# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1060033'
_audit_update_record             
;
2015-07-06 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C56 H82 B N4), 2(C2 F6 N O4 S2), 3(C6 H5 F)'
_chemical_formula_sum            'C67 H89.50 B F7.50 N5 O4 S2'
_chemical_formula_weight         1246.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0096 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0826 0.0763 '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                   13.061(3)
_cell_length_b                   15.613(4)
_cell_length_c                   16.727(4)
_cell_angle_alpha                96.881(7)
_cell_angle_beta                 101.456(6)
_cell_angle_gamma                98.294(7)
_cell_volume                     3269.0(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8186
_cell_measurement_theta_min      2.239
_cell_measurement_theta_max      16.135

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_F_000             1326
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.079
_exptl_absorpt_coefficient_mu    0.088
_shelx_estimated_absorpt_T_min   0.984
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6315
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   'INCOATEC Microsource'
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            160487
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.737
_diffrn_reflns_theta_max         19.609
_diffrn_reflns_theta_full        19.609
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             11676
_reflns_number_gt                9048
_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 v2012.2'
_computing_cell_refinement       'SAINT V8.34A'
_computing_data_reduction        'SAINT V8.34A'
_computing_structure_solution    
'SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_refine_special_details          
'57 SAME/SADI, 3 FLAT and 45 RIGU restrains on the 1.5 molecules of C6H5F; 6 ISOR restraints on C3'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0853P)²+2.8427P] 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         11676
_refine_ls_number_parameters     806
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1601
_refine_ls_wR_factor_gt          0.1455
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.064
_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
B1 B 0.7833(2) 0.32406(17) 0.26044(16) 0.0156(5) Uani 1 1 d D . . . .
H1 H 0.8346(18) 0.3773(15) 0.3082(14) 0.019 Uiso 1 1 d D U . . .
H2 H 0.7318(18) 0.3553(16) 0.2145(14) 0.019 Uiso 1 1 d D U . . .
C2 C 0.71035(18) 0.25374(15) 0.30533(14) 0.0159(5) Uani 1 1 d . . . . .
H2A H 0.6342 0.2505 0.2808 0.019 Uiso 1 1 calc R U . . .
H2B H 0.7280 0.1945 0.2940 0.019 Uiso 1 1 calc R U . . .
C3 C 0.72934(17) 0.28029(14) 0.39408(14) 0.0135(5) Uani 1 1 d . U . . .
N4 N 0.66328(15) 0.31774(12) 0.43281(12) 0.0161(4) Uani 1 1 d . . . . .
C5 C 0.70621(19) 0.33808(16) 0.52244(14) 0.0203(5) Uani 1 1 d . . . . .
H5A H 0.6554 0.3118 0.5532 0.024 Uiso 1 1 calc R U . . .
H5B H 0.7237 0.4021 0.5410 0.024 Uiso 1 1 calc R U . . .
C6 C 0.80652(19) 0.29628(16) 0.53376(14) 0.0201(5) Uani 1 1 d . . . . .
H6A H 0.8691 0.3386 0.5662 0.024 Uiso 1 1 calc R U . . .
H6B H 0.7976 0.2440 0.5615 0.024 Uiso 1 1 calc R U . . .
N7 N 0.81675(15) 0.27206(12) 0.44773(11) 0.0146(4) Uani 1 1 d . . . . .
C8 C 0.55693(18) 0.32799(15) 0.39587(14) 0.0168(5) Uani 1 1 d . . . . .
C9 C 0.53892(19) 0.40880(16) 0.37187(14) 0.0187(5) Uani 1 1 d . . . . .
C10 C 0.4353(2) 0.41586(17) 0.33635(15) 0.0237(6) Uani 1 1 d . . . . .
H10 H 0.4208 0.4696 0.3193 0.028 Uiso 1 1 calc R U . . .
C11 C 0.35262(19) 0.34580(18) 0.32530(15) 0.0256(6) Uani 1 1 d . . . . .
H11 H 0.2825 0.3517 0.3006 0.031 Uiso 1 1 calc R U . . .
C12 C 0.3725(2) 0.26742(18) 0.35030(16) 0.0255(6) Uani 1 1 d . . . . .
H12 H 0.3153 0.2199 0.3423 0.031 Uiso 1 1 calc R U . . .
C13 C 0.47429(19) 0.25644(16) 0.38699(15) 0.0212(5) Uani 1 1 d . . . . .
C14 C 0.62724(19) 0.48800(16) 0.38540(15) 0.0208(5) Uani 1 1 d . . . . .
H14 H 0.6959 0.4692 0.4077 0.025 Uiso 1 1 calc R U . . .
C15 C 0.6356(2) 0.52314(17) 0.30499(16) 0.0259(6) Uani 1 1 d . . . . .
H15A H 0.6953 0.5719 0.3159 0.039 Uiso 1 1 calc R U . . .
H15B H 0.5698 0.5437 0.2828 0.039 Uiso 1 1 calc R U . . .
H15C H 0.6470 0.4764 0.2648 0.039 Uiso 1 1 calc R U . . .
C16 C 0.6100(2) 0.56014(18) 0.44963(17) 0.0290(6) Uani 1 1 d . . . . .
H16A H 0.6655 0.6115 0.4564 0.043 Uiso 1 1 calc R U . . .
H16B H 0.6129 0.5386 0.5026 0.043 Uiso 1 1 calc R U . . .
H16C H 0.5404 0.5764 0.4310 0.043 Uiso 1 1 calc R U . . .
C17 C 0.4928(2) 0.16955(17) 0.41513(16) 0.0255(6) Uani 1 1 d . . . . .
H17 H 0.5682 0.1775 0.4460 0.031 Uiso 1 1 calc R U . . .
C18 C 0.4770(2) 0.09692(18) 0.34230(19) 0.0370(7) Uani 1 1 d . . . . .
H18A H 0.4863 0.0416 0.3627 0.056 Uiso 1 1 calc R U . . .
H18B H 0.5293 0.1114 0.3092 0.056 Uiso 1 1 calc R U . . .
H18C H 0.4054 0.0910 0.3082 0.056 Uiso 1 1 calc R U . . .
C19 C 0.4219(2) 0.1444(2) 0.47451(18) 0.0354(7) Uani 1 1 d . . . . .
H19A H 0.4382 0.0903 0.4944 0.053 Uiso 1 1 calc R U . . .
H19B H 0.3473 0.1353 0.4456 0.053 Uiso 1 1 calc R U . . .
H19C H 0.4351 0.1916 0.5215 0.053 Uiso 1 1 calc R U . . .
C20 C 0.90091(18) 0.22981(14) 0.42643(14) 0.0146(5) Uani 1 1 d . . . . .
C21 C 0.99797(18) 0.28201(15) 0.42490(14) 0.0164(5) Uani 1 1 d . . . . .
C22 C 1.07662(19) 0.23986(16) 0.40177(15) 0.0207(5) Uani 1 1 d . . . . .
H22 H 1.1425 0.2737 0.4000 0.025 Uiso 1 1 calc R U . . .
C23 C 1.0612(2) 0.14955(16) 0.38128(16) 0.0233(6) Uani 1 1 d . . . . .
H23 H 1.1157 0.1223 0.3646 0.028 Uiso 1 1 calc R U . . .
C24 C 0.9664(2) 0.09912(15) 0.38512(15) 0.0219(5) Uani 1 1 d . . . . .
H24 H 0.9570 0.0372 0.3720 0.026 Uiso 1 1 calc R U . . .
C25 C 0.88446(19) 0.13794(15) 0.40799(14) 0.0175(5) Uani 1 1 d . . . . .
C26 C 1.02062(19) 0.38050(15) 0.45324(15) 0.0190(5) Uani 1 1 d . . . . .
H26 H 0.9514 0.4008 0.4528 0.023 Uiso 1 1 calc R U . . .
C27 C 1.0774(2) 0.43105(16) 0.39647(17) 0.0256(6) Uani 1 1 d . . . . .
H27A H 1.0825 0.4941 0.4133 0.038 Uiso 1 1 calc R U . . .
H27B H 1.0372 0.4143 0.3393 0.038 Uiso 1 1 calc R U . . .
H27C H 1.1488 0.4169 0.4007 0.038 Uiso 1 1 calc R U . . .
C28 C 1.0862(2) 0.40020(16) 0.54197(16) 0.0246(6) Uani 1 1 d . . . . .
H28A H 1.0979 0.4633 0.5614 0.037 Uiso 1 1 calc R U . . .
H28B H 1.1548 0.3811 0.5438 0.037 Uiso 1 1 calc R U . . .
H28C H 1.0481 0.3688 0.5776 0.037 Uiso 1 1 calc R U . . .
C29 C 0.7846(2) 0.08006(16) 0.41661(16) 0.0231(6) Uani 1 1 d . . . . .
H29 H 0.7316 0.1184 0.4255 0.028 Uiso 1 1 calc R U . . .
C30 C 0.7353(2) 0.01241(17) 0.33977(17) 0.0301(6) Uani 1 1 d . . . . .
H30A H 0.6693 -0.0211 0.3472 0.045 Uiso 1 1 calc R U . . .
H30B H 0.7850 -0.0275 0.3312 0.045 Uiso 1 1 calc R U . . .
H30C H 0.7201 0.0424 0.2916 0.045 Uiso 1 1 calc R U . . .
C31 C 0.8103(3) 0.03463(19) 0.49317(18) 0.0382(7) Uani 1 1 d . . . . .
H31A H 0.7451 0.0000 0.5008 0.057 Uiso 1 1 calc R U . . .
H31B H 0.8405 0.0790 0.5420 0.057 Uiso 1 1 calc R U . . .
H31C H 0.8616 -0.0040 0.4854 0.057 Uiso 1 1 calc R U . . .
C32 C 0.85810(18) 0.26854(15) 0.20854(14) 0.0161(5) Uani 1 1 d . . . . .
H32A H 0.9340 0.2942 0.2298 0.019 Uiso 1 1 calc R U . . .
H32B H 0.8480 0.2066 0.2176 0.019 Uiso 1 1 calc R U . . .
C33 C 0.82856(17) 0.27252(14) 0.12047(14) 0.0132(5) Uani 1 1 d . . . . .
N34 N 0.74142(15) 0.22752(12) 0.06889(11) 0.0141(4) Uani 1 1 d . . . . .
