# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

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

data_test_a
_database_code_depnum_ccdc_archive 'CCDC 2071470'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_test_a              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
RESPONSE: Reflections affected by beamstop
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        (CAAC)(IiPr)B(CN-Mo(CO)5)
_chemical_name_common            2(CN)-Mo
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H47 B Mo N4 O5, C6 H6'
_chemical_formula_sum            'C41 H53 B Mo N4 O5'
_chemical_formula_weight         788.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.190(6)
_cell_length_b                   14.868(5)
_cell_length_c                   21.174(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4152(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9879
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      25.48


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             1656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.136
_exptl_absorpt_coefficient_mu    0.361
_shelx_estimated_absorpt_T_min   0.892
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5079
_exptl_absorpt_correction_T_max  0.7454
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 1.00 -1.00 0.1120
-1.00 -1.00 1.00 0.1070
1.00 0.00 -1.00 0.1440
-1.00 0.00 1.00 0.1460
-1.00 0.00 -1.00 0.1230
1.00 0.00 1.00 0.1350
0.00 -1.00 -1.00 0.0200
0.00 1.00 1.00 0.0680
1.00 0.00 0.00 0.1610
-1.00 0.00 0.00 0.1480
1.00 1.00 1.00 0.1160
-1.00 1.00 1.00 0.1310
0.00 0.00 -1.00 0.0360
0.00 0.00 1.00 0.0720

_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            26955
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.674
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             8028
_reflns_number_gt                7050
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_max     0.959
_reflns_Friedel_fraction_full    0.959

_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       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_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          
;

 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0191P)²] 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_abs_structure_details 
;
 Flack x determined using 2718 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.065(19)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         8028
_refine_ls_number_parameters     481
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0746
_refine_ls_wR_factor_gt          0.0708
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
C1 C 0.6127(3) 0.6182(2) 0.39310(18) 0.0121(9) Uani 1 1 d . . . . .
N1 N 0.6879(2) 0.60834(18) 0.34814(14) 0.0110(7) Uani 1 1 d . . . . .
C2 C 0.7233(3) 0.6926(2) 0.31700(18) 0.0150(9) Uani 1 1 d . . . . .
C3 C 0.6414(3) 0.7586(2) 0.3390(2) 0.0215(10) Uani 1 1 d . . . . .
H3A H 0.590091 0.766854 0.305359 0.026 Uiso 1 1 calc R U . . .
H3AB H 0.672074 0.817786 0.348543 0.026 Uiso 1 1 calc R U . . .
C4 C 0.5911(3) 0.7197(2) 0.39861(17) 0.0154(8) Uani 1 1 d . . . . .
C5 C 0.8298(3) 0.7195(3) 0.33813(19) 0.0227(9) Uani 1 1 d . . . . .
H5A H 0.848199 0.777102 0.318719 0.034 Uiso 1 1 calc R U . . .
H5B H 0.878305 0.673218 0.325005 0.034 Uiso 1 1 calc R U . . .
H5C H 0.831279 0.725518 0.384213 0.034 Uiso 1 1 calc R U . . .
C6 C 0.7253(4) 0.6839(3) 0.24524(19) 0.0267(11) Uani 1 1 d . . . . .
H6A H 0.751247 0.739683 0.226674 0.040 Uiso 1 1 calc R U . . .
H6B H 0.656456 0.672636 0.229684 0.040 Uiso 1 1 calc R U . . .
H6C H 0.769411 0.633674 0.233253 0.040 Uiso 1 1 calc R U . . .
C7 C 0.6391(3) 0.7587(3) 0.45882(19) 0.0249(11) Uani 1 1 d . . . . .
H7A H 0.633639 0.824408 0.458122 0.037 Uiso 1 1 calc R U . . .
H7B H 0.710712 0.741367 0.460794 0.037 Uiso 1 1 calc R U . . .
H7C H 0.603523 0.735120 0.495931 0.037 Uiso 1 1 calc R U . . .
C8 C 0.4785(3) 0.7434(3) 0.3984(2) 0.0276(11) Uani 1 1 d . . . . .
H8A H 0.470562 0.808881 0.397393 0.041 Uiso 1 1 calc R U . . .
H8B H 0.446441 0.719336 0.436548 0.041 Uiso 1 1 calc R U . . .
H8C H 0.446269 0.717053 0.360983 0.041 Uiso 1 1 calc R U . . .
C9 C 0.7307(3) 0.5219(2) 0.33359(17) 0.0109(8) Uani 1 1 d . . . . .
C10 C 0.8124(3) 0.4891(2) 0.36933(18) 0.0130(9) Uani 1 1 d . . . . .
C11 C 0.8559(3) 0.4069(2) 0.35202(19) 0.0166(9) Uani 1 1 d . . . . .
H11 H 0.912282 0.384363 0.375004 0.020 Uiso 1 1 calc R U . . .
C12 C 0.8176(3) 0.3580(2) 0.30184(19) 0.0175(10) Uani 1 1 d . . . . .
H12 H 0.849665 0.303663 0.289249 0.021 Uiso 1 1 calc R U . . .
C13 C 0.7330(3) 0.3882(2) 0.27011(19) 0.0160(9) Uani 1 1 d . . . . .
H13 H 0.705504 0.352613 0.237001 0.019 Uiso 1 1 calc R U . . .
C14 C 0.6867(3) 0.4696(2) 0.28543(18) 0.0120(9) Uani 1 1 d . . . . .
C15 C 0.8536(3) 0.5356(3) 0.4283(2) 0.0171(9) Uani 1 1 d . . . . .
H15 H 0.815302 0.592986 0.434234 0.021 Uiso 1 1 calc R U . . .
C16 C 0.8365(3) 0.4771(3) 0.48687(19) 0.0233(10) Uani 1 1 d . . . . .
H16A H 0.854894 0.511179 0.524793 0.035 Uiso 1 1 calc R U . . .
H16B H 0.878737 0.423001 0.484074 0.035 Uiso 1 1 calc R U . . .
H16C H 0.764964 0.459663 0.489219 0.035 Uiso 1 1 calc R U . . .
C17 C 0.9669(3) 0.5587(3) 0.4238(2) 0.0255(11) Uani 1 1 d . . . . .
H17A H 0.987419 0.592534 0.461423 0.038 Uiso 1 1 calc R U . . .
H17B H 0.979010 0.595251 0.386048 0.038 Uiso 1 1 calc R U . . .
H17C H 1.006508 0.503074 0.421113 0.038 Uiso 1 1 calc R U . . .
C18 C 0.5883(3) 0.4951(2) 0.25272(17) 0.0157(8) Uani 1 1 d . . . . .
H18 H 0.567798 0.556123 0.267983 0.019 Uiso 1 1 calc R U . . .
C19 C 0.5032(3) 0.4281(3) 0.2702(2) 0.0211(10) Uani 1 1 d . . . . .
H19A H 0.439317 0.447668 0.250890 0.032 Uiso 1 1 calc R U . . .
H19B H 0.495396 0.426033 0.316169 0.032 Uiso 1 1 calc R U . . .
H19C H 0.520804 0.368085 0.254474 0.032 Uiso 1 1 calc R U . . .
C20 C 0.5977(4) 0.4989(3) 0.18060(18) 0.0239(10) Uani 1 1 d . . . . .
H20A H 0.533504 0.519631 0.162406 0.036 Uiso 1 1 calc R U . . .
H20B H 0.613596 0.438828 0.164355 0.036 Uiso 1 1 calc R U . . .
H20C H 0.652020 0.540715 0.168926 0.036 Uiso 1 1 calc R U . . .
B1 B 0.5647(3) 0.5471(3) 0.4308(2) 0.0118(9) Uani 1 1 d . . . . .
C21 C 0.5857(3) 0.4452(2) 0.42584(17) 0.0120(8) Uani 1 1 d . . . . .
N2 N 0.5900(3) 0.36753(17) 0.42770(14) 0.0136(7) Uani 1 1 d . . . . .
C22 C 0.4819(3) 0.5616(2) 0.48329(19) 0.0121(9) Uani 1 1 d . . . . .
N3 N 0.4977(3) 0.5716(2) 0.54607(15) 0.0147(8) Uani 1 1 d . . . . .
C23 C 0.4067(3) 0.5680(2) 0.57861(18) 0.0193(9) Uani 1 1 d . . . . .
H23 H 0.398051 0.572426 0.623046 0.023 Uiso 1 1 calc R U . . .
C24 C 0.3334(3) 0.5573(2) 0.53569(19) 0.0173(10) Uani 1 1 d . . . . .
H24 H 0.262758 0.552772 0.543834 0.021 Uiso 1 1 calc R U . . .
N4 N 0.3798(2) 0.55417(19) 0.47730(15) 0.0137(8) Uani 1 1 d . . . . .
C25 C 0.5991(3) 0.5730(3) 0.57578(19) 0.0229(9) Uani 1 1 d . . . . .
H25 H 0.649986 0.587331 0.542234 0.027 Uiso 1 1 calc R U . . .
C26 C 0.6238(3) 0.4806(3) 0.6018(2) 0.0328(13) Uani 1 1 d . . . . .
H26A H 0.691586 0.481378 0.620781 0.049 Uiso 1 1 calc R U . . .
H26B H 0.622012 0.436330 0.567551 0.049 Uiso 1 1 calc R U . . .
H26C H 0.573721 0.464226 0.634063 0.049 Uiso 1 1 calc R U . . .
C27 C 0.6044(4) 0.6471(3) 0.6258(2) 0.0350(12) Uani 1 1 d . . . . .
H27A H 0.674285 0.652891 0.640980 0.053 Uiso 1 1 calc R U . . .
H27B H 0.559879 0.631592 0.661218 0.053 Uiso 1 1 calc R U . . .
H27C H 0.582427 0.704230 0.607240 0.053 Uiso 1 1 calc R U . . .
C28 C 0.3269(3) 0.5358(3) 0.41666(18) 0.0159(10) Uani 1 1 d . . . . .
H28 H 0.376607 0.544552 0.381543 0.019 Uiso 1 1 calc R U . . .
C29 C 0.2931(4) 0.4373(3) 0.41624(19) 0.0257(11) Uani 1 1 d . . . . .
H29A H 0.259761 0.423651 0.375989 0.039 Uiso 1 1 calc R U . . .
H29B H 0.245440 0.426868 0.451008 0.039 Uiso 1 1 calc R U . . .
H29C H 0.352353 0.398255 0.421459 0.039 Uiso 1 1 calc R U . . .
C30 C 0.2394(3) 0.6002(3) 0.4064(2) 0.0242(11) Uani 1 1 d . . . . .
H30A H 0.211828 0.591702 0.363789 0.036 Uiso 1 1 calc R U . . .
H30B H 0.263446 0.662231 0.410967 0.036 Uiso 1 1 calc R U . . .
H30C H 0.186284 0.588361 0.437639 0.036 Uiso 1 1 calc R U . . .
Mo1 Mo 0.59022(3) 0.21973(2) 0.43265(2) 0.01303(9) Uani 1 1 d . . . . .
C31 C 0.7463(3) 0.2197(3) 0.43958(18) 0.0176(9) Uani 1 1 d . . . . .
C32 C 0.5931(3) 0.2064(2) 0.33644(19) 0.0171(8) Uani 1 1 d . . . . .
C33 C 0.5924(3) 0.0881(2) 0.43800(18) 0.0150(8) Uani 1 1 d . . . . .
C34 C 0.4349(3) 0.2148(3) 0.42375(18) 0.0169(9) Uani 1 1 d . . . . .
C35 C 0.5793(3) 0.2245(3) 0.52997(18) 0.0183(9) Uani 1 1 d . . . . .
O1 O 0.8322(2) 0.2139(2) 0.44394(13) 0.0280(7) Uani 1 1 d . . . . .
O2 O 0.5900(3) 0.19315(17) 0.28339(13) 0.0264(7) Uani 1 1 d . . . . .
O3 O 0.5955(2) 0.00981(15) 0.44049(13) 0.0205(6) Uani 1 1 d . . . . .
O4 O 0.3498(2) 0.20669(18) 0.41656(13) 0.0236(7) Uani 1 1 d . . . . .
O5 O 0.5727(2) 0.2229(2) 0.58348(13) 0.0306(7) Uani 1 1 d . . . . .
C1_1 C 0.2660(4) 0.4743(3) 0.7136(2) 0.0239(11) Uani 1 1 d . . . . .
H1_1 H 0.197931 0.472937 0.698995 0.029 Uiso 1 1 calc R U . . .
C2_1 C 0.3294(4) 0.4018(3) 0.7031(2) 0.0282(11) Uani 1 1 d . . . . .
H2_1 H 0.304691 0.350501 0.681243 0.034 Uiso 1 1 calc R U . . .
C3_1 C 0.4277(3) 0.4034(3) 0.7241(2) 0.0266(11) Uani 1 1 d . . . . .
H3_1 H 0.470492 0.353022 0.716975 0.032 Uiso 1 1 calc R U . . .
C4_1 C 0.4651(3) 0.4781(3) 0.7558(2) 0.0252(11) Uani 1 1 d . . . . .
H4_1 H 0.533298 0.479330 0.770180 0.030 Uiso 1 1 calc R U . . .
C5_1 C 0.4016(4) 0.5511(3) 0.76632(18) 0.0233(10) Uani 1 1 d . . . . .
H5_1 H 0.426345 0.602751 0.787771 0.028 Uiso 1 1 calc R U . . .
C6_1 C 0.3019(3) 0.5486(3) 0.74544(19) 0.0199(10) Uani 1 1 d . . . . .
H6_1 H 0.258316 0.598264 0.753089 0.024 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.382(5) . ?
C1 B1 1.468(5) . ?
C1 C4 1.540(5) . ?
N1 C9 1.437(4) . ?
N1 C2 1.491(4) . ?
C2 C6 1.525(5) . ?
C2 C5 1.528(5) . ?
C2 C3 1.531(5) . ?
C3 C4 1.538(5) . ?
C3 H3A 0.9900 . ?
C3 H3AB 0.9900 . ?
C4 C8 1.526(6) . ?
C4 C7 1.536(5) . ?
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 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.405(5) . ?
C9 C14 1.407(5) . ?
C10 C11 1.399(5) . ?
C10 C15 1.527(6) . ?
C11 C12 1.382(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.378(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(5) . ?
C13 H13 0.9500 . ?
C14 C18 1.519(6) . ?
C15 C16 1.531(5) . ?
C15 C17 1.536(5) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.533(5) . ?
C18 C19 1.547(5) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
B1 C21 1.544(5) . ?
B1 C22 1.573(6) . ?
C21 N2 1.157(4) . ?
N2 Mo1 2.200(3) . ?
C22 N3 1.354(5) . ?
C22 N4 1.357(5) . ?
N3 C23 1.385(5) . ?
N3 C25 1.479(5) . ?
C23 C24 1.337(6) . ?
C23 H23 0.9500 . ?
C24 N4 1.380(5) . ?
C24 H24 0.9500 . ?
N4 C28 1.487(5) . ?
C25 C26 1.516(5) . ?
C25 C27 1.530(5) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.515(5) . ?
C28 C29 1.532(5) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
Mo1 C33 1.961(3) . ?
Mo1 C32 2.047(4) . ?
Mo1 C34 2.058(4) . ?
Mo1 C31 2.063(4) . ?
Mo1 C35 2.067(4) . ?
C31 O1 1.140(4) . ?
C32 O2 1.141(4) . ?
C33 O3 1.166(4) . ?
C34 O4 1.140(4) . ?
C35 O5 1.137(4) . ?
C1_1 C6_1 1.377(6) . ?
C1_1 C2_1 1.383(6) . ?
C1_1 H1_1 0.9500 . ?
C2_1 C3_1 1.371(6) . ?
C2_1 H2_1 0.9500 . ?
C3_1 C4_1 1.389(6) . ?
C3_1 H3_1 0.9500 . ?
C4_1 C5_1 1.389(6) . ?
C4_1 H4_1 0.9500 . ?
C5_1 C6_1 1.387(6) . ?
C5_1 H5_1 0.9500 . ?
C6_1 H6_1 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 B1 127.4(3) . . ?
N1 C1 C4 106.8(3) . . ?
B1 C1 C4 125.8(3) . . ?
C1 N1 C9 121.6(3) . . ?
C1 N1 C2 116.1(3) . . ?
C9 N1 C2 122.3(3) . . ?
N1 C2 C6 112.0(3) . . ?
N1 C2 C5 112.2(3) . . ?
C6 C2 C5 107.3(3) . . ?
N1 C2 C3 100.5(3) . . ?
C6 C2 C3 111.7(3) . . ?
C5 C2 C3 113.1(3) . . ?
C2 C3 C4 108.3(3) . . ?
C2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
C2 C3 H3AB 110.0 . . ?
C4 C3 H3AB 110.0 . . ?
H3A C3 H3AB 108.4 . . ?
C8 C4 C7 108.5(3) . . ?
C8 C4 C3 109.3(3) . . ?
C7 C4 C3 111.2(3) . . ?
C8 C4 C1 113.9(3) . . ?
C7 C4 C1 110.9(3) . . ?
C3 C4 C1 103.1(3) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 121.0(3) . . ?
C10 C9 N1 119.7(3) . . ?
C14 C9 N1 119.2(3) . . ?
C11 C10 C9 118.4(4) . . ?
C11 C10 C15 117.6(4) . . ?
C9 C10 C15 123.9(3) . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C13 C12 C11 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 121.6(4) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C13 C14 C9 117.9(4) . . ?
C13 C14 C18 119.0(3) . . ?
C9 C14 C18 123.0(3) . . ?
C10 C15 C16 110.7(3) . . ?
C10 C15 C17 113.4(4) . . ?
C16 C15 C17 108.7(4) . . ?
C10 C15 H15 108.0 . . ?
C16 C15 H15 108.0 . . ?
C17 C15 H15 108.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C20 113.2(4) . . ?
C14 C18 C19 110.5(3) . . ?
C20 C18 C19 108.7(3) . . ?
C14 C18 H18 108.1 . . ?
C20 C18 H18 108.1 . . ?
C19 C18 H18 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C1 B1 C21 126.3(4) . . ?
C1 B1 C22 125.8(3) . . ?
C21 B1 C22 107.9(3) . . ?
N2 C21 B1 170.5(4) . . ?
C21 N2 Mo1 177.1(3) . . ?
N3 C22 N4 104.7(3) . . ?
N3 C22 B1 127.0(4) . . ?
N4 C22 B1 127.7(4) . . ?
C22 N3 C23 110.6(3) . . ?
C22 N3 C25 124.0(3) . . ?
C23 N3 C25 125.0(3) . . ?
C24 C23 N3 107.0(3) . . ?
C24 C23 H23 126.5 . . ?
N3 C23 H23 126.5 . . ?
C23 C24 N4 107.0(4) . . ?
C23 C24 H24 126.5 . . ?
N4 C24 H24 126.5 . . ?
C22 N4 C24 110.7(3) . . ?
C22 N4 C28 124.1(3) . . ?
C24 N4 C28 124.9(4) . . ?
N3 C25 C26 109.6(3) . . ?
N3 C25 C27 110.2(3) . . ?
C26 C25 C27 113.0(4) . . ?
N3 C25 H25 107.9 . . ?
C26 C25 H25 107.9 . . ?
C27 C25 H25 107.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 C30 111.5(3) . . ?
N4 C28 C29 108.5(3) . . ?
C30 C28 C29 112.4(4) . . ?
N4 C28 H28 108.1 . . ?
C30 C28 H28 108.1 . . ?
C29 C28 H28 108.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C33 Mo1 C32 87.72(14) . . ?
C33 Mo1 C34 89.10(16) . . ?
C32 Mo1 C34 85.63(17) . . ?
C33 Mo1 C31 88.94(16) . . ?
C32 Mo1 C31 92.99(16) . . ?
C34 Mo1 C31 177.65(15) . . ?
C33 Mo1 C35 88.74(15) . . ?
C32 Mo1 C35 175.37(15) . . ?
C34 Mo1 C35 91.33(16) . . ?
C31 Mo1 C35 89.92(16) . . ?
C33 Mo1 N2 179.04(15) . . ?
C32 Mo1 N2 92.84(12) . . ?
C34 Mo1 N2 91.71(14) . . ?
C31 Mo1 N2 90.25(14) . . ?
C35 Mo1 N2 90.74(13) . . ?
O1 C31 Mo1 175.6(3) . . ?
O2 C32 Mo1 174.7(3) . . ?
O3 C33 Mo1 178.6(4) . . ?
O4 C34 Mo1 175.3(4) . . ?
O5 C35 Mo1 176.7(4) . . ?
C6_1 C1_1 C2_1 119.7(4) . . ?
C6_1 C1_1 H1_1 120.1 . . ?
C2_1 C1_1 H1_1 120.1 . . ?
C3_1 C2_1 C1_1 120.4(4) . . ?
C3_1 C2_1 H2_1 119.8 . . ?
C1_1 C2_1 H2_1 119.8 . . ?
C2_1 C3_1 C4_1 120.4(4) . . ?
C2_1 C3_1 H3_1 119.8 . . ?
C4_1 C3_1 H3_1 119.8 . . ?
C5_1 C4_1 C3_1 119.2(4) . . ?
C5_1 C4_1 H4_1 120.4 . . ?
C3_1 C4_1 H4_1 120.4 . . ?
C6_1 C5_1 C4_1 120.0(4) . . ?
C6_1 C5_1 H5_1 120.0 . . ?
C4_1 C5_1 H5_1 120.0 . . ?
C1_1 C6_1 C5_1 120.2(4) . . ?
C1_1 C6_1 H6_1 119.9 . . ?
C5_1 C6_1 H6_1 119.9 . . ?

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
B1 C1 N1 C9 -1.1(6) . . . . ?
C4 C1 N1 C9 176.5(3) . . . . ?
B1 C1 N1 C2 -179.7(4) . . . . ?
C4 C1 N1 C2 -2.1(4) . . . . ?
C1 N1 C2 C6 -130.7(4) . . . . ?
C9 N1 C2 C6 50.7(5) . . . . ?
C1 N1 C2 C5 108.5(4) . . . . ?
C9 N1 C2 C5 -70.1(4) . . . . ?
C1 N1 C2 C3 -12.0(4) . . . . ?
C9 N1 C2 C3 169.4(3) . . . . ?
N1 C2 C3 C4 21.2(4) . . . . ?
C6 C2 C3 C4 140.1(3) . . . . ?
C5 C2 C3 C4 -98.7(4) . . . . ?
C2 C3 C4 C8 -144.5(3) . . . . ?
C2 C3 C4 C7 95.8(4) . . . . ?
C2 C3 C4 C1 -23.0(4) . . . . ?
N1 C1 C4 C8 133.6(3) . . . . ?
B1 C1 C4 C8 -48.8(5) . . . . ?
N1 C1 C4 C7 -103.8(4) . . . . ?
B1 C1 C4 C7 73.9(5) . . . . ?
N1 C1 C4 C3 15.3(4) . . . . ?
B1 C1 C4 C3 -167.0(4) . . . . ?
C1 N1 C9 C10 -86.6(5) . . . . ?
C2 N1 C9 C10 91.9(4) . . . . ?
C1 N1 C9 C14 90.5(4) . . . . ?
C2 N1 C9 C14 -91.0(4) . . . . ?
C14 C9 C10 C11 6.2(6) . . . . ?
N1 C9 C10 C11 -176.8(3) . . . . ?
C14 C9 C10 C15 -170.5(4) . . . . ?
N1 C9 C10 C15 6.5(6) . . . . ?
C9 C10 C11 C12 -1.5(6) . . . . ?
C15 C10 C11 C12 175.4(4) . . . . ?
C10 C11 C12 C13 -3.0(6) . . . . ?
C11 C12 C13 C14 2.9(6) . . . . ?
C12 C13 C14 C9 1.6(6) . . . . ?
C12 C13 C14 C18 -174.6(4) . . . . ?
C10 C9 C14 C13 -6.2(5) . . . . ?
N1 C9 C14 C13 176.7(3) . . . . ?
C10 C9 C14 C18 169.8(4) . . . . ?
N1 C9 C14 C18 -7.3(5) . . . . ?
C11 C10 C15 C16 -62.1(5) . . . . ?
C9 C10 C15 C16 114.6(4) . . . . ?
C11 C10 C15 C17 60.3(5) . . . . ?
C9 C10 C15 C17 -123.0(4) . . . . ?
C13 C14 C18 C20 -58.0(5) . . . . ?
C9 C14 C18 C20 126.1(4) . . . . ?
C13 C14 C18 C19 64.2(5) . . . . ?
C9 C14 C18 C19 -111.8(4) . . . . ?
N1 C1 B1 C21 -2.7(7) . . . . ?
C4 C1 B1 C21 -179.9(4) . . . . ?
N1 C1 B1 C22 177.7(4) . . . . ?
C4 C1 B1 C22 0.6(7) . . . . ?
C1 B1 C22 N3 -93.2(5) . . . . ?
C21 B1 C22 N3 87.2(4) . . . . ?
C1 B1 C22 N4 96.9(5) . . . . ?
C21 B1 C22 N4 -82.7(5) . . . . ?
N4 C22 N3 C23 1.5(4) . . . . ?
B1 C22 N3 C23 -170.2(3) . . . . ?
N4 C22 N3 C25 173.6(3) . . . . ?
B1 C22 N3 C25 1.8(6) . . . . ?
C22 N3 C23 C24 -1.1(4) . . . . ?
C25 N3 C23 C24 -173.0(3) . . . . ?
N3 C23 C24 N4 0.1(4) . . . . ?
N3 C22 N4 C24 -1.5(4) . . . . ?
B1 C22 N4 C24 170.2(3) . . . . ?
N3 C22 N4 C28 -175.7(3) . . . . ?
B1 C22 N4 C28 -4.1(6) . . . . ?
C23 C24 N4 C22 0.9(4) . . . . ?
C23 C24 N4 C28 175.0(3) . . . . ?
C22 N3 C25 C26 -97.6(4) . . . . ?
C23 N3 C25 C26 73.3(5) . . . . ?
C22 N3 C25 C27 137.4(4) . . . . ?
C23 N3 C25 C27 -51.7(5) . . . . ?
C22 N4 C28 C30 -131.7(4) . . . . ?
C24 N4 C28 C30 54.8(5) . . . . ?
C22 N4 C28 C29 103.9(4) . . . . ?
C24 N4 C28 C29 -69.5(5) . . . . ?
C6_1 C1_1 C2_1 C3_1 0.0(7) . . . . ?
C1_1 C2_1 C3_1 C4_1 -0.5(7) . . . . ?
C2_1 C3_1 C4_1 C5_1 0.3(6) . . . . ?
C3_1 C4_1 C5_1 C6_1 0.3(6) . . . . ?
C2_1 C1_1 C6_1 C5_1 0.6(6) . . . . ?
C4_1 C5_1 C6_1 C1_1 -0.8(6) . . . . ?

_refine_diff_density_max         0.525
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.062



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_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_test_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2071472'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_test_a              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report
RESPONSE: Reflections affected by beamstop
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        (CAACH)(IiPr)B(CN)(SPh)
_chemical_name_common            3(CN)
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H53 B N4 S2, C6 H6'
_chemical_formula_sum            'C42 H59 B N4 S2'
_chemical_formula_weight         694.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P c'
_space_group_name_Hall           'P -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'

_cell_length_a                   10.657(7)
_cell_length_b                   16.337(11)
_cell_length_c                   11.950(9)
_cell_angle_alpha                90
_cell_angle_beta                 106.86(2)
_cell_angle_gamma                90
_cell_volume                     1991(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8062
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      26.72


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.191
_exptl_absorpt_coefficient_mu    0.168
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_T_max  0.7454
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 1.00 0.0900
1.00 0.00 -1.00 0.1100
1.00 1.00 1.00 0.0360
-1.00 -1.00 -1.00 0.1040
1.00 0.00 1.00 0.0150
-1.00 0.00 -1.00 0.1230
1.00 -1.00 -1.00 0.0740
-1.00 0.00 0.00 0.0950
-1.00 1.00 1.00 0.0950
0.00 1.00 1.00 0.0780
1.00 0.00 0.00 0.0410
1.00 -1.00 0.00 0.0160
0.00 1.00 0.00 0.0720

_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CMOS area detector (Photon II)'
_diffrn_detector_area_resol_mean 7.5
_diffrn_reflns_number            36025
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.354
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             7672
_reflns_number_gt                7217
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_max     0.964
_reflns_Friedel_fraction_full    0.964

_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       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.38A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.38A (Bruker AXS)'
_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          
;

 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.

