 0.291635 0.642669 0.045 Uiso 1 1 calc R U . . .
C9 C 0.57980(13) 0.25569(3) 0.46234(16) 0.0325(2) Uani 1 1 d . . . . .
H9A H 0.469764 0.253795 0.415663 0.049 Uiso 1 1 calc R U . . .
H9B H 0.625212 0.246002 0.579716 0.049 Uiso 1 1 calc R U . . .
H9C H 0.615552 0.240777 0.391789 0.049 Uiso 1 1 calc R U . . .
C10 C 0.38387(12) 0.32702(3) 0.67484(13) 0.0290(2) Uani 1 1 d . . . . .
H10A H 0.487722 0.325019 0.687716 0.044 Uiso 1 1 calc R U . . .
H10B H 0.365023 0.307116 0.741872 0.044 Uiso 1 1 calc R U . . .
H10C H 0.369006 0.351797 0.715758 0.044 Uiso 1 1 calc R U . . .
C11 C 0.12571(12) 0.32987(3) 0.46867(16) 0.0338(3) Uani 1 1 d . . . . .
H11A H 0.060635 0.331644 0.345793 0.051 Uiso 1 1 calc R U . . .
H11B H 0.121337 0.353653 0.524315 0.051 Uiso 1 1 calc R U . . .
H11C H 0.091084 0.309121 0.517755 0.051 Uiso 1 1 calc R U . . .
C12 C 0.27769(13) 0.30175(4) 0.06153(15) 0.0387(3) Uani 1 1 d . . . . .
H12A H 0.371619 0.316027 0.095095 0.058 Uiso 1 1 calc R U . . .
H12B H 0.197675 0.313798 -0.038037 0.058 Uiso 1 1 calc R U . . .
H12C H 0.292624 0.275805 0.032431 0.058 Uiso 1 1 calc R U . . .
C13 C 0.09642(12) 0.27998(4) 0.15890(17) 0.0386(3) Uani 1 1 d . . . . .
H13A H 0.083256 0.274923 0.262869 0.058 Uiso 1 1 calc R U . . .
H13B H 0.102114 0.256007 0.105402 0.058 Uiso 1 1 calc R U . . .
H13C H 0.010586 0.294720 0.078945 0.058 Uiso 1 1 calc R U . . .
C14 C 0.69685(10) 0.41630(3) 0.64674(11) 0.01959(19) Uani 1 1 d . . . . .
C15 C 0.60188(11) 0.44437(3) 0.66109(12) 0.0224(2) Uani 1 1 d . . . . .
C16 C 0.66552(12) 0.47861(3) 0.73876(13) 0.0270(2) Uani 1 1 d . . . . .
H16 H 0.602240 0.497746 0.749319 0.032 Uiso 1 1 calc R U . . .
C17 C 0.81885(12) 0.48526(3) 0.80070(14) 0.0289(2) Uani 1 1 d . . . . .
H17 H 0.860434 0.508596 0.854544 0.035 Uiso 1 1 calc R U . . .
C18 C 0.91128(11) 0.45753(3) 0.78341(13) 0.0258(2) Uani 1 1 d . . . . .
H18 H 1.016145 0.462296 0.823573 0.031 Uiso 1 1 calc R U . . .
C19 C 0.85304(11) 0.42293(3) 0.70841(12) 0.0215(2) Uani 1 1 d . . . . .
C20 C 0.43465(11) 0.43794(3) 0.59645(14) 0.0262(2) Uani 1 1 d . . . . .
H20A H 0.394893 0.454481 0.658121 0.039 Uiso 1 1 calc R U . . .
H20B H 0.416098 0.411507 0.615265 0.039 Uiso 1 1 calc R U . . .
H20C H 0.384259 0.443641 0.473933 0.039 Uiso 1 1 calc R U . . .
C21 C 0.95428(11) 0.39246(3) 0.69574(13) 0.0245(2) Uani 1 1 d . . . . .
H21A H 1.058516 0.401634 0.744249 0.037 Uiso 1 1 calc R U . . .
H21B H 0.922415 0.385739 0.575430 0.037 Uiso 1 1 calc R U . . .
H21C H 0.947922 0.370146 0.759281 0.037 Uiso 1 1 calc R U . . .
B1 B 0.72274(12) 0.40188(3) 0.24257(13) 0.0200(2) Uani 1 1 d . . . . .
B2 B 0.56560(12) 0.39275(3) 0.27786(13) 0.0194(2) Uani 1 1 d . . . . .
B3 B 0.51966(12) 0.32501(3) 0.42098(13) 0.0198(2) Uani 1 1 d . . . . .
B4 B 0.33188(12) 0.31568(3) 0.36764(15) 0.0215(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 B1 1.4289(13) . ?
N1 C1 1.4528(13) . ?
N1 C2 1.4546(13) . ?
N2 B1 1.4280(14) . ?
N2 C4 1.4528(12) . ?
N2 C3 1.4607(13) . ?
N3 B2 1.4014(13) . ?
N3 C5 1.4598(13) . ?
N3 C6 1.4615(12) . ?
N4 C7 1.2987(12) . ?
N4 C14 1.4215(12) . ?
N5 B3 1.3995(13) . ?
N5 C8 1.4594(12) . ?
N5 C9 1.4595(13) . ?
N6 B4 1.4283(14) . ?
N6 C11 1.4510(12) . ?
N6 C10 1.4544(13) . ?
N8 B4 1.4290(14) . ?
N8 C12 1.4540(14) . ?
N8 C13 1.4541(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 B2 1.6029(14) . ?
C7 B3 1.6070(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.4046(13) . ?
C14 C19 1.4106(13) . ?
C15 C16 1.3963(14) . ?
C15 C20 1.5076(13) . ?
C16 C17 1.3846(15) . ?
C16 H16 0.9500 . ?
C17 C18 1.3883(15) . ?
C17 H17 0.9500 . ?
C18 C19 1.3890(14) . ?
C18 H18 0.9500 . ?
C19 C21 1.5026(14) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
B1 B2 1.7282(15) . ?
B3 B4 1.7298(14) . ?

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 C1 126.07(9) . . ?
B1 N1 C2 122.21(8) . . ?
C1 N1 C2 111.71(8) . . ?
B1 N2 C4 122.16(8) . . ?
B1 N2 C3 124.72(8) . . ?
C4 N2 C3 111.02(8) . . ?
B2 N3 C5 122.45(8) . . ?
B2 N3 C6 126.24(8) . . ?
C5 N3 C6 111.30(8) . . ?
C7 N4 C14 123.59(8) . . ?
B3 N5 C8 125.75(8) . . ?
B3 N5 C9 123.01(8) . . ?
C8 N5 C9 111.09(8) . . ?
B4 N6 C11 127.10(9) . . ?
B4 N6 C10 121.66(8) . . ?
C11 N6 C10 111.04(8) . . ?
B4 N8 C12 121.79(8) . . ?
B4 N8 C13 126.33(9) . . ?
C12 N8 C13 111.35(9) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 B2 124.77(8) . . ?
N4 C7 B3 112.03(8) . . ?
B2 C7 B3 123.18(8) . . ?
N5 C8 H8A 109.5 . . ?
N5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N5 C9 H9A 109.5 . . ?
N5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N6 C10 H10A 109.5 . . ?
N6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N6 C11 H11A 109.5 . . ?
N6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C12 H12A 109.5 . . ?
N8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N8 C13 H13A 109.5 . . ?
N8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 120.29(9) . . ?
C15 C14 N4 120.47(8) . . ?
C19 C14 N4 118.44(8) . . ?
C16 C15 C14 118.67(9) . . ?
C16 C15 C20 120.04(9) . . ?
C14 C15 C20 121.29(9) . . ?
C17 C16 C15 121.42(9) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 119.40(9) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 121.13(9) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C18 C19 C14 119.08(9) . . ?
C18 C19 C21 120.96(9) . . ?
C14 C19 C21 119.95(8) . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 B1 N1 120.93(9) . . ?
N2 B1 B2 119.20(8) . . ?
N1 B1 B2 119.86(8) . . ?
N3 B2 C7 119.78(8) . . ?
N3 B2 B1 119.62(8) . . ?
C7 B2 B1 120.46(8) . . ?
N5 B3 C7 119.43(8) . . ?
N5 B3 B4 119.72(8) . . ?
C7 B3 B4 120.68(8) . . ?
N6 B4 N8 122.12(9) . . ?
N6 B4 B3 117.13(8) . . ?
N8 B4 B3 120.75(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 N4 C7 B2 5.08(14) . . . . ?
C14 N4 C7 B3 -176.23(8) . . . . ?
C7 N4 C14 C15 89.79(11) . . . . ?
C7 N4 C14 C19 -100.39(11) . . . . ?
C19 C14 C15 C16 -0.60(14) . . . . ?
N4 C14 C15 C16 169.02(9) . . . . ?
C19 C14 C15 C20 -179.89(9) . . . . ?
N4 C14 C15 C20 -10.26(14) . . . . ?
C14 C15 C16 C17 0.16(15) . . . . ?
C20 C15 C16 C17 179.46(9) . . . . ?
C15 C16 C17 C18 0.84(16) . . . . ?
C16 C17 C18 C19 -1.41(16) . . . . ?
C17 C18 C19 C14 0.97(15) . . . . ?
C17 C18 C19 C21 -177.74(9) . . . . ?
C15 C14 C19 C18 0.05(14) . . . . ?
N4 C14 C19 C18 -169.78(9) . . . . ?
C15 C14 C19 C21 178.77(9) . . . . ?
N4 C14 C19 C21 8.94(13) . . . . ?
C4 N2 B1 N1 172.18(9) . . . . ?
C3 N2 B1 N1 -25.81(14) . . . . ?
C4 N2 B1 B2 -8.45(13) . . . . ?
C3 N2 B1 B2 153.56(9) . . . . ?
C1 N1 B1 N2 -24.20(15) . . . . ?
C2 N1 B1 N2 157.25(9) . . . . ?
C1 N1 B1 B2 156.43(10) . . . . ?
C2 N1 B1 B2 -22.12(13) . . . . ?
C5 N3 B2 C7 -175.58(9) . . . . ?
C6 N3 B2 C7 4.44(14) . . . . ?
C5 N3 B2 B1 0.16(14) . . . . ?
C6 N3 B2 B1 -179.81(9) . . . . ?
N4 C7 B2 N3 -111.92(11) . . . . ?
B3 C7 B2 N3 69.54(12) . . . . ?
N4 C7 B2 B1 72.37(12) . . . . ?
B3 C7 B2 B1 -106.17(10) . . . . ?
N2 B1 B2 N3 -93.81(11) . . . . ?
N1 B1 B2 N3 85.56(11) . . . . ?
N2 B1 B2 C7 81.90(11) . . . . ?
N1 B1 B2 C7 -98.72(11) . . . . ?
C8 N5 B3 C7 0.16(15) . . . . ?
C9 N5 B3 C7 175.30(9) . . . . ?
C8 N5 B3 B4 -175.03(9) . . . . ?
C9 N5 B3 B4 0.11(14) . . . . ?
N4 C7 B3 N5 -76.75(11) . . . . ?
B2 C7 B3 N5 101.97(11) . . . . ?
N4 C7 B3 B4 98.39(10) . . . . ?
B2 C7 B3 B4 -82.90(11) . . . . ?
C11 N6 B4 N8 -23.45(16) . . . . ?
C10 N6 B4 N8 162.25(9) . . . . ?
C11 N6 B4 B3 157.06(9) . . . . ?
C10 N6 B4 B3 -17.25(13) . . . . ?
C12 N8 B4 N6 166.32(10) . . . . ?
C13 N8 B4 N6 -22.79(16) . . . . ?
C12 N8 B4 B3 -14.20(15) . . . . ?
C13 N8 B4 B3 156.69(10) . . . . ?
N5 B3 B4 N6 102.74(11) . . . . ?
C7 B3 B4 N6 -72.39(12) . . . . ?
N5 B3 B4 N8 -76.76(12) . . . . ?
C7 B3 B4 N8 108.11(11) . . . . ?

_refine_diff_density_max         0.279
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.033


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive
####################################################################### 
# 
# 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_NiHe006_NiHe_a
_database_code_depnum_ccdc_archive 'CCDC 2468867'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2025-07-01 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT041_NiHe006_NiHe_a      
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: asymmetric unit formula versus unit cell formula
;
_vrf_PLAT911_NiHe006_NiHe_a      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         49 Report
RESPONSE: reflections affected by beamstop
;

_audit_creation_method           'CIF-fill 1.6d (K.Radacki, 2005-25)'
_audit_creation_date             2025-04-15
_shelx_SHELXL_version_number     2019/2
_chemical_formula_moiety         'C27 H46 B3 N7 O, 0.5 (C5 H12)'
_chemical_formula_sum            'C29.5 H52 B3 N7 O'
_chemical_formula_weight         553.21
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'


_cell_length_a                   10.9804(3)
_cell_length_b                   12.3739(3)
_cell_length_c                   12.9690(4)
_cell_angle_alpha                69.387(2)
_cell_angle_beta                 79.424(2)
_cell_angle_gamma                79.155(2)
_cell_volume                     1606.59(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18434
_cell_measurement_theta_min      3.6630
_cell_measurement_theta_max      74.3220

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.43.63a (Rigaku Oxford Diffraction, 2023) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_preparation       
;
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0516
0 0 1 0.0378
-1 1 -1 0.1527
1 1 0 0.1029
-1 1 0 0.1902
-1 1 1 0.1803
0 -1 -1 0.0999
-1 -1 -1 0.0791
1 0 -1 0.0915
1 1 -1 0.0889
-1 -1 0 0.0900
0 1 1 0.1094
1 1 1 0.1185
2 -1 -1 0.1311
-2 1 1 0.1948
-1 -2 -2 0.0551
1 2 2 0.0974
1 -1 -2 0.0988
0 1 -2 0.0695
0 -1 2 0.0416
-1 -2 2 0.0435
1 2 -2 0.0750
2 0 1 0.1302
0 2 -1 0.0865
1 0 2 0.0779

_shelx_estimated_absorpt_T_min   0.834
_shelx_estimated_absorpt_T_max   0.953
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
 
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  ω     98.00 129.00   0.50    0.19    --   85.25 122.00 165.72   62
  2  ω    102.00 129.00   0.50    0.19    --   82.28  15.00   0.00   54
  3  ω     63.00  97.00   0.50    0.19    --   82.28  15.00   0.00   68
  4  ω     93.00 133.00   0.50    0.19    --   82.28  15.00-180.00   80
  5  ω     38.00 102.00   0.50    0.19    --   85.25-129.00-110.77  128
  6  ω     42.00  93.00   0.50    0.19    --   85.25 -98.00-158.35  102
  7  ω     36.00 100.00   0.50    0.19    --   82.28-124.00 -15.00  128
  8  ω     55.00  86.00   0.50    0.19    --   82.28 -95.00-120.00   62
  9  ω     25.00  97.00   0.50    0.19    --   71.14-124.00 -15.00  144
 10  ω     40.00  87.00   0.50    0.19    --   82.28 -95.00 -60.00   94
 11  ω     40.00  70.00   0.50    0.19    --   82.28 -95.00 -90.00   60
 12  ω     19.00  84.00   0.50    0.19    --   58.28-124.00 -15.00  130
 13  ω     58.00  90.00   0.50    0.19    --   82.28 -95.00  60.00   64
 14  ω     37.00  93.00   0.50    0.19    --   82.28-112.00  90.00  112
 15  ω     51.00  93.00   0.50    0.19    --   85.25 -97.00 160.45   84
 16  ω     41.00  75.00   0.50    0.19    --   82.28 -95.00 150.00   68
 17  ω     51.00  77.00   0.50    0.19    --   82.28 -95.00 120.00   52
 18  ω     44.00  80.00   0.50    0.19    --   82.28 -95.00  90.00   72
 19  ω     46.00  90.00   0.50    0.19    --   82.28 -95.00 -30.00   88
 20  ω     28.00  79.00   0.50    0.19    --   71.14 -95.00-120.00  102
 21  ω    -94.00 -59.00   0.50    0.19    --  -46.00 -51.00  -3.33   70
 22  ω    -99.00 -64.00   0.50    0.19    --  -50.00 -47.00-107.59   70
 23  ω    -95.00 -60.00   0.50    0.19    --  -46.00 -48.00 108.33   70
 24  ω   -100.00 -63.00   0.50    0.19    --  -50.00 -45.00 121.07   74
 25  ω   -105.00 -65.00   0.50    0.19    --  -54.00 -36.00 -66.08   80
 26  ω   -124.00 -92.00   0.50    0.19    --  -79.50 -63.00-130.01   64
 27  ω   -126.00 -92.00   0.50    0.19    --  -79.50 -57.00-147.71   68
 28  ω   -118.00 -83.00   0.50    0.19    --  -70.00 -54.00 -10.13   70
 29  ω   -127.00 -91.00   0.50    0.19    --  -79.50 -56.00 -11.17   72
 30  ω   -127.00 -92.00   0.50    0.19    --  -79.50 -54.00 -32.68   70
 31  ω   -125.00 -91.00   0.50    0.19    --  -79.50 -61.00  17.56   68
 32  ω   -128.00 -93.00   0.50    0.19    --  -79.50 -50.00-108.91   70
 33  ω   -110.00 -75.00   0.50    0.19    --  -62.00 -51.00  63.92   70
 34  ω   -128.00 -93.00   0.50    0.19    --  -79.50 -50.00 -48.74   70
 35  ω   -127.00 -91.00   0.50    0.19    --  -79.50 -56.00  82.89   72
 36  ω   -128.00 -93.00   0.50    0.19    --  -79.50 -50.00  97.03   70
 37  ω   -127.00 -92.00   0.50    0.19    --  -79.50 -54.00 132.84   70
 38  ω   -107.00 -72.00   0.50    0.19    --  -58.00 -50.00 172.91   70
 39  ω   -130.00 -91.00   0.50    0.19    --  -79.50 -41.00 158.46   78
 40  ω   -129.00 -93.00   0.50    0.19    --  -79.50 -47.00  52.20   72
 41  ω   -111.00 -76.00   0.50    0.19    --  -62.00 -49.00-120.49   70
 42  ω   -124.00 -86.00   0.50    0.19    --  -74.00 -41.00-148.66   76
 43  ω   -126.00 -93.00   0.50    0.19    --  -79.50-120.00-142.36   66
 44  ω   -126.00 -93.00   0.50    0.19    --  -79.50-121.00-120.37   66
 45  ω   -127.00 -90.00   0.50    0.19    --  -79.50-127.00 -63.08   74
 46  ω   -126.00 -93.00   0.50    0.19    --  -79.50-121.00 -43.97   66
 47  ω    -92.00 -31.00   0.50    0.19    --  -76.35 112.00   0.00  122
 48  ω    -98.00 -33.00   0.50    0.19    --  -79.50 119.00-130.69  130
 49  ω    -86.00 -13.00   0.50    0.19    --  -59.96 124.00  63.00  146
 50  ω    -99.00 -32.00   0.50    0.19    --  -79.50 122.00 172.26  134
 51  ω    -95.00 -23.00   0.50    0.19    --  -69.45 124.00  63.00  144
 52  ω    -97.00 -33.00   0.50    0.19    --  -79.50 115.00  60.36  128
 53  ω    -97.00 -33.00   0.50    0.19    --  -79.50 117.00  67.99  128
 54  ω    -99.00 -30.00   0.50    0.19    --  -76.35 124.00  63.00  138
 55  ω    -97.00 -33.00   0.50    0.19    --  -79.50 115.00 -40.14  128
;
_diffrn_orient_matrix_type       
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0239001000
_diffrn_orient_matrix_UB_12      0.0109342000
_diffrn_orient_matrix_UB_13      0.1169672000
_diffrn_orient_matrix_UB_21      0.0397359000
_diffrn_orient_matrix_UB_22      -0.1320691000
_diffrn_orient_matrix_UB_23      0.0505965000
_diffrn_orient_matrix_UB_31      0.1363616000
_diffrn_orient_matrix_UB_32      0.0213647000
_diffrn_orient_matrix_UB_33      -0.0114900000
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            31770
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.671
_diffrn_reflns_theta_max         70.076
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6029
_reflns_number_gt                5288
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
 CrysAlisPro system (CCD 42.72a 64-bit (release 07-10-2022))
;
_computing_cell_refinement       'CrysAlisPro 1.171.43.63a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.63a (Rigaku OD, 2023)'
_computing_structure_solution    "SHELXT 2014/5 (Sheldrick, 2014)'"
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'