C35 C 0.73270(19) 0.24998(16) -0.01549(14) 0.0201(5) Uani 1 1 d . . . . .
H35A H 0.6687 0.2763 -0.0325 0.024 Uiso 1 1 calc R U . . .
H35B H 0.7303 0.1977 -0.0561 0.024 Uiso 1 1 calc R U . . .
C36 C 0.83422(18) 0.31656(15) -0.00688(14) 0.0166(5) Uani 1 1 d . . . . .
H36A H 0.8807 0.2942 -0.0416 0.020 Uiso 1 1 calc R U . . .
H36B H 0.8176 0.3730 -0.0225 0.020 Uiso 1 1 calc R U . . .
N37 N 0.88388(14) 0.32616(12) 0.08118(11) 0.0134(4) Uani 1 1 d . . . . .
C38 C 0.66812(18) 0.15811(14) 0.08829(14) 0.0159(5) Uani 1 1 d . . . . .
C39 C 0.56745(18) 0.17356(15) 0.09609(14) 0.0175(5) Uani 1 1 d . . . . .
C40 C 0.4992(2) 0.10441(17) 0.11495(16) 0.0239(6) Uani 1 1 d . . . . .
H40 H 0.4304 0.1126 0.1212 0.029 Uiso 1 1 calc R U . . .
C41 C 0.5307(2) 0.02442(17) 0.12455(16) 0.0271(6) Uani 1 1 d . . . . .
H41 H 0.4838 -0.0211 0.1382 0.033 Uiso 1 1 calc R U . . .
C42 C 0.6295(2) 0.01037(16) 0.11443(16) 0.0243(6) Uani 1 1 d . . . . .
H42 H 0.6493 -0.0452 0.1202 0.029 Uiso 1 1 calc R U . . .
C43 C 0.70099(19) 0.07687(15) 0.09577(14) 0.0195(5) Uani 1 1 d . . . . .
C44 C 0.52766(18) 0.25823(16) 0.08014(15) 0.0197(5) Uani 1 1 d . . . . .
H44 H 0.5905 0.3034 0.0806 0.024 Uiso 1 1 calc R U . . .
C45 C 0.4544(2) 0.24472(18) -0.00570(16) 0.0283(6) Uani 1 1 d . . . . .
H45A H 0.4361 0.3010 -0.0184 0.042 Uiso 1 1 calc R U . . .
H45B H 0.3895 0.2039 -0.0067 0.042 Uiso 1 1 calc R U . . .
H45C H 0.4906 0.2206 -0.0469 0.042 Uiso 1 1 calc R U . . .
C46 C 0.4705(2) 0.29411(18) 0.14487(17) 0.0288(6) Uani 1 1 d . . . . .
H46A H 0.4490 0.3493 0.1317 0.043 Uiso 1 1 calc R U . . .
H46B H 0.5183 0.3045 0.1995 0.043 Uiso 1 1 calc R U . . .
H46C H 0.4075 0.2515 0.1449 0.043 Uiso 1 1 calc R U . . .
C47 C 0.8069(2) 0.05794(16) 0.07948(16) 0.0228(5) Uani 1 1 d . . . . .
H47 H 0.8546 0.1156 0.0855 0.027 Uiso 1 1 calc R U . . .
C48 C 0.7924(3) 0.0130(2) -0.00927(18) 0.0385(7) Uani 1 1 d . . . . .
H48A H 0.8619 0.0073 -0.0210 0.058 Uiso 1 1 calc R U . . .
H48B H 0.7569 0.0482 -0.0473 0.058 Uiso 1 1 calc R U . . .
H48C H 0.7490 -0.0452 -0.0165 0.058 Uiso 1 1 calc R U . . .
C49 C 0.8623(2) 0.0044(2) 0.13991(18) 0.0357(7) Uani 1 1 d . . . . .
H49A H 0.9320 -0.0013 0.1286 0.053 Uiso 1 1 calc R U . . .
H49B H 0.8193 -0.0539 0.1334 0.053 Uiso 1 1 calc R U . . .
H49C H 0.8712 0.0341 0.1965 0.053 Uiso 1 1 calc R U . . .
C50 C 0.98892(18) 0.37564(14) 0.11373(13) 0.0138(5) Uani 1 1 d . . . . .
C51 C 1.07626(18) 0.33326(15) 0.11182(14) 0.0168(5) Uani 1 1 d . . . . .
C52 C 1.17751(19) 0.38400(16) 0.13895(15) 0.0205(5) Uani 1 1 d . . . . .
H52 H 1.2383 0.3573 0.1382 0.025 Uiso 1 1 calc R U . . .
C53 C 1.1900(2) 0.47268(16) 0.16683(16) 0.0227(5) Uani 1 1 d . . . . .
H53 H 1.2592 0.5063 0.1852 0.027 Uiso 1 1 calc R U . . .
C54 C 1.10214(19) 0.51309(15) 0.16825(15) 0.0210(5) Uani 1 1 d . . . . .
H54 H 1.1122 0.5741 0.1876 0.025 Uiso 1 1 calc R U . . .
C55 C 0.99927(18) 0.46538(15) 0.14168(14) 0.0162(5) Uani 1 1 d . . . . .
C56 C 1.0659(2) 0.23560(15) 0.08183(15) 0.0203(5) Uani 1 1 d . . . . .
H56 H 0.9887 0.2113 0.0613 0.024 Uiso 1 1 calc R U . . .
C57 C 1.1086(2) 0.18763(18) 0.15341(17) 0.0320(6) Uani 1 1 d . . . . .
H57A H 1.0955 0.1245 0.1339 0.048 Uiso 1 1 calc R U . . .
H57B H 1.0723 0.1996 0.1985 0.048 Uiso 1 1 calc R U . . .
H57C H 1.1850 0.2084 0.1733 0.048 Uiso 1 1 calc R U . . .
C58 C 1.1206(2) 0.21788(17) 0.01028(16) 0.0268(6) Uani 1 1 d . . . . .
H58A H 1.1103 0.1546 -0.0080 0.040 Uiso 1 1 calc R U . . .
H58B H 1.1966 0.2412 0.0285 0.040 Uiso 1 1 calc R U . . .
H58C H 1.0898 0.2464 -0.0356 0.040 Uiso 1 1 calc R U . . .
C59 C 0.90481(19) 0.51157(15) 0.14232(15) 0.0193(5) Uani 1 1 d . . . . .
H59 H 0.8390 0.4663 0.1241 0.023 Uiso 1 1 calc R U . . .
C60 C 0.9009(2) 0.57715(17) 0.08086(17) 0.0279(6) Uani 1 1 d . . . . .
H60A H 0.8370 0.6036 0.0793 0.042 Uiso 1 1 calc R U . . .
H60B H 0.8994 0.5467 0.0258 0.042 Uiso 1 1 calc R U . . .
H60C H 0.9639 0.6231 0.0982 0.042 Uiso 1 1 calc R U . . .
C61 C 0.9058(2) 0.55721(17) 0.22869(16) 0.0264(6) Uani 1 1 d . . . . .
H61A H 0.8442 0.5868 0.2264 0.040 Uiso 1 1 calc R U . . .
H61B H 0.9710 0.6004 0.2489 0.040 Uiso 1 1 calc R U . . .
H61C H 0.9027 0.5137 0.2662 0.040 Uiso 1 1 calc R U . . .
C62 C 0.2262(2) 0.22748(19) 0.78424(19) 0.0367(7) Uani 1 1 d D U . . .
F62 F 0.2466(2) 0.23962(19) 0.86541(14) 0.0796(7) Uani 1 1 d D U . . .
C63 C 0.1236(2) 0.2113(2) 0.7444(2) 0.0454(8) Uani 1 1 d D U . . .
H63 H 0.0684 0.2085 0.7739 0.054 Uiso 1 1 calc R U . . .
C64 C 0.1014(3) 0.1992(2) 0.6604(2) 0.0556(9) Uani 1 1 d D U . . .
H64 H 0.0297 0.1877 0.6306 0.067 Uiso 1 1 calc R U . . .
C65 C 0.1829(3) 0.2033(2) 0.6176(2) 0.0597(10) Uani 1 1 d D U . . .
H65 H 0.1671 0.1954 0.5590 0.072 Uiso 1 1 calc R U . . .
C66 C 0.2876(3) 0.2192(2) 0.6618(2) 0.0535(9) Uani 1 1 d D U . . .
H66 H 0.3438 0.2214 0.6334 0.064 Uiso 1 1 calc R U . . .
C67 C 0.3097(2) 0.2318(2) 0.7462(2) 0.0432(8) Uani 1 1 d D U . . .
H67 H 0.3807 0.2430 0.7773 0.052 Uiso 1 1 calc R U . . .
C69 C 0.5912(3) 0.4803(2) -0.0141(2) 0.0514(9) Uani 1 1 d D U . . .
H69 H 0.6563 0.4662 -0.0241 0.062 Uiso 0.5 1 calc R U P A -1
F69 F 0.6706(3) 0.4561(3) -0.0278(2) 0.0534(10) Uani 0.5 1 d D U P B -2
C70 C 0.5854(3) 0.5067(2) 0.0657(2) 0.0506(9) Uani 1 1 d D U . . .
H70 H 0.6450 0.5109 0.1099 0.061 Uiso 1 1 calc R U . . .
C71 C 0.4916(3) 0.5267(2) 0.0798(2) 0.0512(9) Uani 1 1 d D U . . .
H71 H 0.4842 0.5450 0.1343 0.061 Uiso 1 1 calc R U . . .
N73 N 0.28625(19) 0.83818(15) 0.21847(14) 0.0299(5) Uani 1 1 d . . . . .
S74 S 0.16859(5) 0.83549(4) 0.22892(4) 0.02754(17) Uani 1 1 d . . . . .
O75 O 0.14026(15) 0.79386(13) 0.29523(12) 0.0332(5) Uani 1 1 d . . . . .
O76 O 0.09996(17) 0.81366(15) 0.14949(13) 0.0475(6) Uani 1 1 d . . . . .
C77 C 0.1629(2) 0.95148(18) 0.25863(17) 0.0295(6) Uani 1 1 d . . . . .
F78 F 0.23097(13) 0.98525(10) 0.32801(10) 0.0351(4) Uani 1 1 d . . . . .
F79 F 0.06627(14) 0.95998(12) 0.26741(12) 0.0475(5) Uani 1 1 d . . . . .