The asymmetric unit contains one benzene molecule, which was modelled as twofold disordered
in a 56:44 ratio. The benzene rings were idealised with AFIX 66. ADPs were restrained 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)+(0.0357P)²+0.2294P] 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_abs_structure_details 
;
 Flack x determined using 3214 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         7672
_refine_ls_number_parameters     485
_refine_ls_number_restraints     182
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0740
_refine_ls_wR_factor_gt          0.0725
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.052
_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
C1_10 C 0.1530(4) 0.4878(3) 0.6036(5) 0.0439(14) Uani 0.556(5) 1 d G U P A 1
H1_10 H 0.223537 0.522728 0.601493 0.053 Uiso 0.556(5) 1 calc R U P A 1
C2_10 C 0.1464(4) 0.4557(3) 0.7095(3) 0.0400(14) Uani 0.556(5) 1 d G U P A 1
H2_10 H 0.212352 0.468765 0.779737 0.048 Uiso 0.556(5) 1 calc R U P A 1
C3_10 C 0.0432(5) 0.4046(3) 0.7125(2) 0.0314(13) Uani 0.556(5) 1 d G U P A 1
H3_10 H 0.038636 0.382670 0.784888 0.038 Uiso 0.556(5) 1 calc R U P A 1
C4_10 C -0.0534(4) 0.3855(2) 0.6097(4) 0.0277(12) Uani 0.556(5) 1 d G U P A 1
H4_10 H -0.123894 0.350537 0.611797 0.033 Uiso 0.556(5) 1 calc R U P A 1
C5_10 C -0.0467(4) 0.4175(3) 0.5038(3) 0.0267(12) Uani 0.556(5) 1 d G U P A 1
H5_10 H -0.112710 0.404498 0.433552 0.032 Uiso 0.556(5) 1 calc R U P A 1
C6_10 C 0.0565(5) 0.4687(3) 0.5008(3) 0.0362(13) Uani 0.556(5) 1 d G U P A 1
H6_10 H 0.061004 0.490594 0.428398 0.043 Uiso 0.556(5) 1 calc R U P A 1
C1_11 C 0.0109(6) 0.4575(4) 0.4871(3) 0.0377(16) Uani 0.444(5) 1 d G U P A 2
H1_11 H -0.032529 0.468019 0.406972 0.045 Uiso 0.444(5) 1 calc R U P A 2
C2_11 C -0.0496(4) 0.4098(4) 0.5527(6) 0.0378(16) Uani 0.444(5) 1 d G U P A 2
H2_11 H -0.134422 0.387771 0.517528 0.045 Uiso 0.444(5) 1 calc R U P A 2
C3_11 C 0.0139(6) 0.3944(3) 0.6699(6) 0.0367(14) Uani 0.444(5) 1 d G U P A 2
H3_11 H -0.027502 0.361848 0.714780 0.044 Uiso 0.444(5) 1 calc R U P A 2
C4_11 C 0.1379(6) 0.4267(4) 0.7214(3) 0.0322(15) Uani 0.444(5) 1 d G U P A 2
H4_11 H 0.181310 0.416173 0.801478 0.039 Uiso 0.444(5) 1 calc R U P A 2
C5_11 C 0.1984(5) 0.4744(3) 0.6557(5) 0.0330(15) Uani 0.444(5) 1 d G U P A 2
H5_11 H 0.283205 0.496421 0.690924 0.040 Uiso 0.444(5) 1 calc R U P A 2
C6_11 C 0.1349(6) 0.4898(3) 0.5386(5) 0.0363(16) Uani 0.444(5) 1 d G U P A 2
H6_11 H 0.176287 0.522345 0.493672 0.044 Uiso 0.444(5) 1 calc R U P A 2
C1_1 C 0.6429(2) 0.72743(15) 0.4903(2) 0.0137(5) Uani 1 1 d . . . . .
H1_1 H 0.725319 0.760532 0.508317 0.016 Uiso 1 1 calc R U . . .
N1_1 N 0.6400(2) 0.68666(13) 0.60257(17) 0.0148(4) Uani 1 1 d . . . . .
C2_1 C 0.6478(3) 0.59537(15) 0.5924(2) 0.0178(5) Uani 1 1 d . . . . .
C3_1 C 0.7062(2) 0.58431(16) 0.4906(2) 0.0186(5) Uani 1 1 d . . . . .
H3A_1 H 0.676988 0.531708 0.450320 0.022 Uiso 1 1 calc R U . . .
H3AB_1 H 0.803171 0.584200 0.519566 0.022 Uiso 1 1 calc R U . . .
C4_1 C 0.6584(2) 0.65592(15) 0.4064(2) 0.0168(5) Uani 1 1 d . . . . .
C5_1 C 0.5106(3) 0.55646(17) 0.5667(2) 0.0233(6) Uani 1 1 d . . . . .
H5A_1 H 0.515307 0.498671 0.546254 0.035 Uiso 1 1 calc R U . . .
H5B_1 H 0.449576 0.585230 0.501254 0.035 Uiso 1 1 calc R U . . .
H5C_1 H 0.479821 0.560742 0.636152 0.035 Uiso 1 1 calc R U . . .
C6_1 C 0.7364(3) 0.55495(17) 0.7024(2) 0.0232(6) Uani 1 1 d . . . . .
H6A_1 H 0.739436 0.495802 0.689823 0.035 Uiso 1 1 calc R U . . .
H6B_1 H 0.701567 0.565452 0.768474 0.035 Uiso 1 1 calc R U . . .
H6C_1 H 0.825089 0.577690 0.719552 0.035 Uiso 1 1 calc R U . . .
C7_1 C 0.5325(3) 0.63205(16) 0.3096(2) 0.0206(6) Uani 1 1 d . . . . .
H7A_1 H 0.548939 0.582529 0.269760 0.031 Uiso 1 1 calc R U . . .
H7B_1 H 0.507211 0.676858 0.253006 0.031 Uiso 1 1 calc R U . . .
H7C_1 H 0.461552 0.621622 0.344701 0.031 Uiso 1 1 calc R U . . .
C8_1 C 0.7608(3) 0.67739(17) 0.3440(2) 0.0225(6) Uani 1 1 d . . . . .
H8A_1 H 0.781390 0.628519 0.305130 0.034 Uiso 1 1 calc R U . . .
H8B_1 H 0.840667 0.697316 0.401266 0.034 Uiso 1 1 calc R U . . .
H8C_1 H 0.726002 0.720092 0.285649 0.034 Uiso 1 1 calc R U . . .
C9_1 C 0.7021(2) 0.72451(15) 0.7134(2) 0.0150(5) Uani 1 1 d . . . . .
C10_1 C 0.8353(2) 0.74901(15) 0.7495(2) 0.0172(5) Uani 1 1 d . . . . .
C11_1 C 0.8874(3) 0.78577(17) 0.8586(2) 0.0209(6) Uani 1 1 d . . . . .
H11_1 H 0.975643 0.804304 0.880096 0.025 Uiso 1 1 calc R U . . .
C12_1 C 0.8148(3) 0.79603(17) 0.9360(2) 0.0223(6) Uani 1 1 d . . . . .
H12_1 H 0.852445 0.820523 1.010311 0.027 Uiso 1 1 calc R U . . .
C13_1 C 0.6863(3) 0.76997(16) 0.9033(2) 0.0201(6) Uani 1 1 d . . . . .
H13_1 H 0.635966 0.775851 0.956672 0.024 Uiso 1 1 calc R U . . .
C14_1 C 0.6282(2) 0.73513(16) 0.7938(2) 0.0169(5) Uani 1 1 d . . . . .
C15_1 C 0.9306(2) 0.73570(16) 0.6771(2) 0.0183(5) Uani 1 1 d . . . . .
H15_1 H 0.883937 0.704236 0.605364 0.022 Uiso 1 1 calc R U . . .
C16_1 C 0.9727(3) 0.81834(18) 0.6387(2) 0.0246(6) Uani 1 1 d . . . . .
H16A_1 H 1.017629 0.809339 0.578896 0.037 Uiso 1 1 calc R U . . .
H16B_1 H 1.032280 0.845900 0.706299 0.037 Uiso 1 1 calc R U . . .
H16C_1 H 0.895110 0.852572 0.606423 0.037 Uiso 1 1 calc R U . . .
C17_1 C 1.0509(3) 0.68599(19) 0.7448(2) 0.0247(6) Uani 1 1 d . . . . .
H17A_1 H 1.104709 0.673144 0.693129 0.037 Uiso 1 1 calc R U . . .
H17B_1 H 1.022031 0.635023 0.772931 0.037 Uiso 1 1 calc R U . . .
H17C_1 H 1.102662 0.718041 0.811613 0.037 Uiso 1 1 calc R U . . .
C18_1 C 0.4841(2) 0.71211(17) 0.7651(2) 0.0198(6) Uani 1 1 d . . . . .
H18_1 H 0.452707 0.695645 0.680981 0.024 Uiso 1 1 calc R U . . .
C19_1 C 0.4621(3) 0.63991(19) 0.8398(3) 0.0266(6) Uani 1 1 d . . . . .
H19A_1 H 0.368877 0.625439 0.816632 0.040 Uiso 1 1 calc R U . . .
H19B_1 H 0.489930 0.655542 0.922561 0.040 Uiso 1 1 calc R U . . .
H19C_1 H 0.513572 0.592720 0.827924 0.040 Uiso 1 1 calc R U . . .
C20_1 C 0.4030(3) 0.78553(18) 0.7831(2) 0.0235(6) Uani 1 1 d . . . . .
H20A_1 H 0.309784 0.774778 0.745434 0.035 Uiso 1 1 calc R U . . .
H20B_1 H 0.429844 0.834428 0.748478 0.035 Uiso 1 1 calc R U . . .
H20C_1 H 0.417310 0.794428 0.867013 0.035 Uiso 1 1 calc R U . . .
B1_1 B 0.5205(3) 0.79104(17) 0.4380(2) 0.0141(6) Uani 1 1 d . . . . .
N3_1 N 0.5951(2) 0.88173(13) 0.27956(17) 0.0163(5) Uani 1 1 d . . . . .
C21_1 C 0.2965(3) 0.73116(17) 0.4582(2) 0.0213(6) Uani 1 1 d . . . . .
S1_1 S 0.16382(8) 0.69960(6) 0.48133(8) 0.0452(2) Uani 1 1 d . . . . .
C22_1 C 0.5076(2) 0.83019(15) 0.3068(2) 0.0140(5) Uani 1 1 d . . . . .
N2_1 N 0.3913(2) 0.75264(13) 0.43858(17) 0.0155(4) Uani 1 1 d . . . . .
C23_1 C 0.5434(3) 0.91293(17) 0.1688(2) 0.0201(6) Uani 1 1 d . . . . .
H23_1 H 0.584721 0.950764 0.130486 0.024 Uiso 1 1 calc R U . . .
C24_1 C 0.4237(3) 0.88003(16) 0.1247(2) 0.0202(6) Uani 1 1 d . . . . .
H24_1 H 0.364524 0.890329 0.049601 0.024 Uiso 1 1 calc R U . . .
N4_1 N 0.4027(2) 0.82851(13) 0.20888(17) 0.0156(4) Uani 1 1 d . . . . .
C25_1 C 0.7289(2) 0.90491(17) 0.3516(2) 0.0201(6) Uani 1 1 d . . . . .
H25_1 H 0.752509 0.870687 0.424089 0.024 Uiso 1 1 calc R U . . .
C26_1 C 0.8270(3) 0.88738(19) 0.2837(3) 0.0283(6) Uani 1 1 d . . . . .
H26A_1 H 0.916370 0.891228 0.336486 0.042 Uiso 1 1 calc R U . . .
H26B_1 H 0.815599 0.927465 0.220508 0.042 Uiso 1 1 calc R U . . .
H26C_1 H 0.812093 0.832161 0.250407 0.042 Uiso 1 1 calc R U . . .
C27_1 C 0.7343(3) 0.99449(18) 0.3871(3) 0.0278(6) Uani 1 1 d . . . . .
H27A_1 H 0.823577 1.008402 0.433668 0.042 Uiso 1 1 calc R U . . .
H27B_1 H 0.673520 1.004005 0.433538 0.042 Uiso 1 1 calc R U . . .
H27C_1 H 0.709116 1.028814 0.316805 0.042 Uiso 1 1 calc R U . . .
C28_1 C 0.2802(2) 0.77815(17) 0.1841(2) 0.0175(5) Uani 1 1 d . . . . .
H28_1 H 0.294742 0.733491 0.243698 0.021 Uiso 1 1 calc R U . . .
C29_1 C 0.1670(3) 0.83056(18) 0.1950(2) 0.0243(6) Uani 1 1 d . . . . .
H29A_1 H 0.187993 0.853381 0.274144 0.036 Uiso 1 1 calc R U . . .
H29B_1 H 0.087669 0.796933 0.180014 0.036 Uiso 1 1 calc R U . . .
H29C_1 H 0.152073 0.875259 0.137965 0.036 Uiso 1 1 calc R U . . .
C30_1 C 0.2527(3) 0.73886(18) 0.0635(2) 0.0238(6) Uani 1 1 d . . . . .
H30A_1 H 0.329771 0.707642 0.059312 0.036 Uiso 1 1 calc R U . . .
H30B_1 H 0.233602 0.781658 0.003470 0.036 Uiso 1 1 calc R U . . .
H30C_1 H 0.177241 0.702052 0.050342 0.036 Uiso 1 1 calc R U . . .
S2_1 S 0.54074(6) 0.88613(4) 0.54276(5) 0.01605(13) Uani 1 1 d . . . . .
C31_1 C 0.3885(2) 0.93731(16) 0.4783(2) 0.0170(5) Uani 1 1 d . . . . .
C32_1 C 0.2843(2) 0.92480(17) 0.5247(2) 0.0194(5) Uani 1 1 d . . . . .
H32_1 H 0.294303 0.887834 0.588110 0.023 Uiso 1 1 calc R U . . .
C33_1 C 0.1661(3) 0.96550(17) 0.4799(2) 0.0217(6) Uani 1 1 d . . . . .
H33_1 H 0.096448 0.956655 0.513269 0.026 Uiso 1 1 calc R U . . .
C34_1 C 0.1488(3) 1.01910(17) 0.3864(2) 0.0211(6) Uani 1 1 d . . . . .
H34_1 H 0.067804 1.046881 0.355633 0.025 Uiso 1 1 calc R U . . .
C35_1 C 0.2511(3) 1.03159(16) 0.3385(2) 0.0202(5) Uani 1 1 d . . . . .
H35_1 H 0.239968 1.067902 0.274299 0.024 Uiso 1 1 calc R U . . .
C36_1 C 0.3706(3) 0.99107(16) 0.3842(2) 0.0184(5) Uani 1 1 d . . . . .
H36_1 H 0.440275 1.000213 0.350947 0.022 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1_10 C2_10 1.3900 . ?
C1_10 C6_10 1.3900 . ?
C1_10 H1_10 0.9500 . ?
C2_10 C3_10 1.3900 . ?
C2_10 H2_10 0.9500 . ?
C3_10 C4_10 1.3900 . ?
C3_10 H3_10 0.9500 . ?
C4_10 C5_10 1.3900 . ?
C4_10 H4_10 0.9500 . ?
C5_10 C6_10 1.3900 . ?
C5_10 H5_10 0.9500 . ?
C6_10 H6_10 0.9500 . ?
C1_11 C2_11 1.3900 . ?
C1_11 C6_11 1.3900 . ?
C1_11 H1_11 0.9500 . ?
C2_11 C3_11 1.3900 . ?
C2_11 H2_11 0.9500 . ?
C3_11 C4_11 1.3900 . ?
C3_11 H3_11 0.9500 . ?
C4_11 C5_11 1.3900 . ?
C4_11 H4_11 0.9500 . ?
C5_11 C6_11 1.3900 . ?
C5_11 H5_11 0.9500 . ?
C6_11 H6_11 0.9500 . ?
C1_1 N1_1 1.507(3) . ?
C1_1 C4_1 1.578(3) . ?
C1_1 B1_1 1.643(4) . ?
C1_1 H1_1 1.0000 . ?
N1_1 C9_1 1.438(3) . ?
N1_1 C2_1 1.501(3) . ?
C2_1 C6_1 1.528(4) . ?
C2_1 C3_1 1.529(4) . ?
C2_1 C5_1 1.541(4) . ?
C3_1 C4_1 1.531(4) . ?
C3_1 H3A_1 0.9900 . ?
C3_1 H3AB_1 0.9900 . ?
C4_1 C8_1 1.531(3) . ?
C4_1 C7_1 1.546(4) . ?
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 . ?
C7_1 H7A_1 0.9800 . ?
C7_1 H7B_1 0.9800 . ?
C7_1 H7C_1 0.9800 . ?
C8_1 H8A_1 0.9800 . ?
C8_1 H8B_1 0.9800 . ?
C8_1 H8C_1 0.9800 . ?
C9_1 C10_1 1.416(4) . ?
C9_1 C14_1 1.419(3) . ?
C10_1 C11_1 1.396(4) . ?
C10_1 C15_1 1.528(4) . ?
C11_1 C12_1 1.378(4) . ?
C11_1 H11_1 0.9500 . ?
C12_1 C13_1 1.377(4) . ?
C12_1 H12_1 0.9500 . ?
C13_1 C14_1 1.396(4) . ?
C13_1 H13_1 0.9500 . ?
C14_1 C18_1 1.521(4) . ?
C15_1 C16_1 1.534(4) . ?
C15_1 C17_1 1.535(4) . ?
C15_1 H15_1 1.0000 . ?
C16_1 H16A_1 0.9800 . ?
C16_1 H16B_1 0.9800 . ?
C16_1 H16C_1 0.9800 . ?
C17_1 H17A_1 0.9800 . ?
C17_1 H17B_1 0.9800 . ?
C17_1 H17C_1 0.9800 . ?
C18_1 C20_1 1.530(4) . ?
C18_1 C19_1 1.538(4) . ?
C18_1 H18_1 1.0000 . ?
C19_1 H19A_1 0.9800 . ?
C19_1 H19B_1 0.9800 . ?
C19_1 H19C_1 0.9800 . ?
C20_1 H20A_1 0.9800 . ?
C20_1 H20B_1 0.9800 . ?
C20_1 H20C_1 0.9800 . ?
B1_1 N2_1 1.515(3) . ?
B1_1 C22_1 1.661(4) . ?
B1_1 S2_1 1.968(3) . ?
N3_1 C22_1 1.364(3) . ?
N3_1 C23_1 1.376(3) . ?
N3_1 C25_1 1.485(3) . ?
C21_1 N2_1 1.156(3) . ?
C21_1 S1_1 1.603(3) . ?
C22_1 N4_1 1.365(3) . ?
C23_1 C24_1 1.343(4) . ?
C23_1 H23_1 0.9500 . ?
C24_1 N4_1 1.379(3) . ?
C24_1 H24_1 0.9500 . ?
N4_1 C28_1 1.498(3) . ?
C25_1 C27_1 1.520(4) . ?
C25_1 C26_1 1.525(4) . ?
C25_1 H25_1 1.0000 . ?
C26_1 H26A_1 0.9800 . ?
C26_1 H26B_1 0.9800 . ?
C26_1 H26C_1 0.9800 . ?
C27_1 H27A_1 0.9800 . ?
C27_1 H27B_1 0.9800 . ?
C27_1 H27C_1 0.9800 . ?
C28_1 C29_1 1.516(4) . ?
C28_1 C30_1 1.526(4) . ?
C28_1 H28_1 1.0000 . ?
C29_1 H29A_1 0.9800 . ?
C29_1 H29B_1 0.9800 . ?
C29_1 H29C_1 0.9800 . ?
C30_1 H30A_1 0.9800 . ?
C30_1 H30B_1 0.9800 . ?
C30_1 H30C_1 0.9800 . ?
S2_1 C31_1 1.789(3) . ?
C31_1 C32_1 1.393(4) . ?
C31_1 C36_1 1.395(4) . ?
C32_1 C33_1 1.387(4) . ?
C32_1 H32_1 0.9500 . ?
C33_1 C34_1 1.389(4) . ?
C33_1 H33_1 0.9500 . ?
C34_1 C35_1 1.385(4) . ?
C34_1 H34_1 0.9500 . ?
C35_1 C36_1 1.399(4) . ?
C35_1 H35_1 0.9500 . ?
C36_1 H36_1 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2_10 C1_10 C6_10 120.0 . . ?
C2_10 C1_10 H1_10 120.0 . . ?
C6_10 C1_10 H1_10 120.0 . . ?
C3_10 C2_10 C1_10 120.0 . . ?
C3_10 C2_10 H2_10 120.0 . . ?
C1_10 C2_10 H2_10 120.0 . . ?
C2_10 C3_10 C4_10 120.0 . . ?
C2_10 C3_10 H3_10 120.0 . . ?
C4_10 C3_10 H3_10 120.0 . . ?
C5_10 C4_10 C3_10 120.0 . . ?
C5_10 C4_10 H4_10 120.0 . . ?
C3_10 C4_10 H4_10 120.0 . . ?
C4_10 C5_10 C6_10 120.0 . . ?
C4_10 C5_10 H5_10 120.0 . . ?
C6_10 C5_10 H5_10 120.0 . . ?
C5_10 C6_10 C1_10 120.0 . . ?
C5_10 C6_10 H6_10 120.0 . . ?
C1_10 C6_10 H6_10 120.0 . . ?
C2_11 C1_11 C6_11 120.0 . . ?
C2_11 C1_11 H1_11 120.0 . . ?
C6_11 C1_11 H1_11 120.0 . . ?
C1_11 C2_11 C3_11 120.0 . . ?
C1_11 C2_11 H2_11 120.0 . . ?
C3_11 C2_11 H2_11 120.0 . . ?
C2_11 C3_11 C4_11 120.0 . . ?
C2_11 C3_11 H3_11 120.0 . . ?
C4_11 C3_11 H3_11 120.0 . . ?
C5_11 C4_11 C3_11 120.0 . . ?
C5_11 C4_11 H4_11 120.0 . . ?
C3_11 C4_11 H4_11 120.0 . . ?
C6_11 C5_11 C4_11 120.0 . . ?
C6_11 C5_11 H5_11 120.0 . . ?
C4_11 C5_11 H5_11 120.0 . . ?
C5_11 C6_11 C1_11 120.0 . . ?
C5_11 C6_11 H6_11 120.0 . . ?
C1_11 C6_11 H6_11 120.0 . . ?
N1_1 C1_1 C4_1 105.7(2) . . ?
N1_1 C1_1 B1_1 113.52(19) . . ?
C4_1 C1_1 B1_1 116.4(2) . . ?
N1_1 C1_1 H1_1 106.9 . . ?
C4_1 C1_1 H1_1 106.9 . . ?
B1_1 C1_1 H1_1 106.9 . . ?
C9_1 N1_1 C2_1 118.7(2) . . ?
C9_1 N1_1 C1_1 120.5(2) . . ?
C2_1 N1_1 C1_1 110.56(19) . . ?
N1_1 C2_1 C6_1 113.2(2) . . ?
N1_1 C2_1 C3_1 103.1(2) . . ?
C6_1 C2_1 C3_1 109.9(2) . . ?
N1_1 C2_1 C5_1 110.7(2) . . ?
C6_1 C2_1 C5_1 107.9(2) . . ?
C3_1 C2_1 C5_1 112.0(2) . . ?
C2_1 C3_1 C4_1 107.3(2) . . ?
C2_1 C3_1 H3A_1 110.3 . . ?
C4_1 C3_1 H3A_1 110.3 . . ?
C2_1 C3_1 H3AB_1 110.3 . . ?
C4_1 C3_1 H3AB_1 110.3 . . ?
H3A_1 C3_1 H3AB_1 108.5 . . ?
C3_1 C4_1 C8_1 110.3(2) . . ?
C3_1 C4_1 C7_1 110.5(2) . . ?
C8_1 C4_1 C7_1 106.3(2) . . ?
C3_1 C4_1 C1_1 103.0(2) . . ?
C8_1 C4_1 C1_1 111.1(2) . . ?
C7_1 C4_1 C1_1 115.7(2) . . ?
C2_1 C5_1 H5A_1 109.5 . . ?
C2_1 C5_1 H5B_1 109.5 . . ?
H5A_1 C5_1 H5B_1 109.5 . . ?
C2_1 C5_1 H5C_1 109.5 . . ?
H5A_1 C5_1 H5C_1 109.5 . . ?
H5B_1 C5_1 H5C_1 109.5 . . ?
C2_1 C6_1 H6A_1 109.5 . . ?
C2_1 C6_1 H6B_1 109.5 . . ?
H6A_1 C6_1 H6B_1 109.5 . . ?
C2_1 C6_1 H6C_1 109.5 . . ?
H6A_1 C6_1 H6C_1 109.5 . . ?
H6B_1 C6_1 H6C_1 109.5 . . ?
C4_1 C7_1 H7A_1 109.5 . . ?
C4_1 C7_1 H7B_1 109.5 . . ?
H7A_1 C7_1 H7B_1 109.5 . . ?
C4_1 C7_1 H7C_1 109.5 . . ?
H7A_1 C7_1 H7C_1 109.5 . . ?
H7B_1 C7_1 H7C_1 109.5 . . ?
C4_1 C8_1 H8A_1 109.5 . . ?
C4_1 C8_1 H8B_1 109.5 . . ?
H8A_1 C8_1 H8B_1 109.5 . . ?
C4_1 C8_1 H8C_1 109.5 . . ?
H8A_1 C8_1 H8C_1 109.5 . . ?
H8B_1 C8_1 H8C_1 109.5 . . ?
C10_1 C9_1 C14_1 117.7(2) . . ?
C10_1 C9_1 N1_1 123.7(2) . . ?
C14_1 C9_1 N1_1 118.6(2) . . ?
C11_1 C10_1 C9_1 119.8(2) . . ?
C11_1 C10_1 C15_1 116.1(2) . . ?
C9_1 C10_1 C15_1 124.0(2) . . ?
C12_1 C11_1 C10_1 122.1(3) . . ?
C12_1 C11_1 H11_1 119.0 . . ?
C10_1 C11_1 H11_1 119.0 . . ?
C13_1 C12_1 C11_1 118.5(2) . . ?
C13_1 C12_1 H12_1 120.8 . . ?
C11_1 C12_1 H12_1 120.8 . . ?
C12_1 C13_1 C14_1 121.8(2) . . ?
C12_1 C13_1 H13_1 119.1 . . ?
C14_1 C13_1 H13_1 119.1 . . ?
C13_1 C14_1 C9_1 120.1(2) . . ?
C13_1 C14_1 C18_1 117.2(2) . . ?
C9_1 C14_1 C18_1 122.7(2) . . ?
C10_1 C15_1 C16_1 110.1(2) . . ?
C10_1 C15_1 C17_1 111.6(2) . . ?
C16_1 C15_1 C17_1 110.6(2) . . ?
C10_1 C15_1 H15_1 108.1 . . ?
C16_1 C15_1 H15_1 108.1 . . ?
C17_1 C15_1 H15_1 108.1 . . ?
C15_1 C16_1 H16A_1 109.5 . . ?
C15_1 C16_1 H16B_1 109.5 . . ?
H16A_1 C16_1 H16B_1 109.5 . . ?
C15_1 C16_1 H16C_1 109.5 . . ?
H16A_1 C16_1 H16C_1 109.5 . . ?
H16B_1 C16_1 H16C_1 109.5 . . ?
C15_1 C17_1 H17A_1 109.5 . . ?
C15_1 C17_1 H17B_1 109.5 . . ?
H17A_1 C17_1 H17B_1 109.5 . . ?
C15_1 C17_1 H17C_1 109.5 . . ?
H17A_1 C17_1 H17C_1 109.5 . . ?
H17B_1 C17_1 H17C_1 109.5 . . ?
C14_1 C18_1 C20_1 110.4(2) . . ?
C14_1 C18_1 C19_1 111.9(2) . . ?
C20_1 C18_1 C19_1 109.4(2) . . ?
C14_1 C18_1 H18_1 108.3 . . ?
C20_1 C18_1 H18_1 108.3 . . ?
C19_1 C18_1 H18_1 108.3 . . ?
C18_1 C19_1 H19A_1 109.5 . . ?
C18_1 C19_1 H19B_1 109.5 . . ?
H19A_1 C19_1 H19B_1 109.5 . . ?
C18_1 C19_1 H19C_1 109.5 . . ?
H19A_1 C19_1 H19C_1 109.5 . . ?
H19B_1 C19_1 H19C_1 109.5 . . ?
C18_1 C20_1 H20A_1 109.5 . . ?
C18_1 C20_1 H20B_1 109.5 . . ?
H20A_1 C20_1 H20B_1 109.5 . . ?
C18_1 C20_1 H20C_1 109.5 . . ?
H20A_1 C20_1 H20C_1 109.5 . . ?
H20B_1 C20_1 H20C_1 109.5 . . ?
N2_1 B1_1 C1_1 111.0(2) . . ?
N2_1 B1_1 C22_1 109.7(2) . . ?
C1_1 B1_1 C22_1 116.19(19) . . ?
N2_1 B1_1 S2_1 104.83(17) . . ?
C1_1 B1_1 S2_1 109.20(17) . . ?
C22_1 B1_1 S2_1 105.09(18) . . ?
C22_1 N3_1 C23_1 110.4(2) . . ?
C22_1 N3_1 C25_1 128.8(2) . . ?
C23_1 N3_1 C25_1 120.8(2) . . ?
N2_1 C21_1 S1_1 178.0(2) . . ?
N3_1 C22_1 N4_1 104.7(2) . . ?
N3_1 C22_1 B1_1 126.0(2) . . ?
N4_1 C22_1 B1_1 128.6(2) . . ?
C21_1 N2_1 B1_1 167.3(2) . . ?
C24_1 C23_1 N3_1 107.4(2) . . ?
C24_1 C23_1 H23_1 126.3 . . ?
N3_1 C23_1 H23_1 126.3 . . ?
C23_1 C24_1 N4_1 107.1(2) . . ?
C23_1 C24_1 H24_1 126.4 . . ?
N4_1 C24_1 H24_1 126.4 . . ?
C22_1 N4_1 C24_1 110.3(2) . . ?
C22_1 N4_1 C28_1 129.1(2) . . ?
C24_1 N4_1 C28_1 120.5(2) . . ?
N3_1 C25_1 C27_1 111.0(2) . . ?
N3_1 C25_1 C26_1 109.6(2) . . ?
C27_1 C25_1 C26_1 110.7(2) . . ?
N3_1 C25_1 H25_1 108.5 . . ?
C27_1 C25_1 H25_1 108.5 . . ?
C26_1 C25_1 H25_1 108.5 . . ?
C25_1 C26_1 H26A_1 109.5 . . ?
C25_1 C26_1 H26B_1 109.5 . . ?
H26A_1 C26_1 H26B_1 109.5 . . ?
C25_1 C26_1 H26C_1 109.5 . . ?
H26A_1 C26_1 H26C_1 109.5 . . ?
H26B_1 C26_1 H26C_1 109.5 . . ?
C25_1 C27_1 H27A_1 109.5 . . ?
C25_1 C27_1 H27B_1 109.5 . . ?
H27A_1 C27_1 H27B_1 109.5 . . ?
C25_1 C27_1 H27C_1 109.5 . . ?
H27A_1 C27_1 H27C_1 109.5 . . ?
H27B_1 C27_1 H27C_1 109.5 . . ?
N4_1 C28_1 C29_1 110.0(2) . . ?
N4_1 C28_1 C30_1 109.6(2) . . ?
C29_1 C28_1 C30_1 112.3(2) . . ?
N4_1 C28_1 H28_1 108.3 . . ?
C29_1 C28_1 H28_1 108.3 . . ?
C30_1 C28_1 H28_1 108.3 . . ?
C28_1 C29_1 H29A_1 109.5 . . ?
C28_1 C29_1 H29B_1 109.5 . . ?
H29A_1 C29_1 H29B_1 109.5 . . ?
C28_1 C29_1 H29C_1 109.5 . . ?
H29A_1 C29_1 H29C_1 109.5 . . ?
H29B_1 C29_1 H29C_1 109.5 . . ?
C28_1 C30_1 H30A_1 109.5 . . ?
C28_1 C30_1 H30B_1 109.5 . . ?
H30A_1 C30_1 H30B_1 109.5 . . ?
C28_1 C30_1 H30C_1 109.5 . . ?
H30A_1 C30_1 H30C_1 109.5 . . ?
H30B_1 C30_1 H30C_1 109.5 . . ?
C31_1 S2_1 B1_1 100.17(12) . . ?
C32_1 C31_1 C36_1 118.4(2) . . ?
C32_1 C31_1 S2_1 119.2(2) . . ?
C36_1 C31_1 S2_1 122.4(2) . . ?
C33_1 C32_1 C31_1 121.0(2) . . ?
C33_1 C32_1 H32_1 119.5 . . ?
C31_1 C32_1 H32_1 119.5 . . ?
C32_1 C33_1 C34_1 120.4(3) . . ?
C32_1 C33_1 H33_1 119.8 . . ?
C34_1 C33_1 H33_1 119.8 . . ?
C35_1 C34_1 C33_1 119.3(2) . . ?
C35_1 C34_1 H34_1 120.4 . . ?
C33_1 C34_1 H34_1 120.4 . . ?
C34_1 C35_1 C36_1 120.4(2) . . ?
C34_1 C35_1 H35_1 119.8 . . ?
C36_1 C35_1 H35_1 119.8 . . ?
C31_1 C36_1 C35_1 120.5(2) . . ?
C31_1 C36_1 H36_1 119.7 . . ?
C35_1 C36_1 H36_1 119.7 . . ?

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
C6_10 C1_10 C2_10 C3_10 0.0 . . . . ?
C1_10 C2_10 C3_10 C4_10 0.0 . . . . ?
C2_10 C3_10 C4_10 C5_10 0.0 . . . . ?
C3_10 C4_10 C5_10 C6_10 0.0 . . . . ?
C4_10 C5_10 C6_10 C1_10 0.0 . . . . ?
C2_10 C1_10 C6_10 C5_10 0.0 . . . . ?
C6_11 C1_11 C2_11 C3_11 0.0 . . . . ?
C1_11 C2_11 C3_11 C4_11 0.0 . . . . ?
C2_11 C3_11 C4_11 C5_11 0.0 . . . . ?
C3_11 C4_11 C5_11 C6_11 0.0 . . . . ?
C4_11 C5_11 C6_11 C1_11 0.0 . . . . ?
C2_11 C1_11 C6_11 C5_11 0.0 . . . . ?
C4_1 C1_1 N1_1 C9_1 142.8(2) . . . . ?
B1_1 C1_1 N1_1 C9_1 -88.4(3) . . . . ?
C4_1 C1_1 N1_1 C2_1 -1.9(3) . . . . ?
B1_1 C1_1 N1_1 C2_1 126.8(2) . . . . ?
C9_1 N1_1 C2_1 C6_1 -6.2(3) . . . . ?
C1_1 N1_1 C2_1 C6_1 139.2(2) . . . . ?
C9_1 N1_1 C2_1 C3_1 -125.0(2) . . . . ?
C1_1 N1_1 C2_1 C3_1 20.5(3) . . . . ?
C9_1 N1_1 C2_1 C5_1 115.1(2) . . . . ?
C1_1 N1_1 C2_1 C5_1 -99.5(2) . . . . ?
N1_1 C2_1 C3_1 C4_1 -31.9(2) . . . . ?
C6_1 C2_1 C3_1 C4_1 -152.9(2) . . . . ?
C5_1 C2_1 C3_1 C4_1 87.2(3) . . . . ?
C2_1 C3_1 C4_1 C8_1 149.2(2) . . . . ?
C2_1 C3_1 C4_1 C7_1 -93.6(2) . . . . ?
C2_1 C3_1 C4_1 C1_1 30.6(2) . . . . ?
N1_1 C1_1 C4_1 C3_1 -17.4(2) . . . . ?
B1_1 C1_1 C4_1 C3_1 -144.4(2) . . . . ?
N1_1 C1_1 C4_1 C8_1 -135.4(2) . . . . ?
B1_1 C1_1 C4_1 C8_1 97.5(3) . . . . ?
N1_1 C1_1 C4_1 C7_1 103.3(2) . . . . ?
B1_1 C1_1 C4_1 C7_1 -23.7(3) . . . . ?
C2_1 N1_1 C9_1 C10_1 87.2(3) . . . . ?
C1_1 N1_1 C9_1 C10_1 -54.8(3) . . . . ?
C2_1 N1_1 C9_1 C14_1 -90.1(3) . . . . ?
C1_1 N1_1 C9_1 C14_1 127.9(2) . . . . ?
C14_1 C9_1 C10_1 C11_1 -3.0(4) . . . . ?
N1_1 C9_1 C10_1 C11_1 179.7(2) . . . . ?
C14_1 C9_1 C10_1 C15_1 175.1(2) . . . . ?
N1_1 C9_1 C10_1 C15_1 -2.2(4) . . . . ?
C9_1 C10_1 C11_1 C12_1 3.0(4) . . . . ?
C15_1 C10_1 C11_1 C12_1 -175.3(2) . . . . ?
C10_1 C11_1 C12_1 C13_1 -0.9(4) . . . . ?
C11_1 C12_1 C13_1 C14_1 -1.1(4) . . . . ?
C12_1 C13_1 C14_1 C9_1 1.0(4) . . . . ?
C12_1 C13_1 C14_1 C18_1 -177.3(2) . . . . ?
C10_1 C9_1 C14_1 C13_1 1.1(4) . . . . ?
N1_1 C9_1 C14_1 C13_1 178.6(2) . . . . ?
C10_1 C9_1 C14_1 C18_1 179.3(2) . . . . ?
N1_1 C9_1 C14_1 C18_1 -3.2(4) . . . . ?
C11_1 C10_1 C15_1 C16_1 -67.5(3) . . . . ?
C9_1 C10_1 C15_1 C16_1 114.2(3) . . . . ?
C11_1 C10_1 C15_1 C17_1 55.6(3) . . . . ?
C9_1 C10_1 C15_1 C17_1 -122.6(3) . . . . ?
C13_1 C14_1 C18_1 C20_1 53.5(3) . . . . ?
C9_1 C14_1 C18_1 C20_1 -124.8(3) . . . . ?
C13_1 C14_1 C18_1 C19_1 -68.6(3) . . . . ?
C9_1 C14_1 C18_1 C19_1 113.1(3) . . . . ?
N1_1 C1_1 B1_1 N2_1 -47.0(3) . . . . ?
C4_1 C1_1 B1_1 N2_1 76.1(3) . . . . ?
N1_1 C1_1 B1_1 C22_1 -173.3(2) . . . . ?
C4_1 C1_1 B1_1 C22_1 -50.2(3) . . . . ?
N1_1 C1_1 B1_1 S2_1 68.1(2) . . . . ?
C4_1 C1_1 B1_1 S2_1 -168.78(17) . . . . ?
C23_1 N3_1 C22_1 N4_1 1.8(3) . . . . ?
C25_1 N3_1 C22_1 N4_1 -177.9(2) . . . . ?
C23_1 N3_1 C22_1 B1_1 -169.8(2) . . . . ?
C25_1 N3_1 C22_1 B1_1 10.5(4) . . . . ?
N2_1 B1_1 C22_1 N3_1 167.5(2) . . . . ?
C1_1 B1_1 C22_1 N3_1 -65.5(3) . . . . ?
S2_1 B1_1 C22_1 N3_1 55.3(3) . . . . ?
N2_1 B1_1 C22_1 N4_1 -2.1(4) . . . . ?
C1_1 B1_1 C22_1 N4_1 124.9(3) . . . . ?
S2_1 B1_1 C22_1 N4_1 -114.3(2) . . . . ?
C1_1 B1_1 N2_1 C21_1 97.1(12) . . . . ?
C22_1 B1_1 N2_1 C21_1 -133.1(11) . . . . ?
S2_1 B1_1 N2_1 C21_1 -20.7(12) . . . . ?
C22_1 N3_1 C23_1 C24_1 -1.1(3) . . . . ?
C25_1 N3_1 C23_1 C24_1 178.7(2) . . . . ?
N3_1 C23_1 C24_1 N4_1 -0.1(3) . . . . ?
N3_1 C22_1 N4_1 C24_1 -1.9(3) . . . . ?
B1_1 C22_1 N4_1 C24_1 169.4(2) . . . . ?
N3_1 C22_1 N4_1 C28_1 175.5(2) . . . . ?
B1_1 C22_1 N4_1 C28_1 -13.2(4) . . . . ?
C23_1 C24_1 N4_1 C22_1 1.3(3) . . . . ?
C23_1 C24_1 N4_1 C28_1 -176.4(2) . . . . ?
C22_1 N3_1 C25_1 C27_1 -112.3(3) . . . . ?
C23_1 N3_1 C25_1 C27_1 68.0(3) . . . . ?
C22_1 N3_1 C25_1 C26_1 125.2(3) . . . . ?
C23_1 N3_1 C25_1 C26_1 -54.6(3) . . . . ?
C22_1 N4_1 C28_1 C29_1 103.8(3) . . . . ?
C24_1 N4_1 C28_1 C29_1 -79.0(3) . . . . ?
C22_1 N4_1 C28_1 C30_1 -132.3(3) . . . . ?
C24_1 N4_1 C28_1 C30_1 44.9(3) . . . . ?
B1_1 S2_1 C31_1 C32_1 96.6(2) . . . . ?
B1_1 S2_1 C31_1 C36_1 -84.9(2) . . . . ?
C36_1 C31_1 C32_1 C33_1 -0.9(4) . . . . ?
S2_1 C31_1 C32_1 C33_1 177.8(2) . . . . ?
C31_1 C32_1 C33_1 C34_1 0.7(4) . . . . ?
C32_1 C33_1 C34_1 C35_1 -0.1(4) . . . . ?
C33_1 C34_1 C35_1 C36_1 -0.4(4) . . . . ?
C32_1 C31_1 C36_1 C35_1 0.4(4) . . . . ?
S2_1 C31_1 C36_1 C35_1 -178.2(2) . . . . ?
C34_1 C35_1 C36_1 C31_1 0.2(4) . . . . ?