_refine_special_details          
;
 The asymmetric unit contains half a pentane molecule positioned on an 
 inversion center and modelled as twofold disordered (RESI 71/72 PENT) with 
 FVAR refined to a 54:46 ratio and PARTs -1 and -2. ADPs within the disorder 
 were restrained to similarity with SIMU 0.005.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0644P)²+0.4785P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6029
_refine_ls_number_parameters     451
_refine_ls_number_restraints     126
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1172
_refine_ls_wR_factor_gt          0.1130
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_1 B 0.43822(13) 0.76776(12) 0.53183(12) 0.0237(3) Uani 1 1 d . . . . .
N2_1 N 0.40317(10) 0.75372(9) 0.64845(9) 0.0235(2) Uani 1 1 d . . . . .
C3_1 C 0.28290(11) 0.71409(10) 0.68316(10) 0.0228(3) Uani 1 1 d . . . . .
C4_1 C 0.24246(11) 0.70228(10) 0.59499(10) 0.0228(3) Uani 1 1 d . . . . .
N5_1 N 0.33429(10) 0.73560(9) 0.50029(8) 0.0229(2) Uani 1 1 d . . . . .
C1_2 C 0.31350(12) 0.74979(11) 0.39046(10) 0.0252(3) Uani 1 1 d . . . . .
C2_2 C 0.29932(12) 0.86251(12) 0.31326(11) 0.0292(3) Uani 1 1 d . . . . .
C3_2 C 0.28198(15) 0.87599(14) 0.20529(12) 0.0383(3) Uani 1 1 d . . . . .
H3_2 H 0.271530 0.951919 0.152237 0.046 Uiso 1 1 calc R U . . .
C4_2 C 0.27984(16) 0.77993(16) 0.17451(12) 0.0430(4) Uani 1 1 d . . . . .
H4_2 H 0.267963 0.790250 0.100721 0.052 Uiso 1 1 calc R U . . .
C5_2 C 0.29497(14) 0.66908(14) 0.25114(12) 0.0377(3) Uani 1 1 d . . . . .
H5_2 H 0.293570 0.603669 0.229350 0.045 Uiso 1 1 calc R U . . .
C6_2 C 0.31221(12) 0.65195(12) 0.35971(11) 0.0294(3) Uani 1 1 d . . . . .
C7_2 C 0.30191(14) 0.96907(12) 0.34340(12) 0.0326(3) Uani 1 1 d . . . . .
H7A_2 H 0.246909 1.034743 0.299957 0.049 Uiso 1 1 calc R U . . .
H7B_2 H 0.387517 0.988269 0.327088 0.049 Uiso 1 1 calc R U . . .
H7C_2 H 0.272992 0.953467 0.422756 0.049 Uiso 1 1 calc R U . . .
C8_2 C 0.33129(14) 0.53030(12) 0.44077(13) 0.0349(3) Uani 1 1 d . . . . .
H8A_2 H 0.369632 0.476149 0.400401 0.052 Uiso 1 1 calc R U . . .
H8B_2 H 0.250393 0.507925 0.481257 0.052 Uiso 1 1 calc R U . . .
H8C_2 H 0.386279 0.527591 0.493466 0.052 Uiso 1 1 calc R U . . .
C1_3 C 0.47205(12) 0.76848(11) 0.72413(10) 0.0247(3) Uani 1 1 d . . . . .
C2_3 C 0.41601(12) 0.82289(11) 0.80055(11) 0.0270(3) Uani 1 1 d . . . . .
H2_3 H 0.330646 0.855881 0.799339 0.032 Uiso 1 1 calc R U . . .
C3_3 C 0.48200(13) 0.83061(12) 0.87984(11) 0.0291(3) Uani 1 1 d . . . . .
H3_3 H 0.441537 0.867173 0.932670 0.035 Uiso 1 1 calc R U . . .
C4_3 C 0.60682(13) 0.78431(12) 0.88024(11) 0.0279(3) Uani 1 1 d . . . . .
C5_3 C 0.66596(13) 0.73272(12) 0.80172(11) 0.0288(3) Uani 1 1 d . . . . .
H5_3 H 0.752501 0.703662 0.800564 0.035 Uiso 1 1 calc R U . . .
C6_3 C 0.59951(12) 0.72345(11) 0.72528(11) 0.0275(3) Uani 1 1 d . . . . .
H6_3 H 0.640260 0.686317 0.672959 0.033 Uiso 1 1 calc R U . . .
O7_3 O 0.68192(9) 0.78733(9) 0.95376(8) 0.0366(2) Uani 1 1 d . . . . .
C8_3 C 0.62223(16) 0.82472(15) 1.04470(13) 0.0412(4) Uani 1 1 d . . . . .
H8A_3 H 0.683209 0.814113 1.095120 0.062 Uiso 1 1 calc R U . . .
H8B_3 H 0.554346 0.778548 1.084655 0.062 Uiso 1 1 calc R U . . .
H8C_3 H 0.587974 0.907260 1.017025 0.062 Uiso 1 1 calc R U . . .
N1_4 N 0.55039(10) 0.80403(10) 0.46265(9) 0.0269(2) Uani 1 1 d . . . . .
C2_4 C 0.61580(12) 0.89097(12) 0.47202(12) 0.0297(3) Uani 1 1 d . . . . .
H2A_4 H 0.578794 0.910900 0.538839 0.044 Uiso 1 1 calc R U . . .
H2B_4 H 0.608598 0.960976 0.406420 0.044 Uiso 1 1 calc R U . . .
H2C_4 H 0.704215 0.859797 0.477127 0.044 Uiso 1 1 calc R U . . .
C3_4 C 0.59515(13) 0.77677(13) 0.36093(12) 0.0337(3) Uani 1 1 d . . . . .
H3A_4 H 0.557337 0.710323 0.362739 0.051 Uiso 1 1 calc R U . . .
H3B_4 H 0.686332 0.757140 0.354305 0.051 Uiso 1 1 calc R U . . .
H3C_4 H 0.571997 0.844466 0.297102 0.051 Uiso 1 1 calc R U . . .
B1_5 B 0.21837(14) 0.67693(12) 0.80686(12) 0.0241(3) Uani 1 1 d . . . . .
N2_5 N 0.28625(10) 0.59422(9) 0.89155(9) 0.0263(2) Uani 1 1 d . . . . .
C3_5 C 0.39794(13) 0.51801(12) 0.86827(12) 0.0312(3) Uani 1 1 d . . . . .
H3A_5 H 0.409177 0.524329 0.789727 0.047 Uiso 1 1 calc R U . . .
H3B_5 H 0.389049 0.437301 0.914588 0.047 Uiso 1 1 calc R U . . .
H3C_5 H 0.470879 0.541015 0.884816 0.047 Uiso 1 1 calc R U . . .
C4_5 C 0.26902(14) 0.59191(13) 1.00603(11) 0.0347(3) Uani 1 1 d . . . . .
H4A_5 H 0.201320 0.652846 1.016030 0.052 Uiso 1 1 calc R U . . .
H4B_5 H 0.346562 0.605686 1.023709 0.052 Uiso 1 1 calc R U . . .
H4C_5 H 0.247537 0.515645 1.055599 0.052 Uiso 1 1 calc R U . . .
N5_5 N 0.09267(10) 0.72525(10) 0.83284(9) 0.0282(2) Uani 1 1 d . . . . .
C6_5 C 0.00795(13) 0.66561(14) 0.92733(12) 0.0367(3) Uani 1 1 d . . . . .
H6A_5 H 0.049711 0.588297 0.966281 0.055 Uiso 1 1 calc R U . . .
H6B_5 H -0.067001 0.657350 0.901247 0.055 Uiso 1 1 calc R U . . .
H6C_5 H -0.015962 0.711008 0.978150 0.055 Uiso 1 1 calc R U . . .
C7_5 C 0.02768(14) 0.82787(13) 0.75749(12) 0.0354(3) Uani 1 1 d . . . . .
H7A_5 H 0.088728 0.870588 0.699709 0.053 Uiso 1 1 calc R U . . .
H7B_5 H -0.019377 0.878301 0.799067 0.053 Uiso 1 1 calc R U . . .
H7C_5 H -0.030082 0.803825 0.722962 0.053 Uiso 1 1 calc R U . . .
B1_6 B 0.11585(13) 0.65857(13) 0.59509(12) 0.0241(3) Uani 1 1 d . . . . .
N2_6 N 0.08601(10) 0.55021(10) 0.67366(9) 0.0273(2) Uani 1 1 d . . . . .
C3_6 C 0.17641(14) 0.45696(12) 0.73172(12) 0.0325(3) Uani 1 1 d . . . . .
H3A_6 H 0.261222 0.475243 0.700096 0.049 Uiso 1 1 calc R U . . .
H3B_6 H 0.165883 0.383618 0.723507 0.049 Uiso 1 1 calc R U . . .
H3C_6 H 0.163037 0.449184 0.810691 0.049 Uiso 1 1 calc R U . . .
C4_6 C -0.04145(14) 0.52305(14) 0.71431(14) 0.0386(3) Uani 1 1 d . . . . .
H4A_6 H -0.100835 0.592984 0.686059 0.058 Uiso 1 1 calc R U . . .
H4B_6 H -0.053465 0.496440 0.795696 0.058 Uiso 1 1 calc R U . . .
H4C_6 H -0.055621 0.461483 0.688466 0.058 Uiso 1 1 calc R U . . .
N5_6 N 0.03146(10) 0.72810(9) 0.51782(9) 0.0274(2) Uani 1 1 d . . . . .
C6_6 C 0.02318(13) 0.85370(12) 0.46973(12) 0.0313(3) Uani 1 1 d . . . . .
H6A_6 H 0.083942 0.881262 0.498063 0.047 Uiso 1 1 calc R U . . .
H6B_6 H -0.061322 0.889165 0.489890 0.047 Uiso 1 1 calc R U . . .
H6C_6 H 0.041311 0.875645 0.388697 0.047 Uiso 1 1 calc R U . . .
C7_6 C -0.05143(15) 0.68096(13) 0.47387(14) 0.0399(4) Uani 1 1 d . . . . .
H7A_6 H -0.031381 0.595932 0.496956 0.060 Uiso 1 1 calc R U . . .
H7B_6 H -0.040389 0.713260 0.392589 0.060 Uiso 1 1 calc R U . . .
H7C_6 H -0.138335 0.701956 0.502482 0.060 Uiso 1 1 calc R U . . .
C1_71 C -0.1575(14) 0.9665(11) 1.1604(11) 0.050(2) Uani 0.268(3) 1 d . U P A -1
H1A_71 H -0.135439 1.045196 1.139728 0.075 Uiso 0.268(3) 1 calc R U P A -1
H1B_71 H -0.181016 0.936119 1.240958 0.075 Uiso 0.268(3) 1 calc R U P A -1
H1C_71 H -0.228074 0.969117 1.122581 0.075 Uiso 0.268(3) 1 calc R U P A -1
C2_71 C -0.040(2) 0.8833(12) 1.1244(16) 0.0513(19) Uani 0.268(3) 1 d . U P A -1
H2A_71 H 0.027976 0.873011 1.168919 0.062 Uiso 0.268(3) 1 calc R U P A -1
H2B_71 H -0.064449 0.805794 1.138510 0.062 Uiso 0.268(3) 1 calc R U P A -1
C3_71 C 0.0047(9) 0.9361(8) 1.0033(7) 0.0448(14) Uani 0.268(3) 1 d . U P A -1
H3A_71 H -0.064976 0.944709 0.961038 0.054 Uiso 0.268(3) 1 calc R U P A -1
H3B_71 H 0.072566 0.879930 0.981993 0.054 Uiso 0.268(3) 1 calc R U P A -1
C4_71 C 0.0538(8) 1.0562(8) 0.9648(6) 0.0441(14) Uani 0.268(3) 1 d . U P A -1
H4A_71 H -0.013611 1.112940 0.985667 0.053 Uiso 0.268(3) 1 calc R U P A -1
H4B_71 H 0.124318 1.048042 1.005972 0.053 Uiso 0.268(3) 1 calc R U P A -1
C5_71 C 0.0957(15) 1.1040(13) 0.8461(12) 0.055(3) Uani 0.268(3) 1 d . U P A -1
H5A_71 H 0.055855 1.070134 0.805192 0.083 Uiso 0.268(3) 1 calc R U P A -1
H5B_71 H 0.186738 1.085261 0.832526 0.083 Uiso 0.268(3) 1 calc R U P A -1
H5C_71 H 0.072744 1.188808 0.820992 0.083 Uiso 0.268(3) 1 calc R U P A -1
C1_72 C -0.1502(18) 0.9326(19) 1.1923(15) 0.050(3) Uani 0.232(3) 1 d . U P A -2
H1A_72 H -0.143380 0.995870 1.218918 0.075 Uiso 0.232(3) 1 calc R U P A -2
H1B_72 H -0.164482 0.862288 1.255891 0.075 Uiso 0.232(3) 1 calc R U P A -2
H1C_72 H -0.220327 0.955454 1.148524 0.075 Uiso 0.232(3) 1 calc R U P A -2
C2_72 C -0.033(2) 0.9086(12) 1.1219(19) 0.0449(18) Uani 0.232(3) 1 d . U P A -2
H2A_72 H -0.032287 0.833943 1.109549 0.054 Uiso 0.232(3) 1 calc R U P A -2
H2B_72 H 0.039077 0.899631 1.161877 0.054 Uiso 0.232(3) 1 calc R U P A -2
C3_72 C -0.0164(12) 1.0030(19) 1.0112(12) 0.0468(15) Uani 0.232(3) 1 d . U P A
-2
H3A_72 H -0.023238 1.078303 1.024049 0.056 Uiso 0.232(3) 1 calc R U P A -2
H3B_72 H -0.085796 1.008206 0.969783 0.056 Uiso 0.232(3) 1 calc R U P A -2
C4_72 C 0.1080(7) 0.9857(7) 0.9385(6) 0.0464(14) Uani 0.232(3) 1 d . U P A -2
H4A_72 H 0.177604 0.982855 0.978581 0.056 Uiso 0.232(3) 1 calc R U P A -2
H4B_72 H 0.116021 0.909721 0.926646 0.056 Uiso 0.232(3) 1 calc R U P A -2
C5_72 C 0.1200(18) 1.0801(18) 0.8272(16) 0.042(3) Uani 0.232(3) 1 d . U P A -2
H5A_72 H 0.043072 1.094676 0.793446 0.062 Uiso 0.232(3) 1 calc R U P A -2
H5B_72 H 0.190857 1.055343 0.778755 0.062 Uiso 0.232(3) 1 calc R U P A -2
H5C_72 H 0.133873 1.151610 0.837015 0.062 Uiso 0.232(3) 1 calc R U P A -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1_1 N1_4 1.4290(18) . ?
B1_1 N5_1 1.4440(17) . ?
B1_1 N2_1 1.4464(18) . ?
N2_1 C1_3 1.4211(16) . ?
N2_1 C3_1 1.4342(16) . ?
C3_1 C4_1 1.3618(17) . ?
C3_1 B1_5 1.5727(19) . ?
C4_1 N5_1 1.4284(16) . ?
C4_1 B1_6 1.5833(18) . ?
N5_1 C1_2 1.4283(16) . ?
C1_2 C2_2 1.4015(19) . ?
C1_2 C6_2 1.4048(19) . ?
C2_2 C3_2 1.3951(19) . ?
C2_2 C7_2 1.5078(19) . ?
C3_2 C4_2 1.386(2) . ?
C3_2 H3_2 0.9500 . ?
C4_2 C5_2 1.383(2) . ?
C4_2 H4_2 0.9500 . ?
C5_2 C6_2 1.391(2) . ?
C5_2 H5_2 0.9500 . ?
C6_2 C8_2 1.504(2) . ?
C7_2 H7A_2 0.9800 . ?
C7_2 H7B_2 0.9800 . ?
C7_2 H7C_2 0.9800 . ?
C8_2 H8A_2 0.9800 . ?
C8_2 H8B_2 0.9800 . ?
C8_2 H8C_2 0.9800 . ?
C1_3 C2_3 1.3799(19) . ?
C1_3 C6_3 1.4064(19) . ?
C2_3 C3_3 1.4000(19) . ?
C2_3 H2_3 0.9500 . ?
C3_3 C4_3 1.383(2) . ?
C3_3 H3_3 0.9500 . ?
C4_3 O7_3 1.3840(16) . ?
C4_3 C5_3 1.388(2) . ?
C5_3 C6_3 1.3803(18) . ?
C5_3 H5_3 0.9500 . ?
C6_3 H6_3 0.9500 . ?
O7_3 C8_3 1.4217(18) . ?
C8_3 H8A_3 0.9800 . ?
C8_3 H8B_3 0.9800 . ?
C8_3 H8C_3 0.9800 . ?
N1_4 C2_4 1.4502(17) . ?
N1_4 C3_4 1.4521(17) . ?
C2_4 H2A_4 0.9800 . ?
C2_4 H2B_4 0.9800 . ?
C2_4 H2C_4 0.9800 . ?
C3_4 H3A_4 0.9800 . ?
C3_4 H3B_4 0.9800 . ?
C3_4 H3C_4 0.9800 . ?
B1_5 N2_5 1.4253(18) . ?
B1_5 N5_5 1.4271(18) . ?
N2_5 C4_5 1.4526(17) . ?
N2_5 C3_5 1.4539(17) . ?
C3_5 H3A_5 0.9800 . ?
C3_5 H3B_5 0.9800 . ?
C3_5 H3C_5 0.9800 . ?
C4_5 H4A_5 0.9800 . ?
C4_5 H4B_5 0.9800 . ?
C4_5 H4C_5 0.9800 . ?
N5_5 C6_5 1.4542(18) . ?
N5_5 C7_5 1.4553(17) . ?
C6_5 H6A_5 0.9800 . ?
C6_5 H6B_5 0.9800 . ?
C6_5 H6C_5 0.9800 . ?
C7_5 H7A_5 0.9800 . ?
C7_5 H7B_5 0.9800 . ?
C7_5 H7C_5 0.9800 . ?
B1_6 N2_6 1.4227(18) . ?
B1_6 N5_6 1.4272(18) . ?
N2_6 C3_6 1.4545(18) . ?
N2_6 C4_6 1.4599(17) . ?
C3_6 H3A_6 0.9800 . ?
C3_6 H3B_6 0.9800 . ?
C3_6 H3C_6 0.9800 . ?
C4_6 H4A_6 0.9800 . ?
C4_6 H4B_6 0.9800 . ?
C4_6 H4C_6 0.9800 . ?
N5_6 C6_6 1.4483(17) . ?
N5_6 C7_6 1.4552(17) . ?
C6_6 H6A_6 0.9800 . ?
C6_6 H6B_6 0.9800 . ?
C6_6 H6C_6 0.9800 . ?
C7_6 H7A_6 0.9800 . ?
C7_6 H7B_6 0.9800 . ?
C7_6 H7C_6 0.9800 . ?
C1_71 C2_71 1.60(3) . ?
C1_71 H1A_71 0.9800 . ?
C1_71 H1B_71 0.9800 . ?
C1_71 H1C_71 0.9800 . ?
C2_71 C3_71 1.50(2) . ?
C2_71 H2A_71 0.9900 . ?
C2_71 H2B_71 0.9900 . ?
C3_71 C4_71 1.558(10) . ?
C3_71 H3A_71 0.9900 . ?
C3_71 H3B_71 0.9900 . ?
C4_71 C5_71 1.460(16) . ?
C4_71 H4A_71 0.9900 . ?
C4_71 H4B_71 0.9900 . ?
C5_71 H5A_71 0.9800 . ?
C5_71 H5B_71 0.9800 . ?
C5_71 H5C_71 0.9800 . ?
C1_72 C2_72 1.48(3) . ?
C1_72 H1A_72 0.9800 . ?
C1_72 H1B_72 0.9800 . ?
C1_72 H1C_72 0.9800 . ?
C2_72 C3_72 1.50(3) . ?
C2_72 H2A_72 0.9900 . ?
C2_72 H2B_72 0.9900 . ?
C3_72 C4_72 1.536(14) . ?
C3_72 H3A_72 0.9900 . ?
C3_72 H3B_72 0.9900 . ?
C4_72 C5_72 1.50(2) . ?
C4_72 H4A_72 0.9900 . ?
C4_72 H4B_72 0.9900 . ?
C5_72 H5A_72 0.9800 . ?
C5_72 H5B_72 0.9800 . ?
C5_72 H5C_72 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_4 B1_1 N5_1 127.25(12) . . ?
N1_4 B1_1 N2_1 128.36(12) . . ?
N5_1 B1_1 N2_1 104.39(11) . . ?
C1_3 N2_1 C3_1 121.92(10) . . ?
C1_3 N2_1 B1_1 129.28(11) . . ?
C3_1 N2_1 B1_1 108.73(10) . . ?
C4_1 C3_1 N2_1 108.98(11) . . ?
C4_1 C3_1 B1_5 126.51(11) . . ?
N2_1 C3_1 B1_5 124.14(11) . . ?
C3_1 C4_1 N5_1 108.58(11) . . ?
C3_1 C4_1 B1_6 126.67(11) . . ?
N5_1 C4_1 B1_6 124.75(11) . . ?
C1_2 N5_1 C4_1 123.05(10) . . ?
C1_2 N5_1 B1_1 127.04(11) . . ?
C4_1 N5_1 B1_1 109.31(10) . . ?
C2_2 C1_2 C6_2 120.89(12) . . ?
C2_2 C1_2 N5_1 118.75(11) . . ?
C6_2 C1_2 N5_1 120.32(12) . . ?
C3_2 C2_2 C1_2 118.67(13) . . ?
C3_2 C2_2 C7_2 119.23(13) . . ?
C1_2 C2_2 C7_2 122.10(12) . . ?
C4_2 C3_2 C2_2 120.78(14) . . ?
C4_2 C3_2 H3_2 119.6 . . ?
C2_2 C3_2 H3_2 119.6 . . ?
C5_2 C4_2 C3_2 120.03(13) . . ?
C5_2 C4_2 H4_2 120.0 . . ?
C3_2 C4_2 H4_2 120.0 . . ?
C4_2 C5_2 C6_2 120.95(14) . . ?
C4_2 C5_2 H5_2 119.5 . . ?
C6_2 C5_2 H5_2 119.5 . . ?
C5_2 C6_2 C1_2 118.68(13) . . ?
C5_2 C6_2 C8_2 119.89(13) . . ?
C1_2 C6_2 C8_2 121.42(12) . . ?
C2_2 C7_2 H7A_2 109.5 . . ?
C2_2 C7_2 H7B_2 109.5 . . ?
H7A_2 C7_2 H7B_2 109.5 . . ?
C2_2 C7_2 H7C_2 109.5 . . ?
H7A_2 C7_2 H7C_2 109.5 . . ?
H7B_2 C7_2 H7C_2 109.5 . . ?
C6_2 C8_2 H8A_2 109.5 . . ?
C6_2 C8_2 H8B_2 109.5 . . ?
H8A_2 C8_2 H8B_2 109.5 . . ?
C6_2 C8_2 H8C_2 109.5 . . ?
H8A_2 C8_2 H8C_2 109.5 . . ?
H8B_2 C8_2 H8C_2 109.5 . . ?
C2_3 C1_3 C6_3 118.22(12) . . ?
C2_3 C1_3 N2_1 121.63(12) . . ?
C6_3 C1_3 N2_1 120.12(12) . . ?
C1_3 C2_3 C3_3 121.56(12) . . ?
C1_3 C2_3 H2_3 119.2 . . ?
C3_3 C2_3 H2_3 119.2 . . ?
C4_3 C3_3 C2_3 119.13(13) . . ?
C4_3 C3_3 H3_3 120.4 . . ?
C2_3 C3_3 H3_3 120.4 . . ?
C3_3 C4_3 O7_3 124.47(13) . . ?
C3_3 C4_3 C5_3 120.17(12) . . ?
O7_3 C4_3 C5_3 115.34(12) . . ?
C6_3 C5_3 C4_3 120.25(13) . . ?
C6_3 C5_3 H5_3 119.9 . . ?
C4_3 C5_3 H5_3 119.9 . . ?
C5_3 C6_3 C1_3 120.61(13) . . ?
C5_3 C6_3 H6_3 119.7 . . ?
C1_3 C6_3 H6_3 119.7 . . ?
C4_3 O7_3 C8_3 117.32(11) . . ?
O7_3 C8_3 H8A_3 109.5 . . ?
O7_3 C8_3 H8B_3 109.5 . . ?
H8A_3 C8_3 H8B_3 109.5 . . ?
O7_3 C8_3 H8C_3 109.5 . . ?
H8A_3 C8_3 H8C_3 109.5 . . ?
H8B_3 C8_3 H8C_3 109.5 . . ?
B1_1 N1_4 C2_4 123.94(11) . . ?
B1_1 N1_4 C3_4 122.67(11) . . ?
C2_4 N1_4 C3_4 112.13(11) . . ?
N1_4 C2_4 H2A_4 109.5 . . ?
N1_4 C2_4 H2B_4 109.5 . . ?
H2A_4 C2_4 H2B_4 109.5 . . ?
N1_4 C2_4 H2C_4 109.5 . . ?
H2A_4 C2_4 H2C_4 109.5 . . ?
H2B_4 C2_4 H2C_4 109.5 . . ?
N1_4 C3_4 H3A_4 109.5 . . ?
N1_4 C3_4 H3B_4 109.5 . . ?
H3A_4 C3_4 H3B_4 109.5 . . ?
N1_4 C3_4 H3C_4 109.5 . . ?
H3A_4 C3_4 H3C_4 109.5 . . ?
H3B_4 C3_4 H3C_4 109.5 . . ?
N2_5 B1_5 N5_5 120.86(12) . . ?
N2_5 B1_5 C3_1 119.31(12) . . ?
N5_5 B1_5 C3_1 119.83(11) . . ?
B1_5 N2_5 C4_5 124.42(12) . . ?
B1_5 N2_5 C3_5 123.03(11) . . ?
C4_5 N2_5 C3_5 111.43(11) . . ?
N2_5 C3_5 H3A_5 109.5 . . ?
N2_5 C3_5 H3B_5 109.5 . . ?
H3A_5 C3_5 H3B_5 109.5 . . ?
N2_5 C3_5 H3C_5 109.5 . . ?
H3A_5 C3_5 H3C_5 109.5 . . ?
H3B_5 C3_5 H3C_5 109.5 . . ?
N2_5 C4_5 H4A_5 109.5 . . ?
N2_5 C4_5 H4B_5 109.5 . . ?
H4A_5 C4_5 H4B_5 109.5 . . ?
N2_5 C4_5 H4C_5 109.5 . . ?
H4A_5 C4_5 H4C_5 109.5 . . ?
H4B_5 C4_5 H4C_5 109.5 . . ?
B1_5 N5_5 C6_5 123.49(11) . . ?
B1_5 N5_5 C7_5 123.73(12) . . ?
C6_5 N5_5 C7_5 111.80(11) . . ?
N5_5 C6_5 H6A_5 109.5 . . ?
N5_5 C6_5 H6B_5 109.5 . . ?
H6A_5 C6_5 H6B_5 109.5 . . ?
N5_5 C6_5 H6C_5 109.5 . . ?
H6A_5 C6_5 H6C_5 109.5 . . ?
H6B_5 C6_5 H6C_5 109.5 . . ?
N5_5 C7_5 H7A_5 109.5 . . ?
N5_5 C7_5 H7B_5 109.5 . . ?
H7A_5 C7_5 H7B_5 109.5 . . ?
N5_5 C7_5 H7C_5 109.5 . . ?
H7A_5 C7_5 H7C_5 109.5 . . ?
H7B_5 C7_5 H7C_5 109.5 . . ?
N2_6 B1_6 N5_6 120.21(12) . . ?
N2_6 B1_6 C4_1 119.56(11) . . ?
N5_6 B1_6 C4_1 120.22(12) . . ?
B1_6 N2_6 C3_6 124.80(11) . . ?
B1_6 N2_6 C4_6 123.87(12) . . ?
C3_6 N2_6 C4_6 111.09(11) . . ?
N2_6 C3_6 H3A_6 109.5 . . ?
N2_6 C3_6 H3B_6 109.5 . . ?
H3A_6 C3_6 H3B_6 109.5 . . ?
N2_6 C3_6 H3C_6 109.5 . . ?
H3A_6 C3_6 H3C_6 109.5 . . ?
H3B_6 C3_6 H3C_6 109.5 . . ?
N2_6 C4_6 H4A_6 109.5 . . ?
N2_6 C4_6 H4B_6 109.5 . . ?
H4A_6 C4_6 H4B_6 109.5 . . ?
N2_6 C4_6 H4C_6 109.5 . . ?
H4A_6 C4_6 H4C_6 109.5 . . ?
H4B_6 C4_6 H4C_6 109.5 . . ?
B1_6 N5_6 C6_6 123.68(11) . . ?
B1_6 N5_6 C7_6 124.10(12) . . ?
C6_6 N5_6 C7_6 112.14(11) . . ?
N5_6 C6_6 H6A_6 109.5 . . ?
N5_6 C6_6 H6B_6 109.5 . . ?
H6A_6 C6_6 H6B_6 109.5 . . ?
N5_6 C6_6 H6C_6 109.5 . . ?
H6A_6 C6_6 H6C_6 109.5 . . ?
H6B_6 C6_6 H6C_6 109.5 . . ?
N5_6 C7_6 H7A_6 109.5 . . ?
N5_6 C7_6 H7B_6 109.5 . . ?
H7A_6 C7_6 H7B_6 109.5 . . ?
N5_6 C7_6 H7C_6 109.5 . . ?
H7A_6 C7_6 H7C_6 109.5 . . ?
H7B_6 C7_6 H7C_6 109.5 . . ?
C2_71 C1_71 H1A_71 109.5 . . ?
C2_71 C1_71 H1B_71 109.5 . . ?
H1A_71 C1_71 H1B_71 109.5 . . ?
C2_71 C1_71 H1C_71 109.5 . . ?
H1A_71 C1_71 H1C_71 109.5 . . ?
H1B_71 C1_71 H1C_71 109.5 . . ?
C3_71 C2_71 C1_71 109.7(11) . . ?
C3_71 C2_71 H2A_71 109.7 . . ?
C1_71 C2_71 H2A_71 109.7 . . ?
C3_71 C2_71 H2B_71 109.7 . . ?
C1_71 C2_71 H2B_71 109.7 . . ?
H2A_71 C2_71 H2B_71 108.2 . . ?
C2_71 C3_71 C4_71 117.8(8) . . ?
C2_71 C3_71 H3A_71 107.9 . . ?
C4_71 C3_71 H3A_71 107.9 . . ?
C2_71 C3_71 H3B_71 107.9 . . ?
C4_71 C3_71 H3B_71 107.9 . . ?
H3A_71 C3_71 H3B_71 107.2 . . ?
C5_71 C4_71 C3_71 115.6(9) . . ?
C5_71 C4_71 H4A_71 108.4 . . ?
C3_71 C4_71 H4A_71 108.4 . . ?
C5_71 C4_71 H4B_71 108.4 . . ?
C3_71 C4_71 H4B_71 108.4 . . ?
H4A_71 C4_71 H4B_71 107.4 . . ?
C4_71 C5_71 H5A_71 109.5 . . ?
C4_71 C5_71 H5B_71 109.5 . . ?
H5A_71 C5_71 H5B_71 109.5 . . ?
C4_71 C5_71 H5C_71 109.5 . . ?
H5A_71 C5_71 H5C_71 109.5 . . ?
H5B_71 C5_71 H5C_71 109.5 . . ?
C2_72 C1_72 H1A_72 109.5 . . ?
C2_72 C1_72 H1B_72 109.5 . . ?
H1A_72 C1_72 H1B_72 109.5 . . ?
C2_72 C1_72 H1C_72 109.5 . . ?
H1A_72 C1_72 H1C_72 109.5 . . ?
H1B_72 C1_72 H1C_72 109.5 . . ?
C1_72 C2_72 C3_72 113.0(16) . . ?
C1_72 C2_72 H2A_72 109.0 . . ?
C3_72 C2_72 H2A_72 109.0 . . ?
C1_72 C2_72 H2B_72 109.0 . . ?
C3_72 C2_72 H2B_72 109.0 . . ?
H2A_72 C2_72 H2B_72 107.8 . . ?
C2_72 C3_72 C4_72 114.8(13) . . ?
C2_72 C3_72 H3A_72 108.6 . . ?
C4_72 C3_72 H3A_72 108.6 . . ?
C2_72 C3_72 H3B_72 108.6 . . ?
C4_72 C3_72 H3B_72 108.6 . . ?
H3A_72 C3_72 H3B_72 107.5 . . ?
C5_72 C4_72 C3_72 113.5(11) . . ?
C5_72 C4_72 H4A_72 108.9 . . ?
C3_72 C4_72 H4A_72 108.9 . . ?
C5_72 C4_72 H4B_72 108.9 . . ?
C3_72 C4_72 H4B_72 108.9 . . ?
H4A_72 C4_72 H4B_72 107.7 . . ?
C4_72 C5_72 H5A_72 109.5 . . ?
C4_72 C5_72 H5B_72 109.5 . . ?
H5A_72 C5_72 H5B_72 109.5 . . ?
C4_72 C5_72 H5C_72 109.5 . . ?
H5A_72 C5_72 H5C_72 109.5 . . ?
H5B_72 C5_72 H5C_72 109.5 . . ?

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_4 B1_1 N2_1 C1_3 -2.3(2) . . . . ?
N5_1 B1_1 N2_1 C1_3 177.17(11) . . . . ?
N1_4 B1_1 N2_1 C3_1 -179.18(13) . . . . ?
N5_1 B1_1 N2_1 C3_1 0.28(13) . . . . ?
C1_3 N2_1 C3_1 C4_1 -176.78(11) . . . . ?
B1_1 N2_1 C3_1 C4_1 0.39(14) . . . . ?
C1_3 N2_1 C3_1 B1_5 -3.38(18) . . . . ?
B1_1 N2_1 C3_1 B1_5 173.79(11) . . . . ?
N2_1 C3_1 C4_1 N5_1 -0.90(13) . . . . ?
B1_5 C3_1 C4_1 N5_1 -174.11(11) . . . . ?
N2_1 C3_1 C4_1 B1_6 178.80(11) . . . . ?
B1_5 C3_1 C4_1 B1_6 5.6(2) . . . . ?
C3_1 C4_1 N5_1 C1_2 -170.58(11) . . . . ?
B1_6 C4_1 N5_1 C1_2 9.71(18) . . . . ?
C3_1 C4_1 N5_1 B1_1 1.10(14) . . . . ?
B1_6 C4_1 N5_1 B1_1 -178.62(11) . . . . ?
N1_4 B1_1 N5_1 C1_2 -10.1(2) . . . . ?
N2_1 B1_1 N5_1 C1_2 170.44(11) . . . . ?
N1_4 B1_1 N5_1 C4_1 178.64(12) . . . . ?
N2_1 B1_1 N5_1 C4_1 -0.82(13) . . . . ?
C4_1 N5_1 C1_2 C2_2 108.90(14) . . . . ?
B1_1 N5_1 C1_2 C2_2 -61.25(17) . . . . ?
C4_1 N5_1 C1_2 C6_2 -73.52(16) . . . . ?
B1_1 N5_1 C1_2 C6_2 116.34(14) . . . . ?
C6_2 C1_2 C2_2 C3_2 0.9(2) . . . . ?
N5_1 C1_2 C2_2 C3_2 178.50(12) . . . . ?
C6_2 C1_2 C2_2 C7_2 -179.23(12) . . . . ?
N5_1 C1_2 C2_2 C7_2 -1.65(19) . . . . ?
C1_2 C2_2 C3_2 C4_2 -0.5(2) . . . . ?
C7_2 C2_2 C3_2 C4_2 179.62(14) . . . . ?
C2_2 C3_2 C4_2 C5_2 0.0(2) . . . . ?
C3_2 C4_2 C5_2 C6_2 0.1(2) . . . . ?
C4_2 C5_2 C6_2 C1_2 0.2(2) . . . . ?
C4_2 C5_2 C6_2 C8_2 -178.65(14) . . . . ?
C2_2 C1_2 C6_2 C5_2 -0.8(2) . . . . ?
N5_1 C1_2 C6_2 C5_2 -178.32(12) . . . . ?
C2_2 C1_2 C6_2 C8_2 178.09(12) . . . . ?
N5_1 C1_2 C6_2 C8_2 0.55(19) . . . . ?
C3_1 N2_1 C1_3 C2_3 -45.01(17) . . . . ?
B1_1 N2_1 C1_3 C2_3 138.46(14) . . . . ?
C3_1 N2_1 C1_3 C6_3 132.62(13) . . . . ?
B1_1 N2_1 C1_3 C6_3 -43.92(18) . . . . ?
C6_3 C1_3 C2_3 C3_3 -1.93(19) . . . . ?
N2_1 C1_3 C2_3 C3_3 175.74(11) . . . . ?
C1_3 C2_3 C3_3 C4_3 1.1(2) . . . . ?
C2_3 C3_3 C4_3 O7_3 179.51(12) . . . . ?
C2_3 C3_3 C4_3 C5_3 1.1(2) . . . . ?
C3_3 C4_3 C5_3 C6_3 -2.4(2) . . . . ?
O7_3 C4_3 C5_3 C6_3 179.05(11) . . . . ?
C4_3 C5_3 C6_3 C1_3 1.5(2) . . . . ?
C2_3 C1_3 C6_3 C5_3 0.61(19) . . . . ?
N2_1 C1_3 C6_3 C5_3 -177.09(11) . . . . ?
C3_3 C4_3 O7_3 C8_3 9.82(19) . . . . ?
C5_3 C4_3 O7_3 C8_3 -171.66(13) . . . . ?
N5_1 B1_1 N1_4 C2_4 144.52(13) . . . . ?
N2_1 B1_1 N1_4 C2_4 -36.2(2) . . . . ?
N5_1 B1_1 N1_4 C3_4 -21.6(2) . . . . ?
N2_1 B1_1 N1_4 C3_4 157.74(13) . . . . ?
C4_1 C3_1 B1_5 N2_5 120.84(14) . . . . ?
N2_1 C3_1 B1_5 N2_5 -51.39(17) . . . . ?
C4_1 C3_1 B1_5 N5_5 -58.53(18) . . . . ?
N2_1 C3_1 B1_5 N5_5 129.24(13) . . . . ?
N5_5 B1_5 N2_5 C4_5 -31.40(19) . . . . ?
C3_1 B1_5 N2_5 C4_5 149.23(12) . . . . ?
N5_5 B1_5 N2_5 C3_5 161.77(12) . . . . ?
C3_1 B1_5 N2_5 C3_5 -17.59(18) . . . . ?
N2_5 B1_5 N5_5 C6_5 -26.90(19) . . . . ?
C3_1 B1_5 N5_5 C6_5 152.47(12) . . . . ?
N2_5 B1_5 N5_5 C7_5 165.40(13) . . . . ?
C3_1 B1_5 N5_5 C7_5 -15.24(19) . . . . ?
C3_1 C4_1 B1_6 N2_6 -53.70(18) . . . . ?
N5_1 C4_1 B1_6 N2_6 125.96(13) . . . . ?
C3_1 C4_1 B1_6 N5_6 125.50(14) . . . . ?
N5_1 C4_1 B1_6 N5_6 -54.84(18) . . . . ?
N5_6 B1_6 N2_6 C3_6 160.06(12) . . . . ?
C4_1 B1_6 N2_6 C3_6 -20.75(19) . . . . ?
N5_6 B1_6 N2_6 C4_6 -26.18(19) . . . . ?
C4_1 B1_6 N2_6 C4_6 153.01(13) . . . . ?
N2_6 B1_6 N5_6 C6_6 152.54(13) . . . . ?
C4_1 B1_6 N5_6 C6_6 -26.65(19) . . . . ?
N2_6 B1_6 N5_6 C7_6 -30.8(2) . . . . ?
C4_1 B1_6 N5_6 C7_6 150.05(14) . . . . ?
C1_71 C2_71 C3_71 C4_71 62.4(15) . . . . ?
C2_71 C3_71 C4_71 C5_71 -179.7(11) . . . . ?
C1_72 C2_72 C3_72 C4_72 176.2(15) . . . . ?
C2_72 C3_72 C4_72 C5_72 178.6(14) . . . . ?

_refine_diff_density_max         0.329
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.039


_chemical_name_systematic        3-PhOMe
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_NiHe003_NiHe_a
_database_code_depnum_ccdc_archive 'CCDC 2468866'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2025-07-01 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
_audit_creation_method           'CIF-fill 1.3t (K.Radacki, 2005-23)'
_audit_creation_date             2023-03-22
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C21 H45 B4 N7'
_chemical_formula_sum            'C21 H45 B4 N7'
_chemical_formula_weight         438.88
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'


_cell_length_a                   13.5939(2)
_cell_length_b                   16.5266(2)
_cell_length_c                   11.71550(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.6180(10)
_cell_angle_gamma                90
_cell_volume                     2631.86(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16874
_cell_measurement_theta_min      5.3410
_cell_measurement_theta_max      73.7000

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_preparation       
;
 Crystals were grown from saturated solution of pentane at -30?C °C. For 
 data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 1 0.1317
1 -1 -1 0.0277
1 1 0 0.0563
0 1 0 0.0952
0 1 1 0.0551
-1 1 1 0.0238
0 -1 1 0.1254
0 1 -1 0.1372
-1 -1 1 0.0836
1 0 0 0.0593
-1 1 -1 0.1415
1 1 1 0.0694
2 0 -1 0.0467
-2 2 -1 0.1263
2 1 0 0.0523
1 -2 1 0.1314
-1 2 -1 0.1303
-2 1 -1 0.1381
-1 -1 -1 0.1559
0 -2 -1 0.0897
1 -2 0 0.1076
1 -2 -1 0.0607
1 -2 -2 0.0685
0 2 1 0.0534
-1 2 0 0.0919
-2 -2 -1 0.1493
-1 -1 0 0.1266

_shelx_estimated_absorpt_T_min   0.873
_shelx_estimated_absorpt_T_max   0.975
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  ω     37.00  93.00   0.50    0.18    --   82.28-112.00-150.00  112
  2  ω     37.00  93.00   0.50    0.18    --   82.28-112.00 -60.00  112
  3  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00 -60.00  100
  4  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00-150.00  100
  5  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00 -90.00  100
  6  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00-120.00  100
  7  ω     29.00  79.00   0.50    0.18    --   71.34 -95.00-120.00  100
  8  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00   0.00  100
  9  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00  60.00  100
 10  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00 120.00  100
 11  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00 -30.00  100
 12  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00  30.00  100
 13  ω     40.00  90.00   0.50    0.18    --   82.28 -95.00-180.00  100
 14  ω    103.00 131.00   0.50    0.18    --   85.25 114.00 113.82   56
 15  ω     93.00 132.00   0.50    0.18    --   85.25 132.00 -36.71   78
 16  ω     98.00 133.00   0.50    0.18    --   85.25  54.00 -60.82   70
 17  ω     98.00 136.00   0.50    0.18    --   85.25  43.00-122.04   76
 18  ω     46.00 133.00   0.50    0.18    --   82.28  15.00  60.00  174
 19  ω     96.00 137.00   0.50    0.18    --   85.25  35.00 149.31   82
 20  ω     46.00 133.00   0.50    0.18    --   82.28  15.00 150.00  174
 21  ω    -88.00 -51.00   0.50    0.18    --  -38.00 -44.00 175.05   74
 22  ω    -74.00 -39.00   0.50    0.18    --  -26.00 -52.00 -53.95   70
 23  ω    -98.00 -63.00   0.50    0.18    --  -50.00 -51.00-107.63   70
 24  ω    -54.00 -26.00   0.50    0.18    --  -14.00 -59.00-112.23   56
 25  ω    -54.00 -26.00   0.50    0.18    --  -14.00 -55.00  42.53   56
 26  ω   -130.00 -92.00   0.50    0.18    --  -79.50 -42.00 176.73   76
 27  ω   -123.00 -97.00   0.50    0.18    --  -79.50 -66.00 154.82   52
 28  ω   -122.00 -87.00   0.50    0.18    --  -74.00 -53.00 100.61   70
 29  ω   -124.00 -89.00   0.50    0.18    --  -78.00 -60.00  62.50   70
 30  ω   -126.00 -92.00   0.50    0.18    --  -79.50 -57.00  59.38   68
 31  ω   -103.00 -68.00   0.50    0.18    --  -54.00 -50.00 162.37   70
 32  ω   -110.00 -75.00   0.50    0.18    --  -62.00 -52.00  11.96   70
 33  ω   -106.00 -71.00   0.50    0.18    --  -58.00 -51.00  39.01   70
 34  ω   -128.00 -93.00   0.50    0.18    --  -79.50 -49.00  17.66   70
 35  ω   -107.00 -72.00   0.50    0.18    --  -58.00 -47.00 -54.43   70
 36  ω   -125.00 -91.00   0.50    0.18    --  -79.50 -60.00-117.69   68
 37  ω   -129.00 -93.00   0.50    0.18    --  -79.50 -47.00-150.93   72
 38  ω   -129.00 -93.00   0.50    0.18    --  -79.50 -48.00-103.17   72
 39  ω   -130.00 -92.00   0.50    0.18    --  -79.50 -43.00 -58.15   76
 40  ω   -126.00 -96.00   0.50    0.18    --  -79.50-116.00  21.02   60
 41  ω   -126.00 -87.00   0.50    0.18    --  -79.50-133.00 -42.34   78
 42  ω   -126.00 -84.00   0.50    0.18    --  -79.50-138.00 100.69   84
 43  ω   -126.00 -93.00   0.50    0.18    --  -79.50-120.00 134.81   66
 44  ω   -101.00 -31.00   0.50    0.18    --  -78.00 128.00-128.90  140
 45  ω   -100.00 -33.00   0.50    0.18    --  -79.50 123.00 -55.59  134
 46  ω    -97.00 -33.00   0.50    0.18    --  -79.50 116.00  21.35  128
 47  ω    -97.00 -33.00   0.50    0.18    --  -79.50 116.00  64.32  128
 48  ω    -99.00 -32.00   0.50    0.18    --  -79.50 122.00 118.17  134
 49  ω    -97.00 -33.00   0.50    0.18    --  -79.50 117.00 103.31  128
 50  ω    -88.00 -14.00   0.50    0.18    --  -60.16 126.00  60.00  148
 51  ω    -92.00 -31.00   0.50    0.18    --  -76.35 112.00 -60.00  122
;
_diffrn_orient_matrix_type       
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0630359000
_diffrn_orient_matrix_UB_12      -0.0742672000
_diffrn_orient_matrix_UB_13      -0.0318910000
_diffrn_orient_matrix_UB_21      0.0599653000
_diffrn_orient_matrix_UB_22      -0.0111326000
_diffrn_orient_matrix_UB_23      -0.1097591000
_diffrn_orient_matrix_UB_31      0.0726779000
_diffrn_orient_matrix_UB_32      -0.0551929000
_diffrn_orient_matrix_UB_33      0.0650177000
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            24715
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.211
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2405
_reflns_number_gt                2268
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;