F80 F 0.18655(19) 0.99875(13) 0.20086(12) 0.0583(6) Uani 1 1 d . . . . .
S81 S 0.38038(5) 0.82486(4) 0.28864(4) 0.02477(17) Uani 1 1 d . . . . .
O82 O 0.36576(15) 0.83921(12) 0.37102(11) 0.0315(4) Uani 1 1 d . . . . .
O83 O 0.47834(16) 0.86158(13) 0.27114(16) 0.0452(6) Uani 1 1 d . . . . .
C84 C 0.3770(2) 0.70708(17) 0.26692(17) 0.0261(6) Uani 1 1 d . . . . .
F85 F 0.28730(13) 0.66199(10) 0.28001(10) 0.0371(4) Uani 1 1 d . . . . .
F86 F 0.45665(13) 0.68311(10) 0.31908(11) 0.0397(4) Uani 1 1 d . . . . .
F87 F 0.38556(17) 0.68043(12) 0.19155(11) 0.0493(5) 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
B1 C2 1.690(3) . ?
B1 C32 1.692(3) . ?
B1 H1 1.12(2) . ?
B1 H2 1.12(2) . ?
C2 C3 1.454(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.335(3) . ?
C3 N7 1.337(3) . ?
N4 C8 1.444(3) . ?
N4 C5 1.471(3) . ?
C5 C6 1.535(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N7 1.481(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
N7 C20 1.442(3) . ?
C8 C9 1.406(3) . ?
C8 C13 1.408(3) . ?
C9 C10 1.392(3) . ?
C9 C14 1.526(3) . ?
C10 C11 1.388(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(4) . ?
C12 H12 0.9500 . ?
C13 C17 1.524(4) . ?
C14 C15 1.530(3) . ?
C14 C16 1.534(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.521(4) . ?
C17 C19 1.533(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C25 1.406(3) . ?
C20 C21 1.411(3) . ?
C21 C22 1.389(3) . ?
C21 C26 1.522(3) . ?
C22 C23 1.386(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.398(4) . ?
C24 H24 0.9500 . ?
C25 C29 1.518(3) . ?
C26 C28 1.530(4) . ?
C26 C27 1.538(3) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.527(4) . ?
C29 C31 1.540(4) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.458(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 N34 1.329(3) . ?
C33 N37 1.342(3) . ?
N34 C38 1.451(3) . ?
N34 C35 1.481(3) . ?
C35 C36 1.533(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 N37 1.467(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N37 C50 1.439(3) . ?
C38 C39 1.399(3) . ?
C38 C43 1.408(3) . ?
C39 C40 1.405(3) . ?
C39 C44 1.522(3) . ?
C40 C41 1.387(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.379(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.401(3) . ?
C42 H42 0.9500 . ?
C43 C47 1.524(4) . ?
C44 C46 1.530(4) . ?
C44 C45 1.532(3) . ?
C44 H44 1.0000 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C49 1.527(4) . ?
C47 C48 1.527(4) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C55 1.401(3) . ?
C50 C51 1.403(3) . ?
C51 C52 1.398(3) . ?
C51 C56 1.525(3) . ?
C52 C53 1.382(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.389(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.397(3) . ?
C54 H54 0.9500 . ?
C55 C59 1.517(3) . ?
C56 C58 1.528(4) . ?
C56 C57 1.541(4) . ?
C56 H56 1.0000 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C61 1.529(3) . ?
C59 C60 1.534(3) . ?
C59 H59 1.0000 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 F62 1.315(4) . ?
C62 C63 1.345(4) . ?
C62 C67 1.365(4) . ?
C63 C64 1.362(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.393(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.390(5) . ?
C65 H65 0.9500 . ?
C66 C67 1.367(5) . ?
C66 H66 0.9500 . ?
C67 H67 0.9500 . ?
C69 F69 1.208(5) . ?
C69 C71 1.362(5) 2_665 ?
C69 C70 1.368(5) . ?
C69 H69 0.9500 . ?
C70 C71 1.365(5) . ?
C70 H70 0.9500 . ?
C71 C69 1.362(5) 2_665 ?
C71 H71 0.9500 . ?
N73 S74 1.576(2) . ?
N73 S81 1.578(2) . ?
S74 O76 1.420(2) . ?
S74 O75 1.434(2) . ?
S74 C77 1.836(3) . ?
C77 F78 1.313(3) . ?
C77 F79 1.322(3) . ?
C77 F80 1.341(3) . ?
S81 O82 1.424(2) . ?
S81 O83 1.424(2) . ?
S81 C84 1.824(3) . ?
C84 F87 1.311(3) . ?
C84 F86 1.346(3) . ?
C84 F85 1.348(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 B1 C32 109.22(18) . . ?
C2 B1 H1 110.1(13) . . ?
C32 B1 H1 110.5(13) . . ?
C2 B1 H2 111.7(13) . . ?
C32 B1 H2 107.2(13) . . ?
H1 B1 H2 108.0(18) . . ?
C3 C2 B1 112.02(18) . . ?
C3 C2 H2A 109.2 . . ?
B1 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
B1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N4 C3 N7 110.9(2) . . ?
N4 C3 C2 124.8(2) . . ?
N7 C3 C2 124.3(2) . . ?
C3 N4 C8 125.99(19) . . ?
C3 N4 C5 111.52(19) . . ?
C8 N4 C5 122.04(18) . . ?
N4 C5 C6 102.87(18) . . ?
N4 C5 H5A 111.2 . . ?
C6 C5 H5A 111.2 . . ?
N4 C5 H5B 111.2 . . ?
C6 C5 H5B 111.2 . . ?
H5A C5 H5B 109.1 . . ?
N7 C6 C5 102.68(18) . . ?
N7 C6 H6A 111.2 . . ?
C5 C6 H6A 111.2 . . ?
N7 C6 H6B 111.2 . . ?
C5 C6 H6B 111.2 . . ?
H6A C6 H6B 109.1 . . ?
C3 N7 C20 124.77(19) . . ?
C3 N7 C6 110.84(19) . . ?
C20 N7 C6 123.41(18) . . ?
C9 C8 C13 122.4(2) . . ?
C9 C8 N4 119.4(2) . . ?
C13 C8 N4 118.2(2) . . ?
C10 C9 C8 117.6(2) . . ?
C10 C9 C14 119.8(2) . . ?
C8 C9 C14 122.6(2) . . ?
C11 C10 C9 121.2(2) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C12 C11 C10 120.0(2) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 121.6(2) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C8 117.2(2) . . ?
C12 C13 C17 120.1(2) . . ?
C8 C13 C17 122.7(2) . . ?
C9 C14 C15 112.1(2) . . ?
C9 C14 C16 110.1(2) . . ?
C15 C14 C16 110.6(2) . . ?
C9 C14 H14 108.0 . . ?
C15 C14 H14 108.0 . . ?
C16 C14 H14 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C13 111.7(2) . . ?
C18 C17 C19 111.2(2) . . ?
C13 C17 C19 110.8(2) . . ?
C18 C17 H17 107.6 . . ?
C13 C17 H17 107.6 . . ?
C19 C17 H17 107.6 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C25 C20 C21 121.7(2) . . ?
C25 C20 N7 119.34(19) . . ?
C21 C20 N7 118.9(2) . . ?
C22 C21 C20 117.8(2) . . ?
C22 C21 C26 120.0(2) . . ?
C20 C21 C26 122.1(2) . . ?
C23 C22 C21 121.5(2) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C24 C23 C22 120.0(2) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 121.0(2) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C20 117.9(2) . . ?
C24 C25 C29 119.3(2) . . ?
C20 C25 C29 122.7(2) . . ?
C21 C26 C28 109.26(19) . . ?
C21 C26 C27 112.6(2) . . ?
C28 C26 C27 110.5(2) . . ?
C21 C26 H26 108.1 . . ?
C28 C26 H26 108.1 . . ?
C27 C26 H26 108.1 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 C30 112.6(2) . . ?
C25 C29 C31 109.3(2) . . ?
C30 C29 C31 110.5(2) . . ?
C25 C29 H29 108.1 . . ?
C30 C29 H29 108.1 . . ?
C31 C29 H29 108.1 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 B1 110.50(19) . . ?
C33 C32 H32A 109.6 . . ?
B1 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
B1 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
N34 C33 N37 110.56(19) . . ?
N34 C33 C32 125.3(2) . . ?
N37 C33 C32 124.0(2) . . ?
C33 N34 C38 125.53(19) . . ?
C33 N34 C35 111.63(18) . . ?
C38 N34 C35 122.55(18) . . ?
N34 C35 C36 102.85(18) . . ?
N34 C35 H35A 111.2 . . ?
C36 C35 H35A 111.2 . . ?
N34 C35 H35B 111.2 . . ?
C36 C35 H35B 111.2 . . ?
H35A C35 H35B 109.1 . . ?
N37 C36 C35 103.09(17) . . ?
N37 C36 H36A 111.1 . . ?
C35 C36 H36A 111.1 . . ?
N37 C36 H36B 111.1 . . ?
C35 C36 H36B 111.1 . . ?
H36A C36 H36B 109.1 . . ?
C33 N37 C50 126.22(19) . . ?
C33 N37 C36 111.78(18) . . ?
C50 N37 C36 121.00(17) . . ?
C39 C38 C43 123.0(2) . . ?
C39 C38 N34 119.0(2) . . ?
C43 C38 N34 118.0(2) . . ?
C38 C39 C40 117.0(2) . . ?
C38 C39 C44 123.2(2) . . ?
C40 C39 C44 119.6(2) . . ?
C41 C40 C39 121.1(2) . . ?
C41 C40 H40 119.5 . . ?
C39 C40 H40 119.5 . . ?
C42 C41 C40 120.6(2) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C41 C42 C43 120.9(2) . . ?
C41 C42 H42 119.6 . . ?
C43 C42 H42 119.6 . . ?
C42 C43 C38 117.4(2) . . ?
C42 C43 C47 119.8(2) . . ?
C38 C43 C47 122.7(2) . . ?
C39 C44 C46 113.9(2) . . ?
C39 C44 C45 109.8(2) . . ?
C46 C44 C45 109.6(2) . . ?
C39 C44 H44 107.8 . . ?
C46 C44 H44 107.8 . . ?
C45 C44 H44 107.8 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 C49 113.8(2) . . ?
C43 C47 C48 110.2(2) . . ?
C49 C47 C48 110.4(2) . . ?