_refine_diff_density_max         0.174
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.035



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_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_test_a_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2071471'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        (CAAC)(IiPr)B(CN-W(CO)5)
_chemical_name_common            2(CN)-W
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H47 B N4 O5 W'
_chemical_formula_sum            'C35 H47 B N4 O5 W'
_chemical_formula_weight         798.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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                   9.653(4)
_cell_length_b                   10.588(7)
_cell_length_c                   19.881(9)
_cell_angle_alpha                78.11(2)
_cell_angle_beta                 83.576(15)
_cell_angle_gamma                67.077(16)
_cell_volume                     1830.2(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8759
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      25.69


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.226
_exptl_absorpt_coefficient_mu    3.200
_shelx_estimated_absorpt_T_min   0.430
_shelx_estimated_absorpt_T_max   0.532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4106
_exptl_absorpt_correction_T_max  0.7454
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 1.00 0.1310
0.00 -1.00 -1.00 0.0760
-1.00 -1.00 0.00 0.1040
1.00 1.00 1.00 0.1110
-1.00 -1.00 -1.00 0.0940
1.00 0.00 1.00 0.1620
-1.00 0.00 -1.00 0.1590
1.00 -1.00 1.00 0.1420
-1.00 0.00 1.00 0.1640
0.00 1.00 0.00 0.1250
0.00 -1.00 0.00 0.1230
0.00 0.00 -1.00 0.0490
0.00 0.00 1.00 0.1130
1.00 1.00 -1.00 0.1030
-1.00 -1.00 1.00 0.1220
-1.00 1.00 0.00 0.1560
1.00 -1.00 0.00 0.1440

_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            30853
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.047
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        26.000
_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             7190
_reflns_number_gt                6427
_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       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_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          
;

 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0226P)²] 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         7190
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0786
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.002
_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
C1_1 C 0.7130(4) 0.4347(4) 0.8075(2) 0.0130(8) Uani 1 1 d . . . . .
N1_1 N 0.7944(3) 0.3318(4) 0.86111(17) 0.0139(7) Uani 1 1 d . . . . .
C2_1 C 0.8087(5) 0.3935(5) 0.9197(2) 0.0202(10) Uani 1 1 d . . . . .
C3_1 C 0.6695(5) 0.5298(4) 0.9121(2) 0.0220(10) Uani 1 1 d . . . . .
H3A_1 H 0.691216 0.603590 0.927053 0.026 Uiso 1 1 calc R U . . .
H3AB_1 H 0.584152 0.515963 0.940876 0.026 Uiso 1 1 calc R U . . .
C4_1 C 0.6299(5) 0.5720(4) 0.8355(2) 0.0191(9) Uani 1 1 d . . . . .
C5_1 C 0.9544(5) 0.4215(5) 0.9112(2) 0.0273(11) Uani 1 1 d . . . . .
H5A_1 H 0.949617 0.484295 0.942143 0.041 Uiso 1 1 calc R U . . .
H5B_1 H 0.966576 0.464797 0.863536 0.041 Uiso 1 1 calc R U . . .
H5C_1 H 1.040169 0.333384 0.922555 0.041 Uiso 1 1 calc R U . . .
C6_1 C 0.8046(5) 0.3013(5) 0.9891(2) 0.0273(11) Uani 1 1 d . . . . .
H6A_1 H 0.814240 0.346170 1.025817 0.041 Uiso 1 1 calc R U . . .
H6B_1 H 0.888071 0.210813 0.990523 0.041 Uiso 1 1 calc R U . . .
H6C_1 H 0.708933 0.287661 0.995526 0.041 Uiso 1 1 calc R U . . .
C7_1 C 0.4576(5) 0.6319(5) 0.8290(2) 0.0270(11) Uani 1 1 d . . . . .
H7A_1 H 0.412409 0.711826 0.852770 0.040 Uiso 1 1 calc R U . . .
H7B_1 H 0.417840 0.560033 0.849862 0.040 Uiso 1 1 calc R U . . .
H7C_1 H 0.433138 0.661923 0.780313 0.040 Uiso 1 1 calc R U . . .
C8_1 C 0.6874(5) 0.6842(5) 0.7987(2) 0.0276(11) Uani 1 1 d . . . . .
H8A_1 H 0.634968 0.769584 0.817870 0.041 Uiso 1 1 calc R U . . .
H8B_1 H 0.668435 0.703357 0.749511 0.041 Uiso 1 1 calc R U . . .
H8C_1 H 0.795765 0.652010 0.805046 0.041 Uiso 1 1 calc R U . . .
C9_1 C 0.8075(4) 0.1896(4) 0.8689(2) 0.0166(9) Uani 1 1 d . . . . .
C10_1 C 0.6780(4) 0.1551(4) 0.8842(2) 0.0164(9) Uani 1 1 d . . . . .
C11_1 C 0.6929(5) 0.0174(5) 0.8909(2) 0.0196(9) Uani 1 1 d . . . . .
H11_1 H 0.605712 -0.005243 0.899802 0.024 Uiso 1 1 calc R U . . .
C12_1 C 0.8336(5) -0.0885(5) 0.8849(2) 0.0205(10) Uani 1 1 d . . . . .
H12_1 H 0.842522 -0.182659 0.890651 0.025 Uiso 1 1 calc R U . . .
C13_1 C 0.9589(5) -0.0550(5) 0.8707(2) 0.0218(10) Uani 1 1 d . . . . .
H13_1 H 1.054612 -0.127196 0.866881 0.026 Uiso 1 1 calc R U . . .
C14_1 C 0.9492(4) 0.0816(5) 0.8618(2) 0.0170(9) Uani 1 1 d . . . . .
C15_1 C 0.5218(4) 0.2637(5) 0.8946(2) 0.0193(9) Uani 1 1 d . . . . .
H15_1 H 0.533229 0.352696 0.896626 0.023 Uiso 1 1 calc R U . . .
C16_1 C 0.4197(4) 0.2920(5) 0.8355(2) 0.0230(10) Uani 1 1 d . . . . .
H16A_1 H 0.317972 0.355396 0.846394 0.035 Uiso 1 1 calc R U . . .
H16B_1 H 0.416343 0.204118 0.828810 0.035 Uiso 1 1 calc R U . . .
H16C_1 H 0.459156 0.334787 0.793287 0.035 Uiso 1 1 calc R U . . .
C17_1 C 0.4473(5) 0.2199(5) 0.9630(2) 0.0272(11) Uani 1 1 d . . . . .
H17A_1 H 0.351805 0.295647 0.970870 0.041 Uiso 1 1 calc R U . . .
H17B_1 H 0.514293 0.200003 1.000712 0.041 Uiso 1 1 calc R U . . .
H17C_1 H 0.428384 0.136292 0.961168 0.041 Uiso 1 1 calc R U . . .
C18_1 C 1.0939(4) 0.1098(5) 0.8463(2) 0.0212(10) Uani 1 1 d . . . . .
H18_1 H 1.067378 0.212830 0.836561 0.025 Uiso 1 1 calc R U . . .
C19_1 C 1.1816(5) 0.0485(5) 0.7833(2) 0.0269(11) Uani 1 1 d . . . . .
H19A_1 H 1.270958 0.072503 0.773208 0.040 Uiso 1 1 calc R U . . .
H19B_1 H 1.117019 0.087098 0.743491 0.040 Uiso 1 1 calc R U . . .
H19C_1 H 1.212512 -0.053097 0.793134 0.040 Uiso 1 1 calc R U . . .
C20_1 C 1.1938(5) 0.0466(5) 0.9089(2) 0.0278(11) Uani 1 1 d . . . . .
H20A_1 H 1.281789 0.072919 0.900448 0.042 Uiso 1 1 calc R U . . .
H20B_1 H 1.227087 -0.055155 0.916824 0.042 Uiso 1 1 calc R U . . .
H20C_1 H 1.136446 0.081615 0.949587 0.042 Uiso 1 1 calc R U . . .
B1_1 B 0.7155(5) 0.4192(5) 0.7373(2) 0.0138(10) Uani 1 1 d . . . . .
C21_1 C 0.6034(4) 0.5347(4) 0.6870(2) 0.0161(9) Uani 1 1 d . . . . .
N2_1 N 0.5201(3) 0.6157(4) 0.64712(17) 0.0169(8) Uani 1 1 d . . . . .
C22_1 C 0.8356(4) 0.3096(4) 0.6946(2) 0.0116(8) Uani 1 1 d . . . . .
N3_1 N 0.8278(3) 0.1973(3) 0.67513(17) 0.0132(7) Uani 1 1 d . . . . .
C23_1 C 0.9398(4) 0.1501(4) 0.6262(2) 0.0173(9) Uani 1 1 d . . . . .
H23_1 H 0.958331 0.072701 0.604573 0.021 Uiso 1 1 calc R U . . .
C24_1 C 1.0179(4) 0.2342(4) 0.6148(2) 0.0179(9) Uani 1 1 d . . . . .
H24_1 H 1.100977 0.228148 0.583335 0.021 Uiso 1 1 calc R U . . .
N4_1 N 0.9539(3) 0.3309(4) 0.65777(17) 0.0152(8) Uani 1 1 d . . . . .
C25_1 C 0.7060(4) 0.1459(4) 0.6988(2) 0.0156(9) Uani 1 1 d . . . . .
H25_1 H 0.671260 0.167734 0.745904 0.019 Uiso 1 1 calc R U . . .
C26_1 C 0.7600(5) -0.0107(4) 0.7039(2) 0.0220(10) Uani 1 1 d . . . . .
H26A_1 H 0.678430 -0.042032 0.723147 0.033 Uiso 1 1 calc R U . . .
H26B_1 H 0.846257 -0.056666 0.733792 0.033 Uiso 1 1 calc R U . . .
H26C_1 H 0.790094 -0.034439 0.657933 0.033 Uiso 1 1 calc R U . . .
C27_1 C 0.5737(4) 0.2249(5) 0.6514(2) 0.0220(10) Uani 1 1 d . . . . .
H27A_1 H 0.490138 0.194895 0.668315 0.033 Uiso 1 1 calc R U . . .
H27B_1 H 0.604913 0.205446 0.604769 0.033 Uiso 1 1 calc R U . . .
H27C_1 H 0.541223 0.325186 0.650647 0.033 Uiso 1 1 calc R U . . .
C28_1 C 0.9985(4) 0.4484(5) 0.6604(2) 0.0189(9) Uani 1 1 d . . . . .
H28_1 H 0.940889 0.494328 0.699608 0.023 Uiso 1 1 calc R U . . .
C29_1 C 1.1654(5) 0.3957(5) 0.6740(3) 0.0276(11) Uani 1 1 d . . . . .
H29A_1 H 1.191149 0.473479 0.680066 0.041 Uiso 1 1 calc R U . . .
H29B_1 H 1.224413 0.355291 0.634896 0.041 Uiso 1 1 calc R U . . .
H29C_1 H 1.188213 0.324524 0.715780 0.041 Uiso 1 1 calc R U . . .
C30_1 C 0.9579(5) 0.5547(5) 0.5952(3) 0.0367(13) Uani 1 1 d . . . . .
H30A_1 H 0.974528 0.637790 0.600293 0.055 Uiso 1 1 calc R U . . .
H30B_1 H 0.851755 0.580306 0.586151 0.055 Uiso 1 1 calc R U . . .
H30C_1 H 1.020979 0.515099 0.556743 0.055 Uiso 1 1 calc R U . . .
W1_1 W 0.36556(2) 0.78278(2) 0.57724(2) 0.01399(6) Uani 1 1 d . . . . .
C31_1 C 0.3307(4) 0.6458(5) 0.5282(2) 0.0205(10) Uani 1 1 d . . . . .
C32_1 C 0.5474(5) 0.7801(5) 0.5129(2) 0.0215(10) Uani 1 1 d . . . . .
C33_1 C 0.2273(4) 0.9426(5) 0.5152(2) 0.0189(10) Uani 1 1 d . . . . .
C34_1 C 0.3975(4) 0.9200(5) 0.6256(2) 0.0211(10) Uani 1 1 d . . . . .
C35_1 C 0.1966(5) 0.7723(5) 0.6466(2) 0.0251(11) Uani 1 1 d . . . . .
O1_1 O 0.3077(4) 0.5729(3) 0.50023(18) 0.0318(8) Uani 1 1 d . . . . .
O2_1 O 0.6498(3) 0.7794(4) 0.47811(16) 0.0297(8) Uani 1 1 d . . . . .
O3_1 O 0.1483(3) 1.0376(3) 0.47925(16) 0.0273(8) Uani 1 1 d . . . . .
O4_1 O 0.4131(4) 0.9976(4) 0.65307(18) 0.0329(8) Uani 1 1 d . . . . .
O5_1 O 0.1037(4) 0.7637(4) 0.68610(19) 0.0403(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1_1 N1_1 1.408(5) . ?
C1_1 B1_1 1.436(6) . ?
C1_1 C4_1 1.546(5) . ?
N1_1 C9_1 1.437(5) . ?
N1_1 C2_1 1.490(5) . ?
C2_1 C6_1 1.523(6) . ?
C2_1 C5_1 1.532(6) . ?
C2_1 C3_1 1.535(6) . ?
C3_1 C4_1 1.544(6) . ?
C3_1 H3A_1 0.9900 . ?
C3_1 H3AB_1 0.9900 . ?
C4_1 C8_1 1.523(6) . ?
C4_1 C7_1 1.542(6) . ?
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 . ?
C7_1 H7A_1 0.9800 . ?
C7_1 H7B_1 0.9800 . ?
C7_1 H7C_1 0.9800 . ?
C8_1 H8A_1 0.9800 . ?
C8_1 H8B_1 0.9800 . ?
C8_1 H8C_1 0.9800 . ?
C9_1 C14_1 1.415(5) . ?
C9_1 C10_1 1.419(6) . ?
C10_1 C11_1 1.388(6) . ?
C10_1 C15_1 1.522(5) . ?
C11_1 C12_1 1.396(5) . ?
C11_1 H11_1 0.9500 . ?
C12_1 C13_1 1.373(6) . ?
C12_1 H12_1 0.9500 . ?
C13_1 C14_1 1.387(6) . ?
C13_1 H13_1 0.9500 . ?
C14_1 C18_1 1.524(6) . ?
C15_1 C16_1 1.525(5) . ?
C15_1 C17_1 1.537(6) . ?
C15_1 H15_1 1.0000 . ?
C16_1 H16A_1 0.9800 . ?
C16_1 H16B_1 0.9800 . ?
C16_1 H16C_1 0.9800 . ?
C17_1 H17A_1 0.9800 . ?
C17_1 H17B_1 0.9800 . ?
C17_1 H17C_1 0.9800 . ?
C18_1 C20_1 1.533(6) . ?
C18_1 C19_1 1.542(6) . ?
C18_1 H18_1 1.0000 . ?
C19_1 H19A_1 0.9800 . ?
C19_1 H19B_1 0.9800 . ?
C19_1 H19C_1 0.9800 . ?
C20_1 H20A_1 0.9800 . ?
C20_1 H20B_1 0.9800 . ?
C20_1 H20C_1 0.9800 . ?
B1_1 C21_1 1.541(6) . ?
B1_1 C22_1 1.596(5) . ?
C21_1 N2_1 1.156(5) . ?
N2_1 W1_1 2.163(3) . ?
C22_1 N3_1 1.354(5) . ?
C22_1 N4_1 1.356(5) . ?
N3_1 C23_1 1.382(5) . ?
N3_1 C25_1 1.473(5) . ?
C23_1 C24_1 1.346(6) . ?
C23_1 H23_1 0.9500 . ?
C24_1 N4_1 1.382(5) . ?
C24_1 H24_1 0.9500 . ?
N4_1 C28_1 1.479(5) . ?
C25_1 C26_1 1.517(6) . ?
C25_1 C27_1 1.527(5) . ?
C25_1 H25_1 1.0000 . ?
C26_1 H26A_1 0.9800 . ?
C26_1 H26B_1 0.9800 . ?
C26_1 H26C_1 0.9800 . ?
C27_1 H27A_1 0.9800 . ?
C27_1 H27B_1 0.9800 . ?
C27_1 H27C_1 0.9800 . ?
C28_1 C30_1 1.507(6) . ?
C28_1 C29_1 1.522(5) . ?
C28_1 H28_1 1.0000 . ?
C29_1 H29A_1 0.9800 . ?
C29_1 H29B_1 0.9800 . ?
C29_1 H29C_1 0.9800 . ?
C30_1 H30A_1 0.9800 . ?
C30_1 H30B_1 0.9800 . ?
C30_1 H30C_1 0.9800 . ?
W1_1 C33_1 1.978(4) . ?
W1_1 C34_1 2.031(5) . ?
W1_1 C35_1 2.037(5) . ?
W1_1 C32_1 2.047(5) . ?
W1_1 C31_1 2.051(5) . ?
C31_1 O1_1 1.136(5) . ?
C32_1 O2_1 1.140(5) . ?
C33_1 O3_1 1.154(5) . ?
C34_1 O4_1 1.137(5) . ?
C35_1 O5_1 1.142(6) . ?

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_1 C1_1 B1_1 126.1(3) . . ?
N1_1 C1_1 C4_1 108.5(3) . . ?
B1_1 C1_1 C4_1 125.2(4) . . ?
C1_1 N1_1 C9_1 121.4(3) . . ?
C1_1 N1_1 C2_1 111.8(3) . . ?
C9_1 N1_1 C2_1 122.7(3) . . ?
N1_1 C2_1 C6_1 112.5(4) . . ?
N1_1 C2_1 C5_1 110.4(3) . . ?
C6_1 C2_1 C5_1 109.5(4) . . ?
N1_1 C2_1 C3_1 101.8(3) . . ?
C6_1 C2_1 C3_1 111.0(4) . . ?
C5_1 C2_1 C3_1 111.4(4) . . ?
C2_1 C3_1 C4_1 107.3(3) . . ?
C2_1 C3_1 H3A_1 110.2 . . ?
C4_1 C3_1 H3A_1 110.2 . . ?
C2_1 C3_1 H3AB_1 110.2 . . ?
C4_1 C3_1 H3AB_1 110.2 . . ?
H3A_1 C3_1 H3AB_1 108.5 . . ?
C8_1 C4_1 C7_1 107.5(4) . . ?
C8_1 C4_1 C3_1 111.2(4) . . ?
C7_1 C4_1 C3_1 109.8(3) . . ?
C8_1 C4_1 C1_1 110.8(3) . . ?
C7_1 C4_1 C1_1 114.4(3) . . ?
C3_1 C4_1 C1_1 103.1(3) . . ?
C2_1 C5_1 H5A_1 109.5 . . ?
C2_1 C5_1 H5B_1 109.5 . . ?
H5A_1 C5_1 H5B_1 109.5 . . ?
C2_1 C5_1 H5C_1 109.5 . . ?
H5A_1 C5_1 H5C_1 109.5 . . ?
H5B_1 C5_1 H5C_1 109.5 . . ?
C2_1 C6_1 H6A_1 109.5 . . ?
C2_1 C6_1 H6B_1 109.5 . . ?
H6A_1 C6_1 H6B_1 109.5 . . ?
C2_1 C6_1 H6C_1 109.5 . . ?
H6A_1 C6_1 H6C_1 109.5 . . ?
H6B_1 C6_1 H6C_1 109.5 . . ?
C4_1 C7_1 H7A_1 109.5 . . ?
C4_1 C7_1 H7B_1 109.5 . . ?
H7A_1 C7_1 H7B_1 109.5 . . ?
C4_1 C7_1 H7C_1 109.5 . . ?
H7A_1 C7_1 H7C_1 109.5 . . ?
H7B_1 C7_1 H7C_1 109.5 . . ?
C4_1 C8_1 H8A_1 109.5 . . ?
C4_1 C8_1 H8B_1 109.5 . . ?
H8A_1 C8_1 H8B_1 109.5 . . ?
C4_1 C8_1 H8C_1 109.5 . . ?
H8A_1 C8_1 H8C_1 109.5 . . ?
H8B_1 C8_1 H8C_1 109.5 . . ?
C14_1 C9_1 C10_1 118.8(4) . . ?
C14_1 C9_1 N1_1 120.9(4) . . ?
C10_1 C9_1 N1_1 120.3(4) . . ?
C11_1 C10_1 C9_1 119.5(4) . . ?
C11_1 C10_1 C15_1 118.0(4) . . ?
C9_1 C10_1 C15_1 122.5(4) . . ?
C10_1 C11_1 C12_1 121.2(4) . . ?
C10_1 C11_1 H11_1 119.4 . . ?
C12_1 C11_1 H11_1 119.4 . . ?
C13_1 C12_1 C11_1 119.2(4) . . ?
C13_1 C12_1 H12_1 120.4 . . ?
C11_1 C12_1 H12_1 120.4 . . ?
C12_1 C13_1 C14_1 121.7(4) . . ?
C12_1 C13_1 H13_1 119.1 . . ?
C14_1 C13_1 H13_1 119.1 . . ?
C13_1 C14_1 C9_1 119.6(4) . . ?
C13_1 C14_1 C18_1 118.4(4) . . ?
C9_1 C14_1 C18_1 122.0(4) . . ?
C10_1 C15_1 C16_1 112.3(3) . . ?
C10_1 C15_1 C17_1 111.1(4) . . ?
C16_1 C15_1 C17_1 109.8(4) . . ?
C10_1 C15_1 H15_1 107.8 . . ?
C16_1 C15_1 H15_1 107.8 . . ?
C17_1 C15_1 H15_1 107.8 . . ?
C15_1 C16_1 H16A_1 109.5 . . ?
C15_1 C16_1 H16B_1 109.5 . . ?
H16A_1 C16_1 H16B_1 109.5 . . ?
C15_1 C16_1 H16C_1 109.5 . . ?
H16A_1 C16_1 H16C_1 109.5 . . ?
H16B_1 C16_1 H16C_1 109.5 . . ?
C15_1 C17_1 H17A_1 109.5 . . ?
C15_1 C17_1 H17B_1 109.5 . . ?
H17A_1 C17_1 H17B_1 109.5 . . ?
C15_1 C17_1 H17C_1 109.5 . . ?
H17A_1 C17_1 H17C_1 109.5 . . ?
H17B_1 C17_1 H17C_1 109.5 . . ?
C14_1 C18_1 C20_1 109.9(4) . . ?
C14_1 C18_1 C19_1 111.4(4) . . ?
C20_1 C18_1 C19_1 109.4(3) . . ?
C14_1 C18_1 H18_1 108.7 . . ?
C20_1 C18_1 H18_1 108.7 . . ?
C19_1 C18_1 H18_1 108.7 . . ?
C18_1 C19_1 H19A_1 109.5 . . ?
C18_1 C19_1 H19B_1 109.5 . . ?
H19A_1 C19_1 H19B_1 109.5 . . ?
C18_1 C19_1 H19C_1 109.5 . . ?
H19A_1 C19_1 H19C_1 109.5 . . ?
H19B_1 C19_1 H19C_1 109.5 . . ?
C18_1 C20_1 H20A_1 109.5 . . ?
C18_1 C20_1 H20B_1 109.5 . . ?
H20A_1 C20_1 H20B_1 109.5 . . ?
C18_1 C20_1 H20C_1 109.5 . . ?
H20A_1 C20_1 H20C_1 109.5 . . ?
H20B_1 C20_1 H20C_1 109.5 . . ?
C1_1 B1_1 C21_1 119.8(3) . . ?
C1_1 B1_1 C22_1 130.8(4) . . ?
C21_1 B1_1 C22_1 108.6(3) . . ?
N2_1 C21_1 B1_1 176.2(4) . . ?
C21_1 N2_1 W1_1 174.5(3) . . ?
N3_1 C22_1 N4_1 105.4(3) . . ?
N3_1 C22_1 B1_1 129.5(3) . . ?
N4_1 C22_1 B1_1 123.7(4) . . ?
C22_1 N3_1 C23_1 110.1(3) . . ?
C22_1 N3_1 C25_1 123.1(3) . . ?
C23_1 N3_1 C25_1 126.6(3) . . ?
C24_1 C23_1 N3_1 107.3(4) . . ?
C24_1 C23_1 H23_1 126.3 . . ?
N3_1 C23_1 H23_1 126.3 . . ?
C23_1 C24_1 N4_1 106.7(4) . . ?
C23_1 C24_1 H24_1 126.6 . . ?
N4_1 C24_1 H24_1 126.6 . . ?
C22_1 N4_1 C24_1 110.4(3) . . ?
C22_1 N4_1 C28_1 123.7(3) . . ?
C24_1 N4_1 C28_1 125.7(3) . . ?
N3_1 C25_1 C26_1 111.7(3) . . ?
N3_1 C25_1 C27_1 109.0(4) . . ?
C26_1 C25_1 C27_1 112.4(3) . . ?
N3_1 C25_1 H25_1 107.8 . . ?
C26_1 C25_1 H25_1 107.8 . . ?
C27_1 C25_1 H25_1 107.8 . . ?
C25_1 C26_1 H26A_1 109.5 . . ?
C25_1 C26_1 H26B_1 109.5 . . ?
H26A_1 C26_1 H26B_1 109.5 . . ?
C25_1 C26_1 H26C_1 109.5 . . ?
H26A_1 C26_1 H26C_1 109.5 . . ?
H26B_1 C26_1 H26C_1 109.5 . . ?
C25_1 C27_1 H27A_1 109.5 . . ?
C25_1 C27_1 H27B_1 109.5 . . ?
H27A_1 C27_1 H27B_1 109.5 . . ?
C25_1 C27_1 H27C_1 109.5 . . ?
H27A_1 C27_1 H27C_1 109.5 . . ?
H27B_1 C27_1 H27C_1 109.5 . . ?
N4_1 C28_1 C30_1 110.4(4) . . ?
N4_1 C28_1 C29_1 110.5(3) . . ?
C30_1 C28_1 C29_1 111.8(4) . . ?
N4_1 C28_1 H28_1 108.0 . . ?
C30_1 C28_1 H28_1 108.0 . . ?
C29_1 C28_1 H28_1 108.0 . . ?
C28_1 C29_1 H29A_1 109.5 . . ?
C28_1 C29_1 H29B_1 109.5 . . ?
H29A_1 C29_1 H29B_1 109.5 . . ?
C28_1 C29_1 H29C_1 109.5 . . ?
H29A_1 C29_1 H29C_1 109.5 . . ?
H29B_1 C29_1 H29C_1 109.5 . . ?
C28_1 C30_1 H30A_1 109.5 . . ?
C28_1 C30_1 H30B_1 109.5 . . ?
H30A_1 C30_1 H30B_1 109.5 . . ?
C28_1 C30_1 H30C_1 109.5 . . ?
H30A_1 C30_1 H30C_1 109.5 . . ?
H30B_1 C30_1 H30C_1 109.5 . . ?
C33_1 W1_1 C34_1 88.74(18) . . ?
C33_1 W1_1 C35_1 92.88(18) . . ?
C34_1 W1_1 C35_1 90.13(18) . . ?
C33_1 W1_1 C32_1 91.86(17) . . ?
C34_1 W1_1 C32_1 89.76(17) . . ?
C35_1 W1_1 C32_1 175.26(16) . . ?
C33_1 W1_1 C31_1 90.70(18) . . ?
C34_1 W1_1 C31_1 179.32(15) . . ?
C35_1 W1_1 C31_1 89.52(18) . . ?
C32_1 W1_1 C31_1 90.64(17) . . ?
C33_1 W1_1 N2_1 176.96(15) . . ?
C34_1 W1_1 N2_1 88.27(16) . . ?
C35_1 W1_1 N2_1 87.64(15) . . ?
C32_1 W1_1 N2_1 87.62(15) . . ?
C31_1 W1_1 N2_1 92.30(16) . . ?
O1_1 C31_1 W1_1 178.0(4) . . ?
O2_1 C32_1 W1_1 178.6(4) . . ?
O3_1 C33_1 W1_1 178.5(4) . . ?
O4_1 C34_1 W1_1 178.9(4) . . ?
O5_1 C35_1 W1_1 178.6(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
B1_1 C1_1 N1_1 C9_1 -42.1(6) . . . . ?
C4_1 C1_1 N1_1 C9_1 142.5(4) . . . . ?
B1_1 C1_1 N1_1 C2_1 160.3(4) . . . . ?
C4_1 C1_1 N1_1 C2_1 -15.1(4) . . . . ?
C1_1 N1_1 C2_1 C6_1 145.1(4) . . . . ?
C9_1 N1_1 C2_1 C6_1 -12.2(5) . . . . ?
C1_1 N1_1 C2_1 C5_1 -92.2(4) . . . . ?
C9_1 N1_1 C2_1 C5_1 110.5(4) . . . . ?
C1_1 N1_1 C2_1 C3_1 26.2(4) . . . . ?
C9_1 N1_1 C2_1 C3_1 -131.1(4) . . . . ?
N1_1 C2_1 C3_1 C4_1 -26.8(4) . . . . ?
C6_1 C2_1 C3_1 C4_1 -146.8(4) . . . . ?
C5_1 C2_1 C3_1 C4_1 90.8(4) . . . . ?
C2_1 C3_1 C4_1 C8_1 -100.1(4) . . . . ?
C2_1 C3_1 C4_1 C7_1 141.1(4) . . . . ?
C2_1 C3_1 C4_1 C1_1 18.7(4) . . . . ?
N1_1 C1_1 C4_1 C8_1 116.3(4) . . . . ?
B1_1 C1_1 C4_1 C8_1 -59.2(5) . . . . ?
N1_1 C1_1 C4_1 C7_1 -122.0(4) . . . . ?
B1_1 C1_1 C4_1 C7_1 62.6(6) . . . . ?
N1_1 C1_1 C4_1 C3_1 -2.7(4) . . . . ?
B1_1 C1_1 C4_1 C3_1 -178.2(4) . . . . ?
C1_1 N1_1 C9_1 C14_1 116.0(4) . . . . ?
C2_1 N1_1 C9_1 C14_1 -88.9(5) . . . . ?
C1_1 N1_1 C9_1 C10_1 -64.3(5) . . . . ?
C2_1 N1_1 C9_1 C10_1 90.9(5) . . . . ?
C14_1 C9_1 C10_1 C11_1 -0.8(6) . . . . ?
N1_1 C9_1 C10_1 C11_1 179.5(4) . . . . ?
C14_1 C9_1 C10_1 C15_1 178.3(4) . . . . ?
N1_1 C9_1 C10_1 C15_1 -1.4(6) . . . . ?
C9_1 C10_1 C11_1 C12_1 1.9(6) . . . . ?
C15_1 C10_1 C11_1 C12_1 -177.3(4) . . . . ?
C10_1 C11_1 C12_1 C13_1 -1.3(6) . . . . ?
C11_1 C12_1 C13_1 C14_1 -0.3(6) . . . . ?
C12_1 C13_1 C14_1 C9_1 1.4(6) . . . . ?
C12_1 C13_1 C14_1 C18_1 179.8(4) . . . . ?
C10_1 C9_1 C14_1 C13_1 -0.8(6) . . . . ?
N1_1 C9_1 C14_1 C13_1 178.9(4) . . . . ?
C10_1 C9_1 C14_1 C18_1 -179.2(4) . . . . ?
N1_1 C9_1 C14_1 C18_1 0.5(6) . . . . ?
C11_1 C10_1 C15_1 C16_1 -71.6(5) . . . . ?
C9_1 C10_1 C15_1 C16_1 109.3(5) . . . . ?
C11_1 C10_1 C15_1 C17_1 51.8(5) . . . . ?
C9_1 C10_1 C15_1 C17_1 -127.3(4) . . . . ?
C13_1 C14_1 C18_1 C20_1 -66.9(5) . . . . ?
C9_1 C14_1 C18_1 C20_1 111.5(4) . . . . ?
C13_1 C14_1 C18_1 C19_1 54.5(5) . . . . ?
C9_1 C14_1 C18_1 C19_1 -127.2(4) . . . . ?
N1_1 C1_1 B1_1 C21_1 171.5(4) . . . . ?
C4_1 C1_1 B1_1 C21_1 -13.9(6) . . . . ?
N1_1 C1_1 B1_1 C22_1 -20.1(7) . . . . ?
C4_1 C1_1 B1_1 C22_1 154.6(4) . . . . ?
C1_1 B1_1 C22_1 N3_1 104.6(6) . . . . ?
C21_1 B1_1 C22_1 N3_1 -86.0(5) . . . . ?
C1_1 B1_1 C22_1 N4_1 -90.7(6) . . . . ?
C21_1 B1_1 C22_1 N4_1 78.7(5) . . . . ?
N4_1 C22_1 N3_1 C23_1 -0.4(4) . . . . ?
B1_1 C22_1 N3_1 C23_1 166.4(4) . . . . ?
N4_1 C22_1 N3_1 C25_1 -174.7(3) . . . . ?
B1_1 C22_1 N3_1 C25_1 -7.9(6) . . . . ?
C22_1 N3_1 C23_1 C24_1 -0.3(5) . . . . ?
C25_1 N3_1 C23_1 C24_1 173.8(4) . . . . ?
N3_1 C23_1 C24_1 N4_1 0.8(5) . . . . ?
N3_1 C22_1 N4_1 C24_1 0.9(4) . . . . ?
B1_1 C22_1 N4_1 C24_1 -166.8(3) . . . . ?
N3_1 C22_1 N4_1 C28_1 176.8(3) . . . . ?
B1_1 C22_1 N4_1 C28_1 9.0(6) . . . . ?
C23_1 C24_1 N4_1 C22_1 -1.1(5) . . . . ?
C23_1 C24_1 N4_1 C28_1 -176.9(4) . . . . ?
C22_1 N3_1 C25_1 C26_1 -148.9(4) . . . . ?
C23_1 N3_1 C25_1 C26_1 37.8(5) . . . . ?
C22_1 N3_1 C25_1 C27_1 86.3(4) . . . . ?
C23_1 N3_1 C25_1 C27_1 -87.0(5) . . . . ?
C22_1 N4_1 C28_1 C30_1 -107.0(4) . . . . ?
C24_1 N4_1 C28_1 C30_1 68.3(5) . . . . ?
C22_1 N4_1 C28_1 C29_1 128.9(4) . . . . ?
C24_1 N4_1 C28_1 C29_1 -55.9(5) . . . . ?

_refine_diff_density_max         1.652
_refine_diff_density_min         -1.839
_refine_diff_density_rms         0.146



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_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. 
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#######################################################################

data_test_a_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2071473'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_diffrn_ambient_environment      N~2~

_audit_creation_method           'CIF-fill 1.2i (K.Radacki 2005-20)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        (CAAC)(IiPr)B(CN-Cr(CO)5)
_chemical_name_common            2(CN)-Cr
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H47 B Cr N4 O5'
_chemical_formula_sum            'C35 H47 B Cr N4 O5'
_chemical_formula_weight         666.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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                   9.8392(17)
_cell_length_b                   9.9617(20)
_cell_length_c                   19.529(5)
_cell_angle_alpha                84.858(6)
_cell_angle_beta                 84.951(8)
_cell_angle_gamma                71.058(5)
_cell_volume                     1799.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9872
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      26.04


_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            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_F_000             708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.222
_exptl_absorpt_coefficient_mu    0.362
_shelx_estimated_absorpt_T_min   0.886
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7071
_exptl_absorpt_correction_T_max  0.7453


_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_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
0.00 0.00 1.00 0.1010
0.00 0.00 -1.00 0.0430
0.00 1.00 0.00 0.0740
0.00 -1.00 0.00 0.1840
1.00 1.00 0.00 0.1270
-1.00 -1.00 0.00 0.1300
-1.00 0.00 1.00 0.0660
1.00 0.00 -1.00 0.1600
0.00 1.00 1.00 0.0840
0.00 -1.00 -1.00 0.1760
0.00 1.00 -1.00 0.0750
0.00 -1.00 1.00 0.1610
1.00 -1.00 1.00 0.1720
-1.00 1.00 -1.00 0.0490
-1.00 0.00 -1.00 0.0660
1.00 1.00 -1.00 0.0840

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CMOS area detector (Photon II)'
_diffrn_detector_area_resol_mean 7.5
_diffrn_reflns_number            48392
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.345
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7075
_reflns_number_gt                6265
_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       'BIS 6.2.14 / APEX3 ver. 2018.1 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_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          
;
 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger. 