_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_structure_solution    "SHELXT 2014/5 (Sheldrick, 2014)'"
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0526P)²+1.8380P] where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2405
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.1031
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.038
_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_
_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_1 B 0.45234(9) 0.84906(7) 0.35231(10) 0.0168(3) Uani 1 1 d . . . . .
C2_1 C 0.500000 0.80056(9) 0.250000 0.0161(3) Uani 1 2 d S T P . .
B3_1 B 0.57172(9) 0.72317(7) 0.27219(10) 0.0170(3) Uani 1 1 d . . . . .
N4_1 N 0.500000 0.65993(8) 0.250000 0.0176(3) Uani 1 2 d S T P . .
C1_2 C 0.500000 0.57368(9) 0.250000 0.0183(3) Uani 1 2 d S T P . .
C2_2 C 0.55516(8) 0.53139(7) 0.16841(10) 0.0210(3) Uani 1 1 d . . . . .
C3_2 C 0.55455(9) 0.44700(7) 0.17056(11) 0.0266(3) Uani 1 1 d . . . . .
H3_2 H 0.592270 0.417910 0.116480 0.032 Uiso 1 1 calc R U . . .
C4_2 C 0.500000 0.40485(10) 0.250000 0.0298(4) Uani 1 2 d S T P . .
H4_2 H 0.500001 0.347365 0.249998 0.036 Uiso 1 2 calc R U P . .
C5_2 C 0.61425(9) 0.57542(8) 0.08010(10) 0.0254(3) Uani 1 1 d . . . . .
H5A_2 H 0.634055 0.537395 0.020420 0.038 Uiso 1 1 calc R U . . .
H5B_2 H 0.672995 0.598919 0.116227 0.038 Uiso 1 1 calc R U . . .
H5C_2 H 0.574182 0.618635 0.046131 0.038 Uiso 1 1 calc R U . . .
N1_3 N 0.67224(7) 0.71378(6) 0.30003(8) 0.0193(2) Uani 1 1 d . . . . .
C2_3 C 0.71381(9) 0.63802(7) 0.34134(10) 0.0229(3) Uani 1 1 d . . . . .
H2A_3 H 0.663311 0.595728 0.338537 0.034 Uiso 1 1 calc R U . . .
H2B_3 H 0.737031 0.644948 0.420220 0.034 Uiso 1 1 calc R U . . .
H2C_3 H 0.769093 0.622346 0.293111 0.034 Uiso 1 1 calc R U . . .
C3_3 C 0.74313(8) 0.77948(7) 0.30629(10) 0.0227(3) Uani 1 1 d . . . . .
H3A_3 H 0.718126 0.825954 0.262887 0.034 Uiso 1 1 calc R U . . .
H3B_3 H 0.805689 0.761617 0.274008 0.034 Uiso 1 1 calc R U . . .
H3C_3 H 0.753379 0.795163 0.386209 0.034 Uiso 1 1 calc R U . . .
N4_3 N 0.45046(7) 0.81729(6) 0.46763(8) 0.0204(2) Uani 1 1 d . . . . .
C5_3 C 0.53084(9) 0.77429(7) 0.52212(10) 0.0252(3) Uani 1 1 d . . . . .
H5A_3 H 0.589339 0.777619 0.474184 0.038 Uiso 1 1 calc R U . . .
H5B_3 H 0.512497 0.717428 0.532391 0.038 Uiso 1 1 calc R U . . .
H5C_3 H 0.545158 0.798683 0.596712 0.038 Uiso 1 1 calc R U . . .
C6_3 C 0.36391(9) 0.81933(8) 0.53898(10) 0.0276(3) Uani 1 1 d . . . . .
H6A_3 H 0.308906 0.843358 0.496153 0.041 Uiso 1 1 calc R U . . .
H6B_3 H 0.377705 0.851887 0.607208 0.041 Uiso 1 1 calc R U . . .
H6C_3 H 0.346648 0.764111 0.561776 0.041 Uiso 1 1 calc R U . . .
N7_3 N 0.40029(7) 0.92343(6) 0.33247(8) 0.0191(2) Uani 1 1 d . . . . .
C8_3 C 0.37574(9) 0.95740(7) 0.22126(10) 0.0224(3) Uani 1 1 d . . . . .
H8A_3 H 0.388357 0.917065 0.161867 0.034 Uiso 1 1 calc R U . . .
H8B_3 H 0.416251 1.005430 0.207751 0.034 Uiso 1 1 calc R U . . .
H8C_3 H 0.306053 0.972584 0.219202 0.034 Uiso 1 1 calc R U . . .
C9_3 C 0.37955(9) 0.98169(7) 0.42225(10) 0.0243(3) Uani 1 1 d . . . . .
H9A_3 H 0.408763 0.962891 0.494349 0.037 Uiso 1 1 calc R U . . .
H9B_3 H 0.308218 0.987089 0.430759 0.037 Uiso 1 1 calc R U . . .
H9C_3 H 0.407722 1.034297 0.402077 0.037 Uiso 1 1 calc R U . . .


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_1 N7_3 1.4359(15) . ?
B1_1 N4_3 1.4500(15) . ?
B1_1 C2_1 1.5860(14) . ?
C2_1 B3_1 1.6275(16) . ?
C2_1 B3_1 1.6275(16) 2_655 ?
B3_1 N1_3 1.4099(16) . ?
B3_1 N4_1 1.4509(15) . ?
B3_1 B3_1 2.013(3) 2_655 ?
N4_1 C1_2 1.425(2) . ?
C1_2 C2_2 1.4071(14) . ?
C1_2 C2_2 1.4071(14) 2_655 ?
C2_2 C3_2 1.3949(17) . ?
C2_2 C5_2 1.5043(16) . ?
C3_2 C4_2 1.3843(16) . ?
C3_2 H3_2 0.9500 . ?
C4_2 H4_2 0.9500 . ?
C5_2 H5A_2 0.9800 . ?
C5_2 H5B_2 0.9800 . ?
C5_2 H5C_2 0.9800 . ?
N1_3 C3_3 1.4530(14) . ?
N1_3 C2_3 1.4544(14) . ?
C2_3 H2A_3 0.9800 . ?
C2_3 H2B_3 0.9800 . ?
C2_3 H2C_3 0.9800 . ?
C3_3 H3A_3 0.9800 . ?
C3_3 H3B_3 0.9800 . ?
C3_3 H3C_3 0.9800 . ?
N4_3 C5_3 1.4462(15) . ?
N4_3 C6_3 1.4511(15) . ?
C5_3 H5A_3 0.9800 . ?
C5_3 H5B_3 0.9800 . ?
C5_3 H5C_3 0.9800 . ?
C6_3 H6A_3 0.9800 . ?
C6_3 H6B_3 0.9800 . ?
C6_3 H6C_3 0.9800 . ?
N7_3 C8_3 1.4543(14) . ?
N7_3 C9_3 1.4556(14) . ?
C8_3 H8A_3 0.9800 . ?
C8_3 H8B_3 0.9800 . ?
C8_3 H8C_3 0.9800 . ?
C9_3 H9A_3 0.9800 . ?
C9_3 H9B_3 0.9800 . ?
C9_3 H9C_3 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
N7_3 B1_1 N4_3 116.56(10) . . ?
N7_3 B1_1 C2_1 120.99(10) . . ?
N4_3 B1_1 C2_1 122.18(10) . . ?
B1_1 C2_1 B1_1 119.29(13) . 2_655 ?
B1_1 C2_1 B3_1 121.69(7) . . ?
B1_1 C2_1 B3_1 105.60(6) 2_655 . ?
B1_1 C2_1 B3_1 105.60(6) . 2_655 ?
B1_1 C2_1 B3_1 121.69(7) 2_655 2_655 ?
B3_1 C2_1 B3_1 76.39(11) . 2_655 ?
N1_3 B3_1 N4_1 127.58(10) . . ?
N1_3 B3_1 C2_1 134.50(10) . . ?
N4_1 B3_1 C2_1 97.89(9) . . ?
N1_3 B3_1 B3_1 173.50(7) . 2_655 ?
N4_1 B3_1 B3_1 46.08(6) . 2_655 ?
C2_1 B3_1 B3_1 51.80(6) . 2_655 ?
C1_2 N4_1 B3_1 136.08(6) . . ?
C1_2 N4_1 B3_1 136.08(6) . 2_655 ?
B3_1 N4_1 B3_1 87.84(12) . 2_655 ?
C2_2 C1_2 C2_2 120.43(14) . 2_655 ?
C2_2 C1_2 N4_1 119.79(7) . . ?
C2_2 C1_2 N4_1 119.78(7) 2_655 . ?
C3_2 C2_2 C1_2 118.76(11) . . ?
C3_2 C2_2 C5_2 119.96(10) . . ?
C1_2 C2_2 C5_2 121.28(11) . . ?
C4_2 C3_2 C2_2 121.24(12) . . ?
C4_2 C3_2 H3_2 119.4 . . ?
C2_2 C3_2 H3_2 119.4 . . ?
C3_2 C4_2 C3_2 119.57(16) 2_655 . ?
C3_2 C4_2 H4_2 120.2 2_655 . ?
C3_2 C4_2 H4_2 120.2 . . ?
C2_2 C5_2 H5A_2 109.5 . . ?
C2_2 C5_2 H5B_2 109.5 . . ?
H5A_2 C5_2 H5B_2 109.5 . . ?
C2_2 C5_2 H5C_2 109.5 . . ?
H5A_2 C5_2 H5C_2 109.5 . . ?
H5B_2 C5_2 H5C_2 109.5 . . ?
B3_1 N1_3 C3_3 124.75(9) . . ?
B3_1 N1_3 C2_3 122.94(9) . . ?
C3_3 N1_3 C2_3 111.80(9) . . ?
N1_3 C2_3 H2A_3 109.5 . . ?
N1_3 C2_3 H2B_3 109.5 . . ?
H2A_3 C2_3 H2B_3 109.5 . . ?
N1_3 C2_3 H2C_3 109.5 . . ?
H2A_3 C2_3 H2C_3 109.5 . . ?
H2B_3 C2_3 H2C_3 109.5 . . ?
N1_3 C3_3 H3A_3 109.5 . . ?
N1_3 C3_3 H3B_3 109.5 . . ?
H3A_3 C3_3 H3B_3 109.5 . . ?
N1_3 C3_3 H3C_3 109.5 . . ?
H3A_3 C3_3 H3C_3 109.5 . . ?
H3B_3 C3_3 H3C_3 109.5 . . ?
C5_3 N4_3 B1_1 124.64(10) . . ?
C5_3 N4_3 C6_3 111.75(9) . . ?
B1_1 N4_3 C6_3 123.43(10) . . ?
N4_3 C5_3 H5A_3 109.5 . . ?
N4_3 C5_3 H5B_3 109.5 . . ?
H5A_3 C5_3 H5B_3 109.5 . . ?
N4_3 C5_3 H5C_3 109.5 . . ?
H5A_3 C5_3 H5C_3 109.5 . . ?
H5B_3 C5_3 H5C_3 109.5 . . ?
N4_3 C6_3 H6A_3 109.5 . . ?
N4_3 C6_3 H6B_3 109.5 . . ?
H6A_3 C6_3 H6B_3 109.5 . . ?
N4_3 C6_3 H6C_3 109.5 . . ?
H6A_3 C6_3 H6C_3 109.5 . . ?
H6B_3 C6_3 H6C_3 109.5 . . ?
B1_1 N7_3 C8_3 125.68(9) . . ?
B1_1 N7_3 C9_3 123.24(9) . . ?
C8_3 N7_3 C9_3 110.35(9) . . ?
N7_3 C8_3 H8A_3 109.5 . . ?
N7_3 C8_3 H8B_3 109.5 . . ?
H8A_3 C8_3 H8B_3 109.5 . . ?
N7_3 C8_3 H8C_3 109.5 . . ?
H8A_3 C8_3 H8C_3 109.5 . . ?
H8B_3 C8_3 H8C_3 109.5 . . ?
N7_3 C9_3 H9A_3 109.5 . . ?
N7_3 C9_3 H9B_3 109.5 . . ?
H9A_3 C9_3 H9B_3 109.5 . . ?
N7_3 C9_3 H9C_3 109.5 . . ?
H9A_3 C9_3 H9C_3 109.5 . . ?
H9B_3 C9_3 H9C_3 109.5 . . ?

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
N7_3 B1_1 C2_1 B1_1 36.35(8) . . . 2_655 ?
N4_3 B1_1 C2_1 B1_1 -149.81(12) . . . 2_655 ?
N7_3 B1_1 C2_1 B3_1 171.49(10) . . . . ?
N4_3 B1_1 C2_1 B3_1 -14.67(15) . . . . ?
N7_3 B1_1 C2_1 B3_1 -105.10(11) . . . 2_655 ?
N4_3 B1_1 C2_1 B3_1 68.74(11) . . . 2_655 ?
B1_1 C2_1 B3_1 N1_3 -81.99(15) . . . . ?
B1_1 C2_1 B3_1 N1_3 58.31(14) 2_655 . . . ?
B3_1 C2_1 B3_1 N1_3 177.89(17) 2_655 . . . ?
B1_1 C2_1 B3_1 N4_1 100.12(10) . . . . ?
B1_1 C2_1 B3_1 N4_1 -119.58(8) 2_655 . . . ?
B3_1 C2_1 B3_1 N4_1 0.0 2_655 . . . ?
B1_1 C2_1 B3_1 B3_1 100.13(10) . . . 2_655 ?
B1_1 C2_1 B3_1 B3_1 -119.58(8) 2_655 . . 2_655 ?
N1_3 B3_1 N4_1 C1_2 1.90(15) . . . . ?
C2_1 B3_1 N4_1 C1_2 180.000(0) . . . . ?
B3_1 B3_1 N4_1 C1_2 179.999(0) 2_655 . . . ?
N1_3 B3_1 N4_1 B3_1 -178.10(15) . . . 2_655 ?
C2_1 B3_1 N4_1 B3_1 0.0 . . . 2_655 ?
B3_1 N4_1 C1_2 C2_2 -66.47(9) . . . . ?
B3_1 N4_1 C1_2 C2_2 113.53(9) 2_655 . . . ?
B3_1 N4_1 C1_2 C2_2 113.52(9) . . . 2_655 ?
B3_1 N4_1 C1_2 C2_2 -66.48(9) 2_655 . . 2_655 ?
C2_2 C1_2 C2_2 C3_2 -0.41(8) 2_655 . . . ?
N4_1 C1_2 C2_2 C3_2 179.59(8) . . . . ?
C2_2 C1_2 C2_2 C5_2 179.70(12) 2_655 . . . ?
N4_1 C1_2 C2_2 C5_2 -0.30(12) . . . . ?
C1_2 C2_2 C3_2 C4_2 0.85(16) . . . . ?
C5_2 C2_2 C3_2 C4_2 -179.27(9) . . . . ?
C2_2 C3_2 C4_2 C3_2 -0.43(8) . . . 2_655 ?
N4_1 B3_1 N1_3 C3_3 171.33(10) . . . . ?
C2_1 B3_1 N1_3 C3_3 -6.04(19) . . . . ?
N4_1 B3_1 N1_3 C2_3 -17.52(17) . . . . ?
C2_1 B3_1 N1_3 C2_3 165.12(10) . . . . ?
N7_3 B1_1 N4_3 C5_3 -145.51(11) . . . . ?
C2_1 B1_1 N4_3 C5_3 40.40(16) . . . . ?
N7_3 B1_1 N4_3 C6_3 39.72(16) . . . . ?
C2_1 B1_1 N4_3 C6_3 -134.38(11) . . . . ?
N4_3 B1_1 N7_3 C8_3 -166.90(10) . . . . ?
C2_1 B1_1 N7_3 C8_3 7.28(16) . . . . ?
N4_3 B1_1 N7_3 C9_3 23.83(16) . . . . ?
C2_1 B1_1 N7_3 C9_3 -162.00(10) . . . . ?


_chemical_name_systematic        5
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_NiHe002_NiHe_a
_database_code_depnum_ccdc_archive 'CCDC 2468861'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2025-07-01 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_NiHe002_NiHe_a      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         29 Report
RESPONSE: reflections affected by beamstop
;



_audit_creation_method           'CIF-fill 1.3s (K.Radacki, 2005-23)'
_audit_creation_date             2023-03-17
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C19 H39 B3 N6'
_chemical_formula_sum            'C19 H39 B3 N6'
_chemical_formula_weight         383.99
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'


_cell_length_a                   7.7226(2)
_cell_length_b                   10.6260(3)
_cell_length_c                   14.8988(3)
_cell_angle_alpha                81.038(2)
_cell_angle_beta                 80.620(2)
_cell_angle_gamma                78.599(3)
_cell_volume                     1172.76(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10725
_cell_measurement_theta_min      2.9830
_cell_measurement_theta_max      74.0940

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_preparation       
;
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 -1 0.0648
-1 1 0 0.0347
-1 0 -1 0.0528
1 0 -1 0.0705
0 -1 -1 0.0324
0 1 1 0.0032
0 0 -1 0.0690
0 1 0 0.0306
0 1 -1 0.0542
1 -1 1 0.0291
1 -1 -1 0.0588
0 -1 1 0.0788
0 -1 0 0.0519
-1 0 1 0.0771
-1 0 0 0.0597
-1 1 -1 0.0472
-1 -1 -1 0.0647

_shelx_estimated_absorpt_T_min   0.921
_shelx_estimated_absorpt_T_max   0.981
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  ω     28.00  79.00   0.50    0.64    --   71.14 -95.00 120.00  102
  2  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00  30.00  100
  3  ω     28.00  79.00   0.50    0.64    --   71.14 -95.00 -60.00  102
  4  ω     16.00  66.00   0.50    0.64    --   58.28 -95.00-150.00  100
  5  ω     28.00  79.00   0.50    0.64    --   71.14 -95.00-180.00  102
  6  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00-180.00  100
  7  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00-150.00  100
  8  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00-120.00  100
  9  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00   0.00  100
 10  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00 -30.00  100
 11  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00  60.00  100
 12  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00  90.00  100
 13  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00 120.00  100
 14  ω     40.00  90.00   0.50    0.64    --   82.28 -95.00 150.00  100
 15  ω     43.00  91.00   0.50    0.64    --   85.25 -93.00 -82.01   96
 16  ω     51.00 135.00   0.50    0.64    --   85.25  13.00  61.55  168
 17  ω    101.00 132.00   0.50    0.64    --   85.25  49.00  56.62   62
 18  ω     55.00  90.00   0.50    0.64    --   42.00  52.00  94.22   70
 19  ω     44.00  79.00   0.50    0.64    --   30.00  49.00 -50.36   70
 20  ω     76.00 116.00   0.50    0.64    --   64.71  38.00 -28.98   80
 21  ω    101.00 134.00   0.50    0.64    --   85.25  45.00 -91.46   66
 22  ω     70.00 134.00   0.50    0.64    --   82.28  21.00-118.00  128
 23  ω     59.00 123.00   0.50    0.64    --   71.14  21.00-118.00  128
 24  ω     46.00 110.00   0.50    0.64    --   58.28  21.00-118.00  128
 25  ω    -92.00 -31.00   0.50    0.64    --  -76.35 112.00-150.00  122
 26  ω    -98.00 -32.00   0.50    0.64    --  -78.00 118.00 -28.75  132
 27  ω    -97.00 -32.00   0.50    0.64    --  -78.00 114.00  12.36  130
 28  ω    -97.00 -32.00   0.50    0.64    --  -78.00 114.00  73.15  130
 29  ω   -102.00 -32.00   0.50    0.64    --  -79.50 130.00  52.28  140
 30  ω    -97.00 -32.00   0.50    0.64    --  -78.00 114.00  88.67  130
 31  ω   -128.00 -65.00   0.50    0.64    --  -76.35 -21.00  74.00  126
 32  ω   -124.00 -92.00   0.50    0.64    --  -79.50 -63.00 147.07   64
 33  ω   -124.00 -95.00   0.50    0.64    --  -79.50 -65.00  24.38   58
 34  ω   -124.00 -89.00   0.50    0.64    --  -78.00 -60.00 -80.92   70
 35  ω   -126.00 -92.00   0.50    0.64    --  -79.50 -57.00-140.66   68
 36  ω   -127.00 -92.00   0.50    0.64    --  -79.50 -53.00 -98.98   70
 37  ω   -128.00 -93.00   0.50    0.64    --  -79.50 -52.00 -64.99   70
 38  ω   -128.00 -93.00   0.50    0.64    --  -79.50 -51.00 -31.06   70
 39  ω   -107.00 -72.00   0.50    0.64    --  -58.00 -48.00 -33.76   70
 40  ω   -130.00 -91.00   0.50    0.64    --  -79.50 -39.00 -46.51   78
 41  ω   -130.00 -92.00   0.50    0.64    --  -79.50 -43.00  60.06   76
 42  ω   -121.00 -58.00   0.50    0.64    --  -69.45 -21.00  74.00  126
 43  ω   -112.00 -48.00   0.50    0.64    --  -59.96 -21.00  74.00  128
 44  ω   -106.00 -71.00   0.50    0.64    --  -58.00 -52.00 158.28   70
 45  ω   -128.00 -93.00   0.50    0.64    --  -79.50 -52.00 147.73   70
 46  ω   -126.00 -86.00   0.50    0.64    --  -79.50-134.00 115.82   80
 47  ω   -127.00 -90.00   0.50    0.64    --  -79.50-126.00 176.85   74
 48  ω   -126.00 -91.00   0.50    0.64    --  -79.50-124.00 145.96   70
 49  ω   -126.00 -93.00   0.50    0.64    --  -79.50-120.00  48.27   66
 50  ω   -126.00 -93.00   0.50    0.64    --  -79.50-120.00 -96.82   66
;
_diffrn_orient_matrix_type       
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.1012135000
_diffrn_orient_matrix_UB_12      -0.1373012000
_diffrn_orient_matrix_UB_13      0.0273499000
_diffrn_orient_matrix_UB_21      0.1747759000
_diffrn_orient_matrix_UB_22      0.0534593000
_diffrn_orient_matrix_UB_23      -0.0109985000
_diffrn_orient_matrix_UB_31      -0.0375412000
_diffrn_orient_matrix_UB_32      0.0229629000
_diffrn_orient_matrix_UB_33      0.1014741000
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            22823
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.031
_diffrn_reflns_theta_max         70.050
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4417
_reflns_number_gt                3765
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;

_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_structure_solution    "SHELXT 2014/5 (Sheldrick, 2014)'"
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0794P)²+0.1769P] where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4417
_refine_ls_number_parameters     265
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1263
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.041
_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_
_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_1 B 0.21028(19) 0.52914(14) 0.73457(10) 0.0293(3) Uani 1 1 d . . . . .
C2_1 C 0.30494(16) 0.62519(12) 0.75723(8) 0.0267(3) Uani 1 1 d . . . . .
B3_1 B 0.4181(2) 0.51945(14) 0.80907(10) 0.0289(3) Uani 1 1 d . . . . .
N4_1 N 0.32317(14) 0.40780(10) 0.78856(7) 0.0304(3) Uani 1 1 d . . . . .
C5_1 C 0.22025(19) 0.34028(13) 0.86856(10) 0.0375(3) Uani 1 1 d . . . . .
H5A_1 H 0.145137 0.404302 0.905591 0.056 Uiso 1 1 calc R U . . .
H5B_1 H 0.303034 0.281476 0.906020 0.056 Uiso 1 1 calc R U . . .
H5C_1 H 0.144843 0.290611 0.846707 0.056 Uiso 1 1 calc R U . . .
C6_1 C 0.4402(2) 0.31315(13) 0.73143(10) 0.0399(3) Uani 1 1 d . . . . .
H6A_1 H 0.497493 0.359673 0.676084 0.060 Uiso 1 1 calc R U . . .
H6B_1 H 0.368532 0.256760 0.713933 0.060 Uiso 1 1 calc R U . . .
H6C_1 H 0.531847 0.260611 0.766601 0.060 Uiso 1 1 calc R U . . .
N1_2 N 0.56235(15) 0.49209(11) 0.86075(8) 0.0342(3) Uani 1 1 d . . . . .
C2_2 C 0.65887(19) 0.59330(14) 0.86978(10) 0.0385(3) Uani 1 1 d . . . . .
H2A_2 H 0.604555 0.675723 0.837753 0.058 Uiso 1 1 calc R U . . .
H2B_2 H 0.783676 0.570753 0.842803 0.058 Uiso 1 1 calc R U . . .
H2C_2 H 0.653252 0.601481 0.934851 0.058 Uiso 1 1 calc R U . . .
C3_2 C 0.6406(2) 0.36721(14) 0.90571(11) 0.0428(4) Uani 1 1 d . . . . .
H3A_2 H 0.567048 0.302917 0.902992 0.064 Uiso 1 1 calc R U . . .
H3B_2 H 0.646274 0.374236 0.969934 0.064 Uiso 1 1 calc R U . . .
H3C_2 H 0.761195 0.340278 0.874509 0.064 Uiso 1 1 calc R U . . .
N4_2 N 0.07127(15) 0.51898(11) 0.68640(8) 0.0350(3) Uani 1 1 d . . . . .
C5_2 C 0.0145(2) 0.40203(16) 0.67221(11) 0.0471(4) Uani 1 1 d . . . . .
H5A_2 H 0.086744 0.326411 0.703148 0.071 Uiso 1 1 calc R U . . .
H5B_2 H 0.029864 0.395648 0.606379 0.071 Uiso 1 1 calc R U . . .
H5C_2 H -0.111380 0.405086 0.697547 0.071 Uiso 1 1 calc R U . . .
C6_2 C -0.03401(19) 0.63484(15) 0.64426(10) 0.0400(3) Uani 1 1 d . . . . .
H6A_2 H 0.007212 0.711287 0.656372 0.060 Uiso 1 1 calc R U . . .
H6B_2 H -0.159803 0.638595 0.670003 0.060 Uiso 1 1 calc R U . . .
H6C_2 H -0.020632 0.632987 0.577901 0.060 Uiso 1 1 calc R U . . .
C1_3 C 0.29846(16) 0.83361(12) 0.80790(8) 0.0269(3) Uani 1 1 d . . . . .
C2_3 C 0.17515(17) 0.82559(12) 0.88865(9) 0.0304(3) Uani 1 1 d . . . . .
C3_3 C 0.1866(2) 0.89458(13) 0.95879(9) 0.0368(3) Uani 1 1 d . . . . .
H3_3 H 0.104853 0.888438 1.013663 0.044 Uiso 1 1 calc R U . . .
C4_3 C 0.3145(2) 0.97213(14) 0.95048(10) 0.0412(3) Uani 1 1 d . . . . .
H4_3 H 0.320216 1.018870 0.999025 0.049 Uiso 1 1 calc R U . . .
C5_3 C 0.4336(2) 0.98065(13) 0.87081(10) 0.0377(3) Uani 1 1 d . . . . .
H5_3 H 0.520963 1.034119 0.864959 0.045 Uiso 1 1 calc R U . . .
C6_3 C 0.42862(17) 0.91293(12) 0.79910(9) 0.0308(3) Uani 1 1 d . . . . .
C7_3 C 0.02560(18) 0.75012(13) 0.89906(10) 0.0363(3) Uani 1 1 d . . . . .
H7A_3 H -0.071999 0.784939 0.944257 0.055 Uiso 1 1 calc R U . . .
H7B_3 H 0.069244 0.658891 0.919829 0.055 Uiso 1 1 calc R U . . .
H7C_3 H -0.017720 0.757429 0.839860 0.055 Uiso 1 1 calc R U . . .
C8_3 C 0.56538(18) 0.92275(14) 0.71482(10) 0.0367(3) Uani 1 1 d . . . . .
H8A_3 H 0.667410 0.953911 0.729513 0.055 Uiso 1 1 calc R U . . .
H8B_3 H 0.512056 0.983431 0.666027 0.055 Uiso 1 1 calc R U . . .
H8C_3 H 0.605548 0.837286 0.694151 0.055 Uiso 1 1 calc R U . . .
N1_4 N 0.29191(13) 0.76380(9) 0.73475(7) 0.0255(2) Uani 1 1 d . . . . .
B2_4 B 0.27690(18) 0.83018(14) 0.64298(10) 0.0278(3) Uani 1 1 d . . . . .
N3_4 N 0.35266(14) 0.76713(11) 0.56425(7) 0.0318(3) Uani 1 1 d . . . . .
C4_4 C 0.50388(19) 0.66190(13) 0.56224(9) 0.0355(3) Uani 1 1 d . . . . .
H4A_4 H 0.552014 0.647644 0.620642 0.053 Uiso 1 1 calc R U . . .
H4B_4 H 0.596224 0.683936 0.512037 0.053 Uiso 1 1 calc R U . . .
H4C_4 H 0.465724 0.582905 0.552671 0.053 Uiso 1 1 calc R U . . .
C5_4 C 0.2753(2) 0.79447(17) 0.47920(9) 0.0437(4) Uani 1 1 d . . . . .
H5A_4 H 0.166482 0.859638 0.486098 0.066 Uiso 1 1 calc R U . . .
H5B_4 H 0.246203 0.714894 0.464673 0.066 Uiso 1 1 calc R U . . .
H5C_4 H 0.361073 0.827312 0.429467 0.066 Uiso 1 1 calc R U . . .
N6_4 N 0.18279(14) 0.96164(10) 0.63012(7) 0.0312(3) Uani 1 1 d . . . . .
C7_4 C 0.04778(17) 1.02120(13) 0.69801(10) 0.0354(3) Uani 1 1 d . . . . .
H7A_4 H 0.001881 0.953607 0.742762 0.053 Uiso 1 1 calc R U . . .
H7B_4 H -0.050108 1.074536 0.667587 0.053 Uiso 1 1 calc R U . . .
H7C_4 H 0.100374 1.075665 0.729535 0.053 Uiso 1 1 calc R U . . .
C8_4 C 0.2397(2) 1.05699(15) 0.55535(11) 0.0444(4) Uani 1 1 d . . . . .
H8A_4 H 0.341858 1.015417 0.515586 0.067 Uiso 1 1 calc R U . . .
H8B_4 H 0.274054 1.126823 0.580613 0.067 Uiso 1 1 calc R U . . .
H8C_4 H 0.141274 1.092827 0.519593 0.067 Uiso 1 1 calc R U . . .