C43 C47 H47 107.4 . . ?
C49 C47 H47 107.4 . . ?
C48 C47 H47 107.4 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C55 C50 C51 122.9(2) . . ?
C55 C50 N37 118.2(2) . . ?
C51 C50 N37 118.77(19) . . ?
C52 C51 C50 117.7(2) . . ?
C52 C51 C56 119.0(2) . . ?
C50 C51 C56 123.4(2) . . ?
C53 C52 C51 120.6(2) . . ?
C53 C52 H52 119.7 . . ?
C51 C52 H52 119.7 . . ?
C52 C53 C54 120.6(2) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
C53 C54 C55 121.0(2) . . ?
C53 C54 H54 119.5 . . ?
C55 C54 H54 119.5 . . ?
C54 C55 C50 117.2(2) . . ?
C54 C55 C59 119.9(2) . . ?
C50 C55 C59 122.9(2) . . ?
C51 C56 C58 112.22(19) . . ?
C51 C56 C57 110.8(2) . . ?
C58 C56 C57 110.7(2) . . ?
C51 C56 H56 107.6 . . ?
C58 C56 H56 107.6 . . ?
C57 C56 H56 107.6 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C55 C59 C61 112.0(2) . . ?
C55 C59 C60 110.45(19) . . ?
C61 C59 C60 110.6(2) . . ?
C55 C59 H59 107.9 . . ?
C61 C59 H59 107.9 . . ?
C60 C59 H59 107.9 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
F62 C62 C63 117.3(3) . . ?
F62 C62 C67 118.2(3) . . ?
C63 C62 C67 124.5(3) . . ?
C62 C63 C64 117.8(3) . . ?
C62 C63 H63 121.1 . . ?
C64 C63 H63 121.1 . . ?
C63 C64 C65 120.6(3) . . ?
C63 C64 H64 119.7 . . ?
C65 C64 H64 119.7 . . ?
C66 C65 C64 119.2(4) . . ?
C66 C65 H65 120.4 . . ?
C64 C65 H65 120.4 . . ?
C67 C66 C65 120.1(3) . . ?
C67 C66 H66 120.0 . . ?
C65 C66 H66 120.0 . . ?
C62 C67 C66 117.7(3) . . ?
C62 C67 H67 121.1 . . ?
C66 C67 H67 121.1 . . ?
F69 C69 C71 117.0(4) . 2_665 ?
F69 C69 C70 119.4(4) . . ?
C71 C69 C70 123.4(4) 2_665 . ?
C71 C69 H69 118.3 2_665 . ?
C70 C69 H69 118.3 . . ?
C71 C70 C69 118.1(3) . . ?
C71 C70 H70 121.0 . . ?
C69 C70 H70 121.0 . . ?
C69 C71 C70 118.5(3) 2_665 . ?
C69 C71 H71 120.8 2_665 . ?
C70 C71 H71 120.8 . . ?
S74 N73 S81 123.92(14) . . ?
O76 S74 O75 118.80(14) . . ?
O76 S74 N73 108.36(13) . . ?
O75 S74 N73 116.67(12) . . ?
O76 S74 C77 103.38(13) . . ?
O75 S74 C77 104.47(12) . . ?
N73 S74 C77 102.89(13) . . ?
F78 C77 F79 109.0(2) . . ?
F78 C77 F80 107.1(2) . . ?
F79 C77 F80 108.2(2) . . ?
F78 C77 S74 111.54(18) . . ?
F79 C77 S74 109.9(2) . . ?
F80 C77 S74 110.99(19) . . ?
O82 S81 O83 119.31(14) . . ?
O82 S81 N73 116.45(12) . . ?
O83 S81 N73 109.01(13) . . ?
O82 S81 C84 104.31(12) . . ?
O83 S81 C84 103.59(12) . . ?
N73 S81 C84 101.53(12) . . ?
F87 C84 F86 107.5(2) . . ?
F87 C84 F85 108.7(2) . . ?
F86 C84 F85 105.4(2) . . ?
F87 C84 S81 113.32(19) . . ?
F86 C84 S81 110.45(18) . . ?
F85 C84 S81 111.12(17) . . ?

_refine_diff_density_max         0.746
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.068

####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1060034'
_audit_update_record             
;
2015-07-06 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         
'C56 H84 B2 N4, C4 F12 N2 O8 S4, 0.33(C2 H4 Cl4)'
_chemical_formula_sum            'C60.66 H85.32 B2 Cl1.32 F12 N6 O8 S4'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1451.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0096 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0998 0.0984 '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                   12.306(2)
_cell_length_b                   12.691(2)
_cell_length_c                   13.389(2)
_cell_angle_alpha                95.14(2)
_cell_angle_beta                 101.53(2)
_cell_angle_gamma                118.07(2)
_cell_volume                     1766.6(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8182
_cell_measurement_theta_min      2.827
_cell_measurement_theta_max      19.0015
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.146
_shelx_estimated_absorpt_T_min   0.955
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3948
_exptl_absorpt_correction_T_max  0.4251
_exptl_absorpt_process_details   SADABS-2015/1
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_source                   'INCOATEC Microsource'
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            52767
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.508
_diffrn_reflns_theta_max         20.125
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6769
_reflns_number_gt                5126
_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 v2012.2'
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_reduction        'SAINT V8.30C'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_refine_special_details          
'56 DFIX and 100 DANG constraints on the two molecules of disordered N(OTf)2 [NS2O4C2F6], 1 SADI constrain on disordered DCM [CCl2], 477 RIGU and 1002 SIMU constrains on N(OTf)2 and DCM.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1175P)²+2.1303P] 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         6769
_refine_ls_number_parameters     863
_refine_ls_number_restraints     1636
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0745
_refine_ls_wR_factor_ref         0.2259
_refine_ls_wR_factor_gt          0.2054
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.5823(3) 0.5338(3) 0.5304(3) 0.0361(7) Uani 1 1 d . . . . .
H2 H 0.518(3) 0.552(3) 0.453(3) 0.043 Uiso 1 1 d . U . . .
H1 H 0.619(3) 0.484(3) 0.494(3) 0.043 Uiso 1 1 d . U . . .
C8 C 0.2139(3) 0.4377(3) 0.7689(3) 0.0413(7) Uani 1 1 d . . . . .
H8A H 0.1324 0.4156 0.7193 0.062 Uiso 1 1 calc R U . . .
H8B H 0.2508 0.5201 0.8108 0.062 Uiso 1 1 calc R U . . .
H8C H 0.1990 0.3793 0.8148 0.062 Uiso 1 1 calc R U . . .
C2 C 0.6598(3) 0.6524(2) 0.6234(2) 0.0297(6) Uani 1 1 d . . . . .
H2A H 0.7011 0.6311 0.6833 0.036 Uiso 1 1 calc R U . . .
H2B H 0.7293 0.7163 0.6004 0.036 Uiso 1 1 calc R U . . .
C3 C 0.5889(2) 0.7077(2) 0.6621(2) 0.0249(5) Uani 1 1 d . . . . .
N4 N 0.5336(2) 0.67597(19) 0.73821(17) 0.0266(5) Uani 1 1 d . . . . .
C5 C 0.5429(3) 0.5921(2) 0.8014(2) 0.0299(6) Uani 1 1 d . . . . .
C6 C 0.4361(3) 0.4753(2) 0.7850(2) 0.0322(6) Uani 1 1 d . . . . .
C7 C 0.3072(3) 0.4350(3) 0.7087(2) 0.0347(6) Uani 1 1 d . . . . .
H7 H 0.3204 0.4947 0.6621 0.042 Uiso 1 1 calc R U . . .
C9 C 0.2474(3) 0.3073(3) 0.6400(3) 0.0475(8) Uani 1 1 d . . . . .
H9A H 0.1702 0.2903 0.5871 0.071 Uiso 1 1 calc R U . . .
H9B H 0.2245 0.2461 0.6834 0.071 Uiso 1 1 calc R U . . .
H9C H 0.3092 0.3038 0.6056 0.071 Uiso 1 1 calc R U . . .
C10 C 0.4503(3) 0.3968(3) 0.8461(2) 0.0414(7) Uani 1 1 d . . . . .
H10 H 0.3802 0.3167 0.8368 0.050 Uiso 1 1 calc R U . . .
C11 C 0.5642(4) 0.4329(3) 0.9199(3) 0.0483(8) Uani 1 1 d . . . . .
H11 H 0.5719 0.3774 0.9598 0.058 Uiso 1 1 calc R U . . .
C17 C 0.4750(3) 0.7504(3) 0.7610(2) 0.0339(6) Uani 1 1 d . . . . .
H17A H 0.5109 0.7949 0.8347 0.041 Uiso 1 1 calc R U . . .
H17B H 0.3809 0.6991 0.7459 0.041 Uiso 1 1 calc R U . . .
C16 C 0.7815(4) 0.8310(4) 1.0082(3) 0.0659(11) Uani 1 1 d . . . . .
H16A H 0.8500 0.9163 1.0216 0.099 Uiso 1 1 calc R U . . .
H16B H 0.8015 0.7922 1.0636 0.099 Uiso 1 1 calc R U . . .
H16C H 0.7002 0.8281 1.0067 0.099 Uiso 1 1 calc R U . . .
C15 C 0.8962(4) 0.7696(5) 0.9012(4) 0.0835(15) Uani 1 1 d . . . . .
H15A H 0.8862 0.7243 0.8336 0.125 Uiso 1 1 calc R U . . .
H15B H 0.9209 0.7336 0.9570 0.125 Uiso 1 1 calc R U . . .
H15C H 0.9628 0.8552 0.9116 0.125 Uiso 1 1 calc R U . . .
C14 C 0.7703(3) 0.7630(3) 0.9033(3) 0.0530(9) Uani 1 1 d . . . . .
H14 H 0.7508 0.8052 0.8487 0.064 Uiso 1 1 calc R U . . .
C13 C 0.6585(3) 0.6328(3) 0.8781(2) 0.0391(7) Uani 1 1 d . . . . .
C12 C 0.6660(3) 0.5487(4) 0.9356(3) 0.0488(8) Uani 1 1 d . . . . .
H12 H 0.7436 0.5723 0.9867 0.059 Uiso 1 1 calc R U . . .
C18 C 0.5110(3) 0.8387(3) 0.6873(2) 0.0375(7) Uani 1 1 d . . . . .