The CAAC backbone presents a twofold flip-disorder in C3, C7 and C8, modelled in a 
95:5 ratio with ADP restraints SIMU 0.005.
;
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7075
_refine_ls_number_parameters     457
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0775
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.035
_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
C1 C 0.83781(14) 0.23266(13) 0.29771(7) 0.0134(3) Uani 1 1 d . . . . .
C2 C 0.84276(16) 0.19167(15) 0.42297(7) 0.0200(3) Uani 1 1 d . . . . .
C4 C 0.95801(15) 0.09191(14) 0.31283(7) 0.0163(3) Uani 1 1 d . . . . .
C5 C 0.87402(18) 0.28260(17) 0.47486(8) 0.0260(3) Uani 1 1 d . . . . .
H5A H 0.917674 0.221557 0.514578 0.039 Uiso 1 1 calc R U . . .
H5B H 0.783910 0.353545 0.490262 0.039 Uiso 1 1 calc R U . . .
H5C H 0.940483 0.330914 0.452965 0.039 Uiso 1 1 calc R U . . .
C6 C 0.75189(18) 0.10633(17) 0.46174(8) 0.0276(3) Uani 1 1 d . . . . .
H6A H 0.804046 0.048976 0.500401 0.041 Uiso 1 1 calc R U . . .
H6B H 0.733424 0.043643 0.430356 0.041 Uiso 1 1 calc R U . . .
H6C H 0.660167 0.171863 0.479213 0.041 Uiso 1 1 calc R U . . .
C3_11 C 0.98417(17) 0.09856(16) 0.38865(8) 0.0199(3) Uani 0.952(2) 1 d . U P A
1
H3A_11 H 1.013140 0.001826 0.411775 0.024 Uiso 0.952(2) 1 calc R U P A 1
H3AB_11 H 1.061847 0.140264 0.391904 0.024 Uiso 0.952(2) 1 calc R U P A 1
C7_11 C 0.90534(18) -0.03508(15) 0.30340(8) 0.0226(4) Uani 0.952(2) 1 d . U P A
1
H7A_11 H 0.972743 -0.122642 0.323284 0.034 Uiso 0.952(2) 1 calc R U P A 1
H7B_11 H 0.900233 -0.043913 0.254192 0.034 Uiso 0.952(2) 1 calc R U P A 1
H7C_11 H 0.809644 -0.019240 0.326760 0.034 Uiso 0.952(2) 1 calc R U P A 1
C8_11 C 1.09938(16) 0.07187(17) 0.26916(8) 0.0231(4) Uani 0.952(2) 1 d . U P A
1
H8A_11 H 1.172640 -0.014500 0.286316 0.035 Uiso 0.952(2) 1 calc R U P A 1
H8B_11 H 1.131845 0.154228 0.272137 0.035 Uiso 0.952(2) 1 calc R U P A 1
H8C_11 H 1.084157 0.063070 0.221060 0.035 Uiso 0.952(2) 1 calc R U P A 1
C3_12 C 0.927(4) 0.051(3) 0.3902(16) 0.021(3) Uani 0.048(2) 1 d . U P A 2
H3A_12 H 0.869599 -0.014685 0.394714 0.025 Uiso 0.048(2) 1 calc R U P A 2
H3AB_12 H 1.018482 0.004226 0.412829 0.025 Uiso 0.048(2) 1 calc R U P A 2
C7_12 C 0.992(4) -0.026(3) 0.2668(16) 0.023(4) Uani 0.048(2) 1 d . U P A 2
H7A_12 H 1.052730 -0.113498 0.290038 0.035 Uiso 0.048(2) 1 calc R U P A 2
H7B_12 H 1.043522 -0.003187 0.224423 0.035 Uiso 0.048(2) 1 calc R U P A 2
H7C_12 H 0.902595 -0.039646 0.255434 0.035 Uiso 0.048(2) 1 calc R U P A 2
C8_12 C 1.106(3) 0.141(3) 0.3130(16) 0.020(4) Uani 0.048(2) 1 d . U P A 2
H8A_12 H 1.187694 0.058464 0.326238 0.029 Uiso 0.048(2) 1 calc R U P A 2
H8B_12 H 1.089344 0.214310 0.345949 0.029 Uiso 0.048(2) 1 calc R U P A 2
H8C_12 H 1.127349 0.179524 0.266769 0.029 Uiso 0.048(2) 1 calc R U P A 2
C9 C 0.65267(15) 0.40602(14) 0.36842(7) 0.0158(3) Uani 1 1 d . . . . .
C10 C 0.67731(15) 0.53806(15) 0.36878(7) 0.0178(3) Uani 1 1 d . . . . .
C11 C 0.55931(17) 0.66022(15) 0.37679(7) 0.0224(3) Uani 1 1 d . . . . .
H11 H 0.574753 0.749228 0.378167 0.027 Uiso 1 1 calc R U . . .
C12 C 0.42004(17) 0.65473(17) 0.38280(8) 0.0256(3) Uani 1 1 d . . . . .
H12 H 0.340995 0.739079 0.388909 0.031 Uiso 1 1 calc R U . . .
C13 C 0.39633(16) 0.52595(17) 0.37986(8) 0.0240(3) Uani 1 1 d . . . . .
H13 H 0.300421 0.522966 0.383341 0.029 Uiso 1 1 calc R U . . .
C14 C 0.51074(15) 0.40036(15) 0.37188(7) 0.0187(3) Uani 1 1 d . . . . .
C15 C 0.82678(16) 0.55298(15) 0.35620(7) 0.0200(3) Uani 1 1 d . . . . .
H15 H 0.898357 0.455522 0.353549 0.024 Uiso 1 1 calc R U . . .
C16 C 0.86666(19) 0.62590(17) 0.41401(8) 0.0282(3) Uani 1 1 d . . . . .
H16A H 0.966831 0.624353 0.405680 0.042 Uiso 1 1 calc R U . . .
H16B H 0.855450 0.575170 0.458414 0.042 Uiso 1 1 calc R U . . .
H16C H 0.803115 0.724647 0.414761 0.042 Uiso 1 1 calc R U . . .
C17 C 0.83803(17) 0.63688(16) 0.28710(8) 0.0226(3) Uani 1 1 d . . . . .
H17A H 0.937100 0.638091 0.277530 0.034 Uiso 1 1 calc R U . . .
H17B H 0.772651 0.734621 0.289510 0.034 Uiso 1 1 calc R U . . .
H17C H 0.811524 0.591394 0.250220 0.034 Uiso 1 1 calc R U . . .
C18 C 0.47795(16) 0.26404(16) 0.36259(8) 0.0223(3) Uani 1 1 d . . . . .
H18 H 0.571170 0.184251 0.361098 0.027 Uiso 1 1 calc R U . . .
C19 C 0.40857(17) 0.27454(17) 0.29407(8) 0.0262(3) Uani 1 1 d . . . . .
H19A H 0.395389 0.183414 0.287179 0.039 Uiso 1 1 calc R U . . .
H19B H 0.471202 0.297457 0.256173 0.039 Uiso 1 1 calc R U . . .
H19C H 0.314842 0.349444 0.295125 0.039 Uiso 1 1 calc R U . . .
C20 C 0.3799(2) 0.2276(2) 0.42209(9) 0.0358(4) Uani 1 1 d . . . . .
H20A H 0.372415 0.133380 0.416874 0.054 Uiso 1 1 calc R U . . .
H20B H 0.283922 0.298789 0.421220 0.054 Uiso 1 1 calc R U . . .
H20C H 0.420835 0.227506 0.466065 0.054 Uiso 1 1 calc R U . . .
C21 C 0.58351(14) 0.52539(14) 0.19059(7) 0.0150(3) Uani 1 1 d . . . . .
C22 C 0.87640(14) 0.24747(13) 0.15767(7) 0.0127(3) Uani 1 1 d . . . . .
C23 C 0.99966(15) 0.24994(14) 0.05535(7) 0.0162(3) Uani 1 1 d . . . . .
H23 H 1.064731 0.269661 0.020091 0.019 Uiso 1 1 calc R U . . .
C24 C 0.91096(14) 0.17321(14) 0.05022(7) 0.0168(3) Uani 1 1 d . . . . .
H24 H 0.901332 0.128859 0.010655 0.020 Uiso 1 1 calc R U . . .
C25 C 1.05334(14) 0.38289(14) 0.14886(7) 0.0155(3) Uani 1 1 d . . . . .
H25 H 1.024668 0.391472 0.199101 0.019 Uiso 1 1 calc R U . . .
C26 C 1.00675(17) 0.53159(15) 0.11303(8) 0.0234(3) Uani 1 1 d . . . . .
H26A H 1.048947 0.592544 0.134684 0.035 Uiso 1 1 calc R U . . .
H26B H 0.901529 0.571623 0.117147 0.035 Uiso 1 1 calc R U . . .
H26C H 1.039832 0.526208 0.064227 0.035 Uiso 1 1 calc R U . . .
C27 C 1.21544(15) 0.31134(16) 0.14096(7) 0.0204(3) Uani 1 1 d . . . . .
H27A H 1.263949 0.365795 0.163333 0.031 Uiso 1 1 calc R U . . .
H27B H 1.246649 0.307634 0.091905 0.031 Uiso 1 1 calc R U . . .
H27C H 1.240155 0.214483 0.162533 0.031 Uiso 1 1 calc R U . . .
C28 C 0.73191(15) 0.09445(15) 0.13182(7) 0.0183(3) Uani 1 1 d . . . . .
H28 H 0.705921 0.099833 0.182393 0.022 Uiso 1 1 calc R U . . .
C29 C 0.80211(18) -0.06156(16) 0.11716(9) 0.0272(3) Uani 1 1 d . . . . .
H29A H 0.739861 -0.116251 0.137121 0.041 Uiso 1 1 calc R U . . .
H29B H 0.895580 -0.098277 0.137683 0.041 Uiso 1 1 calc R U . . .
H29C H 0.816024 -0.070476 0.067263 0.041 Uiso 1 1 calc R U . . .
C30 C 0.59560(17) 0.16468(19) 0.09397(9) 0.0305(4) Uani 1 1 d . . . . .
H30A H 0.524866 0.116046 0.108704 0.046 Uiso 1 1 calc R U . . .
H30B H 0.618268 0.158472 0.044242 0.046 Uiso 1 1 calc R U . . .
H30C H 0.555703 0.264817 0.104552 0.046 Uiso 1 1 calc R U . . .
C31 C 0.48014(15) 0.82051(15) 0.20559(8) 0.0205(3) Uani 1 1 d . . . . .
C32 C 0.29000(16) 0.67178(16) 0.21035(8) 0.0233(3) Uani 1 1 d . . . . .
C33 C 0.30822(17) 0.85982(16) 0.10609(8) 0.0264(3) Uani 1 1 d . . . . .
C34 C 0.38855(15) 0.59031(15) 0.08254(7) 0.0191(3) Uani 1 1 d . . . . .
C35 C 0.58528(16) 0.71654(15) 0.07983(7) 0.0191(3) Uani 1 1 d . . . . .
B1 B 0.79712(16) 0.29803(15) 0.22984(8) 0.0134(3) Uani 1 1 d . . . . .
N1 N 0.77205(12) 0.27840(12) 0.36196(6) 0.0153(2) Uani 1 1 d . . . . .
N2 N 0.67192(12) 0.42795(11) 0.21400(5) 0.0129(2) Uani 1 1 d . . . . .
N3 N 0.97803(12) 0.29441(11) 0.12154(6) 0.0133(2) Uani 1 1 d . . . . .
N4 N 0.83696(12) 0.17148(12) 0.11340(6) 0.0144(2) Uani 1 1 d . . . . .
O1 O 0.50055(13) 0.90056(11) 0.23830(6) 0.0302(3) Uani 1 1 d . . . . .
O2 O 0.19777(12) 0.65701(14) 0.24664(6) 0.0362(3) Uani 1 1 d . . . . .
O3 O 0.22783(15) 0.96010(13) 0.08076(7) 0.0470(4) Uani 1 1 d . . . . .
O4 O 0.35458(12) 0.53334(12) 0.04209(6) 0.0279(2) Uani 1 1 d . . . . .
O5 O 0.67151(12) 0.72739(13) 0.03839(6) 0.0302(3) Uani 1 1 d . . . . .
Cr1 Cr 0.43779(2) 0.69911(2) 0.14584(2) 0.01512(7) 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
C1 N1 1.4031(17) . ?
C1 B1 1.453(2) . ?
C1 C4 1.5370(18) . ?
C2 N1 1.4904(17) . ?
C2 C5 1.530(2) . ?
C2 C6 1.534(2) . ?
C2 C3_11 1.535(2) . ?
C2 C3_12 1.54(3) . ?
C4 C7_12 1.48(3) . ?
C4 C8_11 1.531(2) . ?
C4 C3_11 1.536(2) . ?
C4 C7_11 1.5450(19) . ?
C4 C3_12 1.56(3) . ?
C4 C8_12 1.68(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C3_11 H3A_11 0.9900 . ?
C3_11 H3AB_11 0.9900 . ?
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 . ?
C3_12 H3A_12 0.9900 . ?
C3_12 H3AB_12 0.9900 . ?
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 . ?
C9 C14 1.411(2) . ?
C9 C10 1.4134(19) . ?
C9 N1 1.4301(18) . ?
C10 C11 1.392(2) . ?
C10 C15 1.522(2) . ?
C11 C12 1.383(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(2) . ?
C13 H13 0.9500 . ?
C14 C18 1.523(2) . ?
C15 C17 1.537(2) . ?
C15 C16 1.538(2) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.535(2) . ?
C18 C20 1.539(2) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 N2 1.1619(18) . ?
C21 Cr1 2.0378(14) . ?
C22 N3 1.3553(17) . ?
C22 N4 1.3558(17) . ?
C22 B1 1.5897(19) . ?
C23 C24 1.348(2) . ?
C23 N3 1.3802(17) . ?
C23 H23 0.9500 . ?
C24 N4 1.3779(18) . ?
C24 H24 0.9500 . ?
C25 N3 1.4794(17) . ?
C25 C27 1.5212(19) . ?
C25 C26 1.5245(19) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 N4 1.4787(17) . ?
C28 C30 1.519(2) . ?
C28 C29 1.524(2) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 O1 1.1411(18) . ?
C31 Cr1 1.9140(15) . ?
C32 O2 1.1411(19) . ?
C32 Cr1 1.9102(16) . ?
C33 O3 1.1557(19) . ?
C33 Cr1 1.8486(16) . ?
C34 O4 1.1437(18) . ?
C34 Cr1 1.9036(15) . ?
C35 O5 1.1443(18) . ?
C35 Cr1 1.8953(15) . ?
B1 N2 1.4995(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 B1 127.92(12) . . ?
N1 C1 C4 106.05(11) . . ?
B1 C1 C4 125.92(12) . . ?
N1 C2 C5 112.41(11) . . ?
N1 C2 C6 112.54(12) . . ?
C5 C2 C6 107.36(12) . . ?
N1 C2 C3_11 100.81(11) . . ?
C5 C2 C3_11 110.11(13) . . ?
C6 C2 C3_11 113.64(13) . . ?
N1 C2 C3_12 100.6(11) . . ?
C5 C2 C3_12 135.4(13) . . ?
C6 C2 C3_12 85.2(13) . . ?
C8_11 C4 C3_11 109.23(12) . . ?
C7_12 C4 C1 121.1(12) . . ?
C8_11 C4 C1 115.50(11) . . ?
C3_11 C4 C1 103.06(11) . . ?
C8_11 C4 C7_11 108.05(12) . . ?
C3_11 C4 C7_11 110.92(12) . . ?
C1 C4 C7_11 110.04(11) . . ?
C7_12 C4 C3_12 114.9(17) . . ?
C1 C4 C3_12 104.2(11) . . ?
C7_12 C4 C8_12 107.5(17) . . ?
C1 C4 C8_12 103.7(10) . . ?
C3_12 C4 C8_12 103.6(18) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C3_11 C4 107.39(12) . . ?
C2 C3_11 H3A_11 110.2 . . ?
C4 C3_11 H3A_11 110.2 . . ?
C2 C3_11 H3AB_11 110.2 . . ?
C4 C3_11 H3AB_11 110.2 . . ?
H3A_11 C3_11 H3AB_11 108.5 . . ?
C4 C7_11 H7A_11 109.5 . . ?
C4 C7_11 H7B_11 109.5 . . ?
H7A_11 C7_11 H7B_11 109.5 . . ?
C4 C7_11 H7C_11 109.5 . . ?
H7A_11 C7_11 H7C_11 109.5 . . ?
H7B_11 C7_11 H7C_11 109.5 . . ?
C4 C8_11 H8A_11 109.5 . . ?
C4 C8_11 H8B_11 109.5 . . ?
H8A_11 C8_11 H8B_11 109.5 . . ?
C4 C8_11 H8C_11 109.5 . . ?
H8A_11 C8_11 H8C_11 109.5 . . ?
H8B_11 C8_11 H8C_11 109.5 . . ?
C2 C3_12 C4 105.9(18) . . ?
C2 C3_12 H3A_12 110.5 . . ?
C4 C3_12 H3A_12 110.5 . . ?
C2 C3_12 H3AB_12 110.5 . . ?
C4 C3_12 H3AB_12 110.5 . . ?
H3A_12 C3_12 H3AB_12 108.7 . . ?
C4 C7_12 H7A_12 109.5 . . ?
C4 C7_12 H7B_12 109.5 . . ?
H7A_12 C7_12 H7B_12 109.5 . . ?
C4 C7_12 H7C_12 109.5 . . ?
H7A_12 C7_12 H7C_12 109.5 . . ?
H7B_12 C7_12 H7C_12 109.5 . . ?
C4 C8_12 H8A_12 109.5 . . ?
C4 C8_12 H8B_12 109.5 . . ?
H8A_12 C8_12 H8B_12 109.5 . . ?
C4 C8_12 H8C_12 109.5 . . ?
H8A_12 C8_12 H8C_12 109.5 . . ?
H8B_12 C8_12 H8C_12 109.5 . . ?
C14 C9 C10 120.24(13) . . ?
C14 C9 N1 119.92(12) . . ?
C10 C9 N1 119.80(12) . . ?
C11 C10 C9 118.60(13) . . ?
C11 C10 C15 118.75(13) . . ?
C9 C10 C15 122.52(12) . . ?
C12 C11 C10 121.40(14) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C12 C11 119.74(14) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 121.18(14) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C9 118.73(13) . . ?
C13 C14 C18 118.83(13) . . ?
C9 C14 C18 122.33(13) . . ?
C10 C15 C17 110.24(12) . . ?
C10 C15 C16 112.87(12) . . ?
C17 C15 C16 109.24(12) . . ?
C10 C15 H15 108.1 . . ?
C17 C15 H15 108.1 . . ?
C16 C15 H15 108.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C19 110.55(12) . . ?
C14 C18 C20 112.68(13) . . ?
C19 C18 C20 109.49(13) . . ?
C14 C18 H18 108.0 . . ?
C19 C18 H18 108.0 . . ?
C20 C18 H18 108.0 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 Cr1 176.61(12) . . ?
N3 C22 N4 105.04(11) . . ?
N3 C22 B1 126.92(11) . . ?
N4 C22 B1 126.84(12) . . ?
C24 C23 N3 107.03(12) . . ?
C24 C23 H23 126.5 . . ?
N3 C23 H23 126.5 . . ?
C23 C24 N4 106.82(12) . . ?
C23 C24 H24 126.6 . . ?
N4 C24 H24 126.6 . . ?
N3 C25 C27 110.13(11) . . ?
N3 C25 C26 109.86(11) . . ?
C27 C25 C26 112.13(12) . . ?
N3 C25 H25 108.2 . . ?
C27 C25 H25 108.2 . . ?
C26 C25 H25 108.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 C30 110.35(12) . . ?
N4 C28 C29 109.24(11) . . ?
C30 C28 C29 112.74(13) . . ?
N4 C28 H28 108.1 . . ?
C30 C28 H28 108.1 . . ?
C29 C28 H28 108.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C31 Cr1 175.33(13) . . ?
O2 C32 Cr1 177.05(13) . . ?
O3 C33 Cr1 179.47(16) . . ?
O4 C34 Cr1 175.40(13) . . ?
O5 C35 Cr1 177.87(12) . . ?
C1 B1 N2 126.65(12) . . ?
C1 B1 C22 127.14(12) . . ?
N2 B1 C22 106.21(11) . . ?
C1 N1 C9 122.17(11) . . ?
C1 N1 C2 115.37(11) . . ?
C9 N1 C2 122.27(11) . . ?
C21 N2 B1 168.77(13) . . ?
C22 N3 C23 110.43(11) . . ?
C22 N3 C25 124.74(11) . . ?
C23 N3 C25 124.81(11) . . ?
C22 N4 C24 110.66(11) . . ?
C22 N4 C28 124.07(11) . . ?
C24 N4 C28 125.25(11) . . ?
C33 Cr1 C35 90.67(7) . . ?
C33 Cr1 C34 88.23(6) . . ?
C35 Cr1 C34 87.34(6) . . ?
C33 Cr1 C32 90.73(7) . . ?
C35 Cr1 C32 176.83(6) . . ?
C34 Cr1 C32 89.86(6) . . ?
C33 Cr1 C31 87.75(6) . . ?
C35 Cr1 C31 91.83(6) . . ?
C34 Cr1 C31 175.88(6) . . ?
C32 Cr1 C31 91.06(6) . . ?
C33 Cr1 C21 178.42(6) . . ?
C35 Cr1 C21 88.78(6) . . ?
C34 Cr1 C21 93.22(6) . . ?
C32 Cr1 C21 89.89(6) . . ?
C31 Cr1 C21 90.79(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C4 C7_12 143.4(15) . . . . ?
B1 C1 C4 C7_12 -33.2(15) . . . . ?
N1 C1 C4 C8_11 -139.31(12) . . . . ?
B1 C1 C4 C8_11 44.13(18) . . . . ?
N1 C1 C4 C3_11 -20.29(14) . . . . ?
B1 C1 C4 C3_11 163.15(13) . . . . ?
N1 C1 C4 C7_11 98.05(13) . . . . ?
B1 C1 C4 C7_11 -78.51(16) . . . . ?
N1 C1 C4 C3_12 12.1(15) . . . . ?
B1 C1 C4 C3_12 -164.4(15) . . . . ?
N1 C1 C4 C8_12 -96.1(11) . . . . ?
B1 C1 C4 C8_12 87.4(11) . . . . ?
N1 C2 C3_11 C4 -23.54(14) . . . . ?
C5 C2 C3_11 C4 -142.44(12) . . . . ?
C6 C2 C3_11 C4 97.09(14) . . . . ?
C8_11 C4 C3_11 C2 150.83(12) . . . . ?
C1 C4 C3_11 C2 27.54(14) . . . . ?
C7_11 C4 C3_11 C2 -90.18(14) . . . . ?
N1 C2 C3_12 C4 27(2) . . . . ?
C5 C2 C3_12 C4 -110.8(16) . . . . ?
C6 C2 C3_12 C4 139.3(19) . . . . ?
C7_12 C4 C3_12 C2 -159.8(19) . . . . ?
C1 C4 C3_12 C2 -25(2) . . . . ?
C8_12 C4 C3_12 C2 83(2) . . . . ?
C14 C9 C10 C11 3.8(2) . . . . ?
N1 C9 C10 C11 -178.49(12) . . . . ?
C14 C9 C10 C15 -172.16(12) . . . . ?
N1 C9 C10 C15 5.5(2) . . . . ?
C9 C10 C11 C12 -1.4(2) . . . . ?
C15 C10 C11 C12 174.72(13) . . . . ?
C10 C11 C12 C13 -0.9(2) . . . . ?
C11 C12 C13 C14 0.9(2) . . . . ?
C12 C13 C14 C9 1.5(2) . . . . ?
C12 C13 C14 C18 -174.63(14) . . . . ?
C10 C9 C14 C13 -3.9(2) . . . . ?
N1 C9 C14 C13 178.46(12) . . . . ?
C10 C9 C14 C18 172.11(12) . . . . ?
N1 C9 C14 C18 -5.6(2) . . . . ?
C11 C10 C15 C17 -64.20(16) . . . . ?
C9 C10 C15 C17 111.79(15) . . . . ?
C11 C10 C15 C16 58.27(18) . . . . ?
C9 C10 C15 C16 -125.75(14) . . . . ?
C13 C14 C18 C19 66.08(17) . . . . ?
C9 C14 C18 C19 -109.89(15) . . . . ?
C13 C14 C18 C20 -56.80(18) . . . . ?
C9 C14 C18 C20 127.23(15) . . . . ?
N3 C23 C24 N4 -0.24(14) . . . . ?
N1 C1 B1 N2 -1.8(2) . . . . ?
C4 C1 B1 N2 174.02(12) . . . . ?
N1 C1 B1 C22 177.70(12) . . . . ?
C4 C1 B1 C22 -6.5(2) . . . . ?
N3 C22 B1 C1 -94.00(17) . . . . ?
N4 C22 B1 C1 100.40(17) . . . . ?
N3 C22 B1 N2 85.58(15) . . . . ?
N4 C22 B1 N2 -80.02(15) . . . . ?
B1 C1 N1 C9 -2.5(2) . . . . ?
C4 C1 N1 C9 -178.96(11) . . . . ?
B1 C1 N1 C2 -177.55(13) . . . . ?
C4 C1 N1 C2 5.98(15) . . . . ?
C14 C9 N1 C1 93.16(16) . . . . ?
C10 C9 N1 C1 -84.52(16) . . . . ?
C14 C9 N1 C2 -92.11(16) . . . . ?
C10 C9 N1 C2 90.21(16) . . . . ?
C5 C2 N1 C1 128.20(13) . . . . ?
C6 C2 N1 C1 -110.43(14) . . . . ?
C3_11 C2 N1 C1 10.98(15) . . . . ?
C3_12 C2 N1 C1 -21.3(14) . . . . ?
C5 C2 N1 C9 -46.86(17) . . . . ?
C6 C2 N1 C9 74.51(16) . . . . ?
C3_11 C2 N1 C9 -164.08(12) . . . . ?
C3_12 C2 N1 C9 163.6(14) . . . . ?
C1 B1 N2 C21 177.6(6) . . . . ?
C22 B1 N2 C21 -2.0(7) . . . . ?
N4 C22 N3 C23 0.93(14) . . . . ?
B1 C22 N3 C23 -167.17(12) . . . . ?
N4 C22 N3 C25 179.98(11) . . . . ?
B1 C22 N3 C25 11.9(2) . . . . ?
C24 C23 N3 C22 -0.44(15) . . . . ?
C24 C23 N3 C25 -179.49(11) . . . . ?
C27 C25 N3 C22 124.58(13) . . . . ?
C26 C25 N3 C22 -111.43(14) . . . . ?
C27 C25 N3 C23 -56.50(16) . . . . ?
C26 C25 N3 C23 67.49(16) . . . . ?
N3 C22 N4 C24 -1.09(14) . . . . ?
B1 C22 N4 C24 167.03(12) . . . . ?
N3 C22 N4 C28 177.26(11) . . . . ?
B1 C22 N4 C28 -14.6(2) . . . . ?
C23 C24 N4 C22 0.85(15) . . . . ?
C23 C24 N4 C28 -177.48(12) . . . . ?
C30 C28 N4 C22 111.77(14) . . . . ?
C29 C28 N4 C22 -123.74(14) . . . . ?
C30 C28 N4 C24 -70.12(17) . . . . ?
C29 C28 N4 C24 54.37(17) . . . . ?

_refine_diff_density_max         0.297
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.042



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_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_AnRe179_ref_a
_database_code_depnum_ccdc_archive 'CCDC 2071474'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_AnRe179_ref_a       
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         14 Report
RESPONSE: Reflections affected by beamstop
;
_audit_creation_method           'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        (CAAC)(IiPr)B(CN)
_chemical_name_common            2(CN)
_chemical_melting_point          ?
_chemical_formula_moiety         '2 (C30 H47 B N4), (C6 H6)'
_chemical_formula_sum            'C66 H100 B2 N8'
_chemical_formula_weight         1027.15

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                   32.7131(2)
_cell_length_b                   9.67986(7)
_cell_length_c                   21.35114(15)
_cell_angle_alpha                90.0
_cell_angle_beta                 108.9322(8)
_cell_angle_gamma                90.0
_cell_volume                     6395.27(8)
_cell_formula_units_Z            4.00
_cell_measurement_temperature    99.99(11)
_cell_measurement_reflns_used    28729
_cell_measurement_theta_min      2.8770
_cell_measurement_theta_max      77.1920
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_F_000             2248.000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.047
_exptl_absorpt_coefficient_mu    0.467
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian

_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99.99(11)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            60303
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.856
_diffrn_reflns_theta_max         77.467
_diffrn_reflns_theta_full        72.130
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13395
_reflns_number_gt                11364
_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 1.171.40.71a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/4 (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          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.

The asymmetric unit contains two half benzene molecules positioned on inversion centers
and two molecules of the compound, one of which presents a twofold disorder in the C2 > C8 CAAC backbone
(RESI 51 and 52 CAAC) modelled with FVAR in a 95:5 ratio, with SIMU 0.01 and SAME restraints.