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_1 N4_2 1.4143(18) . ?
B1_1 C2_1 1.4740(18) . ?
B1_1 N4_1 1.5908(18) . ?
B1_1 B3_1 2.073(2) . ?
C2_1 N1_4 1.4458(15) . ?
C2_1 B3_1 1.4778(19) . ?
B3_1 N1_2 1.4145(18) . ?
B3_1 N4_1 1.6024(17) . ?
N4_1 C6_1 1.4865(17) . ?
N4_1 C5_1 1.4891(16) . ?
C5_1 H5A_1 0.9800 . ?
C5_1 H5B_1 0.9800 . ?
C5_1 H5C_1 0.9800 . ?
C6_1 H6A_1 0.9800 . ?
C6_1 H6B_1 0.9800 . ?
C6_1 H6C_1 0.9800 . ?
N1_2 C3_2 1.4535(17) . ?
N1_2 C2_2 1.4577(17) . ?
C2_2 H2A_2 0.9800 . ?
C2_2 H2B_2 0.9800 . ?
C2_2 H2C_2 0.9800 . ?
C3_2 H3A_2 0.9800 . ?
C3_2 H3B_2 0.9800 . ?
C3_2 H3C_2 0.9800 . ?
N4_2 C6_2 1.4494(18) . ?
N4_2 C5_2 1.4521(17) . ?
C5_2 H5A_2 0.9800 . ?
C5_2 H5B_2 0.9800 . ?
C5_2 H5C_2 0.9800 . ?
C6_2 H6A_2 0.9800 . ?
C6_2 H6B_2 0.9800 . ?
C6_2 H6C_2 0.9800 . ?
C1_3 C2_3 1.4100(18) . ?
C1_3 C6_3 1.4126(17) . ?
C1_3 N1_4 1.4231(16) . ?
C2_3 C3_3 1.3898(19) . ?
C2_3 C7_3 1.5067(18) . ?
C3_3 C4_3 1.386(2) . ?
C3_3 H3_3 0.9500 . ?
C4_3 C5_3 1.381(2) . ?
C4_3 H4_3 0.9500 . ?
C5_3 C6_3 1.3873(19) . ?
C5_3 H5_3 0.9500 . ?
C6_3 C8_3 1.5077(19) . ?
C7_3 H7A_3 0.9800 . ?
C7_3 H7B_3 0.9800 . ?
C7_3 H7C_3 0.9800 . ?
C8_3 H8A_3 0.9800 . ?
C8_3 H8B_3 0.9800 . ?
C8_3 H8C_3 0.9800 . ?
N1_4 B2_4 1.4489(17) . ?
B2_4 N3_4 1.4259(19) . ?
B2_4 N6_4 1.4411(18) . ?
N3_4 C4_4 1.4484(18) . ?
N3_4 C5_4 1.4526(17) . ?
C4_4 H4A_4 0.9800 . ?
C4_4 H4B_4 0.9800 . ?
C4_4 H4C_4 0.9800 . ?
C5_4 H5A_4 0.9800 . ?
C5_4 H5B_4 0.9800 . ?
C5_4 H5C_4 0.9800 . ?
N6_4 C7_4 1.4510(18) . ?
N6_4 C8_4 1.4577(16) . ?
C7_4 H7A_4 0.9800 . ?
C7_4 H7B_4 0.9800 . ?
C7_4 H7C_4 0.9800 . ?
C8_4 H8A_4 0.9800 . ?
C8_4 H8B_4 0.9800 . ?
C8_4 H8C_4 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
N4_2 B1_1 C2_1 141.60(13) . . ?
N4_2 B1_1 N4_1 123.17(11) . . ?
C2_1 B1_1 N4_1 95.23(10) . . ?
N4_2 B1_1 B3_1 172.94(12) . . ?
C2_1 B1_1 B3_1 45.47(7) . . ?
N4_1 B1_1 B3_1 49.76(7) . . ?
N1_4 C2_1 B1_1 134.28(11) . . ?
N1_4 C2_1 B3_1 136.48(11) . . ?
B1_1 C2_1 B3_1 89.22(10) . . ?
N1_2 B3_1 C2_1 143.36(12) . . ?
N1_2 B3_1 N4_1 122.03(11) . . ?
C2_1 B3_1 N4_1 94.59(10) . . ?
N1_2 B3_1 B1_1 171.25(12) . . ?
C2_1 B3_1 B1_1 45.32(7) . . ?
N4_1 B3_1 B1_1 49.28(7) . . ?
C6_1 N4_1 C5_1 110.84(10) . . ?
C6_1 N4_1 B1_1 116.07(10) . . ?
C5_1 N4_1 B1_1 115.12(10) . . ?
C6_1 N4_1 B3_1 114.46(10) . . ?
C5_1 N4_1 B3_1 116.66(10) . . ?
B1_1 N4_1 B3_1 80.96(9) . . ?
N4_1 C5_1 H5A_1 109.5 . . ?
N4_1 C5_1 H5B_1 109.5 . . ?
H5A_1 C5_1 H5B_1 109.5 . . ?
N4_1 C5_1 H5C_1 109.5 . . ?
H5A_1 C5_1 H5C_1 109.5 . . ?
H5B_1 C5_1 H5C_1 109.5 . . ?
N4_1 C6_1 H6A_1 109.5 . . ?
N4_1 C6_1 H6B_1 109.5 . . ?
H6A_1 C6_1 H6B_1 109.5 . . ?
N4_1 C6_1 H6C_1 109.5 . . ?
H6A_1 C6_1 H6C_1 109.5 . . ?
H6B_1 C6_1 H6C_1 109.5 . . ?
B3_1 N1_2 C3_2 127.64(12) . . ?
B3_1 N1_2 C2_2 120.82(11) . . ?
C3_2 N1_2 C2_2 111.45(11) . . ?
N1_2 C2_2 H2A_2 109.5 . . ?
N1_2 C2_2 H2B_2 109.5 . . ?
H2A_2 C2_2 H2B_2 109.5 . . ?
N1_2 C2_2 H2C_2 109.5 . . ?
H2A_2 C2_2 H2C_2 109.5 . . ?
H2B_2 C2_2 H2C_2 109.5 . . ?
N1_2 C3_2 H3A_2 109.5 . . ?
N1_2 C3_2 H3B_2 109.5 . . ?
H3A_2 C3_2 H3B_2 109.5 . . ?
N1_2 C3_2 H3C_2 109.5 . . ?
H3A_2 C3_2 H3C_2 109.5 . . ?
H3B_2 C3_2 H3C_2 109.5 . . ?
B1_1 N4_2 C6_2 119.98(11) . . ?
B1_1 N4_2 C5_2 127.85(12) . . ?
C6_2 N4_2 C5_2 112.17(11) . . ?
N4_2 C5_2 H5A_2 109.5 . . ?
N4_2 C5_2 H5B_2 109.5 . . ?
H5A_2 C5_2 H5B_2 109.5 . . ?
N4_2 C5_2 H5C_2 109.5 . . ?
H5A_2 C5_2 H5C_2 109.5 . . ?
H5B_2 C5_2 H5C_2 109.5 . . ?
N4_2 C6_2 H6A_2 109.5 . . ?
N4_2 C6_2 H6B_2 109.5 . . ?
H6A_2 C6_2 H6B_2 109.5 . . ?
N4_2 C6_2 H6C_2 109.5 . . ?
H6A_2 C6_2 H6C_2 109.5 . . ?
H6B_2 C6_2 H6C_2 109.5 . . ?
C2_3 C1_3 C6_3 119.65(12) . . ?
C2_3 C1_3 N1_4 120.71(11) . . ?
C6_3 C1_3 N1_4 119.64(11) . . ?
C3_3 C2_3 C1_3 118.99(12) . . ?
C3_3 C2_3 C7_3 119.04(12) . . ?
C1_3 C2_3 C7_3 121.89(12) . . ?
C4_3 C3_3 C2_3 121.49(13) . . ?
C4_3 C3_3 H3_3 119.3 . . ?
C2_3 C3_3 H3_3 119.3 . . ?
C5_3 C4_3 C3_3 119.20(13) . . ?
C5_3 C4_3 H4_3 120.4 . . ?
C3_3 C4_3 H4_3 120.4 . . ?
C4_3 C5_3 C6_3 121.52(13) . . ?
C4_3 C5_3 H5_3 119.2 . . ?
C6_3 C5_3 H5_3 119.2 . . ?
C5_3 C6_3 C1_3 119.14(13) . . ?
C5_3 C6_3 C8_3 119.25(12) . . ?
C1_3 C6_3 C8_3 121.59(12) . . ?
C2_3 C7_3 H7A_3 109.5 . . ?
C2_3 C7_3 H7B_3 109.5 . . ?
H7A_3 C7_3 H7B_3 109.5 . . ?
C2_3 C7_3 H7C_3 109.5 . . ?
H7A_3 C7_3 H7C_3 109.5 . . ?
H7B_3 C7_3 H7C_3 109.5 . . ?
C6_3 C8_3 H8A_3 109.5 . . ?
C6_3 C8_3 H8B_3 109.5 . . ?
H8A_3 C8_3 H8B_3 109.5 . . ?
C6_3 C8_3 H8C_3 109.5 . . ?
H8A_3 C8_3 H8C_3 109.5 . . ?
H8B_3 C8_3 H8C_3 109.5 . . ?
C1_3 N1_4 C2_1 116.35(9) . . ?
C1_3 N1_4 B2_4 120.70(10) . . ?
C2_1 N1_4 B2_4 122.93(10) . . ?
N3_4 B2_4 N6_4 118.90(11) . . ?
N3_4 B2_4 N1_4 121.06(12) . . ?
N6_4 B2_4 N1_4 120.04(12) . . ?
B2_4 N3_4 C4_4 124.34(11) . . ?
B2_4 N3_4 C5_4 122.98(12) . . ?
C4_4 N3_4 C5_4 112.47(12) . . ?
N3_4 C4_4 H4A_4 109.5 . . ?
N3_4 C4_4 H4B_4 109.5 . . ?
H4A_4 C4_4 H4B_4 109.5 . . ?
N3_4 C4_4 H4C_4 109.5 . . ?
H4A_4 C4_4 H4C_4 109.5 . . ?
H4B_4 C4_4 H4C_4 109.5 . . ?
N3_4 C5_4 H5A_4 109.5 . . ?
N3_4 C5_4 H5B_4 109.5 . . ?
H5A_4 C5_4 H5B_4 109.5 . . ?
N3_4 C5_4 H5C_4 109.5 . . ?
H5A_4 C5_4 H5C_4 109.5 . . ?
H5B_4 C5_4 H5C_4 109.5 . . ?
B2_4 N6_4 C7_4 124.45(10) . . ?
B2_4 N6_4 C8_4 122.57(11) . . ?
C7_4 N6_4 C8_4 111.81(11) . . ?
N6_4 C7_4 H7A_4 109.5 . . ?
N6_4 C7_4 H7B_4 109.5 . . ?
H7A_4 C7_4 H7B_4 109.5 . . ?
N6_4 C7_4 H7C_4 109.5 . . ?
H7A_4 C7_4 H7C_4 109.5 . . ?
H7B_4 C7_4 H7C_4 109.5 . . ?
N6_4 C8_4 H8A_4 109.5 . . ?
N6_4 C8_4 H8B_4 109.5 . . ?
H8A_4 C8_4 H8B_4 109.5 . . ?
N6_4 C8_4 H8C_4 109.5 . . ?
H8A_4 C8_4 H8C_4 109.5 . . ?
H8B_4 C8_4 H8C_4 109.5 . . ?

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
N4_2 B1_1 C2_1 N1_4 -1.3(3) . . . . ?
N4_1 B1_1 C2_1 N1_4 178.76(13) . . . . ?
B3_1 B1_1 C2_1 N1_4 178.57(18) . . . . ?
N4_2 B1_1 C2_1 B3_1 -179.86(19) . . . . ?
N4_1 B1_1 C2_1 B3_1 0.19(10) . . . . ?
N1_4 C2_1 B3_1 N1_2 -0.3(3) . . . . ?
B1_1 C2_1 B3_1 N1_2 178.2(2) . . . . ?
N1_4 C2_1 B3_1 N4_1 -178.70(14) . . . . ?
B1_1 C2_1 B3_1 N4_1 -0.19(10) . . . . ?
N1_4 C2_1 B3_1 B1_1 -178.51(19) . . . . ?
N4_2 B1_1 N4_1 C6_1 66.97(16) . . . . ?
C2_1 B1_1 N4_1 C6_1 -113.07(12) . . . . ?
B3_1 B1_1 N4_1 C6_1 -112.89(12) . . . . ?
N4_2 B1_1 N4_1 C5_1 -64.85(16) . . . . ?
C2_1 B1_1 N4_1 C5_1 115.11(11) . . . . ?
B3_1 B1_1 N4_1 C5_1 115.29(12) . . . . ?
N4_2 B1_1 N4_1 B3_1 179.86(14) . . . . ?
C2_1 B1_1 N4_1 B3_1 -0.18(9) . . . . ?
N1_2 B3_1 N4_1 C6_1 -64.07(16) . . . . ?
C2_1 B3_1 N4_1 C6_1 114.79(12) . . . . ?
B1_1 B3_1 N4_1 C6_1 114.61(12) . . . . ?
N1_2 B3_1 N4_1 C5_1 67.67(16) . . . . ?
C2_1 B3_1 N4_1 C5_1 -113.47(12) . . . . ?
B1_1 B3_1 N4_1 C5_1 -113.65(12) . . . . ?
N1_2 B3_1 N4_1 B1_1 -178.68(14) . . . . ?
C2_1 B3_1 N4_1 B1_1 0.18(9) . . . . ?
C2_1 B3_1 N1_2 C3_2 178.78(17) . . . . ?
N4_1 B3_1 N1_2 C3_2 -3.1(2) . . . . ?
C2_1 B3_1 N1_2 C2_2 -5.0(3) . . . . ?
N4_1 B3_1 N1_2 C2_2 173.13(11) . . . . ?
C2_1 B1_1 N4_2 C6_2 -4.3(3) . . . . ?
N4_1 B1_1 N4_2 C6_2 175.63(11) . . . . ?
C2_1 B1_1 N4_2 C5_2 175.88(17) . . . . ?
N4_1 B1_1 N4_2 C5_2 -4.2(2) . . . . ?
C6_3 C1_3 C2_3 C3_3 -1.12(19) . . . . ?
N1_4 C1_3 C2_3 C3_3 179.60(11) . . . . ?
C6_3 C1_3 C2_3 C7_3 175.59(11) . . . . ?
N1_4 C1_3 C2_3 C7_3 -3.69(18) . . . . ?
C1_3 C2_3 C3_3 C4_3 0.9(2) . . . . ?
C7_3 C2_3 C3_3 C4_3 -175.89(12) . . . . ?
C2_3 C3_3 C4_3 C5_3 -0.2(2) . . . . ?
C3_3 C4_3 C5_3 C6_3 -0.3(2) . . . . ?
C4_3 C5_3 C6_3 C1_3 0.1(2) . . . . ?
C4_3 C5_3 C6_3 C8_3 -178.20(12) . . . . ?
C2_3 C1_3 C6_3 C5_3 0.63(19) . . . . ?
N1_4 C1_3 C6_3 C5_3 179.92(11) . . . . ?
C2_3 C1_3 C6_3 C8_3 178.87(12) . . . . ?
N1_4 C1_3 C6_3 C8_3 -1.84(18) . . . . ?
C2_3 C1_3 N1_4 C2_1 -56.92(15) . . . . ?
C6_3 C1_3 N1_4 C2_1 123.80(12) . . . . ?
C2_3 C1_3 N1_4 B2_4 124.39(13) . . . . ?
C6_3 C1_3 N1_4 B2_4 -54.89(16) . . . . ?
B1_1 C2_1 N1_4 C1_3 136.38(14) . . . . ?
B3_1 C2_1 N1_4 C1_3 -45.70(19) . . . . ?
B1_1 C2_1 N1_4 B2_4 -45.0(2) . . . . ?
B3_1 C2_1 N1_4 B2_4 132.97(15) . . . . ?
C1_3 N1_4 B2_4 N3_4 149.45(11) . . . . ?
C2_1 N1_4 B2_4 N3_4 -29.16(17) . . . . ?
C1_3 N1_4 B2_4 N6_4 -31.14(16) . . . . ?
C2_1 N1_4 B2_4 N6_4 150.25(11) . . . . ?
N6_4 B2_4 N3_4 C4_4 154.24(12) . . . . ?
N1_4 B2_4 N3_4 C4_4 -26.35(18) . . . . ?
N6_4 B2_4 N3_4 C5_4 -31.49(18) . . . . ?
N1_4 B2_4 N3_4 C5_4 147.92(12) . . . . ?
N3_4 B2_4 N6_4 C7_4 156.42(12) . . . . ?
N1_4 B2_4 N6_4 C7_4 -23.00(18) . . . . ?
N3_4 B2_4 N6_4 C8_4 -36.96(18) . . . . ?
N1_4 B2_4 N6_4 C8_4 143.62(13) . . . . ?


_chemical_name_systematic        4
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_NiHe004_NiHe_a
_database_code_depnum_ccdc_archive 'CCDC 2468863'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2025-07-01 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_NiHe004_NiHe_a      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         44 Report
RESPONSE: reflections affected by beamstop
;

_audit_creation_method           'CIF-fill 1.3w (K.Radacki, 2005-23)'
_audit_creation_date             2023-03-31
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C28 H56 B4 N8'
_chemical_formula_sum            'C28 H56 B4 N8'
_chemical_formula_weight         548.04
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'


_cell_length_a                   10.7702(3)
_cell_length_b                   12.1456(3)
_cell_length_c                   15.0064(3)
_cell_angle_alpha                68.928(2)
_cell_angle_beta                 71.502(2)
_cell_angle_gamma                66.053(2)
_cell_volume                     1639.92(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17409
_cell_measurement_theta_min      3.2120
_cell_measurement_theta_max      74.6700

_exptl_crystal_description       block
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_preparation       
;
 Crystals were grown at -30?C °C from saturated solution in pentane. For 
 data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 2 1 0.0944
1 -2 -1 0.0972
0 -2 1 0.0772
1 1 2 0.0560
-1 0 -2 0.0707
-1 -1 2 0.0357
0 1 -2 0.0412
-1 2 2 0.0911
0 0 -1 0.0487
0 0 1 0.0461
0 2 -1 0.0688
-1 -2 -2 0.0795
1 2 2 0.0767
1 0 2 0.0621
-1 -2 2 0.0444
0 -1 1 0.0641
1 0 -2 0.0899
-1 -1 -1 0.0532
1 1 1 0.0724

_shelx_estimated_absorpt_T_min   0.902
_shelx_estimated_absorpt_T_max   0.956
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  ω     45.00  92.00   0.50    0.50    --   85.25-120.00 160.16   94
  2  ω     39.00  65.00   0.50    0.50    --   85.25-136.00  77.56   52
  3  ω     32.00  98.00   0.50    0.50    --   78.00-118.00   8.65  132
  4  ω     35.00  98.00   0.50    0.50    --   82.00-120.00 -35.81  126
  5  ω     37.00  62.00   0.50    0.50    --   82.28-112.00   0.00   50
  6  ω     37.00  93.00   0.50    0.50    --   82.28-112.00  30.00  112
  7  ω     37.00  62.00   0.50    0.50    --   82.28-112.00 -30.00   50
  8  ω     37.00  93.00   0.50    0.50    --   82.28-112.00 -60.00  112
  9  ω     38.00  66.00   0.50    0.50    --   85.25-128.00 -83.79   56
 10  ω     37.00  62.00   0.50    0.50    --   82.28-112.00-120.00   50
 11  ω     37.00  93.00   0.50    0.50    --   82.28-112.00-150.00  112
 12  ω     53.00  92.00   0.50    0.50    --   85.25 -99.00 -92.99   78
 13  ω     44.00  93.00   0.50    0.50    --   85.25 -98.00  35.22   98
 14  ω     64.00  90.00   0.50    0.50    --   85.25 -99.00  70.30   52
 15  ω     42.00  92.00   0.50    0.50    --   85.25-111.00 110.83  100
 16  ω     40.00  90.00   0.50    0.50    --   82.28 -95.00 120.00  100
 17  ω     48.00  92.00   0.50    0.50    --   85.25 -96.00 136.53   88
 18  ω     44.00  86.00   0.50    0.50    --   82.28 -95.00   0.00   84
 19  ω     40.00  90.00   0.50    0.50    --   82.28 -95.00 -30.00  100
 20  ω     54.00  92.00   0.50    0.50    --   85.25 -96.00-125.32   76
 21  ω     40.00  90.00   0.50    0.50    --   82.28 -95.00-150.00  100
 22  ω     40.00  65.00   0.50    0.50    --   82.28 -95.00-180.00   50
 23  ω     16.00  66.00   0.50    0.50    --   58.28 -95.00-120.00  100
 24  ω     40.00  90.00   0.50    0.50    --   82.28 -95.00  30.00  100
 25  ω     44.00  69.00   0.50    0.50    --   85.25 -72.00 -26.24   50
 26  ω     51.00  82.00   0.50    0.50    --   85.25 -80.00 -76.34   62
 27  ω     45.00  70.00   0.50    0.50    --   85.25 -76.00  33.26   50
 28  ω     45.00  70.00   0.50    0.50    --   85.25 -74.00 128.22   50
 29  ω     97.00 123.00   0.50    0.50    --   85.25 127.00-162.62   52
 30  ω    106.00 132.00   0.50    0.50    --   82.28  15.00  60.00   52
 31  ω    101.00 127.00   0.50    0.50    --   85.25  64.00 133.34   52
 32  ω     98.00 123.00   0.50    0.50    --   85.25  54.00  67.36   50
 33  ω    108.00 133.00   0.50    0.50    --   82.28  15.00 150.00   50
 34  ω    110.00 136.00   0.50    0.50    --   85.25  38.00 107.94   52
 35  ω     46.00 133.00   0.50    0.50    --   82.28  15.00 120.00  174
 36  ω     98.00 136.00   0.50    0.50    --   85.25  43.00 -95.59   76
 37  ω     97.00 131.00   0.50    0.50    --   85.25  59.00-177.27   68
 38  ω     97.00 123.00   0.50    0.50    --   82.28  15.00-180.00   52
 39  ω     64.00 123.00   0.50    0.50    --   82.28  15.00-150.00  118
 40  ω     56.00  91.00   0.50    0.50    --   42.00  51.00-160.96   70
 41  ω     46.00 133.00   0.50    0.50    --   82.28  15.00 -60.00  174
 42  ω     46.00 133.00   0.50    0.50    --   82.28  15.00  30.00  174
 43  ω    -98.00 -33.00   0.50    0.50    --  -79.50 119.00  -2.07  130
 44  ω    -92.00 -31.00   0.50    0.50    --  -76.35 112.00-120.00  122
 45  ω    -97.00 -33.00   0.50    0.50    --  -79.50 116.00  73.12  128
 46  ω    -97.00 -33.00   0.50    0.50    --  -79.50 116.00 126.88  128
 47  ω   -126.00 -92.00   0.50    0.50    --  -79.50 -57.00  12.51   68
 48  ω   -106.00 -71.00   0.50    0.50    --  -58.00 -52.00  75.02   70
 49  ω   -106.00 -71.00   0.50    0.50    --  -58.00 -51.00  42.02   70
 50  ω   -107.00 -72.00   0.50    0.50    --  -58.00 -50.00 110.15   70
 51  ω   -114.00 -79.00   0.50    0.50    --  -66.00 -52.00  19.25   70
 52  ω   -102.00 -67.00   0.50    0.50    --  -54.00 -51.00 -34.90   70
 53  ω   -108.00 -70.00   0.50    0.50    --  -58.00 -41.00 -77.06   76
 54  ω   -128.00 -93.00   0.50    0.50    --  -79.50 -52.00-115.89   70
 55  ω   -127.00 -92.00   0.50    0.50    --  -79.50 -55.00 -68.19   70
 56  ω   -126.00 -88.00   0.50    0.50    --  -79.50-130.00  18.11   76
 57  ω   -126.00 -96.00   0.50    0.50    --  -79.50-116.00  77.19   60
 58  ω   -127.00 -90.00   0.50    0.50    --  -79.50-126.00 -80.21   74
;
_diffrn_orient_matrix_type       
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.1308836000
_diffrn_orient_matrix_UB_12      -0.0267296000
_diffrn_orient_matrix_UB_13      0.0058030000
_diffrn_orient_matrix_UB_21      -0.0820428000
_diffrn_orient_matrix_UB_22      0.0756463000
_diffrn_orient_matrix_UB_23      0.0757962000
_diffrn_orient_matrix_UB_31      -0.0408011000
_diffrn_orient_matrix_UB_32      0.1195611000
_diffrn_orient_matrix_UB_33      -0.0826695000
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            32299
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.222
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5956
_reflns_number_gt                5316
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;

_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_structure_solution    "SHELXT 2014/5 (Sheldrick, 2014)'"
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0604P)²+0.3686P] where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5956
_refine_ls_number_parameters     375
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1070
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.038
_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_
_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_1 B 0.42654(13) 0.23056(12) 0.21809(9) 0.0225(3) Uani 1 1 d . . . . .
C2_1 C 0.37849(11) 0.35511(10) 0.23869(8) 0.0212(2) Uani 1 1 d . . . . .
N3_1 N 0.46569(9) 0.38470(8) 0.27151(7) 0.0208(2) Uani 1 1 d . . . . .
B4_1 B 0.60865(13) 0.30566(12) 0.27574(9) 0.0222(3) Uani 1 1 d . . . . .
C5_1 C 0.65497(11) 0.17733(10) 0.25849(8) 0.0207(2) Uani 1 1 d . . . . .
N6_1 N 0.56564(9) 0.14500(8) 0.23235(7) 0.0208(2) Uani 1 1 d . . . . .
B1_2 B 0.80400(13) 0.07546(11) 0.27261(10) 0.0224(3) Uani 1 1 d . . . . .
N2_2 N 0.81854(10) -0.00953(9) 0.36610(7) 0.0259(2) Uani 1 1 d . . . . .
C3_2 C 0.94781(13) -0.07294(12) 0.40181(10) 0.0348(3) Uani 1 1 d . . . . .
H3A_2 H 1.020989 -0.042570 0.353855 0.052 Uiso 1 1 calc R U . . .
H3B_2 H 0.974293 -0.163210 0.411899 0.052 Uiso 1 1 calc R U . . .
H3C_2 H 0.935051 -0.055686 0.463677 0.052 Uiso 1 1 calc R U . . .
C4_2 C 0.69931(14) -0.02363(13) 0.44372(9) 0.0352(3) Uani 1 1 d . . . . .
H4A_2 H 0.614393 0.021081 0.417316 0.053 Uiso 1 1 calc R U . . .
H4B_2 H 0.694117 0.011036 0.495049 0.053 Uiso 1 1 calc R U . . .
H4C_2 H 0.709185 -0.112484 0.471028 0.053 Uiso 1 1 calc R U . . .
N5_2 N 0.91710(9) 0.07366(8) 0.19116(7) 0.0241(2) Uani 1 1 d . . . . .
C6_2 C 1.03871(12) -0.03447(11) 0.17710(10) 0.0306(3) Uani 1 1 d . . . . .
H6A_2 H 1.028130 -0.108235 0.230040 0.046 Uiso 1 1 calc R U . . .
H6B_2 H 1.121412 -0.019414 0.177222 0.046 Uiso 1 1 calc R U . . .
H6C_2 H 1.048582 -0.048682 0.114548 0.046 Uiso 1 1 calc R U . . .
C7_2 C 0.91686(12) 0.18097(11) 0.10728(9) 0.0287(3) Uani 1 1 d . . . . .
H7A_2 H 0.830719 0.250160 0.117597 0.043 Uiso 1 1 calc R U . . .
H7B_2 H 0.923385 0.158820 0.048875 0.043 Uiso 1 1 calc R U . . .
H7C_2 H 0.996295 0.206441 0.098664 0.043 Uiso 1 1 calc R U . . .
B1_3 B 0.22707(13) 0.45006(12) 0.22571(10) 0.0230(3) Uani 1 1 d . . . . .
N2_3 N 0.19842(10) 0.50236(10) 0.12980(7) 0.0275(2) Uani 1 1 d . . . . .
C3_3 C 0.30479(13) 0.50579(13) 0.04105(9) 0.0346(3) Uani 1 1 d . . . . .
H3A_3 H 0.396289 0.456756 0.057637 0.052 Uiso 1 1 calc R U . . .
H3B_3 H 0.300896 0.592530 0.007700 0.052 Uiso 1 1 calc R U . . .
H3C_3 H 0.288799 0.470400 -0.001927 0.052 Uiso 1 1 calc R U . . .
C4_3 C 0.05970(13) 0.55315(14) 0.10909(10) 0.0377(3) Uani 1 1 d . . . . .
H4A_3 H -0.006138 0.530316 0.168796 0.057 Uiso 1 1 calc R U . . .
H4B_3 H 0.058795 0.518939 0.059361 0.057 Uiso 1 1 calc R U . . .
H4C_3 H 0.033041 0.644387 0.085152 0.057 Uiso 1 1 calc R U . . .
N5_3 N 0.12047(10) 0.47851(9) 0.30772(7) 0.0251(2) Uani 1 1 d . . . . .
C6_3 C 0.12192(12) 0.39659(12) 0.40569(9) 0.0302(3) Uani 1 1 d . . . . .
H6A_3 H 0.200627 0.319107 0.404153 0.045 Uiso 1 1 calc R U . . .
H6B_3 H 0.035327 0.377065 0.431772 0.045 Uiso 1 1 calc R U . . .
H6C_3 H 0.130784 0.438229 0.447359 0.045 Uiso 1 1 calc R U . . .
C7_3 C 0.01013(13) 0.59781(12) 0.30700(10) 0.0368(3) Uani 1 1 d . . . . .
H7A_3 H 0.020273 0.655195 0.241720 0.055 Uiso 1 1 calc R U . . .
H7B_3 H 0.015575 0.633341 0.354293 0.055 Uiso 1 1 calc R U . . .
H7C_3 H -0.079874 0.585361 0.324518 0.055 Uiso 1 1 calc R U . . .
N1_4 N 0.33507(10) 0.18783(9) 0.19254(7) 0.0267(2) Uani 1 1 d . . . . .
C3_4 C 0.21228(14) 0.17110(14) 0.26282(12) 0.0409(3) Uani 1 1 d . . . . .
H3A_4 H 0.226489 0.152911 0.328676 0.061 Uiso 1 1 calc R U . . .
H3B_4 H 0.193877 0.101361 0.257324 0.061 Uiso 1 1 calc R U . . .
H3C_4 H 0.133058 0.247666 0.250204 0.061 Uiso 1 1 calc R U . . .
C2_4 C 0.32227(16) 0.20948(16) 0.09519(11) 0.0454(4) Uani 1 1 d . . . . .
H2A_4 H 0.400091 0.234337 0.048985 0.068 Uiso 1 1 calc R U . . .
H2B_4 H 0.234869 0.276232 0.082926 0.068 Uiso 1 1 calc R U . . .
H2C_4 H 0.323092 0.132721 0.086927 0.068 Uiso 1 1 calc R U . . .
N1_5 N 0.69731(10) 0.35272(9) 0.29794(8) 0.0273(2) Uani 1 1 d . . . . .
C2_5 C 0.81612(12) 0.27018(12) 0.34238(11) 0.0338(3) Uani 1 1 d . . . . .
H2A_5 H 0.793152 0.198850 0.392094 0.051 Uiso 1 1 calc R U . . .
H2B_5 H 0.840470 0.315854 0.372765 0.051 Uiso 1 1 calc R U . . .
H2C_5 H 0.894969 0.240086 0.292280 0.051 Uiso 1 1 calc R U . . .
C3_5 C 0.71740(13) 0.47064(12) 0.23819(10) 0.0334(3) Uani 1 1 d . . . . .
H3A_5 H 0.637519 0.523566 0.207145 0.050 Uiso 1 1 calc R U . . .
H3B_5 H 0.801819 0.454916 0.187876 0.050 Uiso 1 1 calc R U . . .
H3C_5 H 0.726410 0.513063 0.279212 0.050 Uiso 1 1 calc R U . . .
C1_6 C 0.40661(11) 0.48900(10) 0.31503(8) 0.0227(2) Uani 1 1 d . . . . .
C2_6 C 0.37006(12) 0.61372(11) 0.25916(9) 0.0264(3) Uani 1 1 d . . . . .
C3_6 C 0.31389(12) 0.70795(11) 0.30724(10) 0.0323(3) Uani 1 1 d . . . . .
H3_6 H 0.287622 0.792894 0.270368 0.039 Uiso 1 1 calc R U . . .
C4_6 C 0.29577(13) 0.68033(12) 0.40692(11) 0.0360(3) Uani 1 1 d . . . . .
H4_6 H 0.257464 0.745762 0.438267 0.043 Uiso 1 1 calc R U . . .
C5_6 C 0.33357(13) 0.55694(12) 0.46124(10) 0.0327(3) Uani 1 1 d . . . . .
H5_6 H 0.321252 0.538299 0.529981 0.039 Uiso 1 1 calc R U . . .
C6_6 C 0.38959(12) 0.45922(11) 0.41667(9) 0.0258(3) Uani 1 1 d . . . . .
C7_6 C 0.39150(14) 0.65070(12) 0.14981(10) 0.0340(3) Uani 1 1 d . . . . .
H7A_6 H 0.429150 0.719810 0.122596 0.051 Uiso 1 1 calc R U . . .
H7B_6 H 0.302594 0.677274 0.130683 0.051 Uiso 1 1 calc R U . . .
H7C_6 H 0.456737 0.579127 0.124894 0.051 Uiso 1 1 calc R U . . .
C8_6 C 0.42956(13) 0.32674(11) 0.47885(9) 0.0310(3) Uani 1 1 d . . . . .
H8A_6 H 0.368256 0.321922 0.543306 0.046 Uiso 1 1 calc R U . . .
H8B_6 H 0.525773 0.299545 0.485876 0.046 Uiso 1 1 calc R U . . .
H8C_6 H 0.420727 0.272352 0.447918 0.046 Uiso 1 1 calc R U . . .
C1_7 C 0.62326(11) 0.01869(10) 0.21363(8) 0.0227(2) Uani 1 1 d . . . . .
H1_7 H 0.710251 -0.025060 0.240225 0.027 Uiso 1 1 calc R U . . .
C2_7 C 0.53524(12) -0.06671(10) 0.26540(9) 0.0260(3) Uani 1 1 d . . . . .
H2A_7 H 0.450042 -0.032612 0.238663 0.031 Uiso 1 1 calc R U . . .
H2AB_7 H 0.507660 -0.071955 0.335937 0.031 Uiso 1 1 calc R U . . .
C3_7 C 0.62049(13) -0.19674(11) 0.24992(9) 0.0284(3) Uani 1 1 d . . . . .
H3A_7 H 0.702037 -0.232548 0.280888 0.034 Uiso 1 1 calc R U . . .
H3AB_7 H 0.563377 -0.252284 0.281603 0.034 Uiso 1 1 calc R U . . .
C4_7 C 0.66905(14) -0.19098(12) 0.14205(9) 0.0321(3) Uani 1 1 d . . . . .
H4A_7 H 0.587518 -0.162767 0.112421 0.039 Uiso 1 1 calc R U . . .
H4AB_7 H 0.727217 -0.275620 0.134256 0.039 Uiso 1 1 calc R U . . .
C5_7 C 0.75211(14) -0.10203(12) 0.08923(9) 0.0327(3) Uani 1 1 d . . . . .
H5A_7 H 0.776718 -0.095901 0.018606 0.039 Uiso 1 1 calc R U . . .
H5AB_7 H 0.839284 -0.135521 0.113502 0.039 Uiso 1 1 calc R U . . .
C6_7 C 0.66950(13) 0.02800(11) 0.10502(9) 0.0292(3) Uani 1 1 d . . . . .
H6A_7 H 0.727781 0.082546 0.073824 0.035 Uiso 1 1 calc R U . . .
H6AB_7 H 0.587315 0.065619 0.074525 0.035 Uiso 1 1 calc R U . . .