H18A H 0.4339 0.8333 0.6415 0.045 Uiso 1 1 calc R U . . .
H18B H 0.5693 0.9240 0.7267 0.045 Uiso 1 1 calc R U . . .
N19 N 0.5761(2) 0.79619(19) 0.62640(18) 0.0270(5) Uani 1 1 d . . . . .
C20 C 0.6318(3) 0.8584(2) 0.5488(2) 0.0291(6) Uani 1 1 d . . . . .
C21 C 0.7642(3) 0.9443(2) 0.5776(2) 0.0338(6) Uani 1 1 d . . . . .
C22 C 0.8529(3) 0.9747(3) 0.6860(3) 0.0392(7) Uani 1 1 d . . . . .
H22 H 0.8046 0.9139 0.7257 0.047 Uiso 1 1 calc R U . . .
C23 C 0.9725(3) 0.9657(3) 0.6819(3) 0.0532(9) Uani 1 1 d . . . . .
H23A H 0.9461 0.8846 0.6428 0.080 Uiso 1 1 calc R U . . .
H23B H 1.0231 0.9786 0.7531 0.080 Uiso 1 1 calc R U . . .
H23C H 1.0245 1.0283 0.6474 0.080 Uiso 1 1 calc R U . . .
C24 C 0.8930(4) 1.1020(3) 0.7449(3) 0.0560(9) Uani 1 1 d . . . . .
H24A H 0.9367 1.1629 0.7055 0.084 Uiso 1 1 calc R U . . .
H24B H 0.9512 1.1200 0.8138 0.084 Uiso 1 1 calc R U . . .
H24C H 0.8168 1.1046 0.7531 0.084 Uiso 1 1 calc R U . . .
C26 C 0.7363(3) 0.9842(3) 0.4038(3) 0.0451(8) Uani 1 1 d . . . . .
H26 H 0.7723 1.0273 0.3537 0.054 Uiso 1 1 calc R U . . .
C25 C 0.8139(3) 1.0062(3) 0.5020(3) 0.0419(7) Uani 1 1 d . . . . .
H25 H 0.9026 1.0644 0.5187 0.050 Uiso 1 1 calc R U . . .
C29 C 0.4073(3) 0.7491(3) 0.4191(2) 0.0342(6) Uani 1 1 d . . . . .
H29 H 0.3855 0.7029 0.4756 0.041 Uiso 1 1 calc R U . . .
C28 C 0.5514(3) 0.8354(2) 0.4496(2) 0.0329(6) Uani 1 1 d . . . . .
C27 C 0.6073(3) 0.9003(3) 0.3774(2) 0.0404(7) Uani 1 1 d . . . . .
H27 H 0.5554 0.8863 0.3093 0.048 Uiso 1 1 calc R U . . .
C30 C 0.3376(3) 0.8223(3) 0.4090(3) 0.0472(8) Uani 1 1 d . . . . .
H30A H 0.3556 0.8660 0.3523 0.071 Uiso 1 1 calc R U . . .
H30B H 0.3674 0.8813 0.4746 0.071 Uiso 1 1 calc R U . . .
H30C H 0.2451 0.7666 0.3937 0.071 Uiso 1 1 calc R U . . .
C31 C 0.3601(3) 0.6565(3) 0.3160(2) 0.0433(7) Uani 1 1 d . . . . .
H31A H 0.3717 0.6996 0.2584 0.065 Uiso 1 1 calc R U . . .
H31B H 0.2692 0.5967 0.3037 0.065 Uiso 1 1 calc R U . . .
H31C H 0.4096 0.6142 0.3202 0.065 Uiso 1 1 calc R U . . .
N32 N 0.0574(7) 0.4966(7) 0.5330(7) 0.0471(17) Uani 0.3663(19) 1 d D U P A -1
S33 S 0.0794(5) 0.6270(4) 0.5493(3) 0.0283(7) Uani 0.3663(19) 1 d D U P A -1
O34 O 0.2165(6) 0.7026(8) 0.5997(6) 0.0573(19) Uani 0.3663(19) 1 d D U P A -1
O35 O 0.0316(13) 0.6653(13) 0.4654(9) 0.055(3) Uani 0.3663(19) 1 d D U P A -1
C36 C 0.0025(10) 0.6360(10) 0.6510(9) 0.044(2) Uani 0.3663(19) 1 d D U P A -1
F37 F 0.0333(11) 0.5879(11) 0.7289(8) 0.070(2) Uani 0.3663(19) 1 d D U P A -1
F38 F 0.0456(10) 0.7514(8) 0.6928(7) 0.068(2) Uani 0.3663(19) 1 d D U P A -1
F39 F -0.1194(7) 0.5783(9) 0.6147(9) 0.081(2) Uani 0.3663(19) 1 d D U P A -1
S40 S -0.0713(9) 0.3835(8) 0.4542(7) 0.091(3) Uani 0.3663(19) 1 d D U P A -1
O41 O -0.1774(6) 0.3942(7) 0.4197(6) 0.0569(18) Uani 0.3663(19) 1 d D U P A -1
O42 O -0.0820(10) 0.2726(8) 0.4816(10) 0.079(3) Uani 0.3663(19) 1 d D U P A -1
C43 C -0.0183(16) 0.3766(15) 0.3353(12) 0.080(3) Uani 0.3663(19) 1 d D U P A -1
F44 F 0.0153(11) 0.4802(10) 0.3004(9) 0.087(3) Uani 0.3663(19) 1 d D U P A -1
F45 F -0.1072(11) 0.2797(12) 0.2616(9) 0.125(3) Uani 0.3663(19) 1 d D U P A -1
F46 F 0.0775(11) 0.3561(9) 0.3475(9) 0.093(3) Uani 0.3663(19) 1 d D U P A -1
N32' N 0.054(2) 0.5277(16) 0.464(2) 0.075(4) Uani 0.1337(19) 1 d D U P A -2
S33' S -0.0306(9) 0.5754(11) 0.5052(9) 0.078(3) Uani 0.1337(19) 1 d D U P A -2
O34' O -0.008(3) 0.685(2) 0.467(3) 0.088(7) Uani 0.1337(19) 1 d D U P A -2
O35' O -0.1568(15) 0.4877(19) 0.495(2) 0.084(5) Uani 0.1337(19) 1 d D U P A -2
C36' C 0.041(2) 0.647(2) 0.6453(15) 0.083(5) Uani 0.1337(19) 1 d D U P A -2
F37' F -0.014(3) 0.586(3) 0.710(2) 0.114(8) Uani 0.1337(19) 1 d D U P A -2
F38' F 0.1669(17) 0.682(2) 0.6736(19) 0.091(5) Uani 0.1337(19) 1 d D U P A -2
F39' F 0.026(3) 0.746(3) 0.649(2) 0.109(7) Uani 0.1337(19) 1 d D U P A -2
S40' S 0.0285(11) 0.3919(11) 0.4377(12) 0.092(3) Uani 0.1337(19) 1 d D U P A -2
O41' O -0.024(4) 0.325(4) 0.515(3) 0.078(7) Uani 0.1337(19) 1 d D U P A -2
O42' O 0.143(2) 0.398(3) 0.429(3) 0.100(7) Uani 0.1337(19) 1 d D U P A -2
C43' C -0.102(2) 0.302(2) 0.3201(18) 0.108(5) Uani 0.1337(19) 1 d D U P A -2
F44' F -0.121(3) 0.360(3) 0.246(2) 0.123(7) Uani 0.1337(19) 1 d D U P A -2
F45' F -0.207(2) 0.260(3) 0.353(3) 0.123(7) Uani 0.1337(19) 1 d D U P A -2
F46' F -0.112(3) 0.202(2) 0.270(2) 0.122(7) Uani 0.1337(19) 1 d D U P A -2
N47 N 0.531(2) -0.0348(13) 0.9650(12) 0.068(3) Uani 0.266(3) 1 d D U P B -3
S48 S 0.5891(16) 0.1020(13) 0.9571(12) 0.105(3) Uani 0.266(3) 1 d D U P B -3
O49 O 0.541(2) 0.1752(17) 0.998(2) 0.099(5) Uani 0.266(3) 1 d D U P B -3
O50 O 0.627(2) 0.120(2) 0.8642(15) 0.133(6) Uani 0.266(3) 1 d D U P B -3
C51 C 0.7393(18) 0.1585(19) 1.0634(15) 0.130(4) Uani 0.266(3) 1 d D U P B -3
F52 F 0.732(2) 0.0685(17) 1.1132(14) 0.176(6) Uani 0.266(3) 1 d D U P B -3
F53 F 0.8307(17) 0.206(2) 1.021(2) 0.157(6) Uani 0.266(3) 1 d D U P B -3
F54 F 0.7434(18) 0.2448(18) 1.1293(18) 0.158(6) Uani 0.266(3) 1 d D U P B -3
S55 S 0.5198(7) -0.0610(5) 1.0761(3) 0.0616(13) Uani 0.266(3) 1 d D U P B -3
O56 O 0.5464(14) -0.1533(10) 1.0970(9) 0.072(3) Uani 0.266(3) 1 d D U P B -3
O57 O 0.5566(13) 0.0372(9) 1.1607(6) 0.071(3) Uani 0.266(3) 1 d D U P B -3
C58 C 0.3334(15) -0.1540(16) 1.0398(14) 0.095(4) Uani 0.266(3) 1 d D U P B -3
F59 F 0.2958(16) -0.1955(14) 1.1159(11) 0.113(4) Uani 0.266(3) 1 d D U P B -3
F60 F 0.3081(16) -0.2417(13) 0.9633(12) 0.109(4) Uani 0.266(3) 1 d D U P B -3
F61 F 0.2931(15) -0.0793(14) 1.0085(13) 0.112(4) Uani 0.266(3) 1 d D U P B -3
N47' N 0.466(2) 0.0304(15) 1.0210(17) 0.067(3) Uani 0.234(3) 1 d D U P B -4
S48' S 0.5802(16) 0.0931(14) 0.9699(12) 0.107(3) Uani 0.234(3) 1 d D U P B -4
O49' O 0.590(2) 0.2041(16) 0.940(2) 0.142(6) Uani 0.234(3) 1 d D U P B -4
O50' O 0.602(2) 0.0161(14) 0.9008(15) 0.123(5) Uani 0.234(3) 1 d D U P B -4
C51' C 0.729(2) 0.1733(19) 1.0779(16) 0.128(4) Uani 0.234(3) 1 d D U P B -4
F52' F 0.792(2) 0.1229(19) 1.055(2) 0.137(5) Uani 0.234(3) 1 d D U P B -4
F53' F 0.773(2) 0.2848(16) 1.059(2) 0.149(6) Uani 0.234(3) 1 d D U P B -4
F54' F 0.6883(19) 0.1431(19) 1.1621(13) 0.137(5) Uani 0.234(3) 1 d D U P B -4
S55' S 0.4315(8) -0.0959(6) 1.0561(4) 0.0324(13) Uani 0.234(3) 1 d D U P B -4
O56' O 0.5001(16) -0.1480(15) 1.0186(12) 0.051(4) Uani 0.234(3) 1 d D U P B -4
O57' O 0.4433(14) -0.0845(13) 1.1651(7) 0.055(3) Uani 0.234(3) 1 d D U P B -4
C58' C 0.2594(14) -0.2008(16) 1.0040(14) 0.092(4) Uani 0.234(3) 1 d D U P B -4
F59' F 0.2235(16) -0.3038(15) 1.0370(15) 0.132(5) Uani 0.234(3) 1 d D U P B -4
F60' F 0.196(2) -0.221(2) 0.9073(13) 0.140(6) Uani 0.234(3) 1 d D U P B -4
F61' F 0.2029(16) -0.1445(18) 1.0496(14) 0.123(5) Uani 0.234(3) 1 d D U P B -4
C1 C 0.907(2) 0.465(2) 0.9399(12) 0.121(7) Uani 0.33 1 d D U P C -5
H1A H 0.8181 0.4040 0.9375 0.146 Uiso 0.33 1 calc R U P C -5
H1B H 0.9019 0.5230 0.8965 0.146 Uiso 0.33 1 calc R U P C -5
Cl2 Cl 0.9743(5) 0.3927(5) 0.8869(4) 0.0881(13) Uani 0.33 1 d D U P C -5
Cl3 Cl 0.9884(7) 0.5457(7) 1.0681(4) 0.112(2) Uani 0.33 1 d D U P C -5


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C2 1.601(4) . ?