;
_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+1.8263P] 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         13395
_refine_ls_number_parameters     807
_refine_ls_number_restraints     223
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1128
_refine_ls_wR_factor_gt          0.1074
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.039
_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
C1_1 C 0.64218(4) 0.38747(12) 0.23810(5) 0.0218(2) Uani 1 1 d . . . . .
N1_1 N 0.67076(3) 0.42725(10) 0.20430(5) 0.0230(2) Uani 1 1 d . . . . .
C2_1 C 0.70430(4) 0.32365(13) 0.20440(6) 0.0281(3) Uani 1 1 d . . . . .
C3_1 C 0.69848(4) 0.21897(13) 0.25476(6) 0.0285(2) Uani 1 1 d . . . . .
H3A_1 H 0.719114 0.236975 0.298224 0.034 Uiso 1 1 calc R U . . .
H3AB_1 H 0.703097 0.125836 0.241673 0.034 Uiso 1 1 calc R U . . .
C4_1 C 0.65203(4) 0.23471(12) 0.25642(6) 0.0245(2) Uani 1 1 d . . . . .
C5_1 C 0.69733(5) 0.26016(16) 0.13564(7) 0.0389(3) Uani 1 1 d . . . . .
H5A_1 H 0.718516 0.189464 0.139008 0.058 Uiso 1 1 calc R U . . .
H5B_1 H 0.700198 0.330764 0.105769 0.058 Uiso 1 1 calc R U . . .
H5C_1 H 0.668916 0.220632 0.119246 0.058 Uiso 1 1 calc R U . . .
C6_1 C 0.75001(4) 0.38376(16) 0.22790(8) 0.0379(3) Uani 1 1 d . . . . .
H6A_1 H 0.770462 0.312321 0.228376 0.057 Uiso 1 1 calc R U . . .
H6B_1 H 0.756119 0.420591 0.271738 0.057 Uiso 1 1 calc R U . . .
H6C_1 H 0.752133 0.456082 0.198352 0.057 Uiso 1 1 calc R U . . .
C7_1 C 0.65047(4) 0.19250(14) 0.32476(6) 0.0314(3) Uani 1 1 d . . . . .
H7A_1 H 0.662207 0.101278 0.335259 0.047 Uiso 1 1 calc R U . . .
H7B_1 H 0.621045 0.193295 0.324389 0.047 Uiso 1 1 calc R U . . .
H7C_1 H 0.667167 0.256472 0.357443 0.047 Uiso 1 1 calc R U . . .
C8_1 C 0.62056(4) 0.14070(14) 0.20476(7) 0.0322(3) Uani 1 1 d . . . . .
H8A_1 H 0.629528 0.046222 0.213443 0.048 Uiso 1 1 calc R U . . .
H8B_1 H 0.620540 0.165920 0.161264 0.048 Uiso 1 1 calc R U . . .
H8C_1 H 0.591969 0.151320 0.207332 0.048 Uiso 1 1 calc R U . . .
C9_1 C 0.66796(4) 0.56160(12) 0.17554(5) 0.0229(2) Uani 1 1 d . . . . .
C10_1 C 0.69054(4) 0.67387(13) 0.21349(6) 0.0249(2) Uani 1 1 d . . . . .
C11_1 C 0.68627(4) 0.80404(13) 0.18437(6) 0.0295(3) Uani 1 1 d . . . . .
H11_1 H 0.702094 0.877539 0.208378 0.035 Uiso 1 1 calc R U . . .
C12_1 C 0.65901(4) 0.82646(14) 0.12051(6) 0.0318(3) Uani 1 1 d . . . . .
H12_1 H 0.656322 0.914368 0.102038 0.038 Uiso 1 1 calc R U . . .
C13_1 C 0.63585(4) 0.71758(14) 0.08444(6) 0.0304(3) Uani 1 1 d . . . . .
H13_1 H 0.617223 0.733386 0.041756 0.036 Uiso 1 1 calc R U . . .
C14_1 C 0.63971(4) 0.58438(13) 0.11044(6) 0.0260(2) Uani 1 1 d . . . . .
C15_1 C 0.61145(4) 0.47146(14) 0.06875(6) 0.0333(3) Uani 1 1 d . . . . .
H15_1 H 0.617962 0.384863 0.093811 0.040 Uiso 1 1 calc R U . . .
C16_1 C 0.56342(5) 0.50385(17) 0.05424(7) 0.0411(3) Uani 1 1 d . . . . .
H16A_1 H 0.546422 0.425822 0.033007 0.062 Uiso 1 1 calc R U . . .
H16B_1 H 0.555673 0.582844 0.025629 0.062 Uiso 1 1 calc R U . . .
H16C_1 H 0.558066 0.523183 0.094990 0.062 Uiso 1 1 calc R U . . .
C17_1 C 0.62060(6) 0.45050(18) 0.00318(7) 0.0463(4) Uani 1 1 d . . . . .
H17A_1 H 0.603632 0.374728 -0.020643 0.069 Uiso 1 1 calc R U . . .
H17B_1 H 0.650726 0.430657 0.012241 0.069 Uiso 1 1 calc R U . . .
H17C_1 H 0.613169 0.533009 -0.023014 0.069 Uiso 1 1 calc R U . . .
C18_1 C 0.71699(4) 0.66251(14) 0.28656(6) 0.0299(3) Uani 1 1 d . . . . .
H18_1 H 0.716385 0.566054 0.300177 0.036 Uiso 1 1 calc R U . . .
C19_1 C 0.69709(5) 0.75227(16) 0.32842(7) 0.0372(3) Uani 1 1 d . . . . .
H19A_1 H 0.712737 0.738595 0.374524 0.056 Uiso 1 1 calc R U . . .
H19B_1 H 0.667409 0.726623 0.319648 0.056 Uiso 1 1 calc R U . . .
H19C_1 H 0.698681 0.847751 0.317267 0.056 Uiso 1 1 calc R U . . .
C20_1 C 0.76441(4) 0.70497(17) 0.30058(8) 0.0412(3) Uani 1 1 d . . . . .
H20A_1 H 0.780409 0.687290 0.346211 0.062 Uiso 1 1 calc R U . . .
H20B_1 H 0.765832 0.801637 0.291455 0.062 Uiso 1 1 calc R U . . .
H20C_1 H 0.776602 0.652493 0.272823 0.062 Uiso 1 1 calc R U . . .
B1_1 B 0.60837(4) 0.47269(14) 0.24961(6) 0.0221(2) Uani 1 1 d . . . . .
C21_1 C 0.59441(4) 0.62106(13) 0.22453(6) 0.0241(2) Uani 1 1 d . . . . .
N2_1 N 0.57968(4) 0.72976(12) 0.20846(6) 0.0330(2) Uani 1 1 d . . . . .
C22_1 C 0.57877(3) 0.42081(12) 0.29115(5) 0.0213(2) Uani 1 1 d . . . . .
N3_1 N 0.58657(3) 0.43647(10) 0.35704(5) 0.02242(19) Uani 1 1 d . . . . .
C23_1 C 0.55172(4) 0.39016(13) 0.37409(6) 0.0247(2) Uani 1 1 d . . . . .
H23_1 H 0.549428 0.389735 0.416386 0.030 Uiso 1 1 calc R U . . .
C24_1 C 0.52158(4) 0.34566(13) 0.31825(6) 0.0253(2) Uani 1 1 d . . . . .
H24_1 H 0.494599 0.309101 0.314485 0.030 Uiso 1 1 calc R U . . .
N4_1 N 0.53880(3) 0.36519(10) 0.26757(5) 0.0229(2) Uani 1 1 d . . . . .
C25_1 C 0.62520(4) 0.50560(13) 0.40247(5) 0.0240(2) Uani 1 1 d . . . . .
H25_1 H 0.648152 0.501993 0.382296 0.029 Uiso 1 1 calc R U . . .
C26_1 C 0.64103(4) 0.42907(15) 0.46830(6) 0.0316(3) Uani 1 1 d . . . . .
H26A_1 H 0.667065 0.471577 0.496292 0.047 Uiso 1 1 calc R U . . .
H26B_1 H 0.646726 0.334387 0.460616 0.047 Uiso 1 1 calc R U . . .
H26C_1 H 0.619269 0.433024 0.489484 0.047 Uiso 1 1 calc R U . . .
C27_1 C 0.61516(4) 0.65611(14) 0.41048(6) 0.0302(3) Uani 1 1 d . . . . .
H27A_1 H 0.640620 0.701332 0.438633 0.045 Uiso 1 1 calc R U . . .
H27B_1 H 0.592593 0.662208 0.429986 0.045 Uiso 1 1 calc R U . . .
H27C_1 H 0.605918 0.700152 0.367891 0.045 Uiso 1 1 calc R U . . .
C28_1 C 0.51617(4) 0.33498(13) 0.19691(6) 0.0268(2) Uani 1 1 d . . . . .
H28_1 H 0.537213 0.342508 0.173247 0.032 Uiso 1 1 calc R U . . .
C29_1 C 0.49901(4) 0.18809(14) 0.18900(6) 0.0313(3) Uani 1 1 d . . . . .
H29A_1 H 0.487319 0.165934 0.142773 0.047 Uiso 1 1 calc R U . . .
H29B_1 H 0.476758 0.179999 0.209050 0.047 Uiso 1 1 calc R U . . .
H29C_1 H 0.522113 0.125440 0.210181 0.047 Uiso 1 1 calc R U . . .
C30_1 C 0.48075(5) 0.44090(16) 0.16778(7) 0.0380(3) Uani 1 1 d . . . . .
H30A_1 H 0.467032 0.422190 0.121530 0.057 Uiso 1 1 calc R U . . .
H30B_1 H 0.493128 0.531812 0.173111 0.057 Uiso 1 1 calc R U . . .
H30C_1 H 0.459721 0.435545 0.190298 0.057 Uiso 1 1 calc R U . . .
C1_2 C 0.85829(3) 0.38901(12) 0.58832(5) 0.0208(2) Uani 1 1 d . . . . .
N1_2 N 0.83160(3) 0.43109(10) 0.52538(5) 0.02197(19) Uani 1 1 d . . . . .
C2_51 C 0.79809(7) 0.3302(2) 0.48940(9) 0.0261(3) Uani 0.948(2) 1 d D U P A 1
C3_51 C 0.80041(4) 0.22696(14) 0.54480(6) 0.0276(3) Uani 0.948(2) 1 d D U P A 1
H3A_51 H 0.795520 0.133842 0.527150 0.033 Uiso 0.948(2) 1 calc R U P A 1
H3AB_51 H 0.778528 0.248230 0.564990 0.033 Uiso 0.948(2) 1 calc R U P A 1
C4_51 C 0.84577(6) 0.2387(3) 0.59636(8) 0.0248(3) Uani 0.948(2) 1 d D U P A 1
C5_51 C 0.80766(5) 0.26129(18) 0.43061(7) 0.0334(3) Uani 0.948(2) 1 d D U P A 1
H5A_51 H 0.786215 0.192045 0.411580 0.050 Uiso 0.948(2) 1 calc R U P A 1
H5B_51 H 0.835721 0.219094 0.445823 0.050 Uiso 0.948(2) 1 calc R U P A 1
H5C_51 H 0.807007 0.329807 0.397788 0.050 Uiso 0.948(2) 1 calc R U P A 1
C6_51 C 0.75331(5) 0.39496(19) 0.46204(10) 0.0392(4) Uani 0.948(2) 1 d D U P A
1
H6A_51 H 0.732848 0.325888 0.439164 0.059 Uiso 0.948(2) 1 calc R U P A 1
H6B_51 H 0.753905 0.467887 0.431879 0.059 Uiso 0.948(2) 1 calc R U P A 1
H6C_51 H 0.744988 0.431874 0.497855 0.059 Uiso 0.948(2) 1 calc R U P A 1
C7_51 C 0.87801(4) 0.13879(14) 0.58132(8) 0.0303(3) Uani 0.948(2) 1 d D U P A 1
H7A_51 H 0.867704 0.045724 0.580466 0.045 Uiso 0.948(2) 1 calc R U P A 1
H7B_51 H 0.905676 0.147173 0.615064 0.045 Uiso 0.948(2) 1 calc R U P A 1
H7C_51 H 0.880750 0.161197 0.539068 0.045 Uiso 0.948(2) 1 calc R U P A 1
C8_51 C 0.84347(6) 0.20142(16) 0.66478(8) 0.0367(4) Uani 0.948(2) 1 d D U P A 1
H8A_51 H 0.831300 0.110760 0.663338 0.055 Uiso 0.948(2) 1 calc R U P A 1
H8B_51 H 0.825639 0.267346 0.677376 0.055 Uiso 0.948(2) 1 calc R U P A 1
H8C_51 H 0.872022 0.202769 0.696542 0.055 Uiso 0.948(2) 1 calc R U P A 1
C2_52 C 0.7998(12) 0.326(4) 0.4845(15) 0.029(3) Uani 0.052(2) 1 d D U P A 2
C3_52 C 0.8195(7) 0.198(2) 0.5239(10) 0.028(3) Uani 0.052(2) 1 d D U P A 2
H3A_52 H 0.837268 0.150382 0.502037 0.034 Uiso 0.052(2) 1 calc R U P A 2
H3AB_52 H 0.796638 0.135295 0.525352 0.034 Uiso 0.052(2) 1 calc R U P A 2
C4_52 C 0.8471(10) 0.236(5) 0.5945(12) 0.029(3) Uani 0.052(2) 1 d D U P A 2
C5_52 C 0.7951(10) 0.326(3) 0.4107(12) 0.037(5) Uani 0.052(2) 1 d D U P A 2
H5A_52 H 0.775564 0.253220 0.388797 0.055 Uiso 0.052(2) 1 calc R U P A 2
H5B_52 H 0.822788 0.310015 0.405641 0.055 Uiso 0.052(2) 1 calc R U P A 2
H5C_52 H 0.783846 0.412963 0.391526 0.055 Uiso 0.052(2) 1 calc R U P A 2
C6_52 C 0.7562(9) 0.362(3) 0.4917(16) 0.046(6) Uani 0.052(2) 1 d D U P A 2
H6A_52 H 0.734122 0.305595 0.461924 0.068 Uiso 0.052(2) 1 calc R U P A 2
H6B_52 H 0.749893 0.457372 0.481327 0.068 Uiso 0.052(2) 1 calc R U P A 2
H6C_52 H 0.757097 0.344235 0.536396 0.068 Uiso 0.052(2) 1 calc R U P A 2
C7_52 C 0.8857(8) 0.138(3) 0.6220(14) 0.036(4) Uani 0.052(2) 1 d D U P A 2
H7A_52 H 0.876993 0.045370 0.608123 0.054 Uiso 0.052(2) 1 calc R U P A 2
H7B_52 H 0.895815 0.142682 0.669445 0.054 Uiso 0.052(2) 1 calc R U P A 2
H7C_52 H 0.908591 0.165325 0.605492 0.054 Uiso 0.052(2) 1 calc R U P A 2
C8_52 C 0.8196(10) 0.231(3) 0.6405(14) 0.041(5) Uani 0.052(2) 1 d D U P A 2
H8A_52 H 0.810770 0.137112 0.643876 0.061 Uiso 0.052(2) 1 calc R U P A 2
H8B_52 H 0.794476 0.287754 0.622776 0.061 Uiso 0.052(2) 1 calc R U P A 2
H8C_52 H 0.836267 0.263704 0.683599 0.061 Uiso 0.052(2) 1 calc R U P A 2
C9_2 C 0.83602(3) 0.56610(12) 0.50130(5) 0.0210(2) Uani 1 1 d . . . . .
C10_2 C 0.81395(4) 0.67918(12) 0.51741(5) 0.0232(2) Uani 1 1 d . . . . .
C11_2 C 0.81948(4) 0.81000(13) 0.49408(6) 0.0265(2) Uani 1 1 d . . . . .
H11_2 H 0.804078 0.884261 0.502731 0.032 Uiso 1 1 calc R U . . .
C12_2 C 0.84739(4) 0.83162(13) 0.45835(6) 0.0282(2) Uani 1 1 d . . . . .
H12_2 H 0.850803 0.919661 0.443322 0.034 Uiso 1 1 calc R U . . .
C13_2 C 0.87012(4) 0.72182(13) 0.44516(6) 0.0264(2) Uani 1 1 d . . . . .
H13_2 H 0.889388 0.737330 0.422058 0.032 Uiso 1 1 calc R U . . .
C14_2 C 0.86495(4) 0.58820(13) 0.46554(5) 0.0233(2) Uani 1 1 d . . . . .
C15_2 C 0.78656(4) 0.66783(14) 0.56302(6) 0.0269(2) Uani 1 1 d . . . . .
H15_2 H 0.785801 0.570656 0.575465 0.032 Uiso 1 1 calc R U . . .
C16_2 C 0.73993(4) 0.71671(16) 0.52947(7) 0.0353(3) Uani 1 1 d . . . . .
H16A_2 H 0.723689 0.704759 0.559330 0.053 Uiso 1 1 calc R U . . .
H16B_2 H 0.726938 0.663368 0.490116 0.053 Uiso 1 1 calc R U . . .
H16C_2 H 0.739980 0.812579 0.517989 0.053 Uiso 1 1 calc R U . . .
C17_2 C 0.80682(4) 0.75238(15) 0.62645(6) 0.0340(3) Uani 1 1 d . . . . .
H17A_2 H 0.791358 0.735061 0.656950 0.051 Uiso 1 1 calc R U . . .
H17B_2 H 0.805245 0.848952 0.615688 0.051 Uiso 1 1 calc R U . . .
H17C_2 H 0.836510 0.725959 0.646350 0.051 Uiso 1 1 calc R U . . .
C18_2 C 0.89231(4) 0.47368(13) 0.45095(6) 0.0276(2) Uani 1 1 d . . . . .
H18_2 H 0.885052 0.387101 0.468672 0.033 Uiso 1 1 calc R U . . .
C19_2 C 0.88300(4) 0.45542(16) 0.37606(7) 0.0360(3) Uani 1 1 d . . . . .
H19A_2 H 0.899493 0.379063 0.368384 0.054 Uiso 1 1 calc R U . . .
H19B_2 H 0.890938 0.538117 0.358014 0.054 Uiso 1 1 calc R U . . .
H19C_2 H 0.852759 0.437677 0.355031 0.054 Uiso 1 1 calc R U . . .
C20_2 C 0.94071(4) 0.50171(15) 0.48467(7) 0.0338(3) Uani 1 1 d . . . . .
H20A_2 H 0.957115 0.424126 0.478026 0.051 Uiso 1 1 calc R U . . .
H20B_2 H 0.946365 0.515583 0.531240 0.051 Uiso 1 1 calc R U . . .
H20C_2 H 0.948889 0.582922 0.465819 0.051 Uiso 1 1 calc R U . . .
B1_2 B 0.89263(4) 0.46950(14) 0.63519(6) 0.0217(2) Uani 1 1 d . . . . .
C21_2 C 0.90922(4) 0.61515(12) 0.62538(5) 0.0232(2) Uani 1 1 d . . . . .
N2_2 N 0.92550(4) 0.72175(12) 0.62507(5) 0.0323(2) Uani 1 1 d . . . . .
C22_2 C 0.91981(3) 0.41498(12) 0.70675(5) 0.0210(2) Uani 1 1 d . . . . .
N3_2 N 0.95943(3) 0.35622(10) 0.72552(5) 0.02250(19) Uani 1 1 d . . . . .
C23_2 C 0.97457(4) 0.33584(12) 0.79334(6) 0.0247(2) Uani 1 1 d . . . . .
H23_2 H 1.000970 0.297490 0.817936 0.030 Uiso 1 1 calc R U . . .
C24_2 C 0.94350(4) 0.38256(12) 0.81666(5) 0.0246(2) Uani 1 1 d . . . . .
H24_2 H 0.944394 0.382057 0.860645 0.030 Uiso 1 1 calc R U . . .
N4_2 N 0.91015(3) 0.43123(10) 0.76350(4) 0.02222(19) Uani 1 1 d . . . . .
C25_2 C 0.98355(4) 0.32410(13) 0.67952(6) 0.0260(2) Uani 1 1 d . . . . .
H25_2 H 0.963468 0.331838 0.634216 0.031 Uiso 1 1 calc R U . . .
C26_2 C 1.00025(4) 0.17675(14) 0.68970(6) 0.0306(3) Uani 1 1 d . . . . .
H26A_2 H 1.012664 0.153476 0.656039 0.046 Uiso 1 1 calc R U . . .
H26B_2 H 0.976778 0.114970 0.687001 0.046 Uiso 1 1 calc R U . . .
H26C_2 H 1.021854 0.168582 0.732487 0.046 Uiso 1 1 calc R U . . .
C27_2 C 1.01954(5) 0.42851(15) 0.68759(8) 0.0372(3) Uani 1 1 d . . . . .
H27A_2 H 1.034501 0.407976 0.656759 0.056 Uiso 1 1 calc R U . . .
H27B_2 H 1.039421 0.423896 0.731924 0.056 Uiso 1 1 calc R U . . .
H27C_2 H 1.007439 0.519686 0.679193 0.056 Uiso 1 1 calc R U . . .
C28_2 C 0.87124(4) 0.50286(13) 0.76760(6) 0.0256(2) Uani 1 1 d . . . . .
H28_2 H 0.849820 0.504686 0.723156 0.031 Uiso 1 1 calc R U . . .
C29_2 C 0.88268(4) 0.65107(14) 0.78967(6) 0.0310(3) Uani 1 1 d . . . . .
H29A_2 H 0.857309 0.698258 0.791604 0.047 Uiso 1 1 calc R U . . .
H29B_2 H 0.893717 0.696979 0.758649 0.047 Uiso 1 1 calc R U . . .
H29C_2 H 0.904256 0.651668 0.832705 0.047 Uiso 1 1 calc R U . . .
C30_2 C 0.85175(4) 0.42460(16) 0.81306(7) 0.0348(3) Uani 1 1 d . . . . .
H30A_2 H 0.825058 0.467510 0.811901 0.052 Uiso 1 1 calc R U . . .
H30B_2 H 0.871536 0.426427 0.857520 0.052 Uiso 1 1 calc R U . . .
H30C_2 H 0.846386 0.330574 0.798392 0.052 Uiso 1 1 calc R U . . .
C1_3 C 0.4723(3) 0.6108(12) 0.4631(5) 0.043(2) Uani 0.5 1 d G . P B -1
H1_3 H 0.453638 0.676332 0.436957 0.052 Uiso 0.5 1 calc R U P B -1
C2_3 C 0.4657(3) 0.4713(13) 0.4477(4) 0.0341(15) Uani 0.5 1 d G . P B -1
H2_3 H 0.442736 0.443497 0.411183 0.041 Uiso 0.5 1 calc R U P B -1
C3_3 C 0.4936(2) 0.3733(12) 0.4867(4) 0.0351(14) Uani 0.5 1 d G . P B -1
H3_3 H 0.489214 0.279989 0.476410 0.042 Uiso 0.5 1 calc R U P B -1
C4_3 C 0.5280(2) 0.4149(13) 0.5413(4) 0.0311(13) Uani 0.5 1 d G . P B -1
H4_3 H 0.546595 0.349313 0.567411 0.037 Uiso 0.5 1 calc R U P B -1
C5_3 C 0.5345(3) 0.5544(13) 0.5567(5) 0.039(2) Uani 0.5 1 d G . P B -1
H5_3 H 0.557498 0.582147 0.593186 0.047 Uiso 0.5 1 calc R U P B -1
C6_3 C 0.5066(3) 0.6523(12) 0.5176(5) 0.0410(19) Uani 0.5 1 d G . P B -1
H6_3 H 0.511020 0.745659 0.527960 0.049 Uiso 0.5 1 calc R U P B -1
C1_4 C 0.97307(17) 0.4004(10) 1.0076(4) 0.0301(18) Uani 0.5 1 d G . P C -1
H1_4 H 0.955010 0.330038 1.012622 0.036 Uiso 0.5 1 calc R U P C -1
C2_4 C 0.96636(18) 0.5354(10) 1.0243(4) 0.037(2) Uani 0.5 1 d G . P C -1
H2_4 H 0.943799 0.555305 1.040404 0.044 Uiso 0.5 1 calc R U P C -1
C3_4 C 0.99335(19) 0.6405(10) 1.0168(4) 0.0351(19) Uani 0.5 1 d G . P C -1
H3_4 H 0.988857 0.730800 1.027985 0.042 Uiso 0.5 1 calc R U P C -1
C4_4 C 1.02706(18) 0.6107(10) 0.9928(4) 0.045(3) Uani 0.5 1 d G . P C -1
H4_4 H 1.045126 0.681031 0.987786 0.054 Uiso 0.5 1 calc R U P C -1
C5_4 C 1.03378(17) 0.4757(10) 0.9761(4) 0.034(2) Uani 0.5 1 d G . P C -1
H5_4 H 1.056338 0.455765 0.960003 0.041 Uiso 0.5 1 calc R U P C -1
C6_4 C 1.00679(17) 0.3706(10) 0.9836(4) 0.037(2) Uani 0.5 1 d G . P C -1
H6_4 H 1.011281 0.280267 0.972421 0.045 Uiso 0.5 1 calc R U P C -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1_1 N1_1 1.4076(14) . ?
C1_1 B1_1 1.4630(17) . ?
C1_1 C4_1 1.5369(16) . ?
N1_1 C9_1 1.4284(15) . ?
N1_1 C2_1 1.4858(15) . ?
C2_1 C6_1 1.5295(18) . ?
C2_1 C3_1 1.5335(17) . ?
C2_1 C5_1 1.5388(18) . ?
C3_1 C4_1 1.5389(16) . ?
C3_1 H3A_1 0.9700 . ?
C3_1 H3AB_1 0.9700 . ?
C4_1 C7_1 1.5319(16) . ?
C4_1 C8_1 1.5389(17) . ?
C5_1 H5A_1 0.9600 . ?
C5_1 H5B_1 0.9600 . ?
C5_1 H5C_1 0.9600 . ?
C6_1 H6A_1 0.9600 . ?
C6_1 H6B_1 0.9600 . ?
C6_1 H6C_1 0.9600 . ?
C7_1 H7A_1 0.9600 . ?
C7_1 H7B_1 0.9600 . ?
C7_1 H7C_1 0.9600 . ?
C8_1 H8A_1 0.9600 . ?
C8_1 H8B_1 0.9600 . ?
C8_1 H8C_1 0.9600 . ?
C9_1 C10_1 1.4123(17) . ?
C9_1 C14_1 1.4148(16) . ?
C10_1 C11_1 1.3920(18) . ?
C10_1 C18_1 1.5227(17) . ?
C11_1 C12_1 1.3829(19) . ?
C11_1 H11_1 0.9300 . ?
C12_1 C13_1 1.378(2) . ?
C12_1 H12_1 0.9300 . ?
C13_1 C14_1 1.3933(18) . ?
C13_1 H13_1 0.9300 . ?
C14_1 C15_1 1.5190(18) . ?
C15_1 C16_1 1.532(2) . ?
C15_1 C17_1 1.5371(19) . ?
C15_1 H15_1 0.9800 . ?
C16_1 H16A_1 0.9600 . ?
C16_1 H16B_1 0.9600 . ?
C16_1 H16C_1 0.9600 . ?
C17_1 H17A_1 0.9600 . ?
C17_1 H17B_1 0.9600 . ?
C17_1 H17C_1 0.9600 . ?
C18_1 C19_1 1.5347(18) . ?
C18_1 C20_1 1.5373(18) . ?
C18_1 H18_1 0.9800 . ?
C19_1 H19A_1 0.9600 . ?
C19_1 H19B_1 0.9600 . ?
C19_1 H19C_1 0.9600 . ?
C20_1 H20A_1 0.9600 . ?
C20_1 H20B_1 0.9600 . ?
C20_1 H20C_1 0.9600 . ?
B1_1 C21_1 1.5490(18) . ?
B1_1 C22_1 1.5918(16) . ?
C21_1 N2_1 1.1618(16) . ?
C22_1 N4_1 1.3513(14) . ?
C22_1 N3_1 1.3544(14) . ?
N3_1 C23_1 1.3795(14) . ?
N3_1 C25_1 1.4799(14) . ?
C23_1 C24_1 1.3476(17) . ?
C23_1 H23_1 0.9300 . ?
C24_1 N4_1 1.3853(14) . ?
C24_1 H24_1 0.9300 . ?
N4_1 C28_1 1.4782(14) . ?
C25_1 C27_1 1.5153(18) . ?
C25_1 C26_1 1.5231(16) . ?
C25_1 H25_1 0.9800 . ?
C26_1 H26A_1 0.9600 . ?
C26_1 H26B_1 0.9600 . ?
C26_1 H26C_1 0.9600 . ?
C27_1 H27A_1 0.9600 . ?
C27_1 H27B_1 0.9600 . ?
C27_1 H27C_1 0.9600 . ?
C28_1 C29_1 1.5178(18) . ?
C28_1 C30_1 1.5208(18) . ?
C28_1 H28_1 0.9800 . ?
C29_1 H29A_1 0.9600 . ?
C29_1 H29B_1 0.9600 . ?
C29_1 H29C_1 0.9600 . ?
C30_1 H30A_1 0.9600 . ?
C30_1 H30B_1 0.9600 . ?
C30_1 H30C_1 0.9600 . ?
C1_2 N1_2 1.4046(14) . ?
C1_2 B1_2 1.4632(17) . ?
C1_2 C4_51 1.536(3) . ?
C1_2 C4_52 1.54(5) . ?
N1_2 C9_2 1.4287(15) . ?
N1_2 C2_51 1.483(3) . ?
N1_2 C2_52 1.51(5) . ?
C2_51 C6_51 1.525(2) . ?
C2_51 C3_51 1.531(2) . ?
C2_51 C5_51 1.541(2) . ?
C3_51 C4_51 1.538(2) . ?
C3_51 H3A_51 0.9700 . ?
C3_51 H3AB_51 0.9700 . ?
C4_51 C8_51 1.530(2) . ?
C4_51 C7_51 1.540(2) . ?
C5_51 H5A_51 0.9600 . ?
C5_51 H5B_51 0.9600 . ?
C5_51 H5C_51 0.9600 . ?
C6_51 H6A_51 0.9600 . ?
C6_51 H6B_51 0.9600 . ?
C6_51 H6C_51 0.9600 . ?
C7_51 H7A_51 0.9600 . ?
C7_51 H7B_51 0.9600 . ?
C7_51 H7C_51 0.9600 . ?
C8_51 H8A_51 0.9600 . ?
C8_51 H8B_51 0.9600 . ?
C8_51 H8C_51 0.9600 . ?
C2_52 C3_52 1.521(19) . ?
C2_52 C6_52 1.52(2) . ?
C2_52 C5_52 1.532(19) . ?
C3_52 C4_52 1.53(2) . ?
C3_52 H3A_52 0.9700 . ?
C3_52 H3AB_52 0.9700 . ?
C4_52 C8_52 1.53(2) . ?
C4_52 C7_52 1.535(19) . ?
C5_52 H5A_52 0.9600 . ?
C5_52 H5B_52 0.9600 . ?
C5_52 H5C_52 0.9600 . ?
C6_52 H6A_52 0.9600 . ?
C6_52 H6B_52 0.9600 . ?
C6_52 H6C_52 0.9600 . ?
C7_52 H7A_52 0.9600 . ?
C7_52 H7B_52 0.9600 . ?
C7_52 H7C_52 0.9600 . ?
C8_52 H8A_52 0.9600 . ?
C8_52 H8B_52 0.9600 . ?
C8_52 H8C_52 0.9600 . ?
C9_2 C14_2 1.4121(15) . ?
C9_2 C10_2 1.4137(16) . ?
C10_2 C11_2 1.3939(17) . ?
C10_2 C15_2 1.5262(15) . ?
C11_2 C12_2 1.3828(17) . ?
C11_2 H11_2 0.9300 . ?
C12_2 C13_2 1.3774(18) . ?
C12_2 H12_2 0.9300 . ?
C13_2 C14_2 1.3923(17) . ?
C13_2 H13_2 0.9300 . ?
C14_2 C18_2 1.5191(17) . ?
C15_2 C16_2 1.5345(17) . ?
C15_2 C17_2 1.5366(17) . ?
C15_2 H15_2 0.9800 . ?
C16_2 H16A_2 0.9600 . ?
C16_2 H16B_2 0.9600 . ?
C16_2 H16C_2 0.9600 . ?
C17_2 H17A_2 0.9600 . ?
C17_2 H17B_2 0.9600 . ?
C17_2 H17C_2 0.9600 . ?
C18_2 C20_2 1.5358(17) . ?
C18_2 C19_2 1.5377(17) . ?
C18_2 H18_2 0.9800 . ?
C19_2 H19A_2 0.9600 . ?
C19_2 H19B_2 0.9600 . ?
C19_2 H19C_2 0.9600 . ?
C20_2 H20A_2 0.9600 . ?
C20_2 H20B_2 0.9600 . ?
C20_2 H20C_2 0.9600 . ?
B1_2 C21_2 1.5493(17) . ?
B1_2 C22_2 1.5880(16) . ?
C21_2 N2_2 1.1621(16) . ?
C22_2 N3_2 1.3516(15) . ?
C22_2 N4_2 1.3568(14) . ?
N3_2 C23_2 1.3841(14) . ?
N3_2 C25_2 1.4790(14) . ?
C23_2 C24_2 1.3470(17) . ?
C23_2 H23_2 0.9300 . ?
C24_2 N4_2 1.3773(15) . ?
C24_2 H24_2 0.9300 . ?
N4_2 C28_2 1.4770(14) . ?
C25_2 C26_2 1.5175(18) . ?
C25_2 C27_2 1.5183(18) . ?
C25_2 H25_2 0.9800 . ?
C26_2 H26A_2 0.9600 . ?
C26_2 H26B_2 0.9600 . ?
C26_2 H26C_2 0.9600 . ?
C27_2 H27A_2 0.9600 . ?
C27_2 H27B_2 0.9600 . ?
C27_2 H27C_2 0.9600 . ?
C28_2 C29_2 1.5185(18) . ?
C28_2 C30_2 1.5244(17) . ?
C28_2 H28_2 0.9800 . ?
C29_2 H29A_2 0.9600 . ?
C29_2 H29B_2 0.9600 . ?
C29_2 H29C_2 0.9600 . ?
C30_2 H30A_2 0.9600 . ?
C30_2 H30B_2 0.9600 . ?
C30_2 H30C_2 0.9600 . ?
C1_3 C2_3 1.3900 . ?
C1_3 C6_3 1.3900 . ?
C1_3 H1_3 0.9300 . ?
C2_3 C3_3 1.3900 . ?
C2_3 H2_3 0.9300 . ?
C3_3 C4_3 1.3900 . ?
C3_3 H3_3 0.9300 . ?
C4_3 C5_3 1.3900 . ?
C4_3 H4_3 0.9300 . ?
C5_3 C6_3 1.3900 . ?
C5_3 H5_3 0.9300 . ?
C6_3 H6_3 0.9300 . ?
C1_4 C2_4 1.3900 . ?
C1_4 C6_4 1.3900 . ?
C1_4 H1_4 0.9300 . ?
C2_4 C3_4 1.3900 . ?
C2_4 H2_4 0.9300 . ?
C3_4 C4_4 1.3900 . ?
C3_4 H3_4 0.9300 . ?
C4_4 C5_4 1.3900 . ?
C4_4 H4_4 0.9300 . ?
C5_4 C6_4 1.3900 . ?
C5_4 H5_4 0.9300 . ?
C6_4 H6_4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1_1 C1_1 B1_1 126.59(10) . . ?
N1_1 C1_1 C4_1 105.92(9) . . ?
B1_1 C1_1 C4_1 127.39(10) . . ?
C1_1 N1_1 C9_1 120.58(9) . . ?
C1_1 N1_1 C2_1 115.32(9) . . ?
C9_1 N1_1 C2_1 124.02(9) . . ?
N1_1 C2_1 C6_1 112.74(11) . . ?
N1_1 C2_1 C3_1 100.80(9) . . ?
C6_1 C2_1 C3_1 110.60(11) . . ?
N1_1 C2_1 C5_1 112.79(10) . . ?
C6_1 C2_1 C5_1 106.95(11) . . ?
C3_1 C2_1 C5_1 113.03(11) . . ?
C2_1 C3_1 C4_1 107.39(10) . . ?
C2_1 C3_1 H3A_1 110.2 . . ?
C4_1 C3_1 H3A_1 110.2 . . ?
C2_1 C3_1 H3AB_1 110.2 . . ?
C4_1 C3_1 H3AB_1 110.2 . . ?
H3A_1 C3_1 H3AB_1 108.5 . . ?
C7_1 C4_1 C1_1 115.47(10) . . ?
C7_1 C4_1 C3_1 109.51(10) . . ?
C1_1 C4_1 C3_1 102.50(9) . . ?
C7_1 C4_1 C8_1 107.68(10) . . ?
C1_1 C4_1 C8_1 110.50(10) . . ?
C3_1 C4_1 C8_1 111.15(10) . . ?
C2_1 C5_1 H5A_1 109.5 . . ?
C2_1 C5_1 H5B_1 109.5 . . ?
H5A_1 C5_1 H5B_1 109.5 . . ?
C2_1 C5_1 H5C_1 109.5 . . ?
H5A_1 C5_1 H5C_1 109.5 . . ?
H5B_1 C5_1 H5C_1 109.5 . . ?
C2_1 C6_1 H6A_1 109.5 . . ?
C2_1 C6_1 H6B_1 109.5 . . ?
H6A_1 C6_1 H6B_1 109.5 . . ?
C2_1 C6_1 H6C_1 109.5 . . ?
H6A_1 C6_1 H6C_1 109.5 . . ?
H6B_1 C6_1 H6C_1 109.5 . . ?
C4_1 C7_1 H7A_1 109.5 . . ?
C4_1 C7_1 H7B_1 109.5 . . ?
H7A_1 C7_1 H7B_1 109.5 . . ?
C4_1 C7_1 H7C_1 109.5 . . ?
H7A_1 C7_1 H7C_1 109.5 . . ?
H7B_1 C7_1 H7C_1 109.5 . . ?
C4_1 C8_1 H8A_1 109.5 . . ?
C4_1 C8_1 H8B_1 109.5 . . ?
H8A_1 C8_1 H8B_1 109.5 . . ?
C4_1 C8_1 H8C_1 109.5 . . ?
H8A_1 C8_1 H8C_1 109.5 . . ?
H8B_1 C8_1 H8C_1 109.5 . . ?
C10_1 C9_1 C14_1 119.81(11) . . ?
C10_1 C9_1 N1_1 120.35(10) . . ?
C14_1 C9_1 N1_1 119.64(11) . . ?
C11_1 C10_1 C9_1 118.83(11) . . ?
C11_1 C10_1 C18_1 117.67(11) . . ?
C9_1 C10_1 C18_1 123.35(11) . . ?
C12_1 C11_1 C10_1 121.45(12) . . ?
C12_1 C11_1 H11_1 119.3 . . ?
C10_1 C11_1 H11_1 119.3 . . ?
C13_1 C12_1 C11_1 119.52(12) . . ?
C13_1 C12_1 H12_1 120.2 . . ?
C11_1 C12_1 H12_1 120.2 . . ?
C12_1 C13_1 C14_1 121.52(12) . . ?
C12_1 C13_1 H13_1 119.2 . . ?
C14_1 C13_1 H13_1 119.2 . . ?
C13_1 C14_1 C9_1 118.78(11) . . ?
C13_1 C14_1 C15_1 118.25(11) . . ?
C9_1 C14_1 C15_1 122.89(11) . . ?
C14_1 C15_1 C16_1 111.12(11) . . ?
C14_1 C15_1 C17_1 111.56(12) . . ?
C16_1 C15_1 C17_1 109.44(11) . . ?
C14_1 C15_1 H15_1 108.2 . . ?
C16_1 C15_1 H15_1 108.2 . . ?
C17_1 C15_1 H15_1 108.2 . . ?
C15_1 C16_1 H16A_1 109.5 . . ?
C15_1 C16_1 H16B_1 109.5 . . ?
H16A_1 C16_1 H16B_1 109.5 . . ?
C15_1 C16_1 H16C_1 109.5 . . ?
H16A_1 C16_1 H16C_1 109.5 . . ?
H16B_1 C16_1 H16C_1 109.5 . . ?
C15_1 C17_1 H17A_1 109.5 . . ?
C15_1 C17_1 H17B_1 109.5 . . ?
H17A_1 C17_1 H17B_1 109.5 . . ?
C15_1 C17_1 H17C_1 109.5 . . ?
H17A_1 C17_1 H17C_1 109.5 . . ?
H17B_1 C17_1 H17C_1 109.5 . . ?
C10_1 C18_1 C19_1 110.38(11) . . ?
C10_1 C18_1 C20_1 112.48(10) . . ?
C19_1 C18_1 C20_1 109.09(11) . . ?
C10_1 C18_1 H18_1 108.3 . . ?
C19_1 C18_1 H18_1 108.3 . . ?
C20_1 C18_1 H18_1 108.3 . . ?
C18_1 C19_1 H19A_1 109.5 . . ?
C18_1 C19_1 H19B_1 109.5 . . ?
H19A_1 C19_1 H19B_1 109.5 . . ?
C18_1 C19_1 H19C_1 109.5 . . ?
H19A_1 C19_1 H19C_1 109.5 . . ?
H19B_1 C19_1 H19C_1 109.5 . . ?
C18_1 C20_1 H20A_1 109.5 . . ?
C18_1 C20_1 H20B_1 109.5 . . ?
H20A_1 C20_1 H20B_1 109.5 . . ?
C18_1 C20_1 H20C_1 109.5 . . ?
H20A_1 C20_1 H20C_1 109.5 . . ?
H20B_1 C20_1 H20C_1 109.5 . . ?
C1_1 B1_1 C21_1 128.23(10) . . ?
C1_1 B1_1 C22_1 123.05(11) . . ?
C21_1 B1_1 C22_1 108.71(9) . . ?
N2_1 C21_1 B1_1 171.62(11) . . ?
N4_1 C22_1 N3_1 105.37(9) . . ?
N4_1 C22_1 B1_1 127.46(10) . . ?
N3_1 C22_1 B1_1 126.86(10) . . ?
C22_1 N3_1 C23_1 110.15(9) . . ?
C22_1 N3_1 C25_1 124.37(9) . . ?
C23_1 N3_1 C25_1 125.25(9) . . ?
C24_1 C23_1 N3_1 107.48(10) . . ?
C24_1 C23_1 H23_1 126.3 . . ?
N3_1 C23_1 H23_1 126.3 . . ?
C23_1 C24_1 N4_1 106.34(10) . . ?
C23_1 C24_1 H24_1 126.8 . . ?
N4_1 C24_1 H24_1 126.8 . . ?
C22_1 N4_1 C24_1 110.66(9) . . ?
C22_1 N4_1 C28_1 124.24(9) . . ?
C24_1 N4_1 C28_1 125.05(9) . . ?
N3_1 C25_1 C27_1 109.79(9) . . ?
N3_1 C25_1 C26_1 110.32(10) . . ?
C27_1 C25_1 C26_1 112.63(10) . . ?
N3_1 C25_1 H25_1 108.0 . . ?
C27_1 C25_1 H25_1 108.0 . . ?
C26_1 C25_1 H25_1 108.0 . . ?
C25_1 C26_1 H26A_1 109.5 . . ?
C25_1 C26_1 H26B_1 109.5 . . ?
H26A_1 C26_1 H26B_1 109.5 . . ?
C25_1 C26_1 H26C_1 109.5 . . ?
H26A_1 C26_1 H26C_1 109.5 . . ?
H26B_1 C26_1 H26C_1 109.5 . . ?
C25_1 C27_1 H27A_1 109.5 . . ?
C25_1 C27_1 H27B_1 109.5 . . ?
H27A_1 C27_1 H27B_1 109.5 . . ?
C25_1 C27_1 H27C_1 109.5 . . ?
H27A_1 C27_1 H27C_1 109.5 . . ?
H27B_1 C27_1 H27C_1 109.5 . . ?
N4_1 C28_1 C29_1 110.09(10) . . ?
N4_1 C28_1 C30_1 110.30(10) . . ?
C29_1 C28_1 C30_1 112.39(11) . . ?
N4_1 C28_1 H28_1 108.0 . . ?
C29_1 C28_1 H28_1 108.0 . . ?
C30_1 C28_1 H28_1 108.0 . . ?
C28_1 C29_1 H29A_1 109.5 . . ?
C28_1 C29_1 H29B_1 109.5 . . ?
H29A_1 C29_1 H29B_1 109.5 . . ?
C28_1 C29_1 H29C_1 109.5 . . ?
H29A_1 C29_1 H29C_1 109.5 . . ?
H29B_1 C29_1 H29C_1 109.5 . . ?
C28_1 C30_1 H30A_1 109.5 . . ?
C28_1 C30_1 H30B_1 109.5 . . ?
H30A_1 C30_1 H30B_1 109.5 . . ?
C28_1 C30_1 H30C_1 109.5 . . ?
H30A_1 C30_1 H30C_1 109.5 . . ?
H30B_1 C30_1 H30C_1 109.5 . . ?
N1_2 C1_2 B1_2 126.94(10) . . ?
N1_2 C1_2 C4_51 106.03(10) . . ?
B1_2 C1_2 C4_51 126.96(11) . . ?
N1_2 C1_2 C4_52 105.6(9) . . ?
B1_2 C1_2 C4_52 127.2(9) . . ?
C1_2 N1_2 C9_2 120.37(9) . . ?
C1_2 N1_2 C2_51 115.48(11) . . ?
C9_2 N1_2 C2_51 124.05(10) . . ?
C1_2 N1_2 C2_52 117.0(9) . . ?
C9_2 N1_2 C2_52 122.5(9) . . ?
N1_2 C2_51 C6_51 112.63(16) . . ?
N1_2 C2_51 C3_51 100.76(13) . . ?
C6_51 C2_51 C3_51 111.41(17) . . ?
N1_2 C2_51 C5_51 113.30(16) . . ?
C6_51 C2_51 C5_51 106.84(16) . . ?
C3_51 C2_51 C5_51 111.99(16) . . ?
C2_51 C3_51 C4_51 107.41(15) . . ?
C2_51 C3_51 H3A_51 110.2 . . ?
C4_51 C3_51 H3A_51 110.2 . . ?
C2_51 C3_51 H3AB_51 110.2 . . ?
C4_51 C3_51 H3AB_51 110.2 . . ?
H3A_51 C3_51 H3AB_51 108.5 . . ?
C8_51 C4_51 C1_2 115.31(15) . . ?
C8_51 C4_51 C3_51 109.33(16) . . ?
C1_2 C4_51 C3_51 102.72(13) . . ?
C8_51 C4_51 C7_51 107.47(15) . . ?
C1_2 C4_51 C7_51 110.24(15) . . ?
C3_51 C4_51 C7_51 111.80(15) . . ?
C2_51 C5_51 H5A_51 109.5 . . ?
C2_51 C5_51 H5B_51 109.5 . . ?
H5A_51 C5_51 H5B_51 109.5 . . ?
C2_51 C5_51 H5C_51 109.5 . . ?
H5A_51 C5_51 H5C_51 109.5 . . ?
H5B_51 C5_51 H5C_51 109.5 . . ?
C2_51 C6_51 H6A_51 109.5 . . ?
C2_51 C6_51 H6B_51 109.5 . . ?
H6A_51 C6_51 H6B_51 109.5 . . ?
C2_51 C6_51 H6C_51 109.5 . . ?
H6A_51 C6_51 H6C_51 109.5 . . ?
H6B_51 C6_51 H6C_51 109.5 . . ?
C4_51 C7_51 H7A_51 109.5 . . ?
C4_51 C7_51 H7B_51 109.5 . . ?
H7A_51 C7_51 H7B_51 109.5 . . ?
C4_51 C7_51 H7C_51 109.5 . . ?
H7A_51 C7_51 H7C_51 109.5 . . ?
H7B_51 C7_51 H7C_51 109.5 . . ?
C4_51 C8_51 H8A_51 109.5 . . ?
C4_51 C8_51 H8B_51 109.5 . . ?
H8A_51 C8_51 H8B_51 109.5 . . ?
C4_51 C8_51 H8C_51 109.5 . . ?
H8A_51 C8_51 H8C_51 109.5 . . ?
H8B_51 C8_51 H8C_51 109.5 . . ?
N1_2 C2_52 C3_52 98.1(19) . . ?
N1_2 C2_52 C6_52 106(2) . . ?
C3_52 C2_52 C6_52 112(2) . . ?
N1_2 C2_52 C5_52 115(3) . . ?
C3_52 C2_52 C5_52 117(2) . . ?
C6_52 C2_52 C5_52 109(2) . . ?
C2_52 C3_52 C4_52 111(2) . . ?
C2_52 C3_52 H3A_52 109.5 . . ?
C4_52 C3_52 H3A_52 109.5 . . ?
C2_52 C3_52 H3AB_52 109.5 . . ?
C4_52 C3_52 H3AB_52 109.5 . . ?
H3A_52 C3_52 H3AB_52 108.1 . . ?
C3_52 C4_52 C8_52 110(2) . . ?
C3_52 C4_52 C7_52 112(2) . . ?
C8_52 C4_52 C7_52 108(2) . . ?
C3_52 C4_52 C1_2 103.2(19) . . ?
C8_52 C4_52 C1_2 107(2) . . ?
C7_52 C4_52 C1_2 116(2) . . ?
C2_52 C5_52 H5A_52 109.5 . . ?
C2_52 C5_52 H5B_52 109.5 . . ?
H5A_52 C5_52 H5B_52 109.5 . . ?
C2_52 C5_52 H5C_52 109.5 . . ?
H5A_52 C5_52 H5C_52 109.5 . . ?
H5B_52 C5_52 H5C_52 109.5 . . ?
C2_52 C6_52 H6A_52 109.5 . . ?
C2_52 C6_52 H6B_52 109.5 . . ?
H6A_52 C6_52 H6B_52 109.5 . . ?
C2_52 C6_52 H6C_52 109.5 . . ?
H6A_52 C6_52 H6C_52 109.5 . . ?
H6B_52 C6_52 H6C_52 109.5 . . ?
C4_52 C7_52 H7A_52 109.5 . . ?
C4_52 C7_52 H7B_52 109.5 . . ?
H7A_52 C7_52 H7B_52 109.5 . . ?
C4_52 C7_52 H7C_52 109.5 . . ?
H7A_52 C7_52 H7C_52 109.5 . . ?
H7B_52 C7_52 H7C_52 109.5 . . ?
C4_52 C8_52 H8A_52 109.5 . . ?
C4_52 C8_52 H8B_52 109.5 . . ?
H8A_52 C8_52 H8B_52 109.5 . . ?
C4_52 C8_52 H8C_52 109.5 . . ?
H8A_52 C8_52 H8C_52 109.5 . . ?
H8B_52 C8_52 H8C_52 109.5 . . ?
C14_2 C9_2 C10_2 119.94(11) . . ?
C14_2 C9_2 N1_2 119.80(10) . . ?
C10_2 C9_2 N1_2 120.10(10) . . ?
C11_2 C10_2 C9_2 118.73(10) . . ?
C11_2 C10_2 C15_2 117.67(10) . . ?
C9_2 C10_2 C15_2 123.46(11) . . ?
C12_2 C11_2 C10_2 121.34(11) . . ?
C12_2 C11_2 H11_2 119.3 . . ?
C10_2 C11_2 H11_2 119.3 . . ?
C13_2 C12_2 C11_2 119.53(11) . . ?
C13_2 C12_2 H12_2 120.2 . . ?
C11_2 C12_2 H12_2 120.2 . . ?
C12_2 C13_2 C14_2 121.64(11) . . ?
C12_2 C13_2 H13_2 119.2 . . ?
C14_2 C13_2 H13_2 119.2 . . ?
C13_2 C14_2 C9_2 118.71(11) . . ?
C13_2 C14_2 C18_2 118.33(10) . . ?
C9_2 C14_2 C18_2 122.91(11) . . ?
C10_2 C15_2 C16_2 112.37(10) . . ?
C10_2 C15_2 C17_2 110.45(10) . . ?
C16_2 C15_2 C17_2 109.05(10) . . ?
C10_2 C15_2 H15_2 108.3 . . ?
C16_2 C15_2 H15_2 108.3 . . ?
C17_2 C15_2 H15_2 108.3 . . ?
C15_2 C16_2 H16A_2 109.5 . . ?
C15_2 C16_2 H16B_2 109.5 . . ?
H16A_2 C16_2 H16B_2 109.5 . . ?
C15_2 C16_2 H16C_2 109.5 . . ?
H16A_2 C16_2 H16C_2 109.5 . . ?
H16B_2 C16_2 H16C_2 109.5 . . ?
C15_2 C17_2 H17A_2 109.5 . . ?
C15_2 C17_2 H17B_2 109.5 . . ?
H17A_2 C17_2 H17B_2 109.5 . . ?
C15_2 C17_2 H17C_2 109.5 . . ?
H17A_2 C17_2 H17C_2 109.5 . . ?
H17B_2 C17_2 H17C_2 109.5 . . ?
C14_2 C18_2 C20_2 111.18(10) . . ?
C14_2 C18_2 C19_2 111.47(10) . . ?
C20_2 C18_2 C19_2 109.52(10) . . ?
C14_2 C18_2 H18_2 108.2 . . ?
C20_2 C18_2 H18_2 108.2 . . ?
C19_2 C18_2 H18_2 108.2 . . ?
C18_2 C19_2 H19A_2 109.5 . . ?
C18_2 C19_2 H19B_2 109.5 . . ?
H19A_2 C19_2 H19B_2 109.5 . . ?
C18_2 C19_2 H19C_2 109.5 . . ?
H19A_2 C19_2 H19C_2 109.5 . . ?
H19B_2 C19_2 H19C_2 109.5 . . ?
C18_2 C20_2 H20A_2 109.5 . . ?
C18_2 C20_2 H20B_2 109.5 . . ?
H20A_2 C20_2 H20B_2 109.5 . . ?
C18_2 C20_2 H20C_2 109.5 . . ?
H20A_2 C20_2 H20C_2 109.5 . . ?
H20B_2 C20_2 H20C_2 109.5 . . ?
C1_2 B1_2 C21_2 128.10(10) . . ?
C1_2 B1_2 C22_2 123.17(10) . . ?
C21_2 B1_2 C22_2 108.73(9) . . ?
N2_2 C21_2 B1_2 171.93(12) . . ?
N3_2 C22_2 N4_2 105.22(9) . . ?
N3_2 C22_2 B1_2 127.51(9) . . ?
N4_2 C22_2 B1_2 126.92(10) . . ?
C22_2 N3_2 C23_2 110.71(9) . . ?
C22_2 N3_2 C25_2 123.95(9) . . ?
C23_2 N3_2 C25_2 125.30(10) . . ?
C24_2 C23_2 N3_2 106.38(10) . . ?
C24_2 C23_2 H23_2 126.8 . . ?
N3_2 C23_2 H23_2 126.8 . . ?
C23_2 C24_2 N4_2 107.52(10) . . ?
C23_2 C24_2 H24_2 126.2 . . ?
N4_2 C24_2 H24_2 126.2 . . ?
C22_2 N4_2 C24_2 110.17(9) . . ?
C22_2 N4_2 C28_2 124.22(9) . . ?
C24_2 N4_2 C28_2 125.38(9) . . ?
N3_2 C25_2 C26_2 110.31(10) . . ?
N3_2 C25_2 C27_2 110.23(10) . . ?
C26_2 C25_2 C27_2 112.32(10) . . ?
N3_2 C25_2 H25_2 107.9 . . ?
C26_2 C25_2 H25_2 107.9 . . ?
C27_2 C25_2 H25_2 107.9 . . ?
C25_2 C26_2 H26A_2 109.5 . . ?
C25_2 C26_2 H26B_2 109.5 . . ?
H26A_2 C26_2 H26B_2 109.5 . . ?
C25_2 C26_2 H26C_2 109.5 . . ?
H26A_2 C26_2 H26C_2 109.5 . . ?
H26B_2 C26_2 H26C_2 109.5 . . ?
C25_2 C27_2 H27A_2 109.5 . . ?
C25_2 C27_2 H27B_2 109.5 . . ?
H27A_2 C27_2 H27B_2 109.5 . . ?
C25_2 C27_2 H27C_2 109.5 . . ?
H27A_2 C27_2 H27C_2 109.5 . . ?
H27B_2 C27_2 H27C_2 109.5 . . ?
N4_2 C28_2 C29_2 109.36(10) . . ?
N4_2 C28_2 C30_2 110.55(10) . . ?
C29_2 C28_2 C30_2 112.57(10) . . ?
N4_2 C28_2 H28_2 108.1 . . ?
C29_2 C28_2 H28_2 108.1 . . ?
C30_2 C28_2 H28_2 108.1 . . ?
C28_2 C29_2 H29A_2 109.5 . . ?
C28_2 C29_2 H29B_2 109.5 . . ?
H29A_2 C29_2 H29B_2 109.5 . . ?
C28_2 C29_2 H29C_2 109.5 . . ?
H29A_2 C29_2 H29C_2 109.5 . . ?
H29B_2 C29_2 H29C_2 109.5 . . ?
C28_2 C30_2 H30A_2 109.5 . . ?
C28_2 C30_2 H30B_2 109.5 . . ?
H30A_2 C30_2 H30B_2 109.5 . . ?
C28_2 C30_2 H30C_2 109.5 . . ?
H30A_2 C30_2 H30C_2 109.5 . . ?
H30B_2 C30_2 H30C_2 109.5 . . ?
C2_3 C1_3 C6_3 120.0 . . ?
C2_3 C1_3 H1_3 120.0 . . ?
C6_3 C1_3 H1_3 120.0 . . ?
C3_3 C2_3 C1_3 120.0 . . ?
C3_3 C2_3 H2_3 120.0 . . ?
C1_3 C2_3 H2_3 120.0 . . ?
C2_3 C3_3 C4_3 120.0 . . ?
C2_3 C3_3 H3_3 120.0 . . ?
C4_3 C3_3 H3_3 120.0 . . ?
C3_3 C4_3 C5_3 120.0 . . ?
C3_3 C4_3 H4_3 120.0 . . ?
C5_3 C4_3 H4_3 120.0 . . ?
C4_3 C5_3 C6_3 120.0 . . ?
C4_3 C5_3 H5_3 120.0 . . ?
C6_3 C5_3 H5_3 120.0 . . ?
C5_3 C6_3 C1_3 120.0 . . ?
C5_3 C6_3 H6_3 120.0 . . ?
C1_3 C6_3 H6_3 120.0 . . ?
C2_4 C1_4 C6_4 120.0 . . ?
C2_4 C1_4 H1_4 120.0 . . ?
C6_4 C1_4 H1_4 120.0 . . ?
C3_4 C2_4 C1_4 120.0 . . ?
C3_4 C2_4 H2_4 120.0 . . ?
C1_4 C2_4 H2_4 120.0 . . ?
C2_4 C3_4 C4_4 120.0 . . ?
C2_4 C3_4 H3_4 120.0 . . ?
C4_4 C3_4 H3_4 120.0 . . ?
C5_4 C4_4 C3_4 120.0 . . ?
C5_4 C4_4 H4_4 120.0 . . ?
C3_4 C4_4 H4_4 120.0 . . ?
C6_4 C5_4 C4_4 120.0 . . ?
C6_4 C5_4 H5_4 120.0 . . ?
C4_4 C5_4 H5_4 120.0 . . ?
C5_4 C6_4 C1_4 120.0 . . ?
C5_4 C6_4 H6_4 120.0 . . ?
C1_4 C6_4 H6_4 120.0 . . ?