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_1 N6_1 1.4663(15) . ?
B1_1 N1_4 1.4780(15) . ?
B1_1 C2_1 1.5004(17) . ?
C2_1 N3_1 1.3958(14) . ?
C2_1 B1_3 1.5940(16) . ?
N3_1 C1_6 1.4538(14) . ?
N3_1 B4_1 1.4542(15) . ?
B4_1 N1_5 1.4598(16) . ?
B4_1 C5_1 1.5240(16) . ?
C5_1 N6_1 1.3750(14) . ?
C5_1 B1_2 1.6022(15) . ?
N6_1 C1_7 1.4979(13) . ?
B1_2 N2_2 1.4231(17) . ?
B1_2 N5_2 1.4251(16) . ?
N2_2 C4_2 1.4564(16) . ?
N2_2 C3_2 1.4576(15) . ?
C3_2 H3A_2 0.9800 . ?
C3_2 H3B_2 0.9800 . ?
C3_2 H3C_2 0.9800 . ?
C4_2 H4A_2 0.9800 . ?
C4_2 H4B_2 0.9800 . ?
C4_2 H4C_2 0.9800 . ?
N5_2 C7_2 1.4501(15) . ?
N5_2 C6_2 1.4534(14) . ?
C6_2 H6A_2 0.9800 . ?
C6_2 H6B_2 0.9800 . ?
C6_2 H6C_2 0.9800 . ?
C7_2 H7A_2 0.9800 . ?
C7_2 H7B_2 0.9800 . ?
C7_2 H7C_2 0.9800 . ?
B1_3 N2_3 1.4267(16) . ?
B1_3 N5_3 1.4281(16) . ?
N2_3 C4_3 1.4553(15) . ?
N2_3 C3_3 1.4555(16) . ?
C3_3 H3A_3 0.9800 . ?
C3_3 H3B_3 0.9800 . ?
C3_3 H3C_3 0.9800 . ?
C4_3 H4A_3 0.9800 . ?
C4_3 H4B_3 0.9800 . ?
C4_3 H4C_3 0.9800 . ?
N5_3 C6_3 1.4497(15) . ?
N5_3 C7_3 1.4529(15) . ?
C6_3 H6A_3 0.9800 . ?
C6_3 H6B_3 0.9800 . ?
C6_3 H6C_3 0.9800 . ?
C7_3 H7A_3 0.9800 . ?
C7_3 H7B_3 0.9800 . ?
C7_3 H7C_3 0.9800 . ?
N1_4 C2_4 1.4298(17) . ?
N1_4 C3_4 1.4428(17) . ?
C3_4 H3A_4 0.9800 . ?
C3_4 H3B_4 0.9800 . ?
C3_4 H3C_4 0.9800 . ?
C2_4 H2A_4 0.9800 . ?
C2_4 H2B_4 0.9800 . ?
C2_4 H2C_4 0.9800 . ?
N1_5 C2_5 1.4514(15) . ?
N1_5 C3_5 1.4515(16) . ?
C2_5 H2A_5 0.9800 . ?
C2_5 H2B_5 0.9800 . ?
C2_5 H2C_5 0.9800 . ?
C3_5 H3A_5 0.9800 . ?
C3_5 H3B_5 0.9800 . ?
C3_5 H3C_5 0.9800 . ?
C1_6 C2_6 1.4016(17) . ?
C1_6 C6_6 1.4037(16) . ?
C2_6 C3_6 1.3968(17) . ?
C2_6 C7_6 1.5038(18) . ?
C3_6 C4_6 1.3767(19) . ?
C3_6 H3_6 0.9500 . ?
C4_6 C5_6 1.3832(19) . ?
C4_6 H4_6 0.9500 . ?
C5_6 C6_6 1.3977(17) . ?
C5_6 H5_6 0.9500 . ?
C6_6 C8_6 1.5027(17) . ?
C7_6 H7A_6 0.9800 . ?
C7_6 H7B_6 0.9800 . ?
C7_6 H7C_6 0.9800 . ?
C8_6 H8A_6 0.9800 . ?
C8_6 H8B_6 0.9800 . ?
C8_6 H8C_6 0.9800 . ?
C1_7 C6_7 1.5216(16) . ?
C1_7 C2_7 1.5263(16) . ?
C1_7 H1_7 1.0000 . ?
C2_7 C3_7 1.5305(15) . ?
C2_7 H2A_7 0.9900 . ?
C2_7 H2AB_7 0.9900 . ?
C3_7 C4_7 1.5199(17) . ?
C3_7 H3A_7 0.9900 . ?
C3_7 H3AB_7 0.9900 . ?
C4_7 C5_7 1.5214(17) . ?
C4_7 H4A_7 0.9900 . ?
C4_7 H4AB_7 0.9900 . ?
C5_7 C6_7 1.5286(16) . ?
C5_7 H5A_7 0.9900 . ?
C5_7 H5AB_7 0.9900 . ?
C6_7 H6A_7 0.9900 . ?
C6_7 H6AB_7 0.9900 . ?

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
N6_1 B1_1 N1_4 119.42(10) . . ?
N6_1 B1_1 C2_1 117.93(10) . . ?
N1_4 B1_1 C2_1 122.44(10) . . ?
N3_1 C2_1 B1_1 119.46(9) . . ?
N3_1 C2_1 B1_3 120.98(9) . . ?
B1_1 C2_1 B1_3 119.53(10) . . ?
C2_1 N3_1 C1_6 118.66(9) . . ?
C2_1 N3_1 B4_1 122.44(9) . . ?
C1_6 N3_1 B4_1 118.38(9) . . ?
N3_1 B4_1 N1_5 118.35(10) . . ?
N3_1 B4_1 C5_1 117.31(10) . . ?
N1_5 B4_1 C5_1 124.33(10) . . ?
N6_1 C5_1 B4_1 119.64(9) . . ?
N6_1 C5_1 B1_2 117.99(9) . . ?
B4_1 C5_1 B1_2 122.35(9) . . ?
C5_1 N6_1 B1_1 122.58(9) . . ?
C5_1 N6_1 C1_7 115.30(9) . . ?
B1_1 N6_1 C1_7 122.03(9) . . ?
N2_2 B1_2 N5_2 122.48(10) . . ?
N2_2 B1_2 C5_1 118.76(10) . . ?
N5_2 B1_2 C5_1 118.76(10) . . ?
B1_2 N2_2 C4_2 122.20(10) . . ?
B1_2 N2_2 C3_2 125.06(10) . . ?
C4_2 N2_2 C3_2 111.75(10) . . ?
N2_2 C3_2 H3A_2 109.5 . . ?
N2_2 C3_2 H3B_2 109.5 . . ?
H3A_2 C3_2 H3B_2 109.5 . . ?
N2_2 C3_2 H3C_2 109.5 . . ?
H3A_2 C3_2 H3C_2 109.5 . . ?
H3B_2 C3_2 H3C_2 109.5 . . ?
N2_2 C4_2 H4A_2 109.5 . . ?
N2_2 C4_2 H4B_2 109.5 . . ?
H4A_2 C4_2 H4B_2 109.5 . . ?
N2_2 C4_2 H4C_2 109.5 . . ?
H4A_2 C4_2 H4C_2 109.5 . . ?
H4B_2 C4_2 H4C_2 109.5 . . ?
B1_2 N5_2 C7_2 122.26(9) . . ?
B1_2 N5_2 C6_2 125.76(10) . . ?
C7_2 N5_2 C6_2 111.80(9) . . ?
N5_2 C6_2 H6A_2 109.5 . . ?
N5_2 C6_2 H6B_2 109.5 . . ?
H6A_2 C6_2 H6B_2 109.5 . . ?
N5_2 C6_2 H6C_2 109.5 . . ?
H6A_2 C6_2 H6C_2 109.5 . . ?
H6B_2 C6_2 H6C_2 109.5 . . ?
N5_2 C7_2 H7A_2 109.5 . . ?
N5_2 C7_2 H7B_2 109.5 . . ?
H7A_2 C7_2 H7B_2 109.5 . . ?
N5_2 C7_2 H7C_2 109.5 . . ?
H7A_2 C7_2 H7C_2 109.5 . . ?
H7B_2 C7_2 H7C_2 109.5 . . ?
N2_3 B1_3 N5_3 120.39(10) . . ?
N2_3 B1_3 C2_1 118.18(10) . . ?
N5_3 B1_3 C2_1 121.38(10) . . ?
B1_3 N2_3 C4_3 123.98(10) . . ?
B1_3 N2_3 C3_3 124.00(10) . . ?
C4_3 N2_3 C3_3 111.96(10) . . ?
N2_3 C3_3 H3A_3 109.5 . . ?
N2_3 C3_3 H3B_3 109.5 . . ?
H3A_3 C3_3 H3B_3 109.5 . . ?
N2_3 C3_3 H3C_3 109.5 . . ?
H3A_3 C3_3 H3C_3 109.5 . . ?
H3B_3 C3_3 H3C_3 109.5 . . ?
N2_3 C4_3 H4A_3 109.5 . . ?
N2_3 C4_3 H4B_3 109.5 . . ?
H4A_3 C4_3 H4B_3 109.5 . . ?
N2_3 C4_3 H4C_3 109.5 . . ?
H4A_3 C4_3 H4C_3 109.5 . . ?
H4B_3 C4_3 H4C_3 109.5 . . ?
B1_3 N5_3 C6_3 122.96(10) . . ?
B1_3 N5_3 C7_3 124.99(10) . . ?
C6_3 N5_3 C7_3 111.49(10) . . ?
N5_3 C6_3 H6A_3 109.5 . . ?
N5_3 C6_3 H6B_3 109.5 . . ?
H6A_3 C6_3 H6B_3 109.5 . . ?
N5_3 C6_3 H6C_3 109.5 . . ?
H6A_3 C6_3 H6C_3 109.5 . . ?
H6B_3 C6_3 H6C_3 109.5 . . ?
N5_3 C7_3 H7A_3 109.5 . . ?
N5_3 C7_3 H7B_3 109.5 . . ?
H7A_3 C7_3 H7B_3 109.5 . . ?
N5_3 C7_3 H7C_3 109.5 . . ?
H7A_3 C7_3 H7C_3 109.5 . . ?
H7B_3 C7_3 H7C_3 109.5 . . ?
C2_4 N1_4 C3_4 111.87(11) . . ?
C2_4 N1_4 B1_1 124.37(11) . . ?
C3_4 N1_4 B1_1 118.76(10) . . ?
N1_4 C3_4 H3A_4 109.5 . . ?
N1_4 C3_4 H3B_4 109.5 . . ?
H3A_4 C3_4 H3B_4 109.5 . . ?
N1_4 C3_4 H3C_4 109.5 . . ?
H3A_4 C3_4 H3C_4 109.5 . . ?
H3B_4 C3_4 H3C_4 109.5 . . ?
N1_4 C2_4 H2A_4 109.5 . . ?
N1_4 C2_4 H2B_4 109.5 . . ?
H2A_4 C2_4 H2B_4 109.5 . . ?
N1_4 C2_4 H2C_4 109.5 . . ?
H2A_4 C2_4 H2C_4 109.5 . . ?
H2B_4 C2_4 H2C_4 109.5 . . ?
C2_5 N1_5 C3_5 110.94(10) . . ?
C2_5 N1_5 B4_1 122.34(10) . . ?
C3_5 N1_5 B4_1 120.34(10) . . ?
N1_5 C2_5 H2A_5 109.5 . . ?
N1_5 C2_5 H2B_5 109.5 . . ?
H2A_5 C2_5 H2B_5 109.5 . . ?
N1_5 C2_5 H2C_5 109.5 . . ?
H2A_5 C2_5 H2C_5 109.5 . . ?
H2B_5 C2_5 H2C_5 109.5 . . ?
N1_5 C3_5 H3A_5 109.5 . . ?
N1_5 C3_5 H3B_5 109.5 . . ?
H3A_5 C3_5 H3B_5 109.5 . . ?
N1_5 C3_5 H3C_5 109.5 . . ?
H3A_5 C3_5 H3C_5 109.5 . . ?
H3B_5 C3_5 H3C_5 109.5 . . ?
C2_6 C1_6 C6_6 120.94(10) . . ?
C2_6 C1_6 N3_1 122.33(10) . . ?
C6_6 C1_6 N3_1 116.72(10) . . ?
C3_6 C2_6 C1_6 118.38(11) . . ?
C3_6 C2_6 C7_6 118.54(11) . . ?
C1_6 C2_6 C7_6 123.07(11) . . ?
C4_6 C3_6 C2_6 121.40(11) . . ?
C4_6 C3_6 H3_6 119.3 . . ?
C2_6 C3_6 H3_6 119.3 . . ?
C3_6 C4_6 C5_6 119.73(11) . . ?
C3_6 C4_6 H4_6 120.1 . . ?
C5_6 C4_6 H4_6 120.1 . . ?
C4_6 C5_6 C6_6 121.09(12) . . ?
C4_6 C5_6 H5_6 119.5 . . ?
C6_6 C5_6 H5_6 119.5 . . ?
C5_6 C6_6 C1_6 118.45(11) . . ?
C5_6 C6_6 C8_6 119.05(11) . . ?
C1_6 C6_6 C8_6 122.49(10) . . ?
C2_6 C7_6 H7A_6 109.5 . . ?
C2_6 C7_6 H7B_6 109.5 . . ?
H7A_6 C7_6 H7B_6 109.5 . . ?
C2_6 C7_6 H7C_6 109.5 . . ?
H7A_6 C7_6 H7C_6 109.5 . . ?
H7B_6 C7_6 H7C_6 109.5 . . ?
C6_6 C8_6 H8A_6 109.5 . . ?
C6_6 C8_6 H8B_6 109.5 . . ?
H8A_6 C8_6 H8B_6 109.5 . . ?
C6_6 C8_6 H8C_6 109.5 . . ?
H8A_6 C8_6 H8C_6 109.5 . . ?
H8B_6 C8_6 H8C_6 109.5 . . ?
N6_1 C1_7 C6_7 111.46(9) . . ?
N6_1 C1_7 C2_7 116.70(9) . . ?
C6_7 C1_7 C2_7 111.64(9) . . ?
N6_1 C1_7 H1_7 105.3 . . ?
C6_7 C1_7 H1_7 105.3 . . ?
C2_7 C1_7 H1_7 105.3 . . ?
C1_7 C2_7 C3_7 108.73(9) . . ?
C1_7 C2_7 H2A_7 109.9 . . ?
C3_7 C2_7 H2A_7 109.9 . . ?
C1_7 C2_7 H2AB_7 109.9 . . ?
C3_7 C2_7 H2AB_7 109.9 . . ?
H2A_7 C2_7 H2AB_7 108.3 . . ?
C4_7 C3_7 C2_7 111.16(10) . . ?
C4_7 C3_7 H3A_7 109.4 . . ?
C2_7 C3_7 H3A_7 109.4 . . ?
C4_7 C3_7 H3AB_7 109.4 . . ?
C2_7 C3_7 H3AB_7 109.4 . . ?
H3A_7 C3_7 H3AB_7 108.0 . . ?
C3_7 C4_7 C5_7 111.34(10) . . ?
C3_7 C4_7 H4A_7 109.4 . . ?
C5_7 C4_7 H4A_7 109.4 . . ?
C3_7 C4_7 H4AB_7 109.4 . . ?
C5_7 C4_7 H4AB_7 109.4 . . ?
H4A_7 C4_7 H4AB_7 108.0 . . ?
C4_7 C5_7 C6_7 111.14(10) . . ?
C4_7 C5_7 H5A_7 109.4 . . ?
C6_7 C5_7 H5A_7 109.4 . . ?
C4_7 C5_7 H5AB_7 109.4 . . ?
C6_7 C5_7 H5AB_7 109.4 . . ?
H5A_7 C5_7 H5AB_7 108.0 . . ?
C1_7 C6_7 C5_7 109.87(10) . . ?
C1_7 C6_7 H6A_7 109.7 . . ?
C5_7 C6_7 H6A_7 109.7 . . ?
C1_7 C6_7 H6AB_7 109.7 . . ?
C5_7 C6_7 H6AB_7 109.7 . . ?
H6A_7 C6_7 H6AB_7 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6_1 B1_1 C2_1 N3_1 -0.80(16) . . . . ?
N1_4 B1_1 C2_1 N3_1 173.86(10) . . . . ?
N6_1 B1_1 C2_1 B1_3 -179.05(10) . . . . ?
N1_4 B1_1 C2_1 B1_3 -4.39(17) . . . . ?
B1_1 C2_1 N3_1 C1_6 -164.11(10) . . . . ?
B1_3 C2_1 N3_1 C1_6 14.11(15) . . . . ?
B1_1 C2_1 N3_1 B4_1 7.53(16) . . . . ?
B1_3 C2_1 N3_1 B4_1 -174.25(10) . . . . ?
C2_1 N3_1 B4_1 N1_5 171.53(10) . . . . ?
C1_6 N3_1 B4_1 N1_5 -16.81(15) . . . . ?
C2_1 N3_1 B4_1 C5_1 -9.64(16) . . . . ?
C1_6 N3_1 B4_1 C5_1 162.02(10) . . . . ?
N3_1 B4_1 C5_1 N6_1 5.09(16) . . . . ?
N1_5 B4_1 C5_1 N6_1 -176.16(10) . . . . ?
N3_1 B4_1 C5_1 B1_2 -173.13(10) . . . . ?
N1_5 B4_1 C5_1 B1_2 5.63(18) . . . . ?
B4_1 C5_1 N6_1 B1_1 1.31(16) . . . . ?
B1_2 C5_1 N6_1 B1_1 179.60(10) . . . . ?
B4_1 C5_1 N6_1 C1_7 177.86(9) . . . . ?
B1_2 C5_1 N6_1 C1_7 -3.84(14) . . . . ?
N1_4 B1_1 N6_1 C5_1 -178.39(10) . . . . ?
C2_1 B1_1 N6_1 C5_1 -3.57(16) . . . . ?
N1_4 B1_1 N6_1 C1_7 5.28(16) . . . . ?
C2_1 B1_1 N6_1 C1_7 -179.89(10) . . . . ?
N6_1 C5_1 B1_2 N2_2 -89.09(13) . . . . ?
B4_1 C5_1 B1_2 N2_2 89.16(14) . . . . ?
N6_1 C5_1 B1_2 N5_2 91.13(13) . . . . ?
B4_1 C5_1 B1_2 N5_2 -90.62(14) . . . . ?
N5_2 B1_2 N2_2 C4_2 -168.01(11) . . . . ?
C5_1 B1_2 N2_2 C4_2 12.22(16) . . . . ?
N5_2 B1_2 N2_2 C3_2 24.34(18) . . . . ?
C5_1 B1_2 N2_2 C3_2 -155.42(11) . . . . ?
N2_2 B1_2 N5_2 C7_2 -159.13(11) . . . . ?
C5_1 B1_2 N5_2 C7_2 20.64(16) . . . . ?
N2_2 B1_2 N5_2 C6_2 26.25(18) . . . . ?
C5_1 B1_2 N5_2 C6_2 -153.98(11) . . . . ?
N3_1 C2_1 B1_3 N2_3 115.16(12) . . . . ?
B1_1 C2_1 B1_3 N2_3 -66.62(14) . . . . ?
N3_1 C2_1 B1_3 N5_3 -67.51(15) . . . . ?
B1_1 C2_1 B1_3 N5_3 110.71(13) . . . . ?
N5_3 B1_3 N2_3 C4_3 -19.59(18) . . . . ?
C2_1 B1_3 N2_3 C4_3 157.77(11) . . . . ?
N5_3 B1_3 N2_3 C3_3 163.50(12) . . . . ?
C2_1 B1_3 N2_3 C3_3 -19.14(17) . . . . ?
N2_3 B1_3 N5_3 C6_3 154.87(11) . . . . ?
C2_1 B1_3 N5_3 C6_3 -22.40(17) . . . . ?
N2_3 B1_3 N5_3 C7_3 -34.49(18) . . . . ?
C2_1 B1_3 N5_3 C7_3 148.24(12) . . . . ?
N6_1 B1_1 N1_4 C2_4 -94.97(15) . . . . ?
C2_1 B1_1 N1_4 C2_4 90.44(15) . . . . ?
N6_1 B1_1 N1_4 C3_4 112.13(13) . . . . ?
C2_1 B1_1 N1_4 C3_4 -62.46(16) . . . . ?
N3_1 B4_1 N1_5 C2_5 154.15(11) . . . . ?
C5_1 B4_1 N1_5 C2_5 -24.59(18) . . . . ?
N3_1 B4_1 N1_5 C3_5 -56.47(15) . . . . ?
C5_1 B4_1 N1_5 C3_5 124.79(12) . . . . ?
C2_1 N3_1 C1_6 C2_6 -75.16(14) . . . . ?
B4_1 N3_1 C1_6 C2_6 112.86(12) . . . . ?
C2_1 N3_1 C1_6 C6_6 105.90(12) . . . . ?
B4_1 N3_1 C1_6 C6_6 -66.08(13) . . . . ?
C6_6 C1_6 C2_6 C3_6 -1.11(17) . . . . ?
N3_1 C1_6 C2_6 C3_6 179.98(10) . . . . ?
C6_6 C1_6 C2_6 C7_6 177.46(11) . . . . ?
N3_1 C1_6 C2_6 C7_6 -1.45(17) . . . . ?
C1_6 C2_6 C3_6 C4_6 0.74(18) . . . . ?
C7_6 C2_6 C3_6 C4_6 -177.90(11) . . . . ?
C2_6 C3_6 C4_6 C5_6 -0.06(19) . . . . ?
C3_6 C4_6 C5_6 C6_6 -0.3(2) . . . . ?
C4_6 C5_6 C6_6 C1_6 -0.11(18) . . . . ?
C4_6 C5_6 C6_6 C8_6 179.75(12) . . . . ?
C2_6 C1_6 C6_6 C5_6 0.81(17) . . . . ?
N3_1 C1_6 C6_6 C5_6 179.77(10) . . . . ?
C2_6 C1_6 C6_6 C8_6 -179.04(11) . . . . ?
N3_1 C1_6 C6_6 C8_6 -0.08(16) . . . . ?
C5_1 N6_1 C1_7 C6_7 -100.30(11) . . . . ?
B1_1 N6_1 C1_7 C6_7 76.28(13) . . . . ?
C5_1 N6_1 C1_7 C2_7 129.81(10) . . . . ?
B1_1 N6_1 C1_7 C2_7 -53.61(14) . . . . ?
N6_1 C1_7 C2_7 C3_7 -171.34(9) . . . . ?
C6_7 C1_7 C2_7 C3_7 58.85(13) . . . . ?
C1_7 C2_7 C3_7 C4_7 -57.43(13) . . . . ?
C2_7 C3_7 C4_7 C5_7 56.56(14) . . . . ?
C3_7 C4_7 C5_7 C6_7 -55.25(14) . . . . ?
N6_1 C1_7 C6_7 C5_7 169.29(9) . . . . ?
C2_7 C1_7 C6_7 C5_7 -58.23(13) . . . . ?
C4_7 C5_7 C6_7 C1_7 55.52(14) . . . . ?


_chemical_name_systematic        6
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_NiHe001_NiHe_a
_database_code_depnum_ccdc_archive 'CCDC 2468865'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2025-07-01 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_NiHe001_NiHe_a      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         42 Report
RESPONSE: reflections affected by beamstop
;

_audit_creation_method           'CIF-fill 1.3t (K.Radacki, 2005-23)'
_audit_creation_date             2023-03-22
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C26 H50 B3 N7'
_chemical_formula_sum            'C26 H50 B3 N7'
_chemical_formula_weight         493.16
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'


_cell_length_a                   10.7176(2)
_cell_length_b                   11.7085(2)
_cell_length_c                   13.7152(2)
_cell_angle_alpha                89.1930(10)
_cell_angle_beta                 72.7140(10)
_cell_angle_gamma                65.3450(10)
_cell_volume                     1481.51(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19519
_cell_measurement_theta_min      3.4040
_cell_measurement_theta_max      74.8050

_exptl_crystal_description       block
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_preparation       
;
 Crystals were grown from saturated solution of hexane at -30?C °C. For data 
 collection the crystal was immersed in a film of perfluoropolyether oil, 
 mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0308
0 -1 1 0.0705
0 1 -1 0.0985
0 -1 0 0.0667
1 -1 1 0.0978
-1 1 -1 0.1135
-1 0 -1 0.1085
1 0 1 0.1140
-1 -1 -1 0.0850
1 1 1 0.0882
1 -1 0 0.1013
1 0 0 0.1199
-1 0 0 0.0943
-1 -1 0 0.0894
-1 1 1 0.0755
-1 0 1 0.0689
1 1 -1 0.0879
-1 -1 1 0.0787
0 -1 -1 0.0633
0 1 1 0.0804
0 0 -1 0.0271

_shelx_estimated_absorpt_T_min   0.889
_shelx_estimated_absorpt_T_max   0.971
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  ω   -101.00 -32.00   0.50    0.09    --  -79.50 128.00-132.87  138
  2  ω    -98.00 -32.00   0.50    0.09    --  -79.50 120.00-161.74  132
  3  ω    -98.00 -32.00   0.50    0.09    --  -78.00 118.00 -28.10  132
  4  ω    -92.00 -31.00   0.50    0.09    --  -76.35 112.00-150.00  122
  5  ω    -97.00 -33.00   0.50    0.09    --  -79.50 116.00   3.67  128
  6  ω    -82.00 -34.00   0.50    0.09    --  -76.35  92.00  97.00   96
  7  ω    -65.00 -18.00   0.50    0.09    --  -60.16  92.00  97.00   94
  8  ω    -75.00 -28.00   0.50    0.09    --  -69.76  92.00  97.00   94
  9  ω   -102.00 -32.00   0.50    0.09    --  -79.50 129.00 155.58  140
 10  ω    -92.00 -35.00   0.50    0.09    --  -79.50 103.00  99.56  114
 11  ω   -125.00 -91.00   0.50    0.09    --  -79.50 -60.00 138.12   68
 12  ω   -127.00 -92.00   0.50    0.09    --  -79.50 -53.00 167.17   70
 13  ω   -117.00 -83.00   0.50    0.09    --  -70.00 -55.00  67.59   68
 14  ω   -128.00 -93.00   0.50    0.09    --  -79.50 -51.00  57.91   70
 15  ω   -121.00 -86.00   0.50    0.09    --  -74.00 -55.00  33.25   70
 16  ω   -128.00 -93.00   0.50    0.09    --  -79.50 -49.00  43.43   70
 17  ω   -128.00 -93.00   0.50    0.09    --  -79.50 -52.00  21.43   70
 18  ω   -128.00 -93.00   0.50    0.09    --  -79.50 -49.00 -65.56   70
 19  ω   -128.00 -93.00   0.50    0.09    --  -79.50 -49.00-148.45   70
 20  ω   -121.00 -81.00   0.50    0.09    --  -70.00 -37.00-102.00   80
 21  ω   -125.00 -85.00   0.50    0.09    --  -74.00 -37.00 -53.58   80
 22  ω   -127.00 -92.00   0.50    0.09    --  -79.50 -55.00 -23.68   70
 23  ω   -129.00 -93.00   0.50    0.09    --  -79.50 -46.00  81.63   72
 24  ω   -107.00 -72.00   0.50    0.09    --  -58.00 -47.00 172.65   70
 25  ω   -126.00 -91.00   0.50    0.09    --  -79.50-124.00 123.52   70
 26  ω   -126.00 -92.00   0.50    0.09    --  -79.50-123.00  82.26   68
 27  ω   -126.00 -93.00   0.50    0.09    --  -79.50-121.00 -32.36   66
 28  ω   -126.00 -93.00   0.50    0.09    --  -79.50-120.00-155.03   66
 29  ω   -126.00 -93.00   0.50    0.09    --  -79.50-120.00  -9.88   66
 30  ω    -95.00 -60.00   0.50    0.09    --  -46.00 -48.00 114.72   70
 31  ω    -87.00 -52.00   0.50    0.09    --  -38.00 -49.00 175.02   70
 32  ω    -91.00 -56.00   0.50    0.09    --  -42.00 -48.00  70.02   70
 33  ω    -87.00 -52.00   0.50    0.09    --  -38.00 -49.00 -40.11   70
 34  ω    -95.00 -60.00   0.50    0.09    --  -46.00 -49.00-137.20   70
 35  ω     17.00  64.00   0.50    0.09    --   58.57 -92.00 -14.00   94
 36  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00  60.00  100
 37  ω     42.00  93.00   0.50    0.09    --   85.25 -98.00 -42.38  102
 38  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00-180.00  100
 39  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00-120.00  100
 40  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00 -90.00  100
 41  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00  30.00  100
 42  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00 120.00  100
 43  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00 150.00  100
 44  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00  90.00  100
 45  ω     30.00  77.00   0.50    0.09    --   71.34 -92.00 -14.00   94
 46  ω     41.00  88.00   0.50    0.09    --   82.28 -92.00 -14.00   94
 47  ω     40.00  90.00   0.50    0.09    --   82.28 -95.00-150.00  100
 48  ω     46.00 133.00   0.50    0.09    --   82.28  15.00 -90.00  174
 49  ω     99.00 135.00   0.50    0.09    --   85.25  48.00 -72.91   72
 50  ω     91.00 132.00   0.50    0.09    --   85.25 138.00-107.99   82
 51  ω     71.00 137.00   0.50    0.09    --   85.25  19.00  28.96  132
 52  ω     98.00 133.00   0.50    0.09    --   85.25  54.00 162.88   70
;
_diffrn_orient_matrix_type       
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.0755282000
_diffrn_orient_matrix_UB_12      -0.0459321000
_diffrn_orient_matrix_UB_13      0.0820861000
_diffrn_orient_matrix_UB_21      -0.1372762000
_diffrn_orient_matrix_UB_22      -0.0066478000
_diffrn_orient_matrix_UB_23      0.0718364000
_diffrn_orient_matrix_UB_31      0.0576982000
_diffrn_orient_matrix_UB_32      -0.1383730000
_diffrn_orient_matrix_UB_33      -0.0465363000
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            28558
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.402
_diffrn_reflns_theta_max         68.238
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             5386
_reflns_number_gt                4749
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_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.
;