B1 B1 1.755(7) 2_666 ?
B1 H2 1.28(3) . ?
B1 H1 1.07(3) . ?
C8 C7 1.540(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C2 C3 1.488(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N19 1.322(3) . ?
C3 N4 1.326(3) . ?
N4 C5 1.449(3) . ?
N4 C17 1.477(3) . ?
C5 C6 1.402(4) . ?
C5 C13 1.405(4) . ?
C6 C10 1.395(4) . ?
C6 C7 1.521(4) . ?
C7 C9 1.535(4) . ?
C7 H7 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.382(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.371(5) . ?
C11 H11 0.9500 . ?
C17 C18 1.526(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C16 C14 1.526(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C15 C14 1.518(6) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 C13 1.520(5) . ?
C14 H14 1.0000 . ?
C13 C12 1.397(5) . ?
C12 H12 0.9500 . ?
C18 N19 1.479(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
N19 C20 1.447(3) . ?
C20 C28 1.401(4) . ?
C20 C21 1.412(4) . ?
C21 C25 1.397(4) . ?
C21 C22 1.521(4) . ?
C22 C24 1.530(5) . ?
C22 C23 1.540(4) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C26 C27 1.378(5) . ?
C26 C25 1.378(5) . ?
C26 H26 0.9500 . ?
C25 H25 0.9500 . ?
C29 C28 1.521(4) . ?
C29 C30 1.532(4) . ?
C29 C31 1.540(4) . ?
C29 H29 1.0000 . ?
C28 C27 1.399(4) . ?
C27 H27 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N32 S33 1.533(8) . ?
N32 S40 1.614(11) . ?
S33 O35 1.395(10) . ?
S33 O34 1.459(8) . ?
S33 C36 1.832(10) . ?
C36 F39 1.277(12) . ?
C36 F38 1.320(12) . ?
C36 F37 1.333(12) . ?
S40 O41 1.369(10) . ?
S40 O42 1.438(11) . ?
S40 C43 1.848(14) . ?
C43 F46 1.306(15) . ?
C43 F45 1.329(15) . ?
C43 F44 1.340(15) . ?
N32' S40' 1.588(16) . ?
N32' S33' 1.595(16) . ?
S33' O35' 1.389(15) . ?
S33' O34' 1.450(17) . ?
S33' C36' 1.844(17) . ?
C36' F37' 1.299(18) . ?
C36' F39' 1.346(19) . ?
C36' F38' 1.350(18) . ?
S40' O42' 1.405(17) . ?
S40' O41' 1.456(18) . ?
S40' C43' 1.817(17) . ?
C43' F46' 1.318(19) . ?
C43' F44' 1.328(19) . ?
C43' F45' 1.331(19) . ?
N47 S48 1.559(15) . ?
N47 S55 1.570(13) . ?
S48 O50 1.411(16) . ?
S48 O49 1.437(16) . ?
S48 C51 1.864(17) . ?
C51 F53 1.280(18) . ?
C51 F54 1.318(18) . ?
C51 F52 1.351(18) . ?
S55 O56 1.393(9) . ?
S55 O57 1.433(9) . ?
S55 C58 1.949(15) . ?
C58 F59 1.259(16) . ?
C58 F60 1.314(16) . ?
C58 F61 1.323(16) . ?
N47' S48' 1.582(17) . ?
N47' S55' 1.595(13) . ?
S48' O50' 1.434(16) . ?
S48' O49' 1.455(16) . ?
S48' C51' 1.849(18) . ?
C51' F52' 1.270(18) . ?
C51' F53' 1.326(18) . ?
C51' F54' 1.340(18) . ?
S55' O57' 1.425(9) . ?
S55' O56' 1.428(11) . ?
S55' C58' 1.826(15) . ?
C58' F60' 1.305(16) . ?
C58' F59' 1.318(17) . ?
C58' F61' 1.387(18) . ?
C1 Cl2 1.698(13) . ?
C1 Cl3 1.740(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 B1 B1 123.6(3) . 2_666 ?
C2 B1 H2 111.0(15) . . ?
B1 B1 H2 47.0(15) 2_666 . ?
C2 B1 H1 127.6(18) . . ?
B1 B1 H1 108.8(18) 2_666 . ?
H2 B1 H1 103(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C2 B1 118.6(2) . . ?
C3 C2 H2A 107.7 . . ?
B1 C2 H2A 107.7 . . ?
C3 C2 H2B 107.7 . . ?
B1 C2 H2B 107.7 . . ?
H2A C2 H2B 107.1 . . ?
N19 C3 N4 111.9(2) . . ?
N19 C3 C2 124.1(2) . . ?
N4 C3 C2 124.0(2) . . ?
C3 N4 C5 125.4(2) . . ?
C3 N4 C17 110.9(2) . . ?
C5 N4 C17 123.2(2) . . ?
C6 C5 C13 123.0(3) . . ?
C6 C5 N4 118.8(2) . . ?
C13 C5 N4 118.2(2) . . ?
C10 C6 C5 116.8(3) . . ?
C10 C6 C7 120.1(3) . . ?
C5 C6 C7 123.0(2) . . ?
C6 C7 C9 113.1(3) . . ?
C6 C7 C8 109.8(2) . . ?
C9 C7 C8 109.5(2) . . ?
C6 C7 H7 108.1 . . ?
C9 C7 H7 108.1 . . ?
C8 C7 H7 108.1 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C6 121.5(3) . . ?
C11 C10 H10 119.3 . . ?
C6 C10 H10 119.3 . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
N4 C17 C18 103.0(2) . . ?
N4 C17 H17A 111.2 . . ?
C18 C17 H17A 111.2 . . ?
N4 C17 H17B 111.2 . . ?
C18 C17 H17B 111.2 . . ?
H17A C17 H17B 109.1 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C15 C14 C13 113.1(4) . . ?
C15 C14 C16 111.0(3) . . ?
C13 C14 C16 110.0(3) . . ?
C15 C14 H14 107.5 . . ?
C13 C14 H14 107.5 . . ?
C16 C14 H14 107.5 . . ?
C12 C13 C5 116.9(3) . . ?
C12 C13 C14 119.8(3) . . ?
C5 C13 C14 123.3(3) . . ?
C11 C12 C13 121.6(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
N19 C18 C17 103.0(2) . . ?
N19 C18 H18A 111.2 . . ?
C17 C18 H18A 111.2 . . ?
N19 C18 H18B 111.2 . . ?
C17 C18 H18B 111.2 . . ?
H18A C18 H18B 109.1 . . ?
C3 N19 C20 126.7(2) . . ?
C3 N19 C18 110.8(2) . . ?
C20 N19 C18 121.9(2) . . ?
C28 C20 C21 122.5(3) . . ?
C28 C20 N19 118.8(2) . . ?
C21 C20 N19 118.6(2) . . ?
C25 C21 C20 117.1(3) . . ?
C25 C21 C22 119.2(3) . . ?
C20 C21 C22 123.7(3) . . ?
C21 C22 C24 111.0(3) . . ?
C21 C22 C23 112.0(3) . . ?
C24 C22 C23 109.9(3) . . ?
C21 C22 H22 107.9 . . ?
C24 C22 H22 107.9 . . ?
C23 C22 H22 107.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27 C26 C25 120.8(3) . . ?
C27 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C26 C25 C21 121.1(3) . . ?
C26 C25 H25 119.4 . . ?
C21 C25 H25 119.4 . . ?
C28 C29 C30 109.9(2) . . ?
C28 C29 C31 112.2(2) . . ?
C30 C29 C31 109.3(3) . . ?
C28 C29 H29 108.5 . . ?
C30 C29 H29 108.5 . . ?
C31 C29 H29 108.5 . . ?
C27 C28 C20 117.5(3) . . ?
C27 C28 C29 119.2(3) . . ?
C20 C28 C29 123.3(3) . . ?
C26 C27 C28 120.9(3) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
S33 N32 S40 121.9(6) . . ?
O35 S33 O34 115.6(7) . . ?
O35 S33 N32 119.1(8) . . ?
O34 S33 N32 103.6(5) . . ?
O35 S33 C36 107.5(7) . . ?
O34 S33 C36 104.9(5) . . ?
N32 S33 C36 104.8(5) . . ?
F39 C36 F38 111.1(11) . . ?
F39 C36 F37 108.4(10) . . ?
F38 C36 F37 105.8(10) . . ?