_refine_diff_density_max         0.270
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.038



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_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_test_a_tw
_database_code_depnum_ccdc_archive 'CCDC 2071475'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT340_test_a_tw           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00733 Ang.
RESPONSE: Crystal diffracted very poorly at higher angles
;
_vrf_PLAT906_test_a_tw           
;
PROBLEM: Large K Value in the Analysis of Variance ......     13.182 Check
RESPONSE: Crystal diffracted very poorly at higher angles
;
_vrf_PLAT911_test_a_tw           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         15 Report
RESPONSE: reflections affected by beamstop
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[(CAAC)(IiPr)B(CN)][OTf]'
_chemical_name_common            '[2(CN)][OTf]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H50 B F3 N4 O3 S'
_chemical_formula_sum            'C34 H50 B F3 N4 O3 S'
_chemical_formula_weight         662.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   9.430(7)
_cell_length_b                   9.763(7)
_cell_length_c                   20.736(15)
_cell_angle_alpha                95.574(13)
_cell_angle_beta                 96.19(3)
_cell_angle_gamma                101.684(14)
_cell_volume                     1845(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    99(2)
_cell_measurement_reflns_used    8884
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      26.62


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Oxford Cryostream 700).
;
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_F_000             709
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.541
_exptl_crystal_size_mid          0.493
_exptl_crystal_size_min          0.334
_exptl_absorpt_coefficient_mu    0.140
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5953
_exptl_absorpt_correction_T_max  0.7454
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.50 0.2120
1.00 0.00 0.00 0.2370
1.00 0.00 -0.50 0.2300
-1.00 0.00 0.00 0.2260
1.00 1.00 -1.00 0.2330
1.00 -1.00 0.50 0.2770
-1.00 1.00 0.50 0.2330
1.00 0.00 -1.00 0.2320
-1.00 0.00 1.00 0.2030
-1.00 -1.00 1.50 0.2100
1.00 1.00 -1.50 0.2360
-1.00 -1.00 0.50 0.2220
0.00 1.00 0.00 0.2540
0.00 -1.00 0.50 0.2100
0.00 0.00 0.50 0.0860
0.00 0.00 -0.50 0.1670
0.00 -1.00 1.00 0.2180
0.00 1.00 -1.00 0.2840
-1.00 1.00 0.00 0.2350
1.00 -1.00 0.00 0.2670

_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            7248
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.991
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7248
_reflns_number_gt                5811
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_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          
;

 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger. 

The molecule was refined as a two-component twin. A number of reflections affected by the beamstop were omitted.
The structure provides proof of connectivity, however the quality of the data is insufficient for structural discussions.
 
The asymmetric unit contains a twofold disordered triflate counteranion refined to a 66:34 ratio 
(RESI 3 and RESI 31), the ADPs of which were restrained to the same value with similarity restraint SIMU 0.01. 
The half benzene solvent molecule, positionned on an inversion center was also modelled as twofold disordered 
(RESI 2 and 21), refined to a 1:1 ratio with ADPs restrained using SIMU 0.01. 



;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+9.0493P] 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         7248
_refine_ls_number_parameters     559
_refine_ls_number_restraints     426
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0953
_refine_ls_wR_factor_ref         0.2519
_refine_ls_wR_factor_gt          0.2456
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.088
_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
N1 N 0.1883(4) 0.1040(4) 0.17245(19) 0.0171(8) Uani 1 1 d . . . . .
B1 B 0.4462(6) 0.1790(6) 0.2303(3) 0.0183(11) Uani 1 1 d . . . . .
C1 C 0.2836(5) 0.1712(5) 0.2236(2) 0.0175(9) Uani 1 1 d . . . . .
N2 N 0.5992(5) 0.0658(5) 0.1453(2) 0.0263(10) Uani 1 1 d . . . . .
C2 C 0.0302(5) 0.1075(5) 0.1779(2) 0.0223(10) Uani 1 1 d . . . . .
N3 N 0.6097(5) 0.2067(4) 0.3438(2) 0.0231(9) Uani 1 1 d . . . . .
C3 C 0.0415(5) 0.1689(6) 0.2494(2) 0.0253(11) Uani 1 1 d . . . . .
H3A H 0.010542 0.092851 0.276499 0.030 Uiso 1 1 calc R U . . .
H3AB H -0.022474 0.237237 0.253758 0.030 Uiso 1 1 calc R U . . .
N4 N 0.6480(4) 0.3889(4) 0.2929(2) 0.0213(9) Uani 1 1 d . . . . .
C4 C 0.2018(5) 0.2428(5) 0.2721(2) 0.0215(10) Uani 1 1 d . . . . .
C5 C -0.0670(5) -0.0407(6) 0.1637(3) 0.0280(12) Uani 1 1 d . . . . .
H5A H -0.169544 -0.034610 0.163279 0.042 Uiso 1 1 calc R U . . .
H5B H -0.040820 -0.097664 0.197628 0.042 Uiso 1 1 calc R U . . .
H5C H -0.052897 -0.084702 0.120979 0.042 Uiso 1 1 calc R U . . .
C6 C -0.0249(6) 0.1990(6) 0.1297(3) 0.0309(12) Uani 1 1 d . . . . .
H6A H -0.127021 0.200636 0.133962 0.046 Uiso 1 1 calc R U . . .
H6B H -0.017556 0.160257 0.085084 0.046 Uiso 1 1 calc R U . . .
H6C H 0.034548 0.295165 0.139043 0.046 Uiso 1 1 calc R U . . .
C7 C 0.2322(6) 0.4009(5) 0.2652(3) 0.0306(12) Uani 1 1 d . . . . .
H7A H 0.165776 0.445605 0.288923 0.046 Uiso 1 1 calc R U . . .
H7B H 0.216704 0.413776 0.218862 0.046 Uiso 1 1 calc R U . . .
H7C H 0.333435 0.444189 0.283349 0.046 Uiso 1 1 calc R U . . .
C8 C 0.2437(6) 0.2222(6) 0.3436(3) 0.0300(12) Uani 1 1 d . . . . .
H8A H 0.178515 0.259874 0.370900 0.045 Uiso 1 1 calc R U . . .
H8B H 0.344823 0.272100 0.358275 0.045 Uiso 1 1 calc R U . . .
H8C H 0.234416 0.121501 0.347115 0.045 Uiso 1 1 calc R U . . .
C9 C 0.2308(5) 0.0332(5) 0.1146(2) 0.0173(9) Uani 1 1 d . . . . .
C10 C 0.2690(5) 0.1126(5) 0.0632(2) 0.0201(10) Uani 1 1 d . . . . .
C11 C 0.3060(5) 0.0407(6) 0.0082(2) 0.0227(10) Uani 1 1 d . . . . .
H11 H 0.329101 0.089870 -0.027968 0.027 Uiso 1 1 calc R U . . .
C12 C 0.3098(5) -0.0996(6) 0.0051(2) 0.0253(11) Uani 1 1 d . . . . .
H12 H 0.335192 -0.146317 -0.032925 0.030 Uiso 1 1 calc R U . . .
C13 C 0.2769(5) -0.1726(6) 0.0569(2) 0.0240(11) Uani 1 1 d . . . . .
H13 H 0.281454 -0.269247 0.054272 0.029 Uiso 1 1 calc R U . . .
C14 C 0.2373(5) -0.1089(5) 0.1130(2) 0.0204(10) Uani 1 1 d . . . . .
C15 C 0.2796(6) 0.2710(5) 0.0655(3) 0.0244(11) Uani 1 1 d . . . . .
H15 H 0.245429 0.305086 0.106958 0.029 Uiso 1 1 calc R U . . .
C16 C 0.4394(6) 0.3485(6) 0.0657(3) 0.0302(12) Uani 1 1 d . . . . .
H16A H 0.444739 0.450237 0.068304 0.045 Uiso 1 1 calc R U . . .
H16B H 0.474731 0.316270 0.025369 0.045 Uiso 1 1 calc R U . . .
H16C H 0.500144 0.328247 0.103453 0.045 Uiso 1 1 calc R U . . .
C17 C 0.1852(6) 0.3096(6) 0.0078(3) 0.0314(12) Uani 1 1 d . . . . .
H17A H 0.181748 0.409423 0.015507 0.047 Uiso 1 1 calc R U . . .
H17B H 0.086011 0.251735 0.003620 0.047 Uiso 1 1 calc R U . . .
H17C H 0.227651 0.292190 -0.032515 0.047 Uiso 1 1 calc R U . . .
C18 C 0.2137(5) -0.1935(5) 0.1704(2) 0.0211(10) Uani 1 1 d . . . . .
H18 H 0.180682 -0.134395 0.205480 0.025 Uiso 1 1 calc R U . . .
C19 C 0.3556(6) -0.2327(6) 0.1984(3) 0.0259(11) Uani 1 1 d . . . . .
H19A H 0.337494 -0.285792 0.235511 0.039 Uiso 1 1 calc R U . . .
H19B H 0.430459 -0.146584 0.213044 0.039 Uiso 1 1 calc R U . . .
H19C H 0.389539 -0.290669 0.164532 0.039 Uiso 1 1 calc R U . . .
C20 C 0.0959(6) -0.3298(5) 0.1503(3) 0.0283(12) Uani 1 1 d . . . . .
H20A H 0.077406 -0.377634 0.188946 0.042 Uiso 1 1 calc R U . . .
H20B H 0.129846 -0.391968 0.118196 0.042 Uiso 1 1 calc R U . . .
H20C H 0.005565 -0.306480 0.131029 0.042 Uiso 1 1 calc R U . . .
C21 C 0.5269(5) 0.1119(5) 0.1787(2) 0.0198(10) Uani 1 1 d . . . . .
C22 C 0.5613(5) 0.2602(5) 0.2904(2) 0.0184(9) Uani 1 1 d . . . . .
C23 C 0.7256(6) 0.3011(6) 0.3788(3) 0.0291(12) Uani 1 1 d . . . . .
H23 H 0.778431 0.288296 0.418602 0.035 Uiso 1 1 calc R U . . .
C24 C 0.7518(6) 0.4143(6) 0.3472(3) 0.0284(12) Uani 1 1 d . . . . .
H24 H 0.827167 0.496291 0.359751 0.034 Uiso 1 1 calc R U . . .
C25 C 0.5534(6) 0.0606(5) 0.3584(3) 0.0286(12) Uani 1 1 d . . . . .
H25 H 0.459779 0.019911 0.329271 0.034 Uiso 1 1 calc R U . . .
C26 C 0.5236(7) 0.0636(7) 0.4287(3) 0.0397(15) Uani 1 1 d . . . . .
H26A H 0.468866 -0.029208 0.435651 0.060 Uiso 1 1 calc R U . . .
H26B H 0.466156 0.134587 0.438159 0.060 Uiso 1 1 calc R U . . .
H26C H 0.616380 0.087399 0.457790 0.060 Uiso 1 1 calc R U . . .
C27 C 0.6632(8) -0.0283(6) 0.3441(3) 0.0466(17) Uani 1 1 d . . . . .
H27A H 0.625785 -0.125101 0.352710 0.070 Uiso 1 1 calc R U . . .
H27B H 0.755857 0.010965 0.372174 0.070 Uiso 1 1 calc R U . . .
H27C H 0.678991 -0.028362 0.298163 0.070 Uiso 1 1 calc R U . . .
C28 C 0.6423(5) 0.4839(5) 0.2420(3) 0.0258(11) Uani 1 1 d . . . . .
H28 H 0.546809 0.450649 0.213243 0.031 Uiso 1 1 calc R U . . .
C29 C 0.7641(6) 0.4750(7) 0.2002(3) 0.0357(13) Uani 1 1 d . . . . .
H29A H 0.753075 0.529112 0.163249 0.054 Uiso 1 1 calc R U . . .
H29B H 0.758672 0.376254 0.183764 0.054 Uiso 1 1 calc R U . . .
H29C H 0.858870 0.513869 0.226648 0.054 Uiso 1 1 calc R U . . .
C30 C 0.6490(6) 0.6330(6) 0.2726(3) 0.0355(13) Uani 1 1 d . . . . .
H30A H 0.640029 0.693690 0.238103 0.053 Uiso 1 1 calc R U . . .
H30B H 0.742571 0.668440 0.300548 0.053 Uiso 1 1 calc R U . . .
H30C H 0.568857 0.633204 0.299003 0.053 Uiso 1 1 calc R U . . .
C1_2 C 0.561(4) 0.621(3) 0.4591(15) 0.055(4) Uani 0.250(14) 1 d G U P A -1
H1_2 H 0.612346 0.692429 0.437105 0.066 Uiso 0.250(14) 1 calc R U P A -1
C2_2 C 0.638(3) 0.549(4) 0.5000(14) 0.055(4) Uani 0.250(14) 1 d G U P A -1
H2_2 H 0.741400 0.570562 0.505939 0.066 Uiso 0.250(14) 1 calc R U P A -1
C3_2 C 0.562(5) 0.444(3) 0.5323(12) 0.054(4) Uani 0.250(14) 1 d G U P A -1
H3_2 H 0.614866 0.394662 0.560232 0.065 Uiso 0.250(14) 1 calc R U P A -1
C4_2 C 0.411(5) 0.412(3) 0.5236(15) 0.056(4) Uani 0.250(14) 1 d G U P A -1
H4_2 H 0.359277 0.340627 0.545692 0.068 Uiso 0.250(14) 1 calc R U P A -1
C5_2 C 0.334(3) 0.484(3) 0.4828(16) 0.055(4) Uani 0.250(14) 1 d G U P A -1
H5_2 H 0.230221 0.462492 0.476858 0.066 Uiso 0.250(14) 1 calc R U P A -1
C6_2 C 0.409(4) 0.589(3) 0.4505(13) 0.055(4) Uani 0.250(14) 1 d G U P A -1
H6_2 H 0.356753 0.638394 0.422564 0.066 Uiso 0.250(14) 1 calc R U P A -1
C1_21 C 0.590(2) 0.610(3) 0.4759(16) 0.056(4) Uani 0.250(14) 1 d G U P A -2
H1_21 H 0.673153 0.674181 0.466857 0.068 Uiso 0.250(14) 1 calc R U P A -2
C2_21 C 0.606(3) 0.508(3) 0.5168(14) 0.057(4) Uani 0.250(14) 1 d G U P A -2
H2_21 H 0.700584 0.502420 0.535668 0.069 Uiso 0.250(14) 1 calc R U P A -2
C3_21 C 0.484(4) 0.414(2) 0.5301(11) 0.055(4) Uani 0.250(14) 1 d G U P A -2
H3_21 H 0.494764 0.344633 0.557995 0.066 Uiso 0.250(14) 1 calc R U P A -2
C4_21 C 0.345(3) 0.423(2) 0.5024(14) 0.055(4) Uani 0.250(14) 1 d G U P A -2
H4_21 H 0.261512 0.358605 0.511511 0.066 Uiso 0.250(14) 1 calc R U P A -2
C5_21 C 0.329(2) 0.525(3) 0.4616(13) 0.054(4) Uani 0.250(14) 1 d G U P A -2
H5_21 H 0.234078 0.530365 0.442700 0.065 Uiso 0.250(14) 1 calc R U P A -2
C6_21 C 0.451(3) 0.618(2) 0.4483(11) 0.054(4) Uani 0.250(14) 1 d G U P A -2
H6_21 H 0.439897 0.688154 0.420372 0.065 Uiso 0.250(14) 1 calc R U P A -2
S1_3 S 0.1010(6) 0.7746(9) 0.3503(4) 0.0296(11) Uani 0.662(11) 1 d . U P B 1
O1_3 O 0.0181(11) 0.8442(9) 0.3064(3) 0.054(2) Uani 0.662(11) 1 d . U P B 1
O2_3 O 0.044(2) 0.6267(18) 0.3469(6) 0.043(3) Uani 0.662(11) 1 d . U P B 1
O3_3 O 0.2530(10) 0.8228(11) 0.3567(5) 0.057(2) Uani 0.662(11) 1 d . U P B 1
C28_3 C 0.054(2) 0.8406(15) 0.4305(9) 0.041(2) Uani 0.662(11) 1 d . U P B 1
F1_3 F -0.0904(15) 0.7967(13) 0.4320(6) 0.052(3) Uani 0.662(11) 1 d . U P B 1
F2_3 F 0.1151(10) 0.7862(13) 0.4789(4) 0.070(3) Uani 0.662(11) 1 d . U P B 1
F3_3 F 0.0891(13) 0.9767(9) 0.4419(5) 0.076(3) Uani 0.662(11) 1 d . U P B 1
S1_31 S 0.1366(16) 0.767(2) 0.3564(9) 0.041(2) Uani 0.338(11) 1 d . U P B 2
O1_31 O 0.128(2) 0.8843(17) 0.3182(8) 0.061(4) Uani 0.338(11) 1 d . U P B 2
O2_31 O 0.037(4) 0.640(4) 0.3254(11) 0.038(5) Uani 0.338(11) 1 d . U P B 2
O3_31 O 0.2791(16) 0.752(2) 0.3723(9) 0.049(4) Uani 0.338(11) 1 d . U P B 2
C28_31 C 0.067(5) 0.809(3) 0.426(2) 0.046(3) Uani 0.338(11) 1 d . U P B 2
F1_31 F -0.070(3) 0.837(2) 0.4212(12) 0.052(4) Uani 0.338(11) 1 d . U P B 2
F2_31 F 0.075(2) 0.717(2) 0.4682(9) 0.065(4) Uani 0.338(11) 1 d . U P B 2
F3_31 F 0.1493(17) 0.940(2) 0.4617(8) 0.057(4) Uani 0.338(11) 1 d . U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.335(6) . ?
N1 C9 1.460(6) . ?
N1 C2 1.514(6) . ?
B1 C1 1.510(7) . ?
B1 C21 1.548(7) . ?
B1 C22 1.590(7) . ?
C1 C4 1.531(6) . ?
N2 C21 1.146(6) . ?
C2 C6 1.522(7) . ?
C2 C3 1.529(7) . ?
C2 C5 1.530(7) . ?
N3 C22 1.344(6) . ?
N3 C23 1.364(6) . ?
N3 C25 1.490(7) . ?
C3 C4 1.538(7) . ?
C3 H3A 0.9900 . ?
C3 H3AB 0.9900 . ?
N4 C22 1.346(6) . ?
N4 C24 1.379(6) . ?
N4 C28 1.474(6) . ?
C4 C8 1.535(7) . ?
C4 C7 1.535(7) . ?
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 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C14 1.398(7) . ?
C9 C10 1.413(7) . ?
C10 C11 1.395(7) . ?
C10 C15 1.525(7) . ?
C11 C12 1.372(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.375(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(7) . ?
C13 H13 0.9500 . ?
C14 C18 1.523(7) . ?
C15 C17 1.536(7) . ?
C15 C16 1.543(7) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.536(7) . ?
C18 C20 1.540(7) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C23 C24 1.332(8) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.512(8) . ?
C25 C27 1.515(9) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.516(8) . ?
C28 C29 1.523(8) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C1_2 C2_2 1.3900 . ?
C1_2 C6_2 1.3900 . ?
C1_2 H1_2 0.9500 . ?
C2_2 C3_2 1.3900 . ?
C2_2 H2_2 0.9500 . ?
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 H6_2 0.9500 . ?
C1_21 C2_21 1.3900 . ?
C1_21 C6_21 1.3900 . ?
C1_21 H1_21 0.9500 . ?
C2_21 C3_21 1.3900 . ?
C2_21 H2_21 0.9500 . ?
C3_21 C4_21 1.3900 . ?
C3_21 H3_21 0.9500 . ?
C4_21 C5_21 1.3900 . ?
C4_21 H4_21 0.9500 . ?
C5_21 C6_21 1.3900 . ?
C5_21 H5_21 0.9500 . ?
C6_21 H6_21 0.9500 . ?
S1_3 O3_3 1.402(10) . ?
S1_3 O2_3 1.426(19) . ?
S1_3 O1_3 1.442(10) . ?
S1_3 C28_3 1.857(18) . ?
C28_3 F3_3 1.294(16) . ?
C28_3 F2_3 1.31(2) . ?
C28_3 F1_3 1.35(2) . ?
S1_31 O3_31 1.39(2) . ?
S1_31 O2_31 1.44(4) . ?
S1_31 O1_31 1.46(2) . ?
S1_31 C28_31 1.70(4) . ?
C28_31 F2_31 1.32(4) . ?
C28_31 F1_31 1.37(5) . ?
C28_31 F3_31 1.44(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C9 123.5(4) . . ?
C1 N1 C2 115.1(4) . . ?
C9 N1 C2 121.4(4) . . ?
C1 B1 C21 125.0(4) . . ?
C1 B1 C22 125.5(4) . . ?
C21 B1 C22 109.4(4) . . ?
N1 C1 B1 124.8(4) . . ?
N1 C1 C4 108.9(4) . . ?
B1 C1 C4 126.2(4) . . ?
N1 C2 C6 110.4(4) . . ?
N1 C2 C3 100.8(4) . . ?
C6 C2 C3 113.6(4) . . ?
N1 C2 C5 111.1(4) . . ?
C6 C2 C5 108.5(4) . . ?
C3 C2 C5 112.2(4) . . ?
C22 N3 C23 109.8(4) . . ?
C22 N3 C25 124.4(4) . . ?
C23 N3 C25 125.5(4) . . ?
C2 C3 C4 107.6(4) . . ?
C2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
C2 C3 H3AB 110.2 . . ?
C4 C3 H3AB 110.2 . . ?
H3A C3 H3AB 108.5 . . ?
C22 N4 C24 110.0(4) . . ?
C22 N4 C28 125.3(4) . . ?
C24 N4 C28 124.5(4) . . ?
C1 C4 C8 114.0(4) . . ?
C1 C4 C7 108.1(4) . . ?
C8 C4 C7 109.5(4) . . ?
C1 C4 C3 102.7(4) . . ?
C8 C4 C3 109.7(4) . . ?
C7 C4 C3 112.8(4) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C9 C10 122.4(4) . . ?
C14 C9 N1 119.0(4) . . ?
C10 C9 N1 118.5(4) . . ?
C11 C10 C9 116.9(5) . . ?
C11 C10 C15 118.5(4) . . ?
C9 C10 C15 124.5(4) . . ?
C12 C11 C10 121.5(5) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 120.2(5) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C14 121.8(5) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C13 C14 C9 117.2(5) . . ?
C13 C14 C18 118.7(5) . . ?
C9 C14 C18 123.9(4) . . ?
C10 C15 C17 112.6(4) . . ?
C10 C15 C16 110.4(4) . . ?
C17 C15 C16 108.6(4) . . ?
C10 C15 H15 108.4 . . ?
C17 C15 H15 108.4 . . ?
C16 C15 H15 108.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C19 111.3(4) . . ?
C14 C18 C20 111.5(4) . . ?
C19 C18 C20 108.6(4) . . ?
C14 C18 H18 108.5 . . ?
C19 C18 H18 108.5 . . ?
C20 C18 H18 108.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 B1 172.9(5) . . ?
N3 C22 N4 105.7(4) . . ?
N3 C22 B1 127.1(4) . . ?
N4 C22 B1 126.3(4) . . ?
C24 C23 N3 108.0(5) . . ?
C24 C23 H23 126.0 . . ?
N3 C23 H23 126.0 . . ?
C23 C24 N4 106.4(5) . . ?
C23 C24 H24 126.8 . . ?
N4 C24 H24 126.8 . . ?
N3 C25 C26 109.9(4) . . ?
N3 C25 C27 109.1(5) . . ?
C26 C25 C27 111.9(5) . . ?
N3 C25 H25 108.6 . . ?
C26 C25 H25 108.6 . . ?
C27 C25 H25 108.6 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 C30 110.5(4) . . ?
N4 C28 C29 109.5(4) . . ?
C30 C28 C29 112.6(5) . . ?
N4 C28 H28 108.0 . . ?
C30 C28 H28 108.0 . . ?
C29 C28 H28 108.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C2_2 C1_2 C6_2 120.0 . . ?
C2_2 C1_2 H1_2 120.0 . . ?
C6_2 C1_2 H1_2 120.0 . . ?
C1_2 C2_2 C3_2 120.0 . . ?
C1_2 C2_2 H2_2 120.0 . . ?
C3_2 C2_2 H2_2 120.0 . . ?
C4_2 C3_2 C2_2 120.0 . . ?
C4_2 C3_2 H3_2 120.0 . . ?
C2_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 . . ?
C4_2 C5_2 C6_2 120.0 . . ?
C4_2 C5_2 H5_2 120.0 . . ?
C6_2 C5_2 H5_2 120.0 . . ?
C5_2 C6_2 C1_2 120.0 . . ?
C5_2 C6_2 H6_2 120.0 . . ?
C1_2 C6_2 H6_2 120.0 . . ?
C2_21 C1_21 C6_21 120.0 . . ?
C2_21 C1_21 H1_21 120.0 . . ?
C6_21 C1_21 H1_21 120.0 . . ?
C1_21 C2_21 C3_21 120.0 . . ?
C1_21 C2_21 H2_21 120.0 . . ?
C3_21 C2_21 H2_21 120.0 . . ?
C2_21 C3_21 C4_21 120.0 . . ?
C2_21 C3_21 H3_21 120.0 . . ?
C4_21 C3_21 H3_21 120.0 . . ?
C5_21 C4_21 C3_21 120.0 . . ?
C5_21 C4_21 H4_21 120.0 . . ?
C3_21 C4_21 H4_21 120.0 . . ?
C4_21 C5_21 C6_21 120.0 . . ?
C4_21 C5_21 H5_21 120.0 . . ?
C6_21 C5_21 H5_21 120.0 . . ?
C5_21 C6_21 C1_21 120.0 . . ?
C5_21 C6_21 H6_21 120.0 . . ?
C1_21 C6_21 H6_21 120.0 . . ?
O3_3 S1_3 O2_3 118.1(10) . . ?
O3_3 S1_3 O1_3 115.1(8) . . ?
O2_3 S1_3 O1_3 114.0(9) . . ?
O3_3 S1_3 C28_3 103.1(8) . . ?
O2_3 S1_3 C28_3 101.7(8) . . ?
O1_3 S1_3 C28_3 101.2(7) . . ?
F3_3 C28_3 F2_3 109.4(14) . . ?
F3_3 C28_3 F1_3 109.5(13) . . ?
F2_3 C28_3 F1_3 104.2(15) . . ?
F3_3 C28_3 S1_3 112.0(12) . . ?
F2_3 C28_3 S1_3 112.1(10) . . ?
F1_3 C28_3 S1_3 109.4(12) . . ?
O3_31 S1_31 O2_31 114(2) . . ?
O3_31 S1_31 O1_31 112.5(17) . . ?
O2_31 S1_31 O1_31 110.7(17) . . ?
O3_31 S1_31 C28_31 109.1(19) . . ?
O2_31 S1_31 C28_31 104(2) . . ?
O1_31 S1_31 C28_31 105.1(16) . . ?
F2_31 C28_31 F1_31 109(3) . . ?
F2_31 C28_31 F3_31 104(3) . . ?
F1_31 C28_31 F3_31 100(2) . . ?
F2_31 C28_31 S1_31 112(2) . . ?
F1_31 C28_31 S1_31 119(3) . . ?
F3_31 C28_31 S1_31 112(3) . . ?