_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_structure_solution    "SHELXT 2014/5 (Sheldrick, 2014)'"
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_refine_special_details          
;
The molecule had a two-fold disorder of the Xylyl-groups. Therefore the displacement parameters of atoms C1_2 to C1_12 of the residues 2 and 12 were restrained to the same value with similarity restraint SIMU.
The N7-C1_2/12 distances were restrained using the same distance restraint SADI.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0582P)²+0.2951P] where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5386
_refine_ls_number_parameters     388
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1044
_refine_ls_wR_factor_gt          0.1013
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.037
_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_
_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 0.61474(13) 0.45758(12) 0.72927(9) 0.0224(3) Uani 1 1 d . . . . .
N2 N 0.68323(11) 0.05623(9) 0.79784(8) 0.0270(2) Uani 1 1 d . . . . .
C2 C 0.76818(14) 0.56594(12) 0.62682(10) 0.0369(3) Uani 1 1 d . . . . .
H2A H 0.853529 0.566179 0.639234 0.055 Uiso 1 1 calc R U . . .
H2B H 0.714862 0.646881 0.604658 0.055 Uiso 1 1 calc R U . . .
H2C H 0.799076 0.496658 0.572985 0.055 Uiso 1 1 calc R U . . .
B2 B 0.60332(13) 0.13263(12) 0.73581(9) 0.0226(3) Uani 1 1 d . . . . .
N3 N 0.54028(10) 0.08651(9) 0.67723(7) 0.0242(2) Uani 1 1 d . . . . .
C3 C 0.71711(14) 0.10835(12) 0.87666(10) 0.0339(3) Uani 1 1 d . . . . .
H3A H 0.673639 0.087325 0.943823 0.051 Uiso 1 1 calc R U . . .
H3B H 0.678051 0.200614 0.878372 0.051 Uiso 1 1 calc R U . . .
H3C H 0.822485 0.072275 0.860968 0.051 Uiso 1 1 calc R U . . .
B3 B 0.28903(13) 0.37436(12) 0.81188(9) 0.0228(3) Uani 1 1 d . . . . .
N4 N 0.25967(10) 0.29828(9) 0.88885(7) 0.0268(2) Uani 1 1 d . . . . .
C4 C 0.74066(16) -0.08112(12) 0.79165(11) 0.0388(3) Uani 1 1 d . . . . .
H4A H 0.683858 -0.104109 0.852076 0.058 Uiso 1 1 calc R U . . .
H4B H 0.842075 -0.116813 0.789639 0.058 Uiso 1 1 calc R U . . .
H4C H 0.734699 -0.114914 0.729075 0.058 Uiso 1 1 calc R U . . .
N5 N 0.17840(10) 0.45141(9) 0.76979(7) 0.0265(2) Uani 1 1 d . . . . .
C5 C 0.50509(13) 0.14402(12) 0.58876(9) 0.0290(3) Uani 1 1 d . . . . .
H5A H 0.541678 0.208446 0.573427 0.044 Uiso 1 1 calc R U . . .
H5B H 0.399688 0.183694 0.603932 0.044 Uiso 1 1 calc R U . . .
H5C H 0.550130 0.078758 0.529159 0.044 Uiso 1 1 calc R U . . .
N6 N 0.68455(9) 0.32142(8) 0.70824(7) 0.0217(2) Uani 1 1 d . . . . .
C6 C 0.48415(14) -0.00723(11) 0.70589(10) 0.0318(3) Uani 1 1 d . . . . .
H6A H 0.382841 0.027933 0.707703 0.048 Uiso 1 1 calc R U . . .
H6B H 0.490110 -0.029476 0.774042 0.048 Uiso 1 1 calc R U . . .
H6C H 0.541725 -0.083252 0.655214 0.048 Uiso 1 1 calc R U . . .
N7 N 0.46238(9) 0.48932(8) 0.76948(7) 0.0212(2) Uani 1 1 d D . . . .
C7 C 0.14583(14) 0.25572(13) 0.90552(10) 0.0350(3) Uani 1 1 d . . . . .
H7A H 0.072284 0.295336 0.972674 0.052 Uiso 1 1 calc R U . . .
H7B H 0.187825 0.163393 0.903871 0.052 Uiso 1 1 calc R U . . .
H7C H 0.100900 0.279837 0.851201 0.052 Uiso 1 1 calc R U . . .
C8 C 0.34227(14) 0.24803(12) 0.95878(9) 0.0329(3) Uani 1 1 d . . . . .
H8A H 0.276736 0.273333 1.029920 0.049 Uiso 1 1 calc R U . . .
H8B H 0.414547 0.281420 0.949039 0.049 Uiso 1 1 calc R U . . .
H8C H 0.391352 0.155373 0.944626 0.049 Uiso 1 1 calc R U . . .
C008 C 0.44249(12) 0.37605(10) 0.77335(8) 0.0208(2) Uani 1 1 d . . . . .
C9 C 0.20848(13) 0.48535(12) 0.66656(9) 0.0324(3) Uani 1 1 d . . . . .
H9A H 0.170723 0.577674 0.669574 0.049 Uiso 1 1 calc R U . . .
H9B H 0.161714 0.455018 0.628431 0.049 Uiso 1 1 calc R U . . .
H9C H 0.313422 0.446378 0.631643 0.049 Uiso 1 1 calc R U . . .
C009 C 0.57622(11) 0.27614(10) 0.73588(8) 0.0209(2) Uani 1 1 d . . . . .
C10 C 0.02491(13) 0.51515(13) 0.82851(10) 0.0342(3) Uani 1 1 d . . . . .
H10A H 0.010718 0.498952 0.900380 0.051 Uiso 1 1 calc R U . . .
H10B H -0.029051 0.482915 0.799373 0.051 Uiso 1 1 calc R U . . .
H10C H -0.010309 0.606519 0.825329 0.051 Uiso 1 1 calc R U . . .
N1 N 0.67537(10) 0.54840(9) 0.72062(8) 0.0270(2) Uani 1 1 d . . . . .
C1 C 0.61501(14) 0.65390(11) 0.80050(10) 0.0338(3) Uani 1 1 d . . . . .
H1A H 0.561280 0.634323 0.864584 0.051 Uiso 1 1 calc R U . . .
H1B H 0.549322 0.729944 0.779591 0.051 Uiso 1 1 calc R U . . .
H1C H 0.693558 0.668867 0.811398 0.051 Uiso 1 1 calc R U . . .
C1_1 C 0.83770(11) 0.23350(11) 0.66070(9) 0.0248(2) Uani 1 1 d . . . . .
H1_1 H 0.849902 0.148445 0.681997 0.030 Uiso 1 1 calc R U . . .
C2_1 C 0.93606(12) 0.27126(12) 0.70020(9) 0.0283(3) Uani 1 1 d . . . . .
H2A_1 H 0.916939 0.359777 0.688383 0.034 Uiso 1 1 calc R U . . .
H2B_1 H 0.912489 0.267611 0.775312 0.034 Uiso 1 1 calc R U . . .
C3_1 C 1.09626(13) 0.18552(12) 0.64753(11) 0.0356(3) Uani 1 1 d . . . . .
H3A_1 H 1.155636 0.217002 0.672028 0.043 Uiso 1 1 calc R U . . .
H3B_1 H 1.118459 0.098695 0.665905 0.043 Uiso 1 1 calc R U . . .
C4_1 C 1.13486(14) 0.18221(15) 0.53117(11) 0.0439(3) Uani 1 1 d . . . . .
H4A_1 H 1.238848 0.125311 0.498155 0.053 Uiso 1 1 calc R U . . .
H4B_1 H 1.117481 0.268193 0.512307 0.053 Uiso 1 1 calc R U . . .
C5_1 C 1.04299(15) 0.13506(16) 0.49293(12) 0.0520(4) Uani 1 1 d . . . . .
H5A_1 H 1.064581 0.047362 0.508719 0.062 Uiso 1 1 calc R U . . .
H5B_1 H 1.068167 0.133789 0.417286 0.062 Uiso 1 1 calc R U . . .
C6_1 C 0.88145(13) 0.21967(13) 0.54330(10) 0.0339(3) Uani 1 1 d . . . . .
H6A_1 H 0.824783 0.183112 0.520748 0.041 Uiso 1 1 calc R U . . .
H6B_1 H 0.857809 0.304496 0.520172 0.041 Uiso 1 1 calc R U . . .
C1_2 C 0.3458(5) 0.6143(3) 0.8051(3) 0.0239(7) Uani 0.559(6) 1 d DG U P A 1
C2_2 C 0.2699(4) 0.6512(3) 0.9095(3) 0.0228(5) Uani 0.559(6) 1 d G U P A 1
C3_2 C 0.1637(3) 0.7745(3) 0.9440(3) 0.0309(7) Uani 0.559(6) 1 d G U P A 1
H3_2 H 0.111807 0.799727 1.015417 0.037 Uiso 0.559(6) 1 calc R U P A 1
C4_2 C 0.1336(3) 0.86100(18) 0.8741(3) 0.0355(7) Uani 0.559(6) 1 d G U P A 1
H4_2 H 0.061051 0.945293 0.897758 0.043 Uiso 0.559(6) 1 calc R U P A 1
C5_2 C 0.2096(4) 0.8241(2) 0.7697(3) 0.0349(7) Uani 0.559(6) 1 d G U P A 1
H5_2 H 0.188944 0.883237 0.721942 0.042 Uiso 0.559(6) 1 calc R U P A 1
C6_2 C 0.3157(4) 0.7008(3) 0.7352(2) 0.0334(7) Uani 0.559(6) 1 d G U P A 1
C7_2 C 0.3027(8) 0.5614(6) 0.9880(6) 0.0286(10) Uani 0.559(6) 1 d . U P A 1
H7A_2 H 0.241371 0.516326 0.999044 0.043 Uiso 0.559(6) 1 calc R U P A 1
H7B_2 H 0.283103 0.609321 1.053088 0.043 Uiso 0.559(6) 1 calc R U P A 1
H7C_2 H 0.404879 0.500070 0.962939 0.043 Uiso 0.559(6) 1 calc R U P A 1
C8_2 C 0.4006(7) 0.6675(5) 0.6213(5) 0.0376(11) Uani 0.559(6) 1 d . U P A 1
H8A_2 H 0.447935 0.575224 0.603519 0.056 Uiso 0.559(6) 1 calc R U P A 1
H8B_2 H 0.474185 0.699969 0.605323 0.056 Uiso 0.559(6) 1 calc R U P A 1
H8C_2 H 0.334508 0.705710 0.581374 0.056 Uiso 0.559(6) 1 calc R U P A 1
C1_12 C 0.3510(6) 0.6147(3) 0.7888(4) 0.0255(9) Uani 0.441(6) 1 d DG U P A 2
C2_12 C 0.2613(6) 0.6690(4) 0.8885(3) 0.0328(9) Uani 0.441(6) 1 d G U P A 2
C3_12 C 0.1599(4) 0.7951(3) 0.9070(3) 0.0332(8) Uani 0.441(6) 1 d G U P A 2
H3_12 H 0.098625 0.832188 0.975120 0.040 Uiso 0.441(6) 1 calc R U P A 2
C4_12 C 0.1482(3) 0.8668(2) 0.8257(4) 0.0362(9) Uani 0.441(6) 1 d G U P A 2
H4_12 H 0.078855 0.952962 0.838335 0.043 Uiso 0.441(6) 1 calc R U P A 2
C5_12 C 0.2378(4) 0.8125(3) 0.7260(4) 0.0363(8) Uani 0.441(6) 1 d G U P A 2
H5_12 H 0.229810 0.861550 0.670454 0.044 Uiso 0.441(6) 1 calc R U P A 2
C6_12 C 0.3393(5) 0.6865(4) 0.7075(3) 0.0248(7) Uani 0.441(6) 1 d G U P A 2
C7_12 C 0.2776(10) 0.5928(8) 0.9775(8) 0.0363(18) Uani 0.441(6) 1 d . U P A 2
H7A_12 H 0.226960 0.650035 1.042316 0.054 Uiso 0.441(6) 1 calc R U P A 2
H7B_12 H 0.380681 0.546448 0.970258 0.054 Uiso 0.441(6) 1 calc R U P A 2
H7C_12 H 0.235879 0.532621 0.977605 0.054 Uiso 0.441(6) 1 calc R U P A 2
C8_12 C 0.4347(8) 0.6310(6) 0.5977(6) 0.0327(12) Uani 0.441(6) 1 d . U P A 2
H8A_12 H 0.480649 0.538391 0.592853 0.049 Uiso 0.441(6) 1 calc R U P A 2
H8B_12 H 0.509743 0.661884 0.577397 0.049 Uiso 0.441(6) 1 calc R U P A 2
H8C_12 H 0.375646 0.656956 0.551830 0.049 Uiso 0.441(6) 1 calc R U P A 2


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 N7 1.4398(15) . ?
B1 N6 1.4402(15) . ?
B1 N1 1.4471(15) . ?
N2 B2 1.4247(16) . ?
N2 C3 1.4525(15) . ?
N2 C4 1.4558(15) . ?
C2 N1 1.4453(15) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
B2 N3 1.4258(15) . ?
B2 C009 1.5812(16) . ?
N3 C5 1.4509(15) . ?
N3 C6 1.4557(14) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
B3 N4 1.4202(16) . ?
B3 N5 1.4326(16) . ?
B3 C008 1.5795(15) . ?
N4 C8 1.4505(15) . ?
N4 C7 1.4586(14) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N5 C9 1.4444(15) . ?
N5 C10 1.4550(15) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
N6 C009 1.4210(13) . ?
N6 C1_1 1.4671(14) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N7 C1_12 1.418(2) . ?
N7 C008 1.4264(13) . ?
N7 C1_2 1.4400(19) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C008 C009 1.3665(15) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N1 C1 1.4474(16) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1_1 C6_1 1.5278(17) . ?
C1_1 C2_1 1.5281(15) . ?
C1_1 H1_1 1.0000 . ?
C2_1 C3_1 1.5241(16) . ?
C2_1 H2A_1 0.9900 . ?
C2_1 H2B_1 0.9900 . ?
C3_1 C4_1 1.522(2) . ?
C3_1 H3A_1 0.9900 . ?
C3_1 H3B_1 0.9900 . ?
C4_1 C5_1 1.5225(19) . ?
C4_1 H4A_1 0.9900 . ?
C4_1 H4B_1 0.9900 . ?
C5_1 C6_1 1.5276(18) . ?
C5_1 H5A_1 0.9900 . ?
C5_1 H5B_1 0.9900 . ?
C6_1 H6A_1 0.9900 . ?
C6_1 H6B_1 0.9900 . ?
C1_2 C2_2 1.3900 . ?
C1_2 C6_2 1.3900 . ?
C2_2 C3_2 1.3900 . ?
C2_2 C7_2 1.508(6) . ?
C3_2 C4_2 1.3900 . ?
C3_2 H3_2 0.9500 . ?
C4_2 C5_2 1.3900 . ?
C4_2 H4_2 0.9500 . ?
C5_2 C6_2 1.3900 . ?
C5_2 H5_2 0.9500 . ?
C6_2 C8_2 1.515(6) . ?
C7_2 H7A_2 0.9800 . ?
C7_2 H7B_2 0.9800 . ?
C7_2 H7C_2 0.9800 . ?
C8_2 H8A_2 0.9800 . ?
C8_2 H8B_2 0.9800 . ?
C8_2 H8C_2 0.9800 . ?
C1_12 C2_12 1.3900 . ?
C1_12 C6_12 1.3900 . ?
C2_12 C3_12 1.3900 . ?
C2_12 C7_12 1.511(8) . ?
C3_12 C4_12 1.3900 . ?
C3_12 H3_12 0.9500 . ?
C4_12 C5_12 1.3900 . ?
C4_12 H4_12 0.9500 . ?
C5_12 C6_12 1.3900 . ?
C5_12 H5_12 0.9500 . ?
C6_12 C8_12 1.515(6) . ?
C7_12 H7A_12 0.9800 . ?
C7_12 H7B_12 0.9800 . ?
C7_12 H7C_12 0.9800 . ?
C8_12 H8A_12 0.9800 . ?
C8_12 H8B_12 0.9800 . ?
C8_12 H8C_12 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
N7 B1 N6 104.60(9) . . ?
N7 B1 N1 124.61(10) . . ?
N6 B1 N1 130.69(10) . . ?
B2 N2 C3 123.02(10) . . ?
B2 N2 C4 125.53(10) . . ?
C3 N2 C4 111.45(10) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 B2 N3 122.50(10) . . ?
N2 B2 C009 119.09(10) . . ?
N3 B2 C009 118.33(10) . . ?
B2 N3 C5 122.01(9) . . ?
B2 N3 C6 125.40(10) . . ?
C5 N3 C6 111.97(9) . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N4 B3 N5 119.92(10) . . ?
N4 B3 C008 120.38(10) . . ?
N5 B3 C008 119.69(10) . . ?
B3 N4 C8 124.73(10) . . ?
B3 N4 C7 124.51(10) . . ?
C8 N4 C7 110.72(10) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
B3 N5 C9 123.45(10) . . ?
B3 N5 C10 124.25(10) . . ?
C9 N5 C10 112.01(10) . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C009 N6 B1 108.56(9) . . ?
C009 N6 C1_1 120.64(9) . . ?
B1 N6 C1_1 130.69(9) . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1_12 N7 C008 126.0(3) . . ?
C1_12 N7 B1 124.1(3) . . ?
C008 N7 B1 109.46(9) . . ?
C008 N7 C1_2 123.9(3) . . ?
B1 N7 C1_2 126.5(3) . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C009 C008 N7 107.73(9) . . ?
C009 C008 B3 128.63(10) . . ?
N7 C008 B3 123.62(9) . . ?
N5 C9 H9A 109.5 . . ?
N5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C008 C009 N6 109.64(9) . . ?
C008 C009 B2 123.85(9) . . ?
N6 C009 B2 126.20(9) . . ?
N5 C10 H10A 109.5 . . ?
N5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C2 N1 B1 125.39(10) . . ?
C2 N1 C1 112.19(10) . . ?
B1 N1 C1 120.40(10) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N6 C1_1 C6_1 111.53(9) . . ?
N6 C1_1 C2_1 111.46(9) . . ?
C6_1 C1_1 C2_1 112.00(9) . . ?
N6 C1_1 H1_1 107.2 . . ?
C6_1 C1_1 H1_1 107.2 . . ?
C2_1 C1_1 H1_1 107.2 . . ?
C3_1 C2_1 C1_1 112.41(10) . . ?
C3_1 C2_1 H2A_1 109.1 . . ?
C1_1 C2_1 H2A_1 109.1 . . ?
C3_1 C2_1 H2B_1 109.1 . . ?
C1_1 C2_1 H2B_1 109.1 . . ?
H2A_1 C2_1 H2B_1 107.9 . . ?
C4_1 C3_1 C2_1 110.73(10) . . ?
C4_1 C3_1 H3A_1 109.5 . . ?
C2_1 C3_1 H3A_1 109.5 . . ?
C4_1 C3_1 H3B_1 109.5 . . ?
C2_1 C3_1 H3B_1 109.5 . . ?
H3A_1 C3_1 H3B_1 108.1 . . ?
C3_1 C4_1 C5_1 109.85(11) . . ?
C3_1 C4_1 H4A_1 109.7 . . ?
C5_1 C4_1 H4A_1 109.7 . . ?
C3_1 C4_1 H4B_1 109.7 . . ?
C5_1 C4_1 H4B_1 109.7 . . ?
H4A_1 C4_1 H4B_1 108.2 . . ?
C4_1 C5_1 C6_1 111.23(11) . . ?
C4_1 C5_1 H5A_1 109.4 . . ?
C6_1 C5_1 H5A_1 109.4 . . ?
C4_1 C5_1 H5B_1 109.4 . . ?
C6_1 C5_1 H5B_1 109.4 . . ?
H5A_1 C5_1 H5B_1 108.0 . . ?
C5_1 C6_1 C1_1 111.97(11) . . ?
C5_1 C6_1 H6A_1 109.2 . . ?
C1_1 C6_1 H6A_1 109.2 . . ?
C5_1 C6_1 H6B_1 109.2 . . ?
C1_1 C6_1 H6B_1 109.2 . . ?
H6A_1 C6_1 H6B_1 107.9 . . ?
C2_2 C1_2 C6_2 120.0 . . ?
C2_2 C1_2 N7 120.3(2) . . ?
C6_2 C1_2 N7 119.6(2) . . ?
C3_2 C2_2 C1_2 120.0 . . ?
C3_2 C2_2 C7_2 118.4(3) . . ?
C1_2 C2_2 C7_2 121.6(3) . . ?
C2_2 C3_2 C4_2 120.0 . . ?
C2_2 C3_2 H3_2 120.0 . . ?
C4_2 C3_2 H3_2 120.0 . . ?
C5_2 C4_2 C3_2 120.0 . . ?
C5_2 C4_2 H4_2 120.0 . . ?
C3_2 C4_2 H4_2 120.0 . . ?
C6_2 C5_2 C4_2 120.0 . . ?
C6_2 C5_2 H5_2 120.0 . . ?
C4_2 C5_2 H5_2 120.0 . . ?
C5_2 C6_2 C1_2 120.0 . . ?
C5_2 C6_2 C8_2 117.8(3) . . ?
C1_2 C6_2 C8_2 122.1(3) . . ?
C2_2 C7_2 H7A_2 109.5 . . ?
C2_2 C7_2 H7B_2 109.5 . . ?
H7A_2 C7_2 H7B_2 109.5 . . ?
C2_2 C7_2 H7C_2 109.5 . . ?
H7A_2 C7_2 H7C_2 109.5 . . ?
H7B_2 C7_2 H7C_2 109.5 . . ?
C6_2 C8_2 H8A_2 109.5 . . ?
C6_2 C8_2 H8B_2 109.5 . . ?
H8A_2 C8_2 H8B_2 109.5 . . ?
C6_2 C8_2 H8C_2 109.5 . . ?
H8A_2 C8_2 H8C_2 109.5 . . ?
H8B_2 C8_2 H8C_2 109.5 . . ?
C2_12 C1_12 C6_12 120.0 . . ?
C2_12 C1_12 N7 120.7(3) . . ?
C6_12 C1_12 N7 119.1(3) . . ?
C3_12 C2_12 C1_12 120.0 . . ?
C3_12 C2_12 C7_12 119.8(4) . . ?
C1_12 C2_12 C7_12 120.1(4) . . ?
C2_12 C3_12 C4_12 120.0 . . ?
C2_12 C3_12 H3_12 120.0 . . ?
C4_12 C3_12 H3_12 120.0 . . ?
C3_12 C4_12 C5_12 120.0 . . ?
C3_12 C4_12 H4_12 120.0 . . ?
C5_12 C4_12 H4_12 120.0 . . ?
C4_12 C5_12 C6_12 120.0 . . ?
C4_12 C5_12 H5_12 120.0 . . ?
C6_12 C5_12 H5_12 120.0 . . ?
C5_12 C6_12 C1_12 120.0 . . ?
C5_12 C6_12 C8_12 118.3(3) . . ?
C1_12 C6_12 C8_12 121.7(3) . . ?
C2_12 C7_12 H7A_12 109.5 . . ?
C2_12 C7_12 H7B_12 109.5 . . ?
H7A_12 C7_12 H7B_12 109.5 . . ?
C2_12 C7_12 H7C_12 109.5 . . ?
H7A_12 C7_12 H7C_12 109.5 . . ?
H7B_12 C7_12 H7C_12 109.5 . . ?
C6_12 C8_12 H8A_12 109.5 . . ?
C6_12 C8_12 H8B_12 109.5 . . ?
H8A_12 C8_12 H8B_12 109.5 . . ?
C6_12 C8_12 H8C_12 109.5 . . ?
H8A_12 C8_12 H8C_12 109.5 . . ?
H8B_12 C8_12 H8C_12 109.5 . . ?

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
C3 N2 B2 N3 -164.29(11) . . . . ?
C4 N2 B2 N3 15.58(18) . . . . ?
C3 N2 B2 C009 12.53(16) . . . . ?
C4 N2 B2 C009 -167.60(11) . . . . ?
N2 B2 N3 C5 -157.76(11) . . . . ?
C009 B2 N3 C5 25.40(15) . . . . ?
N2 B2 N3 C6 32.03(17) . . . . ?
C009 B2 N3 C6 -144.81(11) . . . . ?
N5 B3 N4 C8 -160.14(11) . . . . ?
C008 B3 N4 C8 19.03(17) . . . . ?
N5 B3 N4 C7 22.51(17) . . . . ?
C008 B3 N4 C7 -158.33(11) . . . . ?
N4 B3 N5 C9 -151.28(11) . . . . ?
C008 B3 N5 C9 29.55(16) . . . . ?
N4 B3 N5 C10 35.43(17) . . . . ?
C008 B3 N5 C10 -143.74(11) . . . . ?
N7 B1 N6 C009 -0.30(12) . . . . ?
N1 B1 N6 C009 176.04(12) . . . . ?
N7 B1 N6 C1_1 175.83(10) . . . . ?
N1 B1 N6 C1_1 -7.8(2) . . . . ?
N6 B1 N7 C1_12 -171.8(3) . . . . ?
N1 B1 N7 C1_12 11.6(3) . . . . ?
N6 B1 N7 C008 0.67(12) . . . . ?
N1 B1 N7 C008 -175.96(10) . . . . ?
N6 B1 N7 C1_2 178.2(2) . . . . ?
N1 B1 N7 C1_2 1.6(3) . . . . ?
C1_12 N7 C008 C009 171.5(3) . . . . ?
B1 N7 C008 C009 -0.80(12) . . . . ?
C1_2 N7 C008 C009 -178.4(2) . . . . ?
C1_12 N7 C008 B3 -6.8(3) . . . . ?
B1 N7 C008 B3 -179.06(10) . . . . ?
C1_2 N7 C008 B3 3.3(3) . . . . ?
N4 B3 C008 C009 54.00(16) . . . . ?
N5 B3 C008 C009 -126.84(12) . . . . ?
N4 B3 C008 N7 -128.13(11) . . . . ?
N5 B3 C008 N7 51.04(15) . . . . ?
N7 C008 C009 N6 0.61(12) . . . . ?
B3 C008 C009 N6 178.75(10) . . . . ?
N7 C008 C009 B2 174.53(10) . . . . ?
B3 C008 C009 B2 -7.33(18) . . . . ?
B1 N6 C009 C008 -0.19(12) . . . . ?
C1_1 N6 C009 C008 -176.78(9) . . . . ?
B1 N6 C009 B2 -173.93(10) . . . . ?
C1_1 N6 C009 B2 9.48(16) . . . . ?
N2 B2 C009 C008 -114.27(12) . . . . ?
N3 B2 C009 C008 62.68(15) . . . . ?
N2 B2 C009 N6 58.63(15) . . . . ?
N3 B2 C009 N6 -124.42(11) . . . . ?
N7 B1 N1 C2 -123.79(13) . . . . ?
N6 B1 N1 C2 60.52(18) . . . . ?
N7 B1 N1 C1 38.72(17) . . . . ?
N6 B1 N1 C1 -136.97(13) . . . . ?
C009 N6 C1_1 C6_1 92.27(12) . . . . ?
B1 N6 C1_1 C6_1 -83.46(14) . . . . ?
C009 N6 C1_1 C2_1 -141.74(10) . . . . ?
B1 N6 C1_1 C2_1 42.53(15) . . . . ?
N6 C1_1 C2_1 C3_1 -176.84(9) . . . . ?
C6_1 C1_1 C2_1 C3_1 -51.11(13) . . . . ?
C1_1 C2_1 C3_1 C4_1 55.34(14) . . . . ?
C2_1 C3_1 C4_1 C5_1 -58.63(15) . . . . ?
C3_1 C4_1 C5_1 C6_1 58.63(18) . . . . ?
C4_1 C5_1 C6_1 C1_1 -54.84(17) . . . . ?
N6 C1_1 C6_1 C5_1 176.30(10) . . . . ?
C2_1 C1_1 C6_1 C5_1 50.60(14) . . . . ?
C008 N7 C1_2 C2_2 68.7(4) . . . . ?
B1 N7 C1_2 C2_2 -108.5(3) . . . . ?
C008 N7 C1_2 C6_2 -115.5(2) . . . . ?
B1 N7 C1_2 C6_2 67.3(4) . . . . ?
C6_2 C1_2 C2_2 C3_2 0.0 . . . . ?
N7 C1_2 C2_2 C3_2 175.9(5) . . . . ?
C6_2 C1_2 C2_2 C7_2 -178.0(5) . . . . ?
N7 C1_2 C2_2 C7_2 -2.2(5) . . . . ?
C1_2 C2_2 C3_2 C4_2 0.0 . . . . ?
C7_2 C2_2 C3_2 C4_2 178.1(5) . . . . ?
C2_2 C3_2 C4_2 C5_2 0.0 . . . . ?
C3_2 C4_2 C5_2 C6_2 0.0 . . . . ?
C4_2 C5_2 C6_2 C1_2 0.0 . . . . ?
C4_2 C5_2 C6_2 C8_2 -176.9(5) . . . . ?
C2_2 C1_2 C6_2 C5_2 0.0 . . . . ?
N7 C1_2 C6_2 C5_2 -175.9(5) . . . . ?
C2_2 C1_2 C6_2 C8_2 176.8(5) . . . . ?
N7 C1_2 C6_2 C8_2 0.9(5) . . . . ?
C008 N7 C1_12 C2_12 74.1(4) . . . . ?
B1 N7 C1_12 C2_12 -114.7(3) . . . . ?
C008 N7 C1_12 C6_12 -110.7(3) . . . . ?
B1 N7 C1_12 C6_12 60.5(5) . . . . ?
C6_12 C1_12 C2_12 C3_12 0.0 . . . . ?
N7 C1_12 C2_12 C3_12 175.2(6) . . . . ?
C6_12 C1_12 C2_12 C7_12 -177.7(7) . . . . ?
N7 C1_12 C2_12 C7_12 -2.5(6) . . . . ?
C1_12 C2_12 C3_12 C4_12 0.0 . . . . ?
C7_12 C2_12 C3_12 C4_12 177.7(7) . . . . ?
C2_12 C3_12 C4_12 C5_12 0.0 . . . . ?
C3_12 C4_12 C5_12 C6_12 0.0 . . . . ?
C4_12 C5_12 C6_12 C1_12 0.0 . . . . ?
C4_12 C5_12 C6_12 C8_12 180.0(6) . . . . ?
C2_12 C1_12 C6_12 C5_12 0.0 . . . . ?
N7 C1_12 C6_12 C5_12 -175.2(6) . . . . ?
C2_12 C1_12 C6_12 C8_12 -180.0(6) . . . . ?
N7 C1_12 C6_12 C8_12 4.8(6) . . . . ?