F39 C36 S33 111.0(8) . . ?
F38 C36 S33 110.0(7) . . ?
F37 C36 S33 110.6(8) . . ?
O41 S40 O42 121.4(8) . . ?
O41 S40 N32 120.2(7) . . ?
O42 S40 N32 107.8(8) . . ?
O41 S40 C43 102.8(8) . . ?
O42 S40 C43 98.8(9) . . ?
N32 S40 C43 100.9(8) . . ?
F46 C43 F45 100.6(13) . . ?
F46 C43 F44 108.1(13) . . ?
F45 C43 F44 111.4(14) . . ?
F46 C43 S40 113.9(12) . . ?
F45 C43 S40 111.3(11) . . ?
F44 C43 S40 111.0(11) . . ?
S40' N32' S33' 129.0(15) . . ?
O35' S33' O34' 117.6(15) . . ?
O35' S33' N32' 116.2(14) . . ?
O34' S33' N32' 107.8(16) . . ?
O35' S33' C36' 106.0(14) . . ?
O34' S33' C36' 97.3(16) . . ?
N32' S33' C36' 110.2(12) . . ?
F37' C36' F39' 108(2) . . ?
F37' C36' F38' 110(2) . . ?
F39' C36' F38' 110(2) . . ?
F37' C36' S33' 117(2) . . ?
F39' C36' S33' 100.9(18) . . ?
F38' C36' S33' 110.8(16) . . ?
O42' S40' O41' 114(2) . . ?
O42' S40' N32' 107.8(16) . . ?
O41' S40' N32' 111(2) . . ?
O42' S40' C43' 111.8(18) . . ?
O41' S40' C43' 101.0(19) . . ?
N32' S40' C43' 111.5(13) . . ?
F46' C43' F44' 105(2) . . ?
F46' C43' F45' 103(2) . . ?
F44' C43' F45' 105(2) . . ?
F46' C43' S40' 119(2) . . ?
F44' C43' S40' 118(2) . . ?
F45' C43' S40' 104.5(18) . . ?
S48 N47 S55 115.7(11) . . ?
O50 S48 O49 119.3(16) . . ?
O50 S48 N47 110.8(14) . . ?
O49 S48 N47 120.3(15) . . ?
O50 S48 C51 106.0(14) . . ?
O49 S48 C51 99.5(14) . . ?
N47 S48 C51 95.7(12) . . ?
F53 C51 F54 109.5(19) . . ?
F53 C51 F52 117(2) . . ?
F54 C51 F52 108.4(19) . . ?
F53 C51 S48 105.6(16) . . ?
F54 C51 S48 104.8(15) . . ?
F52 C51 S48 110.4(15) . . ?
O56 S55 O57 118.4(7) . . ?
O56 S55 N47 111.9(8) . . ?
O57 S55 N47 119.9(7) . . ?
O56 S55 C58 99.5(8) . . ?
O57 S55 C58 105.0(8) . . ?
N47 S55 C58 96.7(9) . . ?
F59 C58 F60 111.7(15) . . ?
F59 C58 F61 113.3(15) . . ?
F60 C58 F61 112.8(16) . . ?
F59 C58 S55 110.8(13) . . ?
F60 C58 S55 101.1(12) . . ?
F61 C58 S55 106.4(12) . . ?
S48' N47' S55' 121.0(14) . . ?
O50' S48' O49' 117.5(15) . . ?
O50' S48' N47' 118.2(14) . . ?
O49' S48' N47' 111.4(15) . . ?
O50' S48' C51' 104.3(14) . . ?
O49' S48' C51' 94.9(14) . . ?
N47' S48' C51' 106.7(13) . . ?
F52' C51' F53' 114(2) . . ?
F52' C51' F54' 113(2) . . ?
F53' C51' F54' 123(2) . . ?
F52' C51' S48' 102.2(16) . . ?
F53' C51' S48' 98.3(15) . . ?
F54' C51' S48' 103.1(15) . . ?
O57' S55' O56' 114.9(9) . . ?
O57' S55' N47' 111.8(10) . . ?
O56' S55' N47' 110.6(11) . . ?
O57' S55' C58' 100.2(9) . . ?
O56' S55' C58' 109.8(10) . . ?
N47' S55' C58' 108.9(10) . . ?
F60' C58' F59' 110.7(17) . . ?
F60' C58' F61' 97.6(17) . . ?
F59' C58' F61' 105.2(17) . . ?
F60' C58' S55' 124.0(16) . . ?
F59' C58' S55' 111.6(12) . . ?
F61' C58' S55' 104.9(12) . . ?
Cl2 C1 Cl3 114.4(11) . . ?
Cl2 C1 H1A 108.7 . . ?
Cl3 C1 H1A 108.7 . . ?
Cl2 C1 H1B 108.7 . . ?
Cl3 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?

_refine_diff_density_max         0.785
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.065

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1060035'
_audit_update_record             
;
2015-07-06 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H81 B2 F6 N5 O4 S2'
_chemical_formula_weight         1112.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0096 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7540(7)
_cell_length_b                   16.4070(14)
_cell_length_c                   18.5100(15)
_cell_angle_alpha                83.780(2)
_cell_angle_beta                 73.470(2)
_cell_angle_gamma                83.410(2)
_cell_volume                     3100.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.104
_exptl_absorpt_coefficient_mu    0.085
_shelx_estimated_absorpt_T_min   0.984
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.56086
_diffrn_radiation_type           AgK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            238549
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.289
_diffrn_reflns_theta_max         22.073
_diffrn_reflns_theta_full        19.665
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15500
_reflns_number_gt                12120
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
'6 SADI constraints for the B-H distances; 471 SAME/SADI and 36 RIGU constraints on the disordered iPr [-C(CH3)2] moieties'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0412P)²+1.3493P] 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         15500
_refine_ls_number_parameters     768
_refine_ls_number_restraints     513
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0999
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   1.024
_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
H5B H 0.4175(15) 0.2794(11) 0.1480(6) 0.041(5) Uiso 1 1 d D . . . .
B0 B 0.49306(17) 0.23578(12) 0.09885(10) 0.0314(4) Uani 1 1 d D . . . .
H0BA H 0.5141(17) 0.1725(9) 0.1245(9) 0.038 Uiso 1 1 d D U . . .
H0BB H 0.4405(16) 0.2375(11) 0.0563(9) 0.038 Uiso 1 1 d D U . . .
C0 C 0.62159(13) 0.28727(9) 0.07330(7) 0.0220(3) Uani 1 1 d . . . . .
H0A H 0.5955 0.3459 0.0616 0.026 Uiso 1 1 calc R U . . .
H0B H 0.6618 0.2838 0.1156 0.026 Uiso 1 1 calc R U . . .
C1 C 0.71706(12) 0.25490(8) 0.00673(7) 0.0187(2) Uani 1 1 d . . . . .
N2 N 0.80155(11) 0.18745(7) 0.00527(6) 0.0204(2) Uani 1 1 d . . . . .
C3 C 0.87303(14) 0.17624(9) -0.06884(7) 0.0241(3) Uani 1 1 d . . . . .
H3 H 0.9391 0.1333 -0.0853 0.029 Uiso 1 1 calc R U . . .
C4 C 0.83127(13) 0.23726(9) -0.11265(7) 0.0233(3) Uani 1 1 d . . . . .
H4 H 0.8620 0.2457 -0.1661 0.028 Uiso 1 1 calc R U . . .
N5 N 0.73457(11) 0.28588(7) -0.06531(6) 0.0190(2) Uani 1 1 d . . . . .
C6 C 0.82724(13) 0.13622(8) 0.06910(7) 0.0220(3) Uani 1 1 d . . . . .
C8 C 0.94268(15) 0.11099(10) 0.16207(9) 0.0323(3) Uani 1 1 d . . . . .
H8 H 0.9968 0.1280 0.1891 0.039 Uiso 1 1 calc R U . . .
C9 C 0.90243(16) 0.03254(10) 0.17771(9) 0.0365(4) Uani 1 1 d . . . . .
H9 H 0.9312 -0.0041 0.2143 0.044 Uiso 1 1 calc R U . . .
C10 C 0.82099(16) 0.00686(9) 0.14083(9) 0.0331(3) Uani 1 1 d . . . . .
H10 H 0.7918 -0.0467 0.1536 0.040 Uiso 1 1 calc R U . . .
C7 C 0.90568(13) 0.16557(9) 0.10755(8) 0.0247(3) Uani 1 1 d D . . . .
C12 C 0.95196(14) 0.25147(9) 0.09095(9) 0.0291(3) Uani 0.568(19) 1 d D U P A 1
H12 H 0.8893 0.2869 0.0676 0.035 Uiso 0.568(19) 1 calc R U P A 1
C13 C 0.9560(11) 0.2910(5) 0.1597(4) 0.0498(17) Uani 0.568(19) 1 d D U P A 1
H13A H 1.0246 0.2617 0.1803 0.075 Uiso 0.568(19) 1 calc R U P A 1
H13B H 0.8717 0.2885 0.1979 0.075 Uiso 0.568(19) 1 calc R U P A 1
H13C H 0.9743 0.3486 0.1457 0.075 Uiso 0.568(19) 1 calc R U P A 1
C14 C 1.0869(6) 0.2497(5) 0.0321(4) 0.0406(13) Uani 0.568(19) 1 d D U P A 1
H14A H 1.0812 0.2281 -0.0141 0.061 Uiso 0.568(19) 1 calc R U P A 1
H14B H 1.1504 0.2142 0.0527 0.061 Uiso 0.568(19) 1 calc R U P A 1
H14C H 1.1146 0.3056 0.0203 0.061 Uiso 0.568(19) 1 calc R U P A 1
C12' C 0.95196(14) 0.25147(9) 0.09095(9) 0.0291(3) Uani 0.432(19) 1 d D U P A 2
H12' H 0.9118 0.2821 0.0523 0.035 Uiso 0.432(19) 1 calc R U P A 2
C13' C 0.9059(10) 0.2982(6) 0.1648(5) 0.0407(17) Uani 0.432(19) 1 d D U P A 2
H13X H 0.9465 0.2698 0.2028 0.061 Uiso 0.432(19) 1 calc R U P A 2
H13Y H 0.8109 0.2995 0.1844 0.061 Uiso 0.432(19) 1 calc R U P A 2
H13Z H 0.9314 0.3547 0.1533 0.061 Uiso 0.432(19) 1 calc R U P A 2
C14' C 1.0981(8) 0.2507(7) 0.0610(11) 0.067(3) Uani 0.432(19) 1 d D U P A 2
H14X H 1.1273 0.2248 0.0130 0.101 Uiso 0.432(19) 1 calc R U P A 2
H14Y H 1.1391 0.2195 0.0977 0.101 Uiso 0.432(19) 1 calc R U P A 2
H14Z H 1.1229 0.3073 0.0529 0.101 Uiso 0.432(19) 1 calc R U P A 2
C11 C 0.78064(14) 0.05836(9) 0.08498(8) 0.0260(3) Uani 1 1 d D . . . .