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
C9 N1 C1 B1 -2.4(7) . . . . ?
C2 N1 C1 B1 178.3(4) . . . . ?
C9 N1 C1 C4 175.2(4) . . . . ?
C2 N1 C1 C4 -4.1(5) . . . . ?
C21 B1 C1 N1 0.7(8) . . . . ?
C22 B1 C1 N1 179.1(4) . . . . ?
C21 B1 C1 C4 -176.6(5) . . . . ?
C22 B1 C1 C4 1.9(8) . . . . ?
C1 N1 C2 C6 110.6(5) . . . . ?
C9 N1 C2 C6 -68.7(6) . . . . ?
C1 N1 C2 C3 -9.9(5) . . . . ?
C9 N1 C2 C3 170.8(4) . . . . ?
C1 N1 C2 C5 -129.0(4) . . . . ?
C9 N1 C2 C5 51.7(6) . . . . ?
N1 C2 C3 C4 19.6(5) . . . . ?
C6 C2 C3 C4 -98.6(5) . . . . ?
C5 C2 C3 C4 137.9(4) . . . . ?
N1 C1 C4 C8 134.7(4) . . . . ?
B1 C1 C4 C8 -47.7(7) . . . . ?
N1 C1 C4 C7 -103.3(5) . . . . ?
B1 C1 C4 C7 74.3(6) . . . . ?
N1 C1 C4 C3 16.1(5) . . . . ?
B1 C1 C4 C3 -166.3(5) . . . . ?
C2 C3 C4 C1 -22.2(5) . . . . ?
C2 C3 C4 C8 -143.8(4) . . . . ?
C2 C3 C4 C7 93.9(5) . . . . ?
C1 N1 C9 C14 90.2(6) . . . . ?
C2 N1 C9 C14 -90.6(5) . . . . ?
C1 N1 C9 C10 -87.6(5) . . . . ?
C2 N1 C9 C10 91.7(5) . . . . ?
C14 C9 C10 C11 3.6(7) . . . . ?
N1 C9 C10 C11 -178.7(4) . . . . ?
C14 C9 C10 C15 -173.1(4) . . . . ?
N1 C9 C10 C15 4.5(7) . . . . ?
C9 C10 C11 C12 -2.1(7) . . . . ?
C15 C10 C11 C12 174.9(4) . . . . ?
C10 C11 C12 C13 -0.1(7) . . . . ?
C11 C12 C13 C14 0.9(7) . . . . ?
C12 C13 C14 C9 0.5(7) . . . . ?
C12 C13 C14 C18 -175.4(4) . . . . ?
C10 C9 C14 C13 -2.9(7) . . . . ?
N1 C9 C14 C13 179.5(4) . . . . ?
C10 C9 C14 C18 172.8(4) . . . . ?
N1 C9 C14 C18 -4.8(7) . . . . ?
C11 C10 C15 C17 57.7(6) . . . . ?
C9 C10 C15 C17 -125.5(5) . . . . ?
C11 C10 C15 C16 -63.9(6) . . . . ?
C9 C10 C15 C16 112.9(5) . . . . ?
C13 C14 C18 C19 63.8(6) . . . . ?
C9 C14 C18 C19 -111.8(5) . . . . ?
C13 C14 C18 C20 -57.6(6) . . . . ?
C9 C14 C18 C20 126.7(5) . . . . ?
C23 N3 C22 N4 -0.3(6) . . . . ?
C25 N3 C22 N4 -174.8(4) . . . . ?
C23 N3 C22 B1 169.5(5) . . . . ?
C25 N3 C22 B1 -5.0(8) . . . . ?
C24 N4 C22 N3 1.0(5) . . . . ?
C28 N4 C22 N3 175.8(4) . . . . ?
C24 N4 C22 B1 -168.8(5) . . . . ?
C28 N4 C22 B1 5.9(8) . . . . ?
C1 B1 C22 N3 92.9(6) . . . . ?
C21 B1 C22 N3 -88.4(6) . . . . ?
C1 B1 C22 N4 -99.4(6) . . . . ?
C21 B1 C22 N4 79.3(6) . . . . ?
C22 N3 C23 C24 -0.6(6) . . . . ?
C25 N3 C23 C24 173.9(5) . . . . ?
N3 C23 C24 N4 1.1(6) . . . . ?
C22 N4 C24 C23 -1.3(6) . . . . ?
C28 N4 C24 C23 -176.2(5) . . . . ?
C22 N3 C25 C26 -133.2(5) . . . . ?
C23 N3 C25 C26 53.2(7) . . . . ?
C22 N3 C25 C27 103.9(6) . . . . ?
C23 N3 C25 C27 -69.8(7) . . . . ?
C22 N4 C28 C30 134.9(5) . . . . ?
C24 N4 C28 C30 -51.1(6) . . . . ?
C22 N4 C28 C29 -100.6(6) . . . . ?
C24 N4 C28 C29 73.5(6) . . . . ?
C6_2 C1_2 C2_2 C3_2 0.0 . . . . ?
C1_2 C2_2 C3_2 C4_2 0.0 . . . . ?
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 . . . . ?
C2_2 C1_2 C6_2 C5_2 0.0 . . . . ?
C6_21 C1_21 C2_21 C3_21 0.0 . . . . ?
C1_21 C2_21 C3_21 C4_21 0.0 . . . . ?
C2_21 C3_21 C4_21 C5_21 0.0 . . . . ?
C3_21 C4_21 C5_21 C6_21 0.0 . . . . ?
C4_21 C5_21 C6_21 C1_21 0.0 . . . . ?
C2_21 C1_21 C6_21 C5_21 0.0 . . . . ?
O3_3 S1_3 C28_3 F3_3 60.8(14) . . . . ?
O2_3 S1_3 C28_3 F3_3 -176.3(14) . . . . ?
O1_3 S1_3 C28_3 F3_3 -58.6(15) . . . . ?
O3_3 S1_3 C28_3 F2_3 -62.6(14) . . . . ?
O2_3 S1_3 C28_3 F2_3 60.3(14) . . . . ?
O1_3 S1_3 C28_3 F2_3 178.0(11) . . . . ?
O3_3 S1_3 C28_3 F1_3 -177.7(12) . . . . ?
O2_3 S1_3 C28_3 F1_3 -54.7(14) . . . . ?
O1_3 S1_3 C28_3 F1_3 62.9(12) . . . . ?
O3_31 S1_31 C28_31 F2_31 -55(3) . . . . ?
O2_31 S1_31 C28_31 F2_31 67(3) . . . . ?
O1_31 S1_31 C28_31 F2_31 -176(2) . . . . ?
O3_31 S1_31 C28_31 F1_31 176(3) . . . . ?
O2_31 S1_31 C28_31 F1_31 -61(3) . . . . ?
O1_31 S1_31 C28_31 F1_31 55(3) . . . . ?
O3_31 S1_31 C28_31 F3_31 61(3) . . . . ?
O2_31 S1_31 C28_31 F3_31 -176(3) . . . . ?
O1_31 S1_31 C28_31 F3_31 -60(3) . . . . ?

_refine_diff_density_max         0.493
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.096



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_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_MaHa098_StHa_b_a
_database_code_depnum_ccdc_archive 'CCDC 2071476'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;

_audit_creation_method           'CIF-fill 1.2n (K.Radacki 2005-21)'
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(CAAC)(IiPr)BH(CN)][SPh]'
_chemical_name_common            '[2(CN)-H][PhS]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H47 B N4, C6 H5 S, 0.5 (C7 H8)'
_chemical_formula_sum            'C39.50 H57 B N4 S'
_chemical_formula_weight         630.76

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'
S S 0.3331 0.5567 '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                   9.78460(10)
_cell_length_b                   11.33740(10)
_cell_length_c                   17.2083(2)
_cell_angle_alpha                95.3960(10)
_cell_angle_beta                 95.5070(10)
_cell_angle_gamma                99.3500(10)
_cell_volume                     1863.18(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    44427
_cell_measurement_theta_min      2.6420
_cell_measurement_theta_max      77.0120


_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    1.124
_exptl_crystal_F_000             686
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.087
_exptl_absorpt_coefficient_mu    0.997
_shelx_estimated_absorpt_T_min   0.734
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.34689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.41.73a (Rigaku Oxford Diffraction, 2020) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK 
scaling algorithm.
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 2 0.1332
1 -1 2 0.1206
-1 1 -2 0.1039
-2 1 0 0.1468
2 -1 -1 0.1617
1 -1 -2 0.1164
1 -2 2 0.1215
2 -1 0 0.1653
1 0 -2 0.1186
-1 0 2 0.1165
1 0 0 0.1667
-1 0 0 0.1582
-1 0 -2 0.1239
1 0 2 0.1247
0 0 -1 0.0451
0 0 1 0.0422
2 1 2 0.1338
2 1 -2 0.1361
-2 -1 0 0.1544
-2 -1 2 0.1400
-1 -1 -1 0.1331
0 1 2 0.0328
0 -1 -2 0.0675
1 2 -2 0.0805
-1 -2 2 0.1152
0 2 1 0.0250
0 -2 -1 0.0778
0 2 -1 0.0314
0 -2 1 0.0765

_exptl_absorpt_special_details   ?
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(8)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'microfocus sealed tube (PhotonJet)'
_diffrn_measurement_device_type  'Rigaku OD XtaLAB Synergy-S'

_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 
   # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
 --------------------------------------------------------------------------
   1  ω    -30.00  27.00   0.50    0.16    --  -47.45  24.00 -68.00  114
   2  ω   -122.00 -34.00   0.50    0.16    --  -47.45 -24.00 126.00  176
   3  ω     35.00 122.00   0.50    0.16    --   47.45  24.00 -68.00  174
   4  ω   -160.00 -73.00   0.50    0.65    --  -86.25 -24.00 126.00  174
   5  ω     95.00 178.00   0.50    0.65    --  107.75  24.00 -68.00  166
   6  ω    -70.00  25.00   0.50    0.16    --  -47.45  77.00 -30.00  190
   7  ω    -26.00  28.00   0.50    0.16    --  -47.45  19.00  90.00  108
   8  ω   -120.00 -70.00   0.50    0.16    --  -47.45-125.00 -60.00  100
   9  ω   -120.00 -70.00   0.50    0.16    --  -47.45-125.00 -30.00  100
  10  ω    -27.00  30.00   0.50    0.16    --   47.45 -24.00 126.00  114
  11  ω     31.00  95.00   0.50    0.16    --   47.45-125.00 -30.00  128
  12  ω    -51.00 -14.00   0.50    0.65    --  -86.25  45.00 -90.00   74
  13  ω    -51.00 -14.00   0.50    0.65    --  -86.25  45.00-180.00   74
  14  ω    -71.00 -13.00   0.50    0.65    --  -86.25  61.00  90.00  116
  15  ω     35.00 109.00   0.50    0.65    --  107.75 -94.00 120.00  148
  16  ω     95.00 178.00   0.50    0.65    --  107.75  45.00-120.00  166
  17  ω     35.00 109.00   0.50    0.65    --  107.75 -94.00 -60.00  148
  18  ω     35.00 109.00   0.50    0.65    --  107.75 -94.00 -90.00  148
  19  ω     35.00 117.00   0.50    0.65    --  107.75-125.00 -60.00  164
  20  ω     95.00 178.00   0.50    0.65    --  107.75  30.00  30.00  166
  21  ω     36.00 123.00   0.50    0.65    --  107.75-133.00 116.25  174
  22  ω     35.00  71.00   0.50    0.65    --  107.75 -61.00  60.00   72
  23  ω     35.00 109.00   0.50    0.65    --  107.75 -94.00 150.00  148
  24  ω     35.00 106.00   0.50    0.65    --  107.75 -77.00 150.00  142
  25  ω     35.00 109.00   0.50    0.65    --  107.75 -94.00-180.00  148
  26  ω     92.00 178.00   0.50    0.65    --  107.75 125.00 150.00  172
  27  ω     35.00 117.00   0.50    0.65    --  107.75-125.00   0.00  164
  28  ω     35.00  83.00   0.50    0.65    --  107.75 -68.00-118.87   96
  29  ω     95.00 178.00   0.50    0.65    --  107.75  30.00  90.00  166
  30  ω     92.00 178.00   0.50    0.65    --  107.75 125.00-150.00  172
  31  ω     35.00 106.00   0.50    0.65    --  107.75 -77.00-180.00  142
  32  ω     35.00 109.00   0.50    0.65    --  107.75 -94.00-150.00  148
  33  ω     35.00 117.00   0.50    0.65    --  107.75-125.00 -90.00  164
  34  ω     95.00 178.00   0.50    0.65    --  107.75  30.00-180.00  166
  35  ω     35.00 117.00   0.50    0.65    --  107.75-125.00-120.00  164
  36  ω     35.00  68.00   0.50    0.65    --  107.75 -59.00-115.25   66
  37  ω     88.00 178.00   0.50    0.65    --  107.75  71.00 173.45  180
  38  ω     95.00 178.00   0.50    0.65    --  107.75  45.00 120.00  166
  39  ω     95.00 178.00   0.50    0.65    --  107.75  30.00 -30.00  166
  40  ω     92.00 178.00   0.50    0.65    --  107.75 125.00  90.00  172
  41  ω     35.00  71.00   0.50    0.65    --  107.75 -61.00  90.00   72
  42  ω     35.00 132.00   0.50    0.65    --  107.75 -79.00  52.47  194
  43  ω     38.00 125.00   0.50    0.65    --  107.75-136.00-107.49  174
  44  ω     95.00 178.00   0.50    0.65    --  107.75  45.00-150.00  166
  45  ω     95.00 178.00   0.50    0.65    --  107.75  45.00   0.00  166
  46  ω     36.00 123.00   0.50    0.65    --  107.75-133.00  28.67  174
  47  ω     35.00 106.00   0.50    0.65    --  107.75 -77.00 120.00  142
  48  ω     35.00  71.00   0.50    0.65    --  107.75 -61.00 -30.00   72
  49  ω     35.00 117.00   0.50    0.65    --  107.75-125.00 120.00  164
  50  ω     90.00 178.00   0.50    0.65    --  107.75  65.00 152.50  176
  51  ω     92.00 178.00   0.50    0.65    --  107.75 125.00 120.00  172
  52  ω     35.00 106.00   0.50    0.65    --  107.75 -77.00-120.00  142
  53  ω     35.00 106.00   0.50    0.65    --  107.75 -77.00 -30.00  142
  54  ω     35.00 117.00   0.50    0.65    --  107.75-125.00  60.00  164
  55  ω     35.00 109.00   0.50    0.65    --  107.75 -94.00  30.00  148
  56  ω     35.00 117.00   0.50    0.65    --  107.75-125.00-180.00  164
  57  ω     35.00 117.00   0.50    0.65    --  107.75-125.00 150.00  164
  58  ω     94.00 178.00   0.50    0.65    --  107.75  15.00 -90.00  168
  59  ω     92.00 178.00   0.50    0.65    --  107.75 125.00  60.00  172
  60  ω     35.00 109.00   0.50    0.65    --  107.75 -94.00  60.00  148
  61  ω     35.00 106.00   0.50    0.65    --  107.75 -77.00-150.00  142
  62  ω     85.00 178.00   0.50    0.65    --  107.75  77.00 150.00  186
  63  ω     35.00 133.00   0.50    0.65    --  107.75 -83.00  12.53  196
  64  ω   -120.00 -25.00   0.50    0.16    --  -47.45 -77.00-150.00  190
  65  ω   -120.00 -25.00   0.50    0.16    --  -47.45 -77.00  60.00  190
  66  ω   -120.00 -32.00   0.50    0.16    --  -47.45 -57.00 120.00  176
  67  ω   -120.00 -25.00   0.50    0.16    --  -47.45 -77.00   0.00  190
  68  ω   -120.00 -25.00   0.50    0.16    --  -47.45 -77.00 -90.00  190
  69  ω   -120.00 -25.00   0.50    0.16    --  -47.45 -77.00 -60.00  190
  70  ω   -120.00 -25.00   0.50    0.16    --  -47.45 -77.00 120.00  190
  71  ω   -120.00 -25.00   0.50    0.16    --  -47.45 -77.00  30.00  190
  72  ω     35.00 121.00   0.50    0.16    --   47.45  37.00 -30.00  172
  73  ω     35.00 121.00   0.50    0.16    --   47.45  37.00-180.00  172
  74  ω   -159.00 -64.00   0.50    0.65    --  -86.25 -75.00 -84.88  190
  75  ω   -159.00 -64.00   0.50    0.65    --  -86.25 -75.00 -38.16  190
  76  ω   -159.00 -61.00   0.50    0.65    --  -86.25 -83.00 126.92  196
  77  ω   -159.00 -61.00   0.50    0.65    --  -86.25 -83.00  11.96  196
  78  ω   -159.00 -62.00   0.50    0.65    --  -86.25 -79.00  59.23  194
  79  ω   -159.00 -63.00   0.50    0.65    --  -86.25 -77.00  90.00  192
  80  ω   -159.00 -62.00   0.50    0.65    --  -86.25 -79.00-131.44  194

;

_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'HPAD area detector (HyPix 6000)'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            79195
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_av_R_equivalents  0.0715
_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       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.596
_diffrn_reflns_theta_max         78.007
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7909
_reflns_number_gt                7153
_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 1.171.41.73a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.

The asymmetric unit contains half a toluene molecule positioned on an inversion center,
the benzene ring of which was modelled using AFIX 66.