_chemical_name_systematic        3-Cy
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_NiHe005_NiHe_a
_database_code_depnum_ccdc_archive 'CCDC 2468862'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2025-07-01 deposited with the CCDC.	2025-08-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_STRVA01_NiHe005_NiHe_a      
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: chirality is irrelevant for this compound
;
_vrf_PLAT601_NiHe005_NiHe_a      
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS   <=         37 Ang**3
RESPONSE: no solvent detected in voids
;
_vrf_PLAT911_NiHe005_NiHe_a      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         28 Report
RESPONSE: reflections affected by beamstop
;

_audit_creation_method           'CIF-fill 1.4a (K.Radacki, 2005-23)'
_audit_creation_date             2023-04-13
_shelx_SHELXL_version_number     2018/3
_chemical_formula_moiety         'C28 H48 B3 N7'
_chemical_formula_sum            'C28 H48 B3 N7'
_chemical_formula_weight         515.16
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'


_cell_length_a                   19.26690(10)
_cell_length_b                   10.93410(10)
_cell_length_c                   30.2037(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.6820(10)
_cell_angle_gamma                90
_cell_volume                     6272.27(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    42279
_cell_measurement_theta_min      2.9570
_cell_measurement_theta_max      74.8780

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.429
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.43.63a (Rigaku Oxford Diffraction, 2023) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_preparation       
;
 Crystals were grown at -30?C °C from saturated solution in pentane. For 
 data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.1425
-1 -1 1 0.1447
-1 0 -1 0.1219
-1 0 1 0.1608
1 0 0 0.1922
0 0 -1 0.0286
0 0 1 0.0692
1 -1 -1 0.0774
0 1 1 0.1439
-1 1 -1 0.1132
0 -1 0 0.1295
0 1 0 0.1414
1 1 1 0.1408
-1 -1 -1 0.1292
0 -1 1 0.1302
0 1 -1 0.1331
1 1 -1 0.1556
1 0 -1 0.1556
1 2 0 0.1416
-1 0 -2 0.0893
-2 1 2 0.1313
-1 1 2 0.1270
1 0 2 0.1452
0 1 2 0.1333

_shelx_estimated_absorpt_T_min   0.838
_shelx_estimated_absorpt_T_max   0.952
_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  ω     42.00  93.00   0.50    0.14    --   85.25 -98.00 -35.07  102
  2  ω     39.00 101.00   0.50    0.14    --   85.25-125.00  49.61  124
  3  ω     42.00  93.00   0.50    0.14    --   85.25 -98.00  88.88  102
  4  ω     42.00  93.00   0.50    0.14    --   85.25 -97.00 168.12  102
  5  ω     37.00  93.00   0.50    0.14    --   82.28-112.00 120.00  112
  6  ω     40.00  90.00   0.50    0.14    --   82.28 -95.00 120.00  100
  7  ω     40.00  90.00   0.50    0.14    --   82.28 -95.00  60.00  100
  8  ω     40.00  90.00   0.50    0.14    --   82.28 -95.00  30.00  100
  9  ω     40.00  90.00   0.50    0.14    --   82.28 -95.00 -60.00  100
 10  ω     40.00  90.00   0.50    0.14    --   82.28 -95.00 -90.00  100
 11  ω     40.00  90.00   0.50    0.14    --   82.28 -95.00-120.00  100
 12  ω     40.00  90.00   0.50    0.14    --   82.28 -95.00-150.00  100
 13  ω     16.00  66.00   0.50    0.14    --   58.57 -95.00-120.00  100
 14  ω     50.00 135.00   0.50    0.14    --   85.25  14.00  24.57  170
 15  ω     73.00 137.00   0.50    0.14    --   85.25  21.00-141.65  128
 16  ω     97.00 132.00   0.50    0.14    --   85.25 124.00-137.56   70
 17  ω     98.00 132.00   0.50    0.14    --   85.25 122.00 -81.21   68
 18  ω    102.00 131.00   0.50    0.14    --   85.25 115.00  -6.85   58
 19  ω     59.00  94.00   0.50    0.14    --   46.00  52.00  74.19   70
 20  ω     34.00  60.00   0.50    0.14    --   22.00  59.00  48.38   52
 21  ω     34.00  60.00   0.50    0.14    --   22.00  59.00   8.45   52
 22  ω     34.00  60.00   0.50    0.14    --   22.00  57.00 -46.95   52
 23  ω   -102.00 -33.00   0.50    0.14    --  -79.50 132.00  71.53  138
 24  ω    -93.00 -35.00   0.50    0.14    --  -79.50 106.00 117.52  116
 25  ω    -99.00 -32.00   0.50    0.14    --  -79.50 121.00  -3.51  134
 26  ω   -100.00 -33.00   0.50    0.14    --  -79.50 123.00 -71.61  134
 27  ω    -97.00 -33.00   0.50    0.14    --  -79.50 117.00-167.61  128
 28  ω    -91.00 -35.00   0.50    0.14    --  -79.50 101.00 -66.37  112
 29  ω   -131.00 -68.00   0.50    0.14    --  -79.50 -21.00 -25.26  126
 30  ω   -125.00 -91.00   0.50    0.14    --  -79.50 -60.00 -55.55   68
 31  ω   -125.00 -91.00   0.50    0.14    --  -79.50 -60.00-158.28   68
 32  ω   -126.00 -91.00   0.50    0.14    --  -79.50 -58.00 -27.66   70
 33  ω   -125.00 -91.00   0.50    0.14    --  -79.50 -61.00  17.46   68
 34  ω   -122.00 -87.00   0.50    0.14    --  -74.00 -52.00  94.06   70
 35  ω   -124.00 -94.00   0.50    0.14    --  -79.50 -64.00 155.41   60
 36  ω    -74.00 -39.00   0.50    0.14    --  -26.00 -52.00 115.24   70
 37  ω   -102.00 -67.00   0.50    0.14    --  -54.00 -52.00  65.61   70
 38  ω   -128.00 -93.00   0.50    0.14    --  -79.50 -50.00  60.77   70
 39  ω   -110.00 -75.00   0.50    0.14    --  -62.00 -51.00 -42.04   70
 40  ω   -106.00 -71.00   0.50    0.14    --  -58.00 -51.00-170.41   70
 41  ω    -74.00 -39.00   0.50    0.14    --  -26.00 -51.00-158.85   70
 42  ω   -124.00 -87.00   0.50    0.14    --  -74.00 -44.00 -95.88   74
 43  ω   -129.00 -92.00   0.50    0.14    --  -79.50 -44.00-141.22   74
 44  ω   -130.00 -90.00   0.50    0.14    --  -79.50 -38.00-118.37   80
 45  ω   -107.00 -72.00   0.50    0.14    --  -58.00 -50.00 -71.72   70
 46  ω   -119.00 -84.00   0.50    0.14    --  -70.00 -47.00 128.71   70
 47  ω   -120.00 -83.00   0.50    0.14    --  -70.00 -45.00 162.53   74
 48  ω   -130.00 -91.00   0.50    0.14    --  -79.50 -41.00 107.23   78
 49  ω   -126.00 -93.00   0.50    0.14    --  -79.50-120.00 -68.50   66
 50  ω   -126.00 -85.00   0.50    0.14    --  -79.50-136.00-173.31   82
 51  ω   -126.00 -85.00   0.50    0.14    --  -79.50-137.00-136.36   82
 52  ω   -126.00 -86.00   0.50    0.14    --  -79.50-134.00  59.66   80
 53  ω   -127.00 -90.00   0.50    0.14    --  -79.50-126.00 136.77   74
;
_diffrn_orient_matrix_type       
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.0454475000
_diffrn_orient_matrix_UB_12      -0.0728553000
_diffrn_orient_matrix_UB_13      -0.0281429000
_diffrn_orient_matrix_UB_21      -0.0298839000
_diffrn_orient_matrix_UB_22      -0.1205522000
_diffrn_orient_matrix_UB_23      0.0153836000
_diffrn_orient_matrix_UB_31      -0.0601594000
_diffrn_orient_matrix_UB_32      0.0048352000
_diffrn_orient_matrix_UB_33      -0.0405839000
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            57795
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.968
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_point_group_measured_fraction_full 0.884
_reflns_number_total             10126
_reflns_number_gt                9917
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_max     0.770
_reflns_Friedel_fraction_full    0.772
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal class for the 
 calculation of statistics and refinement. _reflns_Friedel_fraction is 
 defined as the number of unique Friedel pairs measured divided by the number 
 that would be possible theoretically, ignoring centric projections and 
 systematic absences. Completness statistics refer to single and composite 
 reflections containing twin component 1 only.
;

_computing_data_collection       
;
 CrysAlisPro system (CCD 42.72a 64-bit (release 07-10-2022))
;
_computing_cell_refinement       'CrysAlisPro 1.171.43.63a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.63a (Rigaku OD, 2023)'
_computing_structure_solution    "SHELXT 2014/5 (Sheldrick, 2014)'"
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'


_refine_special_details          
;
 Refined as a 2-component inversion twin. The BASF parameter was refined to 
 33.9%.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0466P)²+1.0685P] where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.34(19)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         10126
_refine_ls_number_parameters     714
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0716
_refine_ls_wR_factor_gt          0.0712
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.144
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.028
_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_
_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_1 B 0.56173(10) 0.26137(17) 0.62674(7) 0.0234(4) Uani 1 1 d . . . . .
N2_1 N 0.54044(7) 0.36788(12) 0.64920(5) 0.0218(3) Uani 1 1 d . . . . .
C3_1 C 0.58241(9) 0.46953(14) 0.64006(6) 0.0211(3) Uani 1 1 d . . . . .
C4_1 C 0.62735(9) 0.43209(14) 0.61240(6) 0.0210(3) Uani 1 1 d . . . . .
N5_1 N 0.61681(7) 0.30363(12) 0.60392(5) 0.0219(3) Uani 1 1 d . . . . .
B1_2 B 0.67936(11) 0.51531(18) 0.59041(7) 0.0234(4) Uani 1 1 d . . . . .
N2_2 N 0.75049(8) 0.47879(13) 0.58934(5) 0.0276(3) Uani 1 1 d . . . . .
C4_2 C 0.78778(11) 0.5076(2) 0.55270(8) 0.0395(5) Uani 1 1 d . . . . .
H4A_2 H 0.756531 0.552959 0.529428 0.059 Uiso 1 1 calc R U . . .
H4B_2 H 0.802799 0.431592 0.539914 0.059 Uiso 1 1 calc R U . . .
H4C_2 H 0.829184 0.557574 0.564007 0.059 Uiso 1 1 calc R U . . .
N5_2 N 0.65465(8) 0.62914(13) 0.57078(5) 0.0270(3) Uani 1 1 d . . . . .
C6_2 C 0.58120(11) 0.66084(18) 0.55613(7) 0.0333(4) Uani 1 1 d . . . . .
H6A_2 H 0.552215 0.586946 0.555218 0.050 Uiso 1 1 calc R U . . .
H6B_2 H 0.575376 0.697302 0.526092 0.050 Uiso 1 1 calc R U . . .
H6C_2 H 0.566441 0.719688 0.577192 0.050 Uiso 1 1 calc R U . . .
C7_2 C 0.70070(12) 0.73366(17) 0.56842(7) 0.0377(5) Uani 1 1 d . . . . .
H7A_2 H 0.747943 0.714837 0.584614 0.057 Uiso 1 1 calc R U . . .
H7B_2 H 0.681968 0.804987 0.582138 0.057 Uiso 1 1 calc R U . . .
H7C_2 H 0.703175 0.751499 0.536931 0.057 Uiso 1 1 calc R U . . .
C3_2 C 0.79100(10) 0.39953(17) 0.62247(7) 0.0336(4) Uani 1 1 d . . . . .
H3A_2 H 0.762173 0.375795 0.644881 0.050 Uiso 1 1 calc R U . . .
H3B_2 H 0.833028 0.443009 0.637309 0.050 Uiso 1 1 calc R U . . .
H3C_2 H 0.805212 0.326159 0.607640 0.050 Uiso 1 1 calc R U . . .
B1_3 B 0.57684(10) 0.60144(17) 0.66062(6) 0.0225(4) Uani 1 1 d . . . . .
N2_3 N 0.50967(8) 0.65871(13) 0.65930(5) 0.0264(3) Uani 1 1 d . . . . .
C3_3 C 0.44884(10) 0.63317(17) 0.62560(7) 0.0311(4) Uani 1 1 d . . . . .
H3A_3 H 0.461010 0.571235 0.604737 0.047 Uiso 1 1 calc R U . . .
H3B_3 H 0.433771 0.708292 0.609041 0.047 Uiso 1 1 calc R U . . .
H3C_3 H 0.410480 0.602652 0.640163 0.047 Uiso 1 1 calc R U . . .
C4_3 C 0.49257(12) 0.73892(18) 0.69432(8) 0.0375(5) Uani 1 1 d . . . . .
H4A_3 H 0.534278 0.749721 0.717494 0.056 Uiso 1 1 calc R U . . .
H4B_3 H 0.454539 0.702522 0.707775 0.056 Uiso 1 1 calc R U . . .
H4C_3 H 0.477360 0.818580 0.681305 0.056 Uiso 1 1 calc R U . . .
N5_3 N 0.63958(8) 0.66217(13) 0.68093(5) 0.0255(3) Uani 1 1 d . . . . .
C6_3 C 0.70659(10) 0.60290(17) 0.69668(7) 0.0300(4) Uani 1 1 d . . . . .
H6A_3 H 0.699792 0.514122 0.697154 0.045 Uiso 1 1 calc R U . . .
H6B_3 H 0.725478 0.631639 0.727050 0.045 Uiso 1 1 calc R U . . .
H6C_3 H 0.739758 0.622933 0.676459 0.045 Uiso 1 1 calc R U . . .
C7_3 C 0.64619(11) 0.79470(16) 0.68409(7) 0.0343(4) Uani 1 1 d . . . . .
H7A_3 H 0.603149 0.832800 0.668068 0.051 Uiso 1 1 calc R U . . .
H7B_3 H 0.686520 0.821169 0.670590 0.051 Uiso 1 1 calc R U . . .
H7C_3 H 0.653341 0.819296 0.715730 0.051 Uiso 1 1 calc R U . . .
N1_4 N 0.53359(8) 0.14050(13) 0.62692(5) 0.0282(3) Uani 1 1 d . . . . .
C2_4 C 0.50449(11) 0.09047(17) 0.66427(7) 0.0364(4) Uani 1 1 d . . . . .
H2A_4 H 0.508465 0.151094 0.688462 0.055 Uiso 1 1 calc R U . . .
H2B_4 H 0.530531 0.016512 0.675300 0.055 Uiso 1 1 calc R U . . .
H2C_4 H 0.454805 0.069964 0.654310 0.055 Uiso 1 1 calc R U . . .
C3_4 C 0.53457(11) 0.05388(17) 0.59063(7) 0.0362(4) Uani 1 1 d . . . . .
H3A_4 H 0.546157 0.096782 0.564338 0.054 Uiso 1 1 calc R U . . .
H3B_4 H 0.488147 0.015526 0.582844 0.054 Uiso 1 1 calc R U . . .
H3C_4 H 0.570070 -0.009184 0.600216 0.054 Uiso 1 1 calc R U . . .
C1_5 C 0.48308(9) 0.37588(14) 0.67358(6) 0.0236(3) Uani 1 1 d . . . . .
C2_5 C 0.41495(9) 0.35029(15) 0.65065(6) 0.0265(4) Uani 1 1 d . . . . .
C3_5 C 0.35931(10) 0.35252(17) 0.67512(7) 0.0318(4) Uani 1 1 d . . . . .
H3_5 H 0.313027 0.333521 0.660419 0.038 Uiso 1 1 calc R U . . .
C4_5 C 0.37054(11) 0.38184(19) 0.72023(7) 0.0360(5) Uani 1 1 d . . . . .
H4_5 H 0.332102 0.383909 0.736217 0.043 Uiso 1 1 calc R U . . .
C5_5 C 0.43778(11) 0.40816(18) 0.74205(7) 0.0332(4) Uani 1 1 d . . . . .
H5_5 H 0.444934 0.429842 0.772940 0.040 Uiso 1 1 calc R U . . .
C6_5 C 0.49544(10) 0.40351(15) 0.71958(6) 0.0269(4) Uani 1 1 d . . . . .
C7_5 C 0.40046(10) 0.32151(17) 0.60128(7) 0.0311(4) Uani 1 1 d . . . . .
H7A_5 H 0.352148 0.345543 0.588731 0.047 Uiso 1 1 calc R U . . .
H7B_5 H 0.406261 0.233538 0.596887 0.047 Uiso 1 1 calc R U . . .
H7C_5 H 0.433523 0.366702 0.586043 0.047 Uiso 1 1 calc R U . . .
C8_5 C 0.56862(10) 0.42421(18) 0.74480(6) 0.0314(4) Uani 1 1 d . . . . .
H8A_5 H 0.570001 0.404944 0.776628 0.047 Uiso 1 1 calc R U . . .
H8B_5 H 0.581862 0.509945 0.741750 0.047 Uiso 1 1 calc R U . . .
H8C_5 H 0.601708 0.371229 0.732481 0.047 Uiso 1 1 calc R U . . .
C1_6 C 0.66314(9) 0.22918(15) 0.58315(6) 0.0215(3) Uani 1 1 d . . . . .
C2_6 C 0.66568(10) 0.24127(15) 0.53725(6) 0.0256(4) Uani 1 1 d . . . . .
C3_6 C 0.71205(11) 0.16647(17) 0.51853(7) 0.0315(4) Uani 1 1 d . . . . .
H3_6 H 0.715387 0.175234 0.487670 0.038 Uiso 1 1 calc R U . . .
C4_6 C 0.75303(10) 0.08019(17) 0.54408(7) 0.0335(4) Uani 1 1 d . . . . .
H4_6 H 0.783810 0.029419 0.530748 0.040 Uiso 1 1 calc R U . . .
C5_6 C 0.74915(9) 0.06791(16) 0.58905(7) 0.0301(4) Uani 1 1 d . . . . .
H5_6 H 0.777281 0.008011 0.606433 0.036 Uiso 1 1 calc R U . . .
C6_6 C 0.70470(9) 0.14182(15) 0.60946(6) 0.0252(4) Uani 1 1 d . . . . .
C7_6 C 0.61839(11) 0.32931(18) 0.50823(6) 0.0339(4) Uani 1 1 d . . . . .
H7A_6 H 0.615090 0.305754 0.476641 0.051 Uiso 1 1 calc R U . . .
H7B_6 H 0.637830 0.412096 0.512561 0.051 Uiso 1 1 calc R U . . .
H7C_6 H 0.571387 0.327499 0.516564 0.051 Uiso 1 1 calc R U . . .
C8_6 C 0.70401(10) 0.12765(16) 0.65904(6) 0.0305(4) Uani 1 1 d . . . . .
H8A_6 H 0.748672 0.091803 0.673611 0.046 Uiso 1 1 calc R U . . .
H8B_6 H 0.665060 0.073935 0.663516 0.046 Uiso 1 1 calc R U . . .
H8C_6 H 0.697846 0.207998 0.672225 0.046 Uiso 1 1 calc R U . . .
B1_7 B 0.33480(10) 0.88494(17) 0.37040(7) 0.0227(4) Uani 1 1 d . . . . .
N2_7 N 0.36978(7) 0.98059(12) 0.34974(5) 0.0215(3) Uani 1 1 d . . . . .
C3_7 C 0.44409(9) 0.96493(15) 0.36179(6) 0.0212(3) Uani 1 1 d . . . . .
C4_7 C 0.45695(9) 0.86518(14) 0.38919(6) 0.0210(3) Uani 1 1 d . . . . .
N5_7 N 0.39097(7) 0.81287(12) 0.39479(5) 0.0212(3) Uani 1 1 d . . . . .
B1_8 B 0.53217(10) 0.81532(18) 0.41054(6) 0.0234(4) Uani 1 1 d . . . . .
N2_8 N 0.55010(8) 0.69014(13) 0.40539(5) 0.0255(3) Uani 1 1 d . . . . .
C3_8 C 0.51477(10) 0.61261(16) 0.36996(6) 0.0294(4) Uani 1 1 d . . . . .
H3A_8 H 0.479190 0.660306 0.350206 0.044 Uiso 1 1 calc R U . . .
H3B_8 H 0.491919 0.544715 0.383072 0.044 Uiso 1 1 calc R U . . .
H3C_8 H 0.549212 0.580153 0.352546 0.044 Uiso 1 1 calc R U . . .
C4_8 C 0.60198(11) 0.62212(18) 0.43648(7) 0.0360(4) Uani 1 1 d . . . . .
H4A_8 H 0.622480 0.675609 0.461303 0.054 Uiso 1 1 calc R U . . .
H4B_8 H 0.639237 0.592781 0.420707 0.054 Uiso 1 1 calc R U . . .
H4C_8 H 0.579149 0.552184 0.448374 0.054 Uiso 1 1 calc R U . . .
N5_8 N 0.58245(8) 0.89834(14) 0.43390(5) 0.0265(3) Uani 1 1 d . . . . .
C6_8 C 0.56483(10) 1.01154(18) 0.45476(7) 0.0331(4) Uani 1 1 d . . . . .
H6A_8 H 0.513616 1.017527 0.452582 0.050 Uiso 1 1 calc R U . . .
H6B_8 H 0.582030 1.081253 0.439317 0.050 Uiso 1 1 calc R U . . .
H6C_8 H 0.586977 1.012103 0.486443 0.050 Uiso 1 1 calc R U . . .
C7_8 C 0.65814(10) 0.88754(19) 0.43548(7) 0.0352(4) Uani 1 1 d . . . . .
H7A_8 H 0.668013 0.818027 0.417021 0.053 Uiso 1 1 calc R U . . .
H7B_8 H 0.681203 0.874571 0.466598 0.053 Uiso 1 1 calc R U . . .
H7C_8 H 0.676165 0.962758 0.423889 0.053 Uiso 1 1 calc R U . . .
B1_9 B 0.50032(10) 1.05104(17) 0.34507(7) 0.0228(4) Uani 1 1 d . . . . .
N2_9 N 0.55368(8) 0.99787(13) 0.32353(5) 0.0249(3) Uani 1 1 d . . . . .
C3_9 C 0.55008(10) 0.87597(16) 0.30390(6) 0.0298(4) Uani 1 1 d . . . . .
H3A_9 H 0.502737 0.842364 0.303130 0.045 Uiso 1 1 calc R U . . .
H3B_9 H 0.584664 0.822818 0.322084 0.045 Uiso 1 1 calc R U . . .
H3C_9 H 0.560411 0.880661 0.273262 0.045 Uiso 1 1 calc R U . . .
C4_9 C 0.62147(10) 1.05527(18) 0.32243(7) 0.0336(4) Uani 1 1 d . . . . .
H4A_9 H 0.625652 1.129564 0.340841 0.050 Uiso 1 1 calc R U . . .
H4B_9 H 0.625099 1.076592 0.291390 0.050 Uiso 1 1 calc R U . . .
H4C_9 H 0.659322 0.998343 0.334328 0.050 Uiso 1 1 calc R U . . .
N5_9 N 0.49710(8) 1.18001(12) 0.35110(5) 0.0255(3) Uani 1 1 d . . . . .
C6_9 C 0.46439(10) 1.23759(16) 0.38582(7) 0.0325(4) Uani 1 1 d . . . . .
H6A_9 H 0.447056 1.174340 0.404200 0.049 Uiso 1 1 calc R U . . .
H6B_9 H 0.424939 1.288625 0.371790 0.049 Uiso 1 1 calc R U . . .
H6C_9 H 0.499136 1.288589 0.404861 0.049 Uiso 1 1 calc R U . . .
C7_9 C 0.51823(11) 1.27096(17) 0.32072(8) 0.0373(5) Uani 1 1 d . . . . .
H7A_9 H 0.535301 1.229615 0.295844 0.056 Uiso 1 1 calc R U . . .
H7B_9 H 0.555867 1.322013 0.337054 0.056 Uiso 1 1 calc R U . . .
H7C_9 H 0.477733 1.322453 0.308837 0.056 Uiso 1 1 calc R U . . .
N1_10 N 0.26096(8) 0.86615(13) 0.36766(5) 0.0256(3) Uani 1 1 d . . . . .
C2_10 C 0.23085(10) 0.81113(17) 0.40376(6) 0.0301(4) Uani 1 1 d . . . . .
H2A_10 H 0.266558 0.807783 0.430982 0.045 Uiso 1 1 calc R U . . .
H2B_10 H 0.214814 0.728093 0.395158 0.045 Uiso 1 1 calc R U . . .
H2C_10 H 0.190809 0.860322 0.409557 0.045 Uiso 1 1 calc R U . . .
C3_10 C 0.20940(10) 0.90200(18) 0.32939(7) 0.0310(4) Uani 1 1 d . . . . .
H3A_10 H 0.233318 0.939778 0.306671 0.047 Uiso 1 1 calc R U . . .
H3B_10 H 0.176523 0.960837 0.338968 0.047 Uiso 1 1 calc R U . . .
H3C_10 H 0.183407 0.829672 0.316599 0.047 Uiso 1 1 calc R U . . .
C1_11 C 0.38494(9) 0.70030(15) 0.41798(6) 0.0232(3) Uani 1 1 d . . . . .
C2_11 C 0.40651(9) 0.69429(16) 0.46456(6) 0.0265(4) Uani 1 1 d . . . . .
C3_11 C 0.40156(10) 0.58253(18) 0.48611(7) 0.0339(4) Uani 1 1 d . . . . .
H3_11 H 0.417254 0.576616 0.517586 0.041 Uiso 1 1 calc R U . . .
C4_11 C 0.37428(11) 0.48048(18) 0.46252(8) 0.0379(5) Uani 1 1 d . . . . .
H4_11 H 0.371829 0.404732 0.477588 0.045 Uiso 1 1 calc R U . . .
C5_11 C 0.35058(11) 0.48914(16) 0.41688(7) 0.0338(4) Uani 1 1 d . . . . .
H5_11 H 0.330481 0.419281 0.400941 0.041 Uiso 1 1 calc R U . . .
C6_11 C 0.35549(9) 0.59816(16) 0.39369(6) 0.0274(4) Uani 1 1 d . . . . .
C7_11 C 0.43123(10) 0.80668(18) 0.49144(6) 0.0316(4) Uani 1 1 d . . . . .
H7A_11 H 0.428805 0.792258 0.523171 0.047 Uiso 1 1 calc R U . . .
H7B_11 H 0.401037 0.876112 0.480431 0.047 Uiso 1 1 calc R U . . .
H7C_11 H 0.479949 0.824825 0.488234 0.047 Uiso 1 1 calc R U . . .
C8_11 C 0.32959(11) 0.60258(17) 0.34382(7) 0.0325(4) Uani 1 1 d . . . . .
H8A_11 H 0.332744 0.520815 0.331013 0.049 Uiso 1 1 calc R U . . .
H8B_11 H 0.358678 0.659648 0.329863 0.049 Uiso 1 1 calc R U . . .
H8C_11 H 0.280500 0.630156 0.338112 0.049 Uiso 1 1 calc R U . . .
C1_12 C 0.33754(9) 1.08382(15) 0.32576(6) 0.0236(3) Uani 1 1 d . . . . .
C2_12 C 0.34228(9) 1.10107(16) 0.28027(6) 0.0280(4) Uani 1 1 d . . . . .
C3_12 C 0.30818(11) 1.20149(18) 0.25797(7) 0.0357(4) Uani 1 1 d . . . . .
H3_12 H 0.312239 1.215949 0.227493 0.043 Uiso 1 1 calc R U . . .
C4_12 C 0.26842(11) 1.28072(19) 0.27941(8) 0.0410(5) Uani 1 1 d . . . . .
H4_12 H 0.245027 1.348145 0.263587 0.049 Uiso 1 1 calc R U . . .
C5_12 C 0.26301(10) 1.26116(17) 0.32381(8) 0.0353(4) Uani 1 1 d . . . . .
H5_12 H 0.235146 1.314996 0.338213 0.042 Uiso 1 1 calc R U . . .
C6_12 C 0.29760(9) 1.16400(16) 0.34797(7) 0.0280(4) Uani 1 1 d . . . . .
C7_12 C 0.38148(11) 1.01283(18) 0.25535(6) 0.0322(4) Uani 1 1 d . . . . .
H7A_12 H 0.362854 1.017407 0.223140 0.048 Uiso 1 1 calc R U . . .
H7B_12 H 0.375532 0.929566 0.266125 0.048 Uiso 1 1 calc R U . . .
H7C_12 H 0.431626 1.033974 0.260540 0.048 Uiso 1 1 calc R U . . .
C8_12 C 0.29180(10) 1.14715(17) 0.39672(7) 0.0321(4) Uani 1 1 d . . . . .
H8A_12 H 0.280516 1.225708 0.409425 0.048 Uiso 1 1 calc R U . . .
H8B_12 H 0.336664 1.116755 0.413184 0.048 Uiso 1 1 calc R U . . .
H8C_12 H 0.254441 1.088027 0.399259 0.048 Uiso 1 1 calc R U . . .


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_1 N1_4 1.429(2) . ?
B1_1 N5_1 1.436(2) . ?
B1_1 N2_1 1.442(2) . ?
N2_1 C3_1 1.429(2) . ?
N2_1 C1_5 1.430(2) . ?
C3_1 C4_1 1.363(2) . ?
C3_1 B1_3 1.581(2) . ?
C4_1 N5_1 1.436(2) . ?
C4_1 B1_2 1.580(2) . ?
N5_1 C1_6 1.429(2) . ?
B1_2 N5_2 1.425(2) . ?
B1_2 N2_2 1.433(2) . ?
N2_2 C3_2 1.449(2) . ?
N2_2 C4_2 1.452(2) . ?
C4_2 H4A_2 0.9800 . ?
C4_2 H4B_2 0.9800 . ?
C4_2 H4C_2 0.9800 . ?
N5_2 C6_2 1.452(3) . ?
N5_2 C7_2 1.456(2) . ?
C6_2 H6A_2 0.9800 . ?
C6_2 H6B_2 0.9800 . ?
C6_2 H6C_2 0.9800 . ?
C7_2 H7A_2 0.9800 . ?
C7_2 H7B_2 0.9800 . ?
C7_2 H7C_2 0.9800 . ?
C3_2 H3A_2 0.9800 . ?
C3_2 H3B_2 0.9800 . ?
C3_2 H3C_2 0.9800 . ?
B1_3 N5_3 1.425(3) . ?
B1_3 N2_3 1.432(2) . ?
N2_3 C3_3 1.444(3) . ?
N2_3 C4_3 1.454(2) . ?
C3_3 H3A_3 0.9800 . ?
C3_3 H3B_3 0.9800 . ?
C3_3 H3C_3 0.9800 . ?
C4_3 H4A_3 0.9800 . ?
C4_3 H4B_3 0.9800 . ?
C4_3 H4C_3 0.9800 . ?
N5_3 C6_3 1.451(2) . ?
N5_3 C7_3 1.456(2) . ?
C6_3 H6A_3 0.9800 . ?
C6_3 H6B_3 0.9800 . ?
C6_3 H6C_3 0.9800 . ?
C7_3 H7A_3 0.9800 . ?
C7_3 H7B_3 0.9800 . ?
C7_3 H7C_3 0.9800 . ?
N1_4 C2_4 1.449(2) . ?
N1_4 C3_4 1.451(2) . ?
C2_4 H2A_4 0.9800 . ?
C2_4 H2B_4 0.9800 . ?
C2_4 H2C_4 0.9800 . ?
C3_4 H3A_4 0.9800 . ?
C3_4 H3B_4 0.9800 . ?
C3_4 H3C_4 0.9800 . ?
C1_5 C6_5 1.403(3) . ?
C1_5 C2_5 1.406(3) . ?
C2_5 C3_5 1.401(2) . ?
C2_5 C7_5 1.503(3) . ?
C3_5 C4_5 1.381(3) . ?
C3_5 H3_5 0.9500 . ?
C4_5 C5_5 1.381(3) . ?
C4_5 H4_5 0.9500 . ?
C5_5 C6_5 1.397(2) . ?
C5_5 H5_5 0.9500 . ?
C6_5 C8_5 1.503(3) . ?
C7_5 H7A_5 0.9800 . ?
C7_5 H7B_5 0.9800 . ?
C7_5 H7C_5 0.9800 . ?
C8_5 H8A_5 0.9800 . ?
C8_5 H8B_5 0.9800 . ?
C8_5 H8C_5 0.9800 . ?
C1_6 C2_6 1.402(2) . ?
C1_6 C6_6 1.404(2) . ?
C2_6 C3_6 1.399(3) . ?
C2_6 C7_6 1.502(3) . ?
C3_6 C4_6 1.380(3) . ?
C3_6 H3_6 0.9500 . ?
C4_6 C5_6 1.379(3) . ?
C4_6 H4_6 0.9500 . ?
C5_6 C6_6 1.394(2) . ?
C5_6 H5_6 0.9500 . ?
C6_6 C8_6 1.508(3) . ?
C7_6 H7A_6 0.9800 . ?
C7_6 H7B_6 0.9800 . ?
C7_6 H7C_6 0.9800 . ?
C8_6 H8A_6 0.9800 . ?
C8_6 H8B_6 0.9800 . ?
C8_6 H8C_6 0.9800 . ?
B1_7 N1_10 1.426(2) . ?
B1_7 N5_7 1.437(2) . ?
B1_7 N2_7 1.442(2) . ?
N2_7 C1_12 1.426(2) . ?
N2_7 C3_7 1.427(2) . ?
C3_7 C4_7 1.366(2) . ?
C3_7 B1_9 1.581(2) . ?
C4_7 N5_7 1.430(2) . ?
C4_7 B1_8 1.581(3) . ?
N5_7 C1_11 1.431(2) . ?
B1_8 N5_8 1.425(3) . ?
B1_8 N2_8 1.426(2) . ?
N2_8 C3_8 1.443(2) . ?
N2_8 C4_8 1.455(2) . ?
C3_8 H3A_8 0.9800 . ?
C3_8 H3B_8 0.9800 . ?
C3_8 H3C_8 0.9800 . ?
C4_8 H4A_8 0.9800 . ?
C4_8 H4B_8 0.9800 . ?
C4_8 H4C_8 0.9800 . ?
N5_8 C6_8 1.455(2) . ?
N5_8 C7_8 1.456(2) . ?
C6_8 H6A_8 0.9800 . ?
C6_8 H6B_8 0.9800 . ?
C6_8 H6C_8 0.9800 . ?
C7_8 H7A_8 0.9800 . ?
C7_8 H7B_8 0.9800 . ?
C7_8 H7C_8 0.9800 . ?
B1_9 N5_9 1.425(2) . ?
B1_9 N2_9 1.429(2) . ?
N2_9 C4_9 1.454(2) . ?
N2_9 C3_9 1.456(2) . ?
C3_9 H3A_9 0.9800 . ?
C3_9 H3B_9 0.9800 . ?
C3_9 H3C_9 0.9800 . ?
C4_9 H4A_9 0.9800 . ?
C4_9 H4B_9 0.9800 . ?
C4_9 H4C_9 0.9800 . ?
N5_9 C6_9 1.455(2) . ?
N5_9 C7_9 1.457(2) . ?
C6_9 H6A_9 0.9800 . ?
C6_9 H6B_9 0.9800 . ?
C6_9 H6C_9 0.9800 . ?
C7_9 H7A_9 0.9800 . ?
C7_9 H7B_9 0.9800 . ?
C7_9 H7C_9 0.9800 . ?
N1_10 C3_10 1.446(2) . ?
N1_10 C2_10 1.449(2) . ?
C2_10 H2A_10 0.9800 . ?
C2_10 H2B_10 0.9800 . ?
C2_10 H2C_10 0.9800 . ?
C3_10 H3A_10 0.9800 . ?
C3_10 H3B_10 0.9800 . ?
C3_10 H3C_10 0.9800 . ?
C1_11 C2_11 1.400(3) . ?
C1_11 C6_11 1.403(2) . ?
C2_11 C3_11 1.395(3) . ?
C2_11 C7_11 1.505(3) . ?
C3_11 C4_11 1.379(3) . ?
C3_11 H3_11 0.9500 . ?
C4_11 C5_11 1.381(3) . ?
C4_11 H4_11 0.9500 . ?
C5_11 C6_11 1.394(3) . ?
C5_11 H5_11 0.9500 . ?
C6_11 C8_11 1.506(3) . ?
C7_11 H7A_11 0.9800 . ?
C7_11 H7B_11 0.9800 . ?
C7_11 H7C_11 0.9800 . ?
C8_11 H8A_11 0.9800 . ?
C8_11 H8B_11 0.9800 . ?
C8_11 H8C_11 0.9800 . ?
C1_12 C2_12 1.405(3) . ?
C1_12 C6_12 1.409(2) . ?
C2_12 C3_12 1.394(3) . ?
C2_12 C7_12 1.503(3) . ?
C3_12 C4_12 1.387(3) . ?
C3_12 H3_12 0.9500 . ?
C4_12 C5_12 1.379(3) . ?
C4_12 H4_12 0.9500 . ?
C5_12 C6_12 1.393(3) . ?
C5_12 H5_12 0.9500 . ?
C6_12 C8_12 1.507(3) . ?
C7_12 H7A_12 0.9800 . ?
C7_12 H7B_12 0.9800 . ?
C7_12 H7C_12 0.9800 . ?
C8_12 H8A_12 0.9800 . ?
C8_12 H8B_12 0.9800 . ?
C8_12 H8C_12 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_4 B1_1 N5_1 127.67(16) . . ?
N1_4 B1_1 N2_1 127.39(16) . . ?
N5_1 B1_1 N2_1 104.94(14) . . ?
C3_1 N2_1 C1_5 124.30(13) . . ?
C3_1 N2_1 B1_1 108.81(13) . . ?
C1_5 N2_1 B1_1 126.69(14) . . ?
C4_1 C3_1 N2_1 108.86(14) . . ?
C4_1 C3_1 B1_3 127.35(14) . . ?
N2_1 C3_1 B1_3 123.77(14) . . ?
C3_1 C4_1 N5_1 108.53(13) . . ?
C3_1 C4_1 B1_2 126.70(14) . . ?
N5_1 C4_1 B1_2 124.67(14) . . ?
C1_6 N5_1 B1_1 126.46(14) . . ?
C1_6 N5_1 C4_1 123.75(13) . . ?
B1_1 N5_1 C4_1 108.84(13) . . ?
N5_2 B1_2 N2_2 119.19(16) . . ?
N5_2 B1_2 C4_1 119.11(16) . . ?
N2_2 B1_2 C4_1 121.70(16) . . ?
B1_2 N2_2 C3_2 123.87(15) . . ?
B1_2 N2_2 C4_2 123.68(17) . . ?
C3_2 N2_2 C4_2 112.21(16) . . ?
N2_2 C4_2 H4A_2 109.5 . . ?
N2_2 C4_2 H4B_2 109.5 . . ?
H4A_2 C4_2 H4B_2 109.5 . . ?
N2_2 C4_2 H4C_2 109.5 . . ?
H4A_2 C4_2 H4C_2 109.5 . . ?
H4B_2 C4_2 H4C_2 109.5 . . ?
B1_2 N5_2 C6_2 125.13(15) . . ?
B1_2 N5_2 C7_2 122.82(16) . . ?
C6_2 N5_2 C7_2 111.62(15) . . ?
N5_2 C6_2 H6A_2 109.5 . . ?
N5_2 C6_2 H6B_2 109.5 . . ?
H6A_2 C6_2 H6B_2 109.5 . . ?
N5_2 C6_2 H6C_2 109.5 . . ?
H6A_2 C6_2 H6C_2 109.5 . . ?
H6B_2 C6_2 H6C_2 109.5 . . ?
N5_2 C7_2 H7A_2 109.5 . . ?
N5_2 C7_2 H7B_2 109.5 . . ?
H7A_2 C7_2 H7B_2 109.5 . . ?
N5_2 C7_2 H7C_2 109.5 . . ?
H7A_2 C7_2 H7C_2 109.5 . . ?
H7B_2 C7_2 H7C_2 109.5 . . ?
N2_2 C3_2 H3A_2 109.5 . . ?
N2_2 C3_2 H3B_2 109.5 . . ?
H3A_2 C3_2 H3B_2 109.5 . . ?
N2_2 C3_2 H3C_2 109.5 . . ?
H3A_2 C3_2 H3C_2 109.5 . . ?
H3B_2 C3_2 H3C_2 109.5 . . ?
N5_3 B1_3 N2_3 120.37(16) . . ?
N5_3 B1_3 C3_1 119.06(15) . . ?
N2_3 B1_3 C3_1 120.57(16) . . ?
B1_3 N2_3 C3_3 123.87(15) . . ?
B1_3 N2_3 C4_3 123.91(17) . . ?
C3_3 N2_3 C4_3 111.91(15) . . ?
N2_3 C3_3 H3A_3 109.5 . . ?
N2_3 C3_3 H3B_3 109.5 . . ?
H3A_3 C3_3 H3B_3 109.5 . . ?
N2_3 C3_3 H3C_3 109.5 . . ?
H3A_3 C3_3 H3C_3 109.5 . . ?
H3B_3 C3_3 H3C_3 109.5 . . ?
N2_3 C4_3 H4A_3 109.5 . . ?
N2_3 C4_3 H4B_3 109.5 . . ?
H4A_3 C4_3 H4B_3 109.5 . . ?
N2_3 C4_3 H4C_3 109.5 . . ?
H4A_3 C4_3 H4C_3 109.5 . . ?
H4B_3 C4_3 H4C_3 109.5 . . ?
B1_3 N5_3 C6_3 125.22(14) . . ?
B1_3 N5_3 C7_3 123.40(16) . . ?
C6_3 N5_3 C7_3 111.08(15) . . ?
N5_3 C6_3 H6A_3 109.5 . . ?
N5_3 C6_3 H6B_3 109.5 . . ?
H6A_3 C6_3 H6B_3 109.5 . . ?
N5_3 C6_3 H6C_3 109.5 . . ?
H6A_3 C6_3 H6C_3 109.5 . . ?
H6B_3 C6_3 H6C_3 109.5 . . ?
N5_3 C7_3 H7A_3 109.5 . . ?
N5_3 C7_3 H7B_3 109.5 . . ?
H7A_3 C7_3 H7B_3 109.5 . . ?
N5_3 C7_3 H7C_3 109.5 . . ?
H7A_3 C7_3 H7C_3 109.5 . . ?
H7B_3 C7_3 H7C_3 109.5 . . ?
B1_1 N1_4 C2_4 123.29(16) . . ?
B1_1 N1_4 C3_4 123.21(15) . . ?
C2_4 N1_4 C3_4 113.43(15) . . ?
N1_4 C2_4 H2A_4 109.5 . . ?
N1_4 C2_4 H2B_4 109.5 . . ?
H2A_4 C2_4 H2B_4 109.5 . . ?
N1_4 C2_4 H2C_4 109.5 . . ?
H2A_4 C2_4 H2C_4 109.5 . . ?
H2B_4 C2_4 H2C_4 109.5 . . ?
N1_4 C3_4 H3A_4 109.5 . . ?
N1_4 C3_4 H3B_4 109.5 . . ?
H3A_4 C3_4 H3B_4 109.5 . . ?
N1_4 C3_4 H3C_4 109.5 . . ?
H3A_4 C3_4 H3C_4 109.5 . . ?
H3B_4 C3_4 H3C_4 109.5 . . ?
C6_5 C1_5 C2_5 121.33(15) . . ?
C6_5 C1_5 N2_1 120.41(16) . . ?
C2_5 C1_5 N2_1 118.20(16) . . ?
C3_5 C2_5 C1_5 118.07(17) . . ?
C3_5 C2_5 C7_5 119.74(17) . . ?
C1_5 C2_5 C7_5 122.19(15) . . ?
C4_5 C3_5 C2_5 121.20(18) . . ?
C4_5 C3_5 H3_5 119.4 . . ?
C2_5 C3_5 H3_5 119.4 . . ?
C3_5 C4_5 C5_5 119.86(17) . . ?
C3_5 C4_5 H4_5 120.1 . . ?
C5_5 C4_5 H4_5 120.1 . . ?
C4_5 C5_5 C6_5 121.29(18) . . ?
C4_5 C5_5 H5_5 119.4 . . ?
C6_5 C5_5 H5_5 119.4 . . ?
C5_5 C6_5 C1_5 118.21(17) . . ?
C5_5 C6_5 C8_5 120.23(17) . . ?
C1_5 C6_5 C8_5 121.54(15) . . ?
C2_5 C7_5 H7A_5 109.5 . . ?
C2_5 C7_5 H7B_5 109.5 . . ?
H7A_5 C7_5 H7B_5 109.5 . . ?
C2_5 C7_5 H7C_5 109.5 . . ?
H7A_5 C7_5 H7C_5 109.5 . . ?
H7B_5 C7_5 H7C_5 109.5 . . ?
C6_5 C8_5 H8A_5 109.5 . . ?
C6_5 C8_5 H8B_5 109.5 . . ?
H8A_5 C8_5 H8B_5 109.5 . . ?
C6_5 C8_5 H8C_5 109.5 . . ?
H8A_5 C8_5 H8C_5 109.5 . . ?
H8B_5 C8_5 H8C_5 109.5 . . ?
C2_6 C1_6 C6_6 120.83(15) . . ?
C2_6 C1_6 N5_1 120.59(15) . . ?
C6_6 C1_6 N5_1 118.57(15) . . ?
C3_6 C2_6 C1_6 118.39(17) . . ?
C3_6 C2_6 C7_6 120.32(17) . . ?
C1_6 C2_6 C7_6 121.25(16) . . ?
C4_6 C3_6 C2_6 121.20(17) . . ?
C4_6 C3_6 H3_6 119.4 . . ?
C2_6 C3_6 H3_6 119.4 . . ?
C5_6 C4_6 C3_6 119.78(16) . . ?
C5_6 C4_6 H4_6 120.1 . . ?
C3_6 C4_6 H4_6 120.1 . . ?
C4_6 C5_6 C6_6 121.19(17) . . ?
C4_6 C5_6 H5_6 119.4 . . ?
C6_6 C5_6 H5_6 119.4 . . ?
C5_6 C6_6 C1_6 118.59(16) . . ?
C5_6 C6_6 C8_6 119.22(16) . . ?
C1_6 C6_6 C8_6 122.18(15) . . ?
C2_6 C7_6 H7A_6 109.5 . . ?
C2_6 C7_6 H7B_6 109.5 . . ?
H7A_6 C7_6 H7B_6 109.5 . . ?
C2_6 C7_6 H7C_6 109.5 . . ?
H7A_6 C7_6 H7C_6 109.5 . . ?
H7B_6 C7_6 H7C_6 109.5 . . ?
C6_6 C8_6 H8A_6 109.5 . . ?
C6_6 C8_6 H8B_6 109.5 . . ?
H8A_6 C8_6 H8B_6 109.5 . . ?
C6_6 C8_6 H8C_6 109.5 . . ?
H8A_6 C8_6 H8C_6 109.5 . . ?
H8B_6 C8_6 H8C_6 109.5 . . ?
N1_10 B1_7 N5_7 127.48(16) . . ?
N1_10 B1_7 N2_7 127.85(16) . . ?
N5_7 B1_7 N2_7 104.66(15) . . ?
C1_12 N2_7 C3_7 123.86(13) . . ?
C1_12 N2_7 B1_7 126.78(14) . . ?
C3_7 N2_7 B1_7 108.93(14) . . ?
C4_7 C3_7 N2_7 108.80(14) . . ?
C4_7 C3_7 B1_9 127.21(15) . . ?
N2_7 C3_7 B1_9 124.00(14) . . ?
C3_7 C4_7 N5_7 108.46(14) . . ?
C3_7 C4_7 B1_8 125.65(15) . . ?
N5_7 C4_7 B1_8 125.89(14) . . ?
C4_7 N5_7 C1_11 123.30(14) . . ?
C4_7 N5_7 B1_7 109.14(13) . . ?
C1_11 N5_7 B1_7 127.33(14) . . ?
N5_8 B1_8 N2_8 120.55(17) . . ?
N5_8 B1_8 C4_7 118.85(15) . . ?
N2_8 B1_8 C4_7 120.58(16) . . ?
B1_8 N2_8 C3_8 123.49(16) . . ?
B1_8 N2_8 C4_8 124.93(16) . . ?
C3_8 N2_8 C4_8 111.43(15) . . ?
N2_8 C3_8 H3A_8 109.5 . . ?
N2_8 C3_8 H3B_8 109.5 . . ?
H3A_8 C3_8 H3B_8 109.5 . . ?
N2_8 C3_8 H3C_8 109.5 . . ?
H3A_8 C3_8 H3C_8 109.5 . . ?
H3B_8 C3_8 H3C_8 109.5 . . ?
N2_8 C4_8 H4A_8 109.5 . . ?
N2_8 C4_8 H4B_8 109.5 . . ?
H4A_8 C4_8 H4B_8 109.5 . . ?
N2_8 C4_8 H4C_8 109.5 . . ?
H4A_8 C4_8 H4C_8 109.5 . . ?
H4B_8 C4_8 H4C_8 109.5 . . ?
B1_8 N5_8 C6_8 124.60(15) . . ?
B1_8 N5_8 C7_8 123.95(15) . . ?
C6_8 N5_8 C7_8 111.11(15) . . ?
N5_8 C6_8 H6A_8 109.5 . . ?
N5_8 C6_8 H6B_8 109.5 . . ?
H6A_8 C6_8 H6B_8 109.5 . . ?
N5_8 C6_8 H6C_8 109.5 . . ?
H6A_8 C6_8 H6C_8 109.5 . . ?
H6B_8 C6_8 H6C_8 109.5 . . ?
N5_8 C7_8 H7A_8 109.5 . . ?
N5_8 C7_8 H7B_8 109.5 . . ?
H7A_8 C7_8 H7B_8 109.5 . . ?
N5_8 C7_8 H7C_8 109.5 . . ?
H7A_8 C7_8 H7C_8 109.5 . . ?
H7B_8 C7_8 H7C_8 109.5 . . ?
N5_9 B1_9 N2_9 120.72(15) . . ?
N5_9 B1_9 C3_7 120.13(15) . . ?
N2_9 B1_9 C3_7 119.15(15) . . ?
B1_9 N2_9 C4_9 123.51(15) . . ?
B1_9 N2_9 C3_9 124.69(14) . . ?
C4_9 N2_9 C3_9 111.55(14) . . ?
N2_9 C3_9 H3A_9 109.5 . . ?
N2_9 C3_9 H3B_9 109.5 . . ?
H3A_9 C3_9 H3B_9 109.5 . . ?
N2_9 C3_9 H3C_9 109.5 . . ?
H3A_9 C3_9 H3C_9 109.5 . . ?
H3B_9 C3_9 H3C_9 109.5 . . ?
N2_9 C4_9 H4A_9 109.5 . . ?
N2_9 C4_9 H4B_9 109.5 . . ?
H4A_9 C4_9 H4B_9 109.5 . . ?
N2_9 C4_9 H4C_9 109.5 . . ?
H4A_9 C4_9 H4C_9 109.5 . . ?
H4B_9 C4_9 H4C_9 109.5 . . ?
B1_9 N5_9 C6_9 123.64(14) . . ?
B1_9 N5_9 C7_9 124.93(16) . . ?
C6_9 N5_9 C7_9 111.07(14) . . ?
N5_9 C6_9 H6A_9 109.5 . . ?
N5_9 C6_9 H6B_9 109.5 . . ?
H6A_9 C6_9 H6B_9 109.5 . . ?
N5_9 C6_9 H6C_9 109.5 . . ?
H6A_9 C6_9 H6C_9 109.5 . . ?
H6B_9 C6_9 H6C_9 109.5 . . ?
N5_9 C7_9 H7A_9 109.5 . . ?
N5_9 C7_9 H7B_9 109.5 . . ?
H7A_9 C7_9 H7B_9 109.5 . . ?
N5_9 C7_9 H7C_9 109.5 . . ?
H7A_9 C7_9 H7C_9 109.5 . . ?
H7B_9 C7_9 H7C_9 109.5 . . ?
B1_7 N1_10 C3_10 123.51(15) . . ?
B1_7 N1_10 C2_10 122.53(15) . . ?
C3_10 N1_10 C2_10 113.95(14) . . ?
N1_10 C2_10 H2A_10 109.5 . . ?
N1_10 C2_10 H2B_10 109.5 . . ?
H2A_10 C2_10 H2B_10 109.5 . . ?
N1_10 C2_10 H2C_10 109.5 . . ?
H2A_10 C2_10 H2C_10 109.5 . . ?
H2B_10 C2_10 H2C_10 109.5 . . ?
N1_10 C3_10 H3A_10 109.5 . . ?
N1_10 C3_10 H3B_10 109.5 . . ?
H3A_10 C3_10 H3B_10 109.5 . . ?
N1_10 C3_10 H3C_10 109.5 . . ?
H3A_10 C3_10 H3C_10 109.5 . . ?
H3B_10 C3_10 H3C_10 109.5 . . ?
C2_11 C1_11 C6_11 120.92(16) . . ?
C2_11 C1_11 N5_7 119.85(15) . . ?
C6_11 C1_11 N5_7 119.20(15) . . ?
C3_11 C2_11 C1_11 118.56(17) . . ?
C3_11 C2_11 C7_11 120.22(17) . . ?
C1_11 C2_11 C7_11 121.15(16) . . ?
C4_11 C3_11 C2_11 121.15(19) . . ?
C4_11 C3_11 H3_11 119.4 . . ?
C2_11 C3_11 H3_11 119.4 . . ?
C3_11 C4_11 C5_11 119.58(17) . . ?
C3_11 C4_11 H4_11 120.2 . . ?
C5_11 C4_11 H4_11 120.2 . . ?
C4_11 C5_11 C6_11 121.42(19) . . ?
C4_11 C5_11 H5_11 119.3 . . ?
C6_11 C5_11 H5_11 119.3 . . ?
C5_11 C6_11 C1_11 118.28(18) . . ?
C5_11 C6_11 C8_11 119.41(17) . . ?
C1_11 C6_11 C8_11 122.31(16) . . ?
C2_11 C7_11 H7A_11 109.5 . . ?
C2_11 C7_11 H7B_11 109.5 . . ?
H7A_11 C7_11 H7B_11 109.5 . . ?
C2_11 C7_11 H7C_11 109.5 . . ?
H7A_11 C7_11 H7C_11 109.5 . . ?
H7B_11 C7_11 H7C_11 109.5 . . ?
C6_11 C8_11 H8A_11 109.5 . . ?
C6_11 C8_11 H8B_11 109.5 . . ?
H8A_11 C8_11 H8B_11 109.5 . . ?
C6_11 C8_11 H8C_11 109.5 . . ?
H8A_11 C8_11 H8C_11 109.5 . . ?
H8B_11 C8_11 H8C_11 109.5 . . ?
C2_12 C1_12 C6_12 120.84(16) . . ?
C2_12 C1_12 N2_7 120.58(15) . . ?
C6_12 C1_12 N2_7 118.48(15) . . ?
C3_12 C2_12 C1_12 118.40(17) . . ?
C3_12 C2_12 C7_12 119.96(17) . . ?
C1_12 C2_12 C7_12 121.62(16) . . ?
C4_12 C3_12 C2_12 121.26(19) . . ?
C4_12 C3_12 H3_12 119.4 . . ?
C2_12 C3_12 H3_12 119.4 . . ?
C5_12 C4_12 C3_12 119.68(18) . . ?
C5_12 C4_12 H4_12 120.2 . . ?
C3_12 C4_12 H4_12 120.2 . . ?
C4_12 C5_12 C6_12 121.31(18) . . ?
C4_12 C5_12 H5_12 119.3 . . ?
C6_12 C5_12 H5_12 119.3 . . ?
C5_12 C6_12 C1_12 118.46(18) . . ?
C5_12 C6_12 C8_12 119.83(17) . . ?
C1_12 C6_12 C8_12 121.71(16) . . ?
C2_12 C7_12 H7A_12 109.5 . . ?
C2_12 C7_12 H7B_12 109.5 . . ?
H7A_12 C7_12 H7B_12 109.5 . . ?
C2_12 C7_12 H7C_12 109.5 . . ?
H7A_12 C7_12 H7C_12 109.5 . . ?
H7B_12 C7_12 H7C_12 109.5 . . ?
C6_12 C8_12 H8A_12 109.5 . . ?
C6_12 C8_12 H8B_12 109.5 . . ?
H8A_12 C8_12 H8B_12 109.5 . . ?
C6_12 C8_12 H8C_12 109.5 . . ?
H8A_12 C8_12 H8C_12 109.5 . . ?
H8B_12 C8_12 H8C_12 109.5 . . ?

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_4 B1_1 N2_1 C3_1 -179.98(18) . . . . ?
N5_1 B1_1 N2_1 C3_1 -0.49(19) . . . . ?
N1_4 B1_1 N2_1 C1_5 -5.0(3) . . . . ?
N5_1 B1_1 N2_1 C1_5 174.52(16) . . . . ?
C1_5 N2_1 C3_1 C4_1 -173.84(16) . . . . ?
B1_1 N2_1 C3_1 C4_1 1.32(19) . . . . ?
C1_5 N2_1 C3_1 B1_3 7.6(3) . . . . ?
B1_1 N2_1 C3_1 B1_3 -177.25(16) . . . . ?
N2_1 C3_1 C4_1 N5_1 -1.59(19) . . . . ?
B1_3 C3_1 C4_1 N5_1 176.91(16) . . . . ?
N2_1 C3_1 C4_1 B1_2 174.85(16) . . . . ?
B1_3 C3_1 C4_1 B1_2 -6.7(3) . . . . ?
N1_4 B1_1 N5_1 C1_6 -11.8(3) . . . . ?
N2_1 B1_1 N5_1 C1_6 168.67(15) . . . . ?
N1_4 B1_1 N5_1 C4_1 179.03(18) . . . . ?
N2_1 B1_1 N5_1 C4_1 -0.46(19) . . . . ?
C3_1 C4_1 N5_1 C1_6 -168.20(15) . . . . ?
B1_2 C4_1 N5_1 C1_6 15.3(3) . . . . ?
C3_1 C4_1 N5_1 B1_1 1.29(19) . . . . ?
B1_2 C4_1 N5_1 B1_1 -175.24(16) . . . . ?
C3_1 C4_1 B1_2 N5_2 -44.4(3) . . . . ?
N5_1 C4_1 B1_2 N5_2 131.46(18) . . . . ?
C3_1 C4_1 B1_2 N2_2 136.13(19) . . . . ?
N5_1 C4_1 B1_2 N2_2 -48.0(3) . . . . ?
N5_2 B1_2 N2_2 C3_2 152.19(17) . . . . ?
C4_1 B1_2 N2_2 C3_2 -28.4(3) . . . . ?
N5_2 B1_2 N2_2 C4_2 -33.9(3) . . . . ?
C4_1 B1_2 N2_2 C4_2 145.57(17) . . . . ?
N2_2 B1_2 N5_2 C6_2 158.84(17) . . . . ?
C4_1 B1_2 N5_2 C6_2 -20.6(3) . . . . ?
N2_2 B1_2 N5_2 C7_2 -29.3(3) . . . . ?
C4_1 B1_2 N5_2 C7_2 151.24(17) . . . . ?
C4_1 C3_1 B1_3 N5_3 -47.3(3) . . . . ?
N2_1 C3_1 B1_3 N5_3 130.97(17) . . . . ?
C4_1 C3_1 B1_3 N2_3 133.34(19) . . . . ?
N2_1 C3_1 B1_3 N2_3 -48.4(2) . . . . ?
N5_3 B1_3 N2_3 C3_3 153.49(16) . . . . ?
C3_1 B1_3 N2_3 C3_3 -27.2(2) . . . . ?
N5_3 B1_3 N2_3 C4_3 -33.5(3) . . . . ?
C3_1 B1_3 N2_3 C4_3 145.79(17) . . . . ?
N2_3 B1_3 N5_3 C6_3 160.06(16) . . . . ?
C3_1 B1_3 N5_3 C6_3 -19.3(2) . . . . ?
N2_3 B1_3 N5_3 C7_3 -26.8(3) . . . . ?
C3_1 B1_3 N5_3 C7_3 153.85(16) . . . . ?
N5_1 B1_1 N1_4 C2_4 150.19(19) . . . . ?
N2_1 B1_1 N1_4 C2_4 -30.4(3) . . . . ?
N5_1 B1_1 N1_4 C3_4 -26.6(3) . . . . ?
N2_1 B1_1 N1_4 C3_4 152.75(19) . . . . ?
C3_1 N2_1 C1_5 C6_5 -67.8(2) . . . . ?
B1_1 N2_1 C1_5 C6_5 117.87(19) . . . . ?
C3_1 N2_1 C1_5 C2_5 114.81(18) . . . . ?
B1_1 N2_1 C1_5 C2_5 -59.5(2) . . . . ?
C6_5 C1_5 C2_5 C3_5 -0.3(2) . . . . ?
N2_1 C1_5 C2_5 C3_5 177.02(15) . . . . ?
C6_5 C1_5 C2_5 C7_5 179.47(16) . . . . ?
N2_1 C1_5 C2_5 C7_5 -3.2(2) . . . . ?
C1_5 C2_5 C3_5 C4_5 1.5(3) . . . . ?
C7_5 C2_5 C3_5 C4_5 -178.24(17) . . . . ?
C2_5 C3_5 C4_5 C5_5 -0.8(3) . . . . ?
C3_5 C4_5 C5_5 C6_5 -1.2(3) . . . . ?
C4_5 C5_5 C6_5 C1_5 2.4(3) . . . . ?
C4_5 C5_5 C6_5 C8_5 -175.85(17) . . . . ?
C2_5 C1_5 C6_5 C5_5 -1.6(2) . . . . ?
N2_1 C1_5 C6_5 C5_5 -178.90(15) . . . . ?
C2_5 C1_5 C6_5 C8_5 176.62(16) . . . . ?
N2_1 C1_5 C6_5 C8_5 -0.6(2) . . . . ?
B1_1 N5_1 C1_6 C2_6 120.80(19) . . . . ?
C4_1 N5_1 C1_6 C2_6 -71.6(2) . . . . ?
B1_1 N5_1 C1_6 C6_6 -57.7(2) . . . . ?
C4_1 N5_1 C1_6 C6_6 109.93(18) . . . . ?
C6_6 C1_6 C2_6 C3_6 -1.7(2) . . . . ?
N5_1 C1_6 C2_6 C3_6 179.84(15) . . . . ?
C6_6 C1_6 C2_6 C7_6 176.38(17) . . . . ?
N5_1 C1_6 C2_6 C7_6 -2.1(2) . . . . ?
C1_6 C2_6 C3_6 C4_6 1.8(3) . . . . ?
C7_6 C2_6 C3_6 C4_6 -176.29(18) . . . . ?
C2_6 C3_6 C4_6 C5_6 -0.8(3) . . . . ?
C3_6 C4_6 C5_6 C6_6 -0.4(3) . . . . ?
C4_6 C5_6 C6_6 C1_6 0.5(3) . . . . ?
C4_6 C5_6 C6_6 C8_6 -178.07(17) . . . . ?
C2_6 C1_6 C6_6 C5_6 0.6(2) . . . . ?
N5_1 C1_6 C6_6 C5_6 179.07(15) . . . . ?
C2_6 C1_6 C6_6 C8_6 179.10(16) . . . . ?
N5_1 C1_6 C6_6 C8_6 -2.4(2) . . . . ?
N1_10 B1_7 N2_7 C1_12 6.8(3) . . . . ?
N5_7 B1_7 N2_7 C1_12 -172.80(15) . . . . ?
N1_10 B1_7 N2_7 C3_7 179.44(17) . . . . ?
N5_7 B1_7 N2_7 C3_7 -0.12(18) . . . . ?
C1_12 N2_7 C3_7 C4_7 172.38(15) . . . . ?
B1_7 N2_7 C3_7 C4_7 -0.57(18) . . . . ?
C1_12 N2_7 C3_7 B1_9 -7.9(2) . . . . ?
B1_7 N2_7 C3_7 B1_9 179.15(15) . . . . ?
N2_7 C3_7 C4_7 N5_7 1.02(17) . . . . ?
B1_9 C3_7 C4_7 N5_7 -178.69(15) . . . . ?
N2_7 C3_7 C4_7 B1_8 -179.69(15) . . . . ?
B1_9 C3_7 C4_7 B1_8 0.6(3) . . . . ?
C3_7 C4_7 N5_7 C1_11 173.80(14) . . . . ?
B1_8 C4_7 N5_7 C1_11 -5.5(2) . . . . ?
C3_7 C4_7 N5_7 B1_7 -1.11(18) . . . . ?
B1_8 C4_7 N5_7 B1_7 179.61(16) . . . . ?
N1_10 B1_7 N5_7 C4_7 -178.83(17) . . . . ?
N2_7 B1_7 N5_7 C4_7 0.73(18) . . . . ?
N1_10 B1_7 N5_7 C1_11 6.5(3) . . . . ?
N2_7 B1_7 N5_7 C1_11 -173.92(14) . . . . ?
C3_7 C4_7 B1_8 N5_8 50.7(2) . . . . ?
N5_7 C4_7 B1_8 N5_8 -130.14(17) . . . . ?
C3_7 C4_7 B1_8 N2_8 -127.50(18) . . . . ?
N5_7 C4_7 B1_8 N2_8 51.7(2) . . . . ?
N5_8 B1_8 N2_8 C3_8 -156.29(16) . . . . ?
C4_7 B1_8 N2_8 C3_8 21.9(2) . . . . ?
N5_8 B1_8 N2_8 C4_8 28.4(3) . . . . ?
C4_7 B1_8 N2_8 C4_8 -153.40(17) . . . . ?
N2_8 B1_8 N5_8 C6_8 -157.17(17) . . . . ?
C4_7 B1_8 N5_8 C6_8 24.6(3) . . . . ?
N2_8 B1_8 N5_8 C7_8 30.2(3) . . . . ?
C4_7 B1_8 N5_8 C7_8 -148.04(17) . . . . ?
C4_7 C3_7 B1_9 N5_9 -127.20(19) . . . . ?
N2_7 C3_7 B1_9 N5_9 53.1(2) . . . . ?
C4_7 C3_7 B1_9 N2_9 53.4(3) . . . . ?
N2_7 C3_7 B1_9 N2_9 -126.23(18) . . . . ?
N5_9 B1_9 N2_9 C4_9 25.3(3) . . . . ?
C3_7 B1_9 N2_9 C4_9 -155.31(17) . . . . ?
N5_9 B1_9 N2_9 C3_9 -160.80(17) . . . . ?
C3_7 B1_9 N2_9 C3_9 18.6(3) . . . . ?
N2_9 B1_9 N5_9 C6_9 -155.88(18) . . . . ?
C3_7 B1_9 N5_9 C6_9 24.8(3) . . . . ?
N2_9 B1_9 N5_9 C7_9 31.6(3) . . . . ?
C3_7 B1_9 N5_9 C7_9 -147.71(18) . . . . ?
N5_7 B1_7 N1_10 C3_10 -151.08(18) . . . . ?
N2_7 B1_7 N1_10 C3_10 29.5(3) . . . . ?
N5_7 B1_7 N1_10 C2_10 30.2(3) . . . . ?
N2_7 B1_7 N1_10 C2_10 -149.26(18) . . . . ?
C4_7 N5_7 C1_11 C2_11 69.4(2) . . . . ?
B1_7 N5_7 C1_11 C2_11 -116.67(19) . . . . ?
C4_7 N5_7 C1_11 C6_11 -112.42(18) . . . . ?
B1_7 N5_7 C1_11 C6_11 61.5(2) . . . . ?
C6_11 C1_11 C2_11 C3_11 3.3(2) . . . . ?
N5_7 C1_11 C2_11 C3_11 -178.50(15) . . . . ?
C6_11 C1_11 C2_11 C7_11 -173.69(16) . . . . ?
N5_7 C1_11 C2_11 C7_11 4.5(2) . . . . ?
C1_11 C2_11 C3_11 C4_11 -1.8(3) . . . . ?
C7_11 C2_11 C3_11 C4_11 175.30(17) . . . . ?
C2_11 C3_11 C4_11 C5_11 -0.8(3) . . . . ?
C3_11 C4_11 C5_11 C6_11 2.0(3) . . . . ?
C4_11 C5_11 C6_11 C1_11 -0.4(3) . . . . ?
C4_11 C5_11 C6_11 C8_11 179.34(17) . . . . ?
C2_11 C1_11 C6_11 C5_11 -2.3(2) . . . . ?
N5_7 C1_11 C6_11 C5_11 179.54(15) . . . . ?
C2_11 C1_11 C6_11 C8_11 177.98(16) . . . . ?
N5_7 C1_11 C6_11 C8_11 -0.2(2) . . . . ?
C3_7 N2_7 C1_12 C2_12 69.9(2) . . . . ?
B1_7 N2_7 C1_12 C2_12 -118.42(19) . . . . ?
C3_7 N2_7 C1_12 C6_12 -113.63(18) . . . . ?
B1_7 N2_7 C1_12 C6_12 58.0(2) . . . . ?
C6_12 C1_12 C2_12 C3_12 1.8(3) . . . . ?
N2_7 C1_12 C2_12 C3_12 178.18(16) . . . . ?
C6_12 C1_12 C2_12 C7_12 -176.74(16) . . . . ?
N2_7 C1_12 C2_12 C7_12 -0.4(3) . . . . ?
C1_12 C2_12 C3_12 C4_12 -2.1(3) . . . . ?
C7_12 C2_12 C3_12 C4_12 176.45(19) . . . . ?
C2_12 C3_12 C4_12 C5_12 0.8(3) . . . . ?
C3_12 C4_12 C5_12 C6_12 0.9(3) . . . . ?
C4_12 C5_12 C6_12 C1_12 -1.2(3) . . . . ?
C4_12 C5_12 C6_12 C8_12 178.62(18) . . . . ?
C2_12 C1_12 C6_12 C5_12 -0.2(3) . . . . ?
N2_7 C1_12 C6_12 C5_12 -176.62(16) . . . . ?
C2_12 C1_12 C6_12 C8_12 179.99(17) . . . . ?
N2_7 C1_12 C6_12 C8_12 3.6(2) . . . . ?


_chemical_name_systematic        3-Xyl
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