The PhS- anion was modelled as twofold disordered, with parts refined to a 55:45 ratio.
The benzene rings of both parts were idealised with AFIX 66 and ADPs restrained with SIMU 0.01.
The ADPs of C2_15 were additionally restrained with ISOR 0.001. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0934P)²+0.5166P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7909
_refine_ls_number_parameters     487
_refine_ls_number_restraints     216
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1551
_refine_ls_wR_factor_gt          0.1515
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.087
_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
S1_5 S 0.1522(7) 0.2687(5) 0.0655(4) 0.0319(6) Uani 0.550(15) 1 d . U P A 1
C2_5 C 0.0545(6) 0.2579(5) 0.1465(3) 0.0391(14) Uani 0.550(15) 1 d G U P A 1
C3_5 C -0.0513(7) 0.1605(5) 0.1481(4) 0.0317(11) Uani 0.550(15) 1 d G U P A 1
H3_5 H -0.065579 0.094788 0.107924 0.038 Uiso 0.550(15) 1 calc R U P A 1
C4_5 C -0.1363(7) 0.1592(5) 0.2084(4) 0.0373(10) Uani 0.550(15) 1 d G U P A 1
H4_5 H -0.208587 0.092574 0.209428 0.045 Uiso 0.550(15) 1 calc R U P A 1
C5_5 C -0.1154(7) 0.2553(5) 0.2671(3) 0.0360(11) Uani 0.550(15) 1 d G U P A 1
H5_5 H -0.173430 0.254364 0.308342 0.043 Uiso 0.550(15) 1 calc R U P A 1
C6_5 C -0.0095(8) 0.3527(4) 0.2656(2) 0.0335(11) Uani 0.550(15) 1 d G U P A 1
H6_5 H 0.004735 0.418369 0.305753 0.040 Uiso 0.550(15) 1 calc R U P A 1
C7_5 C 0.0754(6) 0.3540(4) 0.2053(3) 0.0265(8) Uani 0.550(15) 1 d G U P A 1
H7_5 H 0.147745 0.420585 0.204249 0.032 Uiso 0.550(15) 1 calc R U P A 1
S1_15 S 0.1523(8) 0.2513(6) 0.0529(4) 0.0271(6) Uani 0.450(15) 1 d . U P A 2
C2_15 C 0.0606(6) 0.2627(6) 0.1379(3) 0.0147(9) Uani 0.450(15) 1 d G U P A 2
C3_15 C -0.0479(8) 0.1730(6) 0.1496(4) 0.0323(14) Uani 0.450(15) 1 d G U P A 2
H3_15 H -0.077727 0.105714 0.111038 0.039 Uiso 0.450(15) 1 calc R U P A 2
C4_15 C -0.1129(8) 0.1816(7) 0.2178(5) 0.0368(11) Uani 0.450(15) 1 d G U P A 2
H4_15 H -0.187056 0.120309 0.225831 0.044 Uiso 0.450(15) 1 calc R U P A 2
C5_15 C -0.0693(10) 0.2800(7) 0.2743(3) 0.0425(13) Uani 0.450(15) 1 d G U P A 2
H5_15 H -0.113702 0.285965 0.320857 0.051 Uiso 0.450(15) 1 calc R U P A 2
C6_15 C 0.0392(10) 0.3698(6) 0.2625(3) 0.0414(13) Uani 0.450(15) 1 d G U P A 2
H6_15 H 0.068982 0.437028 0.301091 0.050 Uiso 0.450(15) 1 calc R U P A 2
C7_15 C 0.1041(7) 0.3611(5) 0.1943(4) 0.0369(12) Uani 0.450(15) 1 d G U P A 2
H7_15 H 0.178313 0.422435 0.186298 0.044 Uiso 0.450(15) 1 calc R U P A 2
C1_6 C 0.8436(5) 0.3536(4) 0.5751(3) 0.0648(11) Uani 0.5 1 d . . P B -1
H1A_6 H 0.747790 0.336522 0.549213 0.097 Uiso 0.5 1 calc R U P B -1
H1B_6 H 0.844094 0.388155 0.629567 0.097 Uiso 0.5 1 calc R U P B -1
H1C_6 H 0.881847 0.278874 0.574617 0.097 Uiso 0.5 1 calc R U P B -1
C2_6 C 0.9281(5) 0.4383(2) 0.5338(2) 0.0462(11) Uani 0.5 1 d G . P B -1
C3_6 C 0.8824(4) 0.5471(3) 0.5268(2) 0.0491(12) Uani 0.5 1 d G . P B -1
H3_6 H 0.798777 0.560982 0.547148 0.059 Uiso 0.5 1 calc R U P B -1
C4_6 C 0.9590(5) 0.63556(18) 0.4901(2) 0.0501(11) Uani 0.5 1 d G . P B -1
H4_6 H 0.927716 0.709909 0.485370 0.060 Uiso 0.5 1 calc R U P B -1
C5_6 C 1.0813(5) 0.6152(2) 0.4604(2) 0.0479(12) Uani 0.5 1 d G . P B -1
H5_6 H 1.133613 0.675712 0.435299 0.058 Uiso 0.5 1 calc R U P B -1
C6_6 C 1.1270(5) 0.5065(3) 0.4673(2) 0.0523(13) Uani 0.5 1 d G . P B -1
H6_6 H 1.210571 0.492587 0.447005 0.063 Uiso 0.5 1 calc R U P B -1
C7_6 C 1.0504(5) 0.41800(19) 0.5040(2) 0.0473(11) Uani 0.5 1 d G . P B -1
H7_6 H 1.081633 0.343658 0.508782 0.057 Uiso 0.5 1 calc R U P B -1
C1 C 0.60766(16) 0.79713(12) 0.21729(8) 0.0312(3) Uani 1 1 d . . . . .
N1 N 0.69966(13) 0.79267(11) 0.27613(7) 0.0290(3) Uani 1 1 d . . . . .
B1 B 0.44071(19) 0.78399(16) 0.22007(10) 0.0333(4) Uani 1 1 d . . . . .
H1 H 0.4076(18) 0.6842(16) 0.2088(10) 0.033(4) Uiso 1 1 d . . . . .
C2 C 0.67430(18) 0.78956(14) 0.14050(9) 0.0358(3) Uani 1 1 d . . . . .
N2 N 0.33582(16) 0.84694(15) 0.35672(8) 0.0451(3) Uani 1 1 d . . . . .
C3 C 0.83085(18) 0.81115(15) 0.16854(9) 0.0383(4) Uani 1 1 d . . . . .
H3A H 0.878448 0.758142 0.135428 0.046 Uiso 1 1 calc R U . . .
H3AB H 0.872663 0.895787 0.165000 0.046 Uiso 1 1 calc R U . . .
N3 N 0.33716(14) 0.95953(11) 0.15364(7) 0.0331(3) Uani 1 1 d . . . . .
C4 C 0.84702(16) 0.78318(14) 0.25380(9) 0.0350(3) Uani 1 1 d . . . . .
N4 N 0.25566(14) 0.78145(11) 0.09650(7) 0.0329(3) Uani 1 1 d . . . . .
C5 C 0.6403(2) 0.88226(16) 0.08521(9) 0.0421(4) Uani 1 1 d . . . . .
H5A H 0.698040 0.880378 0.041789 0.063 Uiso 1 1 calc R U . . .
H5B H 0.659447 0.962779 0.114371 0.063 Uiso 1 1 calc R U . . .
H5C H 0.541576 0.862754 0.064211 0.063 Uiso 1 1 calc R U . . .
C6 C 0.6236(2) 0.66245(15) 0.09715(9) 0.0418(4) Uani 1 1 d . . . . .
H6A H 0.672993 0.652554 0.050666 0.063 Uiso 1 1 calc R U . . .
H6B H 0.523212 0.651550 0.080917 0.063 Uiso 1 1 calc R U . . .
H6C H 0.642518 0.602385 0.132294 0.063 Uiso 1 1 calc R U . . .
C7 C 0.95929(17) 0.87321(16) 0.30458(11) 0.0427(4) Uani 1 1 d . . . . .
H7A H 1.050534 0.865473 0.287626 0.064 Uiso 1 1 calc R U . . .
H7B H 0.958510 0.857542 0.359590 0.064 Uiso 1 1 calc R U . . .
H7C H 0.941455 0.954855 0.299358 0.064 Uiso 1 1 calc R U . . .
C8 C 0.87657(18) 0.65696(16) 0.26372(10) 0.0402(4) Uani 1 1 d . . . . .
H8A H 0.970413 0.651066 0.250129 0.060 Uiso 1 1 calc R U . . .
H8B H 0.807929 0.597688 0.229002 0.060 Uiso 1 1 calc R U . . .
H8C H 0.870346 0.641105 0.318391 0.060 Uiso 1 1 calc R U . . .
C9 C 0.67037(14) 0.78173(12) 0.35737(8) 0.0275(3) Uani 1 1 d . . . . .
C10 C 0.61631(15) 0.66747(13) 0.37814(8) 0.0296(3) Uani 1 1 d . . . . .
C11 C 0.59675(18) 0.65994(14) 0.45681(9) 0.0375(3) Uani 1 1 d . . . . .
H11 H 0.560606 0.584140 0.472716 0.045 Uiso 1 1 calc R U . . .
C12 C 0.6282(2) 0.75901(15) 0.51210(9) 0.0417(4) Uani 1 1 d . . . . .
H12 H 0.616243 0.750568 0.565548 0.050 Uiso 1 1 calc R U . . .
C13 C 0.67744(17) 0.87104(14) 0.48995(9) 0.0356(3) Uani 1 1 d . . . . .
H13 H 0.697429 0.939198 0.528370 0.043 Uiso 1 1 calc R U . . .
C14 C 0.69804(15) 0.88523(13) 0.41211(8) 0.0295(3) Uani 1 1 d . . . . .
C15 C 0.57223(16) 0.55275(13) 0.32160(9) 0.0334(3) Uani 1 1 d . . . . .
H15 H 0.592779 0.571418 0.267828 0.040 Uiso 1 1 calc R U . . .
C16 C 0.41531(18) 0.50624(15) 0.31877(12) 0.0457(4) Uani 1 1 d . . . . .
H16A H 0.386755 0.439966 0.276557 0.069 Uiso 1 1 calc R U . . .
H16B H 0.363741 0.571525 0.308822 0.069 Uiso 1 1 calc R U . . .
H16C H 0.395232 0.477515 0.369123 0.069 Uiso 1 1 calc R U . . .
C17 C 0.65020(18) 0.45125(14) 0.34426(10) 0.0378(3) Uani 1 1 d . . . . .
H17A H 0.625934 0.382732 0.303357 0.057 Uiso 1 1 calc R U . . .
H17B H 0.623369 0.425960 0.394373 0.057 Uiso 1 1 calc R U . . .
H17C H 0.750922 0.480467 0.349464 0.057 Uiso 1 1 calc R U . . .
C18 C 0.74033(16) 1.01320(13) 0.39202(9) 0.0328(3) Uani 1 1 d . . . . .
H18 H 0.754178 1.009579 0.335072 0.039 Uiso 1 1 calc R U . . .
C19 C 0.62427(18) 1.08661(14) 0.40625(9) 0.0379(3) Uani 1 1 d . . . . .
H19A H 0.647854 1.165598 0.387525 0.057 Uiso 1 1 calc R U . . .
H19B H 0.615053 1.097123 0.462581 0.057 Uiso 1 1 calc R U . . .
H19C H 0.535927 1.043909 0.377728 0.057 Uiso 1 1 calc R U . . .
C20 C 0.87581(18) 1.07841(15) 0.44013(11) 0.0435(4) Uani 1 1 d . . . . .
H20A H 0.902477 1.157619 0.422255 0.065 Uiso 1 1 calc R U . . .
H20B H 0.949911 1.031002 0.433091 0.065 Uiso 1 1 calc R U . . .
H20C H 0.861749 1.088330 0.495829 0.065 Uiso 1 1 calc R U . . .
C21 C 0.38737(16) 0.82130(14) 0.30184(9) 0.0348(3) Uani 1 1 d . . . . .
C22 C 0.35060(16) 0.84247(13) 0.15409(8) 0.0332(3) Uani 1 1 d . . . . .
C23 C 0.23228(16) 0.97093(13) 0.09622(8) 0.0336(3) Uani 1 1 d . . . . .
H23 H 0.202394 1.043450 0.084232 0.040 Uiso 1 1 calc R U . . .
C24 C 0.18087(17) 0.85960(13) 0.06069(9) 0.0337(3) Uani 1 1 d . . . . .
H24 H 0.107324 0.838465 0.019004 0.040 Uiso 1 1 calc R U . . .
C25 C 0.41971(17) 1.06311(14) 0.20523(9) 0.0375(3) Uani 1 1 d . . . . .
H25 H 0.495688 1.034260 0.237388 0.045 Uiso 1 1 calc R U . . .
C26 C 0.3274(2) 1.11629(16) 0.26063(10) 0.0441(4) Uani 1 1 d . . . . .
H26A H 0.382997 1.184634 0.294955 0.066 Uiso 1 1 calc R U . . .
H26B H 0.288557 1.054844 0.292680 0.066 Uiso 1 1 calc R U . . .
H26C H 0.251291 1.143598 0.229890 0.066 Uiso 1 1 calc R U . . .
C27 C 0.48619(19) 1.15668(15) 0.15558(11) 0.0434(4) Uani 1 1 d . . . . .
H27A H 0.552375 1.218910 0.189570 0.065 Uiso 1 1 calc R U . . .
H27B H 0.413443 1.193547 0.129021 0.065 Uiso 1 1 calc R U . . .
H27C H 0.535415 1.117651 0.116296 0.065 Uiso 1 1 calc R U . . .
C28 C 0.22793(17) 0.64982(13) 0.07063(9) 0.0349(3) Uani 1 1 d . . . . .
H28 H 0.298062 0.611872 0.101085 0.042 Uiso 1 1 calc R U . . .
C29 C 0.24569(18) 0.62833(14) -0.01623(9) 0.0376(3) Uani 1 1 d . . . . .
H29A H 0.234285 0.541687 -0.032167 0.056 Uiso 1 1 calc R U . . .
H29B H 0.338947 0.667279 -0.025199 0.056 Uiso 1 1 calc R U . . .
H29C H 0.175272 0.662189 -0.047215 0.056 Uiso 1 1 calc R U . . .
C30 C 0.0842(2) 0.59529(15) 0.08830(11) 0.0433(4) Uani 1 1 d . . . . .
H30A H 0.069514 0.507840 0.075093 0.065 Uiso 1 1 calc R U . . .
H30B H 0.013780 0.628655 0.056983 0.065 Uiso 1 1 calc R U . . .
H30C H 0.076266 0.614050 0.144275 0.065 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1_5 C2_5 1.768(7) . ?
C2_5 C3_5 1.3900 . ?
C2_5 C7_5 1.3900 . ?
C3_5 C4_5 1.3900 . ?
C3_5 H3_5 0.9500 . ?
C4_5 C5_5 1.3900 . ?
C4_5 H4_5 0.9500 . ?
C5_5 C6_5 1.3900 . ?
C5_5 H5_5 0.9500 . ?
C6_5 C7_5 1.3900 . ?
C6_5 H6_5 0.9500 . ?
C7_5 H7_5 0.9500 . ?
S1_15 C2_15 1.793(8) . ?
C2_15 C3_15 1.3900 . ?
C2_15 C7_15 1.3900 . ?
C3_15 C4_15 1.3900 . ?
C3_15 H3_15 0.9500 . ?
C4_15 C5_15 1.3900 . ?
C4_15 H4_15 0.9500 . ?
C5_15 C6_15 1.3900 . ?
C5_15 H5_15 0.9500 . ?
C6_15 C7_15 1.3900 . ?
C6_15 H6_15 0.9500 . ?
C7_15 H7_15 0.9500 . ?
C1_6 C2_6 1.447(6) . ?
C1_6 H1A_6 0.9800 . ?
C1_6 H1B_6 0.9800 . ?
C1_6 H1C_6 0.9800 . ?
C2_6 C3_6 1.3900 . ?
C2_6 C7_6 1.3900 . ?
C3_6 C4_6 1.3900 . ?
C3_6 H3_6 0.9500 . ?
C4_6 C5_6 1.3900 . ?
C4_6 H4_6 0.9500 . ?
C5_6 C6_6 1.3900 . ?
C5_6 H5_6 0.9500 . ?
C6_6 C7_6 1.3900 . ?
C6_6 H6_6 0.9500 . ?
C7_6 H7_6 0.9500 . ?
C1 N1 1.2990(19) . ?
C1 C2 1.530(2) . ?
C1 B1 1.622(2) . ?
N1 C9 1.4663(17) . ?
N1 C4 1.5450(18) . ?
B1 C21 1.591(2) . ?
B1 C22 1.627(2) . ?
B1 H1 1.118(18) . ?
C2 C3 1.534(2) . ?
C2 C5 1.537(2) . ?
C2 C6 1.541(2) . ?
N2 C21 1.148(2) . ?
C3 C4 1.529(2) . ?
C3 H3A 0.9900 . ?
C3 H3AB 0.9900 . ?
N3 C22 1.3554(18) . ?
N3 C23 1.3852(18) . ?
N3 C25 1.476(2) . ?
C4 C7 1.515(2) . ?
C4 C8 1.527(2) . ?
N4 C22 1.345(2) . ?
N4 C24 1.3881(17) . ?
N4 C28 1.4897(19) . ?
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 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C14 1.406(2) . ?
C9 C10 1.409(2) . ?
C10 C11 1.394(2) . ?
C10 C15 1.524(2) . ?
C11 C12 1.376(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(2) . ?
C13 H13 0.9500 . ?
C14 C18 1.524(2) . ?
C15 C16 1.535(2) . ?
C15 C17 1.5398(19) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.531(2) . ?
C18 C19 1.538(2) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C23 C24 1.345(2) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.524(2) . ?
C25 C27 1.527(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.512(2) . ?
C28 C29 1.523(2) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
C3_5 C2_5 C7_5 120.0 . . ?
C3_5 C2_5 S1_5 120.8(3) . . ?
C7_5 C2_5 S1_5 118.9(3) . . ?
C2_5 C3_5 C4_5 120.0 . . ?
C2_5 C3_5 H3_5 120.0 . . ?
C4_5 C3_5 H3_5 120.0 . . ?
C3_5 C4_5 C5_5 120.0 . . ?
C3_5 C4_5 H4_5 120.0 . . ?
C5_5 C4_5 H4_5 120.0 . . ?
C4_5 C5_5 C6_5 120.0 . . ?
C4_5 C5_5 H5_5 120.0 . . ?
C6_5 C5_5 H5_5 120.0 . . ?
C7_5 C6_5 C5_5 120.0 . . ?
C7_5 C6_5 H6_5 120.0 . . ?
C5_5 C6_5 H6_5 120.0 . . ?
C6_5 C7_5 C2_5 120.0 . . ?
C6_5 C7_5 H7_5 120.0 . . ?
C2_5 C7_5 H7_5 120.0 . . ?
C3_15 C2_15 C7_15 120.0 . . ?
C3_15 C2_15 S1_15 121.3(4) . . ?
C7_15 C2_15 S1_15 118.6(4) . . ?
C2_15 C3_15 C4_15 120.0 . . ?
C2_15 C3_15 H3_15 120.0 . . ?
C4_15 C3_15 H3_15 120.0 . . ?
C3_15 C4_15 C5_15 120.0 . . ?
C3_15 C4_15 H4_15 120.0 . . ?
C5_15 C4_15 H4_15 120.0 . . ?
C4_15 C5_15 C6_15 120.0 . . ?
C4_15 C5_15 H5_15 120.0 . . ?
C6_15 C5_15 H5_15 120.0 . . ?
C7_15 C6_15 C5_15 120.0 . . ?
C7_15 C6_15 H6_15 120.0 . . ?
C5_15 C6_15 H6_15 120.0 . . ?
C6_15 C7_15 C2_15 120.0 . . ?
C6_15 C7_15 H7_15 120.0 . . ?
C2_15 C7_15 H7_15 120.0 . . ?
C2_6 C1_6 H1A_6 109.5 . . ?
C2_6 C1_6 H1B_6 109.5 . . ?
H1A_6 C1_6 H1B_6 109.5 . . ?
C2_6 C1_6 H1C_6 109.5 . . ?
H1A_6 C1_6 H1C_6 109.5 . . ?
H1B_6 C1_6 H1C_6 109.5 . . ?
C3_6 C2_6 C7_6 120.0 . . ?
C3_6 C2_6 C1_6 115.8(3) . . ?
C7_6 C2_6 C1_6 124.1(3) . . ?
C4_6 C3_6 C2_6 120.0 . . ?
C4_6 C3_6 H3_6 120.0 . . ?
C2_6 C3_6 H3_6 120.0 . . ?
C3_6 C4_6 C5_6 120.0 . . ?
C3_6 C4_6 H4_6 120.0 . . ?
C5_6 C4_6 H4_6 120.0 . . ?
C4_6 C5_6 C6_6 120.0 . . ?
C4_6 C5_6 H5_6 120.0 . . ?
C6_6 C5_6 H5_6 120.0 . . ?
C5_6 C6_6 C7_6 120.0 . . ?
C5_6 C6_6 H6_6 120.0 . . ?
C7_6 C6_6 H6_6 120.0 . . ?
C6_6 C7_6 C2_6 120.0 . . ?
C6_6 C7_6 H7_6 120.0 . . ?
C2_6 C7_6 H7_6 120.0 . . ?
N1 C1 C2 109.88(13) . . ?
N1 C1 B1 125.96(13) . . ?
C2 C1 B1 122.98(13) . . ?
C1 N1 C9 125.46(12) . . ?
C1 N1 C4 114.85(12) . . ?
C9 N1 C4 119.26(11) . . ?
C21 B1 C1 117.64(13) . . ?
C21 B1 C22 106.17(11) . . ?
C1 B1 C22 118.26(13) . . ?
C21 B1 H1 105.1(9) . . ?
C1 B1 H1 101.2(9) . . ?
C22 B1 H1 107.0(9) . . ?
C1 C2 C3 103.15(12) . . ?
C1 C2 C5 114.47(12) . . ?
C3 C2 C5 110.64(14) . . ?
C1 C2 C6 108.06(13) . . ?
C3 C2 C6 111.82(13) . . ?
C5 C2 C6 108.66(13) . . ?
C4 C3 C2 107.44(12) . . ?
C4 C3 H3A 110.2 . . ?
C2 C3 H3A 110.2 . . ?
C4 C3 H3AB 110.2 . . ?
C2 C3 H3AB 110.2 . . ?
H3A C3 H3AB 108.5 . . ?
C22 N3 C23 110.20(12) . . ?
C22 N3 C25 126.81(12) . . ?
C23 N3 C25 123.00(12) . . ?
C7 C4 C8 108.33(13) . . ?
C7 C4 C3 112.32(14) . . ?
C8 C4 C3 114.30(13) . . ?
C7 C4 N1 112.18(12) . . ?
C8 C4 N1 109.37(12) . . ?
C3 C4 N1 100.20(11) . . ?
C22 N4 C24 110.27(12) . . ?
C22 N4 C28 128.10(12) . . ?
C24 N4 C28 121.63(13) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C9 C10 122.16(12) . . ?
C14 C9 N1 119.02(12) . . ?
C10 C9 N1 118.82(12) . . ?
C11 C10 C9 116.98(13) . . ?
C11 C10 C15 117.29(13) . . ?
C9 C10 C15 125.69(13) . . ?
C12 C11 C10 121.94(14) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C11 C12 C13 120.08(14) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 120.96(14) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C9 117.79(13) . . ?
C13 C14 C18 117.16(13) . . ?
C9 C14 C18 124.94(12) . . ?
C10 C15 C16 110.90(13) . . ?
C10 C15 C17 112.51(12) . . ?
C16 C15 C17 107.99(13) . . ?
C10 C15 H15 108.4 . . ?
C16 C15 H15 108.4 . . ?
C17 C15 H15 108.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C20 112.55(12) . . ?
C14 C18 C19 110.24(13) . . ?
C20 C18 C19 108.65(13) . . ?
C14 C18 H18 108.4 . . ?
C20 C18 H18 108.4 . . ?
C19 C18 H18 108.4 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 B1 173.11(16) . . ?
N4 C22 N3 105.69(12) . . ?
N4 C22 B1 126.11(13) . . ?
N3 C22 B1 127.30(13) . . ?
C24 C23 N3 106.83(12) . . ?
C24 C23 H23 126.6 . . ?
N3 C23 H23 126.6 . . ?
C23 C24 N4 107.01(13) . . ?
C23 C24 H24 126.5 . . ?
N4 C24 H24 126.5 . . ?
N3 C25 C26 109.90(14) . . ?
N3 C25 C27 109.88(13) . . ?
C26 C25 C27 111.44(14) . . ?
N3 C25 H25 108.5 . . ?
C26 C25 H25 108.5 . . ?
C27 C25 H25 108.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 C30 109.85(12) . . ?
N4 C28 C29 109.62(12) . . ?
C30 C28 C29 112.29(14) . . ?
N4 C28 H28 108.3 . . ?
C30 C28 H28 108.3 . . ?
C29 C28 H28 108.3 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_refine_diff_density_max         0.706
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.052



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_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_AnRe150_ref2_a
_database_code_depnum_ccdc_archive 'CCDC 2071477'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2021-03-18 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_audit_creation_method           'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[(CAAC)(IiPr)B(NCS)][OTf]'
_chemical_name_common            '[2(NCS)][OTf]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H47 B N4 S, C F3 O3 S'
_chemical_formula_sum            'C31 H47 B F3 N4 O3 S2'
_chemical_formula_weight         655.65

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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a                   12.31193(8)
_cell_length_b                   15.53996(11)
_cell_length_c                   36.3830(2)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     6961.04(8)
_cell_formula_units_Z            8.00
_cell_measurement_temperature    99.9(6)
_cell_measurement_reflns_used    29337
_cell_measurement_theta_min      2.4590
_cell_measurement_theta_max      76.9930
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_F_000             2792.000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.142
_exptl_absorpt_coefficient_mu    1.827
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian

_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99.9(6)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            58073
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.4288
_diffrn_reflns_theta_max         72.118

_diffrn_reflns_theta_full        74.3338
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.9982
_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             6847
_reflns_number_gt                6484
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2014/4 (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          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.


;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0571P)²+5.0390P] 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         6847
_refine_ls_number_parameters     409
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1188
_refine_ls_wR_factor_gt          0.1172
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
C1 C 0.42755(12) 0.50664(10) 0.36640(4) 0.0169(3) Uani 1 1 d . . . . .
N1 N 0.49797(10) 0.49557(8) 0.33863(3) 0.0169(3) Uani 1 1 d . . . . .
C2 C 0.56603(13) 0.41447(10) 0.34168(4) 0.0216(3) Uani 1 1 d . . . . .
C3 C 0.49715(14) 0.36294(11) 0.36878(5) 0.0236(3) Uani 1 1 d . . . . .
H3A H 0.543380 0.328580 0.384618 0.028 Uiso 1 1 calc R U . . .
H3AB H 0.448483 0.324681 0.355647 0.028 Uiso 1 1 calc R U . . .
C4 C 0.43165(13) 0.42801(10) 0.39176(4) 0.0202(3) Uani 1 1 d . . . . .
C5 C 0.57771(16) 0.36958(12) 0.30467(5) 0.0299(4) Uani 1 1 d . . . . .
H5A H 0.507544 0.351240 0.296246 0.045 Uiso 1 1 calc R U . . .
H5B H 0.624322 0.320435 0.307284 0.045 Uiso 1 1 calc R U . . .
H5C H 0.608634 0.408776 0.287168 0.045 Uiso 1 1 calc R U . . .
C6 C 0.67892(14) 0.43570(12) 0.35653(5) 0.0295(4) Uani 1 1 d . . . . .
H6A H 0.672107 0.467610 0.379009 0.044 Uiso 1 1 calc R U . . .
H6B H 0.717731 0.469543 0.338791 0.044 Uiso 1 1 calc R U . . .
H6C H 0.717896 0.383290 0.361137 0.044 Uiso 1 1 calc R U . . .
C7 C 0.31830(14) 0.39093(12) 0.39971(5) 0.0281(4) Uani 1 1 d . . . . .
H7A H 0.279949 0.382878 0.376995 0.042 Uiso 1 1 calc R U . . .
H7B H 0.278637 0.430148 0.415057 0.042 Uiso 1 1 calc R U . . .
H7C H 0.325527 0.336623 0.412043 0.042 Uiso 1 1 calc R U . . .
C8 C 0.48695(15) 0.44963(12) 0.42838(4) 0.0277(4) Uani 1 1 d . . . . .
H8A H 0.555544 0.476890 0.423703 0.042 Uiso 1 1 calc R U . . .
H8B H 0.498474 0.397667 0.442104 0.042 Uiso 1 1 calc R U . . .
H8C H 0.441453 0.487866 0.442251 0.042 Uiso 1 1 calc R U . . .
C9 C 0.51154(12) 0.55520(10) 0.30822(4) 0.0186(3) Uani 1 1 d . . . . .
C10 C 0.58434(13) 0.62439(10) 0.31124(4) 0.0220(3) Uani 1 1 d . . . . .
C11 C 0.59708(15) 0.67822(11) 0.28068(5) 0.0288(4) Uani 1 1 d . . . . .
H11 H 0.646403 0.723461 0.281851 0.035 Uiso 1 1 calc R U . . .
C12 C 0.53841(16) 0.66574(12) 0.24904(5) 0.0308(4) Uani 1 1 d . . . . .
H12 H 0.549201 0.701549 0.228887 0.037 Uiso 1 1 calc R U . . .
C13 C 0.46350(15) 0.59999(12) 0.24722(5) 0.0286(4) Uani 1 1 d . . . . .
H13 H 0.422132 0.593437 0.226016 0.034 Uiso 1 1 calc R U . . .
C14 C 0.44809(13) 0.54280(11) 0.27651(4) 0.0220(3) Uani 1 1 d . . . . .
C15 C 0.64438(13) 0.64833(11) 0.34624(5) 0.0247(3) Uani 1 1 d . . . . .
H15 H 0.626182 0.605843 0.365170 0.030 Uiso 1 1 calc R U . . .
C16 C 0.60861(15) 0.73733(12) 0.35997(5) 0.0322(4) Uani 1 1 d . . . . .
H16A H 0.531241 0.737894 0.363244 0.048 Uiso 1 1 calc R U . . .
H16B H 0.628744 0.780241 0.342248 0.048 Uiso 1 1 calc R U . . .
H16C H 0.643462 0.749523 0.382987 0.048 Uiso 1 1 calc R U . . .
C17 C 0.76813(15) 0.64832(13) 0.34108(6) 0.0339(4) Uani 1 1 d . . . . .
H17A H 0.791227 0.592731 0.332620 0.051 Uiso 1 1 calc R U . . .
H17B H 0.802718 0.661030 0.364092 0.051 Uiso 1 1 calc R U . . .
H17C H 0.787842 0.691176 0.323282 0.051 Uiso 1 1 calc R U . . .
C18 C 0.36021(14) 0.47512(11) 0.27333(5) 0.0249(3) Uani 1 1 d . . . . .
H18 H 0.365718 0.436804 0.294642 0.030 Uiso 1 1 calc R U . . .
C19 C 0.37321(16) 0.42044(13) 0.23831(5) 0.0325(4) Uani 1 1 d . . . . .
H19A H 0.445231 0.396840 0.237466 0.049 Uiso 1 1 calc R U . . .
H19B H 0.361412 0.455901 0.217078 0.049 Uiso 1 1 calc R U . . .
H19C H 0.321109 0.374485 0.238556 0.049 Uiso 1 1 calc R U . . .
C20 C 0.24760(15) 0.51725(13) 0.27384(5) 0.0308(4) Uani 1 1 d . . . . .
H20A H 0.240413 0.551961 0.295535 0.046 Uiso 1 1 calc R U . . .
H20B H 0.192707 0.473375 0.273871 0.046 Uiso 1 1 calc R U . . .
H20C H 0.239181 0.552785 0.252450 0.046 Uiso 1 1 calc R U . . .
B1 B 0.35634(14) 0.58472(12) 0.37189(5) 0.0181(3) Uani 1 1 d . . . . .
N2 N 0.34747(11) 0.65429(9) 0.34534(4) 0.0209(3) Uani 1 1 d . . . . .
C21 C 0.32714(15) 0.71408(12) 0.32706(5) 0.0277(4) Uani 1 1 d . . . . .
S1 S 0.30053(6) 0.79418(4) 0.30171(2) 0.05227(18) Uani 1 1 d . . . . .
N3 N 0.17243(11) 0.59047(9) 0.40772(4) 0.0199(3) Uani 1 1 d . . . . .
N4 N 0.30826(11) 0.64434(9) 0.43758(3) 0.0194(3) Uani 1 1 d . . . . .
C22 C 0.28106(12) 0.60175(10) 0.40664(4) 0.0184(3) Uani 1 1 d . . . . .
C23 C 0.13107(13) 0.62661(11) 0.43948(4) 0.0236(3) Uani 1 1 d . . . . .
H23 H 0.058564 0.627681 0.446633 0.028 Uiso 1 1 calc R U . . .
C24 C 0.21600(13) 0.66012(11) 0.45818(4) 0.0230(3) Uani 1 1 d . . . . .
H24 H 0.212950 0.688458 0.480668 0.028 Uiso 1 1 calc R U . . .
C25 C 0.10853(13) 0.55028(11) 0.37781(4) 0.0230(3) Uani 1 1 d . . . . .
H25 H 0.158787 0.518750 0.361846 0.028 Uiso 1 1 calc R U . . .
C26 C 0.02721(15) 0.48646(12) 0.39338(5) 0.0324(4) Uani 1 1 d . . . . .
H26A H -0.005591 0.454761 0.373641 0.049 Uiso 1 1 calc R U . . .
H26B H -0.028004 0.516924 0.406718 0.049 Uiso 1 1 calc R U . . .
H26C H 0.063817 0.447366 0.409626 0.049 Uiso 1 1 calc R U . . .
C27 C 0.05470(14) 0.62039(13) 0.35507(5) 0.0300(4) Uani 1 1 d . . . . .
H27A H 0.109083 0.659299 0.346055 0.045 Uiso 1 1 calc R U . . .
H27B H 0.003889 0.651347 0.370094 0.045 Uiso 1 1 calc R U . . .
H27C H 0.017127 0.594786 0.334698 0.045 Uiso 1 1 calc R U . . .
C28 C 0.41929(13) 0.67660(11) 0.44624(4) 0.0216(3) Uani 1 1 d . . . . .
H28 H 0.471053 0.648020 0.429823 0.026 Uiso 1 1 calc R U . . .
C29 C 0.42360(15) 0.77261(12) 0.43886(5) 0.0279(4) Uani 1 1 d . . . . .
H29A H 0.496048 0.793261 0.443027 0.042 Uiso 1 1 calc R U . . .
H29B H 0.374261 0.801763 0.455065 0.042 Uiso 1 1 calc R U . . .
H29C H 0.403206 0.783577 0.413830 0.042 Uiso 1 1 calc R U . . .
C30 C 0.44987(14) 0.65524(12) 0.48566(4) 0.0275(4) Uani 1 1 d . . . . .
H30A H 0.524561 0.670059 0.489813 0.041 Uiso 1 1 calc R U . . .
H30B H 0.439789 0.594786 0.489899 0.041 Uiso 1 1 calc R U . . .
H30C H 0.404563 0.687365 0.502183 0.041 Uiso 1 1 calc R U . . .
C32_1 C 0.30028(17) 0.95760(14) 0.51896(6) 0.0369(4) Uani 1 1 d . . . . .
F1_1 F 0.21930(12) 0.97503(11) 0.49598(4) 0.0587(4) Uani 1 1 d . . . . .
F2_1 F 0.31637(13) 1.02691(9) 0.53959(4) 0.0558(4) Uani 1 1 d . . . . .
F3_1 F 0.38981(12) 0.94652(10) 0.49881(4) 0.0573(4) Uani 1 1 d . . . . .
S2_1 S 0.27049(3) 0.86277(3) 0.54678(2) 0.02636(12) Uani 1 1 d . . . . .
O1_1 O 0.24584(12) 0.79842(10) 0.51960(4) 0.0412(3) Uani 1 1 d . . . . .
O2_1 O 0.17957(11) 0.88987(10) 0.56858(4) 0.0371(3) Uani 1 1 d . . . . .
O3_1 O 0.37000(11) 0.84892(10) 0.56683(4) 0.0373(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
C1 N1 1.342(2) . ?
C1 B1 1.510(2) . ?
C1 C4 1.532(2) . ?
N1 C9 1.4529(19) . ?
N1 C2 1.5175(19) . ?
C2 C5 1.523(2) . ?
C2 C3 1.527(2) . ?
C2 C6 1.527(2) . ?
C3 C4 1.540(2) . ?
C3 H3A 0.9700 . ?
C3 H3AB 0.9700 . ?
C4 C8 1.534(2) . ?
C4 C7 1.537(2) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.404(2) . ?
C9 C14 1.406(2) . ?
C10 C11 1.400(2) . ?
C10 C15 1.519(2) . ?
C11 C12 1.373(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.378(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.401(2) . ?
C13 H13 0.9300 . ?
C14 C18 1.513(2) . ?
C15 C16 1.535(2) . ?
C15 C17 1.535(2) . ?
C15 H15 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C20 1.533(2) . ?
C18 C19 1.540(2) . ?
C18 H18 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
B1 N2 1.454(2) . ?
B1 C22 1.590(2) . ?
N2 C21 1.170(2) . ?
C21 S1 1.5835(18) . ?
N3 C22 1.349(2) . ?
N3 C23 1.382(2) . ?
N3 C25 1.481(2) . ?
N4 C22 1.348(2) . ?
N4 C24 1.383(2) . ?
N4 C28 1.490(2) . ?
C23 C24 1.352(2) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.519(2) . ?
C25 C27 1.520(2) . ?
C25 H25 0.9800 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.517(2) . ?
C28 C30 1.520(2) . ?
C28 H28 0.9800 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C32_1 F2_1 1.328(2) . ?
C32_1 F1_1 1.329(2) . ?
C32_1 F3_1 1.335(3) . ?
C32_1 S2_1 1.825(2) . ?
S2_1 O2_1 1.4351(13) . ?
S2_1 O1_1 1.4386(14) . ?
S2_1 O3_1 1.4421(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 B1 125.27(14) . . ?
N1 C1 C4 109.26(13) . . ?
B1 C1 C4 125.47(13) . . ?
C1 N1 C9 124.46(13) . . ?
C1 N1 C2 114.08(12) . . ?
C9 N1 C2 121.45(12) . . ?
N1 C2 C5 111.59(13) . . ?
N1 C2 C3 100.14(12) . . ?
C5 C2 C3 112.52(14) . . ?
N1 C2 C6 110.42(13) . . ?
C5 C2 C6 109.01(14) . . ?
C3 C2 C6 112.96(14) . . ?
C2 C3 C4 107.27(13) . . ?
C2 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
C2 C3 H3AB 110.3 . . ?
C4 C3 H3AB 110.3 . . ?
H3A C3 H3AB 108.5 . . ?
C1 C4 C8 111.30(13) . . ?
C1 C4 C7 112.48(13) . . ?
C8 C4 C7 108.76(14) . . ?
C1 C4 C3 102.36(12) . . ?
C8 C4 C3 112.51(14) . . ?
C7 C4 C3 109.36(14) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 121.57(14) . . ?
C10 C9 N1 120.14(14) . . ?
C14 C9 N1 118.27(14) . . ?
C11 C10 C9 117.84(16) . . ?
C11 C10 C15 117.70(15) . . ?
C9 C10 C15 124.32(14) . . ?
C12 C11 C10 121.50(17) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C12 C13 119.81(16) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 121.64(16) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C13 C14 C9 117.51(16) . . ?
C13 C14 C18 118.66(15) . . ?
C9 C14 C18 123.71(14) . . ?
C10 C15 C16 110.72(15) . . ?
C10 C15 C17 112.35(14) . . ?
C16 C15 C17 108.95(15) . . ?
C10 C15 H15 108.2 . . ?
C16 C15 H15 108.2 . . ?
C17 C15 H15 108.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 C20 110.41(14) . . ?
C14 C18 C19 111.87(14) . . ?
C20 C18 C19 109.86(14) . . ?
C14 C18 H18 108.2 . . ?
C20 C18 H18 108.2 . . ?
C19 C18 H18 108.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 B1 C1 123.58(14) . . ?
N2 B1 C22 111.14(13) . . ?
C1 B1 C22 125.27(14) . . ?
C21 N2 B1 169.90(16) . . ?
N2 C21 S1 179.00(16) . . ?
C22 N3 C23 109.67(13) . . ?
C22 N3 C25 124.05(13) . . ?
C23 N3 C25 126.16(13) . . ?
C22 N4 C24 109.61(13) . . ?
C22 N4 C28 124.74(13) . . ?
C24 N4 C28 125.41(13) . . ?
N4 C22 N3 106.60(13) . . ?
N4 C22 B1 126.93(14) . . ?
N3 C22 B1 125.41(13) . . ?
C24 C23 N3 107.00(14) . . ?
C24 C23 H23 126.5 . . ?
N3 C23 H23 126.5 . . ?
C23 C24 N4 107.12(14) . . ?
C23 C24 H24 126.4 . . ?
N4 C24 H24 126.4 . . ?
N3 C25 C26 110.59(14) . . ?
N3 C25 C27 109.22(14) . . ?
C26 C25 C27 112.56(14) . . ?
N3 C25 H25 108.1 . . ?
C26 C25 H25 108.1 . . ?
C27 C25 H25 108.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 C29 109.00(13) . . ?
N4 C28 C30 110.70(13) . . ?
C29 C28 C30 111.92(14) . . ?
N4 C28 H28 108.4 . . ?
C29 C28 H28 108.4 . . ?
C30 C28 H28 108.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
F2_1 C32_1 F1_1 107.59(18) . . ?
F2_1 C32_1 F3_1 106.96(18) . . ?
F1_1 C32_1 F3_1 107.47(17) . . ?
F2_1 C32_1 S2_1 111.82(14) . . ?
F1_1 C32_1 S2_1 111.27(15) . . ?
F3_1 C32_1 S2_1 111.50(15) . . ?
O2_1 S2_1 O1_1 114.79(9) . . ?
O2_1 S2_1 O3_1 115.27(8) . . ?
O1_1 S2_1 O3_1 115.03(9) . . ?
O2_1 S2_1 C32_1 103.09(9) . . ?
O1_1 S2_1 C32_1 102.86(9) . . ?
O3_1 S2_1 C32_1 103.32(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
B1 C1 N1 C9 -4.0(2) . . . . ?
C4 C1 N1 C9 176.51(13) . . . . ?
B1 C1 N1 C2 174.98(14) . . . . ?
C4 C1 N1 C2 -4.50(17) . . . . ?
C1 N1 C2 C5 138.39(15) . . . . ?
C9 N1 C2 C5 -42.58(19) . . . . ?
C1 N1 C2 C3 19.10(16) . . . . ?
C9 N1 C2 C3 -161.87(13) . . . . ?
C1 N1 C2 C6 -100.21(15) . . . . ?
C9 N1 C2 C6 78.82(17) . . . . ?
N1 C2 C3 C4 -25.68(15) . . . . ?
C5 C2 C3 C4 -144.29(14) . . . . ?
C6 C2 C3 C4 91.76(16) . . . . ?
N1 C1 C4 C8 108.24(15) . . . . ?
B1 C1 C4 C8 -71.24(19) . . . . ?
N1 C1 C4 C7 -129.42(14) . . . . ?
B1 C1 C4 C7 51.1(2) . . . . ?
N1 C1 C4 C3 -12.17(16) . . . . ?
B1 C1 C4 C3 168.35(14) . . . . ?
C2 C3 C4 C1 23.98(16) . . . . ?
C2 C3 C4 C8 -95.58(16) . . . . ?
C2 C3 C4 C7 143.44(14) . . . . ?
C1 N1 C9 C10 87.70(19) . . . . ?
C2 N1 C9 C10 -91.23(18) . . . . ?
C1 N1 C9 C14 -90.64(18) . . . . ?
C2 N1 C9 C14 90.44(17) . . . . ?
C14 C9 C10 C11 -3.8(2) . . . . ?
N1 C9 C10 C11 177.87(14) . . . . ?
C14 C9 C10 C15 171.80(15) . . . . ?
N1 C9 C10 C15 -6.5(2) . . . . ?
C9 C10 C11 C12 1.8(3) . . . . ?
C15 C10 C11 C12 -174.13(16) . . . . ?
C10 C11 C12 C13 1.3(3) . . . . ?
C11 C12 C13 C14 -2.5(3) . . . . ?
C12 C13 C14 C9 0.5(2) . . . . ?
C12 C13 C14 C18 176.79(16) . . . . ?
C10 C9 C14 C13 2.7(2) . . . . ?
N1 C9 C14 C13 -178.96(14) . . . . ?
C10 C9 C14 C18 -173.36(15) . . . . ?
N1 C9 C14 C18 4.9(2) . . . . ?
C11 C10 C15 C16 60.1(2) . . . . ?
C9 C10 C15 C16 -115.52(17) . . . . ?
C11 C10 C15 C17 -61.9(2) . . . . ?
C9 C10 C15 C17 122.41(18) . . . . ?
C13 C14 C18 C20 -68.11(19) . . . . ?
C9 C14 C18 C20 107.93(18) . . . . ?
C13 C14 C18 C19 54.6(2) . . . . ?
C9 C14 C18 C19 -129.39(17) . . . . ?
N1 C1 B1 N2 6.6(2) . . . . ?
C4 C1 B1 N2 -173.99(14) . . . . ?
N1 C1 B1 C22 -174.02(14) . . . . ?
C4 C1 B1 C22 5.4(2) . . . . ?
C1 B1 N2 C21 167.3(9) . . . . ?
C22 B1 N2 C21 -12.2(10) . . . . ?
C24 N4 C22 N3 -0.16(18) . . . . ?
C28 N4 C22 N3 -174.75(14) . . . . ?
C24 N4 C22 B1 168.49(15) . . . . ?
C28 N4 C22 B1 -6.1(2) . . . . ?
C23 N3 C22 N4 0.29(18) . . . . ?
C25 N3 C22 N4 176.61(14) . . . . ?
C23 N3 C22 B1 -168.58(15) . . . . ?
C25 N3 C22 B1 7.7(2) . . . . ?
N2 B1 C22 N4 -89.35(19) . . . . ?
C1 B1 C22 N4 91.2(2) . . . . ?
N2 B1 C22 N3 77.3(2) . . . . ?
C1 B1 C22 N3 -102.16(19) . . . . ?
C22 N3 C23 C24 -0.31(19) . . . . ?
C25 N3 C23 C24 -176.53(15) . . . . ?
N3 C23 C24 N4 0.20(19) . . . . ?
C22 N4 C24 C23 -0.03(19) . . . . ?
C28 N4 C24 C23 174.51(15) . . . . ?
C22 N3 C25 C26 135.39(16) . . . . ?
C23 N3 C25 C26 -48.9(2) . . . . ?
C22 N3 C25 C27 -100.21(18) . . . . ?
C23 N3 C25 C27 75.5(2) . . . . ?
C22 N4 C28 C29 101.76(17) . . . . ?
C24 N4 C28 C29 -71.98(19) . . . . ?
C22 N4 C28 C30 -134.72(16) . . . . ?
C24 N4 C28 C30 51.5(2) . . . . ?
F2_1 C32_1 S2_1 O2_1 55.04(16) . . . . ?
F1_1 C32_1 S2_1 O2_1 -65.30(16) . . . . ?
F3_1 C32_1 S2_1 O2_1 174.73(14) . . . . ?
F2_1 C32_1 S2_1 O1_1 174.68(15) . . . . ?
F1_1 C32_1 S2_1 O1_1 54.34(17) . . . . ?
F3_1 C32_1 S2_1 O1_1 -65.62(16) . . . . ?
F2_1 C32_1 S2_1 O3_1 -65.32(17) . . . . ?
F1_1 C32_1 S2_1 O3_1 174.34(15) . . . . ?
F3_1 C32_1 S2_1 O3_1 54.38(16) . . . . ?

_refine_diff_density_max         0.356
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.051



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