C15 C 0.69292(16) 0.02880(9) 0.04403(9) 0.0322(3) Uani 1 1 d D . . . .
H15 H 0.6609 0.0774 0.0146 0.039 Uiso 1 1 calc R U . . .
C16 C 0.7700(2) -0.03333(12) -0.01189(11) 0.0512(5) Uani 1 1 d D . . . .
H16A H 0.8424 -0.0073 -0.0485 0.077 Uiso 1 1 calc R U . . .
H16B H 0.7127 -0.0515 -0.0386 0.077 Uiso 1 1 calc R U . . .
H16C H 0.8044 -0.0809 0.0156 0.077 Uiso 1 1 calc R U . . .
C17 C 0.57419(18) -0.00891(11) 0.09869(11) 0.0428(4) Uani 1 1 d D . . . .
H17A H 0.5180 -0.0245 0.0700 0.064 Uiso 1 1 calc R U . . .
H17B H 0.5255 0.0315 0.1340 0.064 Uiso 1 1 calc R U . . .
H17C H 0.6032 -0.0578 0.1270 0.064 Uiso 1 1 calc R U . . .
C18 C 0.66482(13) 0.35828(8) -0.09189(7) 0.0196(3) Uani 1 1 d . . . . .
C20 C 0.64002(17) 0.50367(9) -0.11805(8) 0.0323(3) Uani 1 1 d . . . . .
H20 H 0.6622 0.5574 -0.1152 0.039 Uiso 1 1 calc R U . . .
C21 C 0.54595(16) 0.49392(9) -0.15290(9) 0.0333(3) Uani 1 1 d . . . . .
H21 H 0.5058 0.5408 -0.1750 0.040 Uiso 1 1 calc R U . . .
C22 C 0.50932(15) 0.41675(9) -0.15605(8) 0.0284(3) Uani 1 1 d . . . . .
H22 H 0.4435 0.4114 -0.1798 0.034 Uiso 1 1 calc R U . . .
C19 C 0.70317(15) 0.43598(9) -0.08690(8) 0.0255(3) Uani 1 1 d D . . . .
C24 C 0.81163(17) 0.44602(10) -0.05201(8) 0.0334(4) Uani 0.580(14) 1 d D U P B
1
H24 H 0.8084 0.4026 -0.0094 0.040 Uiso 0.580(14) 1 calc R U P B 1
C25 C 0.9398(5) 0.4352(4) -0.1076(3) 0.0351(11) Uani 0.580(14) 1 d D U P B 1
H25A H 0.9506 0.3811 -0.1274 0.053 Uiso 0.580(14) 1 calc R U P B 1
H25B H 1.0084 0.4391 -0.0831 0.053 Uiso 0.580(14) 1 calc R U P B 1
H25C H 0.9457 0.4783 -0.1492 0.053 Uiso 0.580(14) 1 calc R U P B 1
C26 C 0.7869(5) 0.5320(3) -0.0189(4) 0.0393(11) Uani 0.580(14) 1 d D U P B 1
H26A H 0.8010 0.5754 -0.0604 0.059 Uiso 0.580(14) 1 calc R U P B 1
H26B H 0.8472 0.5352 0.0115 0.059 Uiso 0.580(14) 1 calc R U P B 1
H26C H 0.6971 0.5392 0.0130 0.059 Uiso 0.580(14) 1 calc R U P B 1
C24' C 0.81163(17) 0.44602(10) -0.05201(8) 0.0334(4) Uani 0.420(14) 1 d D U P B
2
H24' H 0.8331 0.3899 -0.0293 0.040 Uiso 0.420(14) 1 calc R U P B 2
C25' C 0.9416(7) 0.4683(7) -0.1146(4) 0.0417(18) Uani 0.420(14) 1 d D U P B 2
H25X H 0.9604 0.4310 -0.1551 0.062 Uiso 0.420(14) 1 calc R U P B 2
H25Y H 1.0141 0.4623 -0.0916 0.062 Uiso 0.420(14) 1 calc R U P B 2
H25Z H 0.9304 0.5252 -0.1357 0.062 Uiso 0.420(14) 1 calc R U P B 2
C26' C 0.7837(8) 0.4996(9) 0.0094(6) 0.071(3) Uani 0.420(14) 1 d D U P B 2
H26X H 0.7601 0.5559 -0.0089 0.106 Uiso 0.420(14) 1 calc R U P B 2
H26Y H 0.8611 0.4987 0.0275 0.106 Uiso 0.420(14) 1 calc R U P B 2
H26Z H 0.7113 0.4802 0.0508 0.106 Uiso 0.420(14) 1 calc R U P B 2
C23 C 0.56750(13) 0.34643(8) -0.12477(7) 0.0214(3) Uani 1 1 d D . . . .
C27 C 0.52618(14) 0.26167(9) -0.12809(8) 0.0245(3) Uani 1 1 d D . . . .
H27 H 0.5667 0.2219 -0.0946 0.029 Uiso 1 1 calc R U . . .
C28 C 0.57547(17) 0.23361(10) -0.20812(9) 0.0350(4) Uani 1 1 d D . . . .
H28A H 0.5352 0.2707 -0.2419 0.052 Uiso 1 1 calc R U . . .
H28B H 0.5525 0.1775 -0.2080 0.052 Uiso 1 1 calc R U . . .
H28C H 0.6703 0.2347 -0.2258 0.052 Uiso 1 1 calc R U . . .
C29 C 0.37863(15) 0.26031(10) -0.09811(9) 0.0328(3) Uani 1 1 d D . . . .
H29A H 0.3365 0.2985 -0.1303 0.049 Uiso 1 1 calc R U . . .
H29B H 0.3500 0.2770 -0.0463 0.049 Uiso 1 1 calc R U . . .
H29C H 0.3548 0.2045 -0.0986 0.049 Uiso 1 1 calc R U . . .
B30 B 0.36141(15) 0.26713(10) 0.21795(8) 0.0230(3) Uani 1 1 d D . . . .
H3BA H 0.3015(14) 0.2150(9) 0.2255(9) 0.028 Uiso 1 1 d D U . . .
H3BB H 0.3038(14) 0.3272(8) 0.2233(9) 0.028 Uiso 1 1 d D U . . .
C30 C 0.46854(12) 0.25400(8) 0.26639(7) 0.0176(2) Uani 1 1 d . . . . .
H30A H 0.5272 0.2038 0.2521 0.021 Uiso 1 1 calc R U . . .
H30B H 0.5220 0.3015 0.2546 0.021 Uiso 1 1 calc R U . . .
C31 C 0.40269(11) 0.24616(7) 0.34765(7) 0.0149(2) Uani 1 1 d . . . . .
N32 N 0.38004(10) 0.17523(6) 0.39136(6) 0.0148(2) Uani 1 1 d . . . . .
C33 C 0.31261(12) 0.19257(8) 0.46467(7) 0.0174(2) Uani 1 1 d . . . . .
H33 H 0.2849 0.1536 0.5065 0.021 Uiso 1 1 calc R U . . .
C34 C 0.29399(12) 0.27506(8) 0.46519(7) 0.0179(2) Uani 1 1 d . . . . .
H34 H 0.2506 0.3053 0.5076 0.022 Uiso 1 1 calc R U . . .
N35 N 0.34994(10) 0.30751(6) 0.39241(6) 0.0155(2) Uani 1 1 d . . . . .
C36 C 0.43476(12) 0.09433(7) 0.36819(7) 0.0154(2) Uani 1 1 d . . . . .
C38 C 0.41783(14) -0.03018(8) 0.31868(7) 0.0231(3) Uani 1 1 d . . . . .
H38 H 0.3707 -0.0647 0.3001 0.028 Uiso 1 1 calc R U . . .
C39 C 0.54327(14) -0.05694(8) 0.32216(8) 0.0258(3) Uani 1 1 d . . . . .
H39 H 0.5812 -0.1092 0.3054 0.031 Uiso 1 1 calc R U . . .
C40 C 0.61377(13) -0.00853(8) 0.34972(8) 0.0238(3) Uani 1 1 d . . . . .
H40 H 0.6992 -0.0281 0.3522 0.029 Uiso 1 1 calc R U . . .
C37 C 0.35960(12) 0.04654(8) 0.34193(7) 0.0177(2) Uani 1 1 d D . . . .
C42 C 0.22004(13) 0.07526(8) 0.34170(8) 0.0214(3) Uani 1 1 d D . . . .
H42 H 0.2120 0.1368 0.3370 0.026 Uiso 1 1 calc R U . . .
C43 C 0.12405(13) 0.04723(9) 0.41633(8) 0.0253(3) Uani 1 1 d D . . . .
H43A H 0.0352 0.0676 0.4154 0.038 Uiso 1 1 calc R U . . .
H43B H 0.1446 0.0692 0.4584 0.038 Uiso 1 1 calc R U . . .
H43C H 0.1310 -0.0130 0.4230 0.038 Uiso 1 1 calc R U . . .
C44 C 0.18286(16) 0.04675(10) 0.27562(9) 0.0336(3) Uani 1 1 d D . . . .
H44A H 0.0945 0.0700 0.2763 0.050 Uiso 1 1 calc R U . . .
H44B H 0.1861 -0.0135 0.2800 0.050 Uiso 1 1 calc R U . . .
H44C H 0.2441 0.0654 0.2280 0.050 Uiso 1 1 calc R U . . .
C41 C 0.56057(12) 0.06888(8) 0.37397(7) 0.0181(2) Uani 1 1 d D . . . .
C45 C 0.63664(12) 0.12091(8) 0.40629(7) 0.0212(3) Uani 1 1 d D . . . .
H45 H 0.5795 0.1716 0.4236 0.025 Uiso 1 1 calc R U . . .
C46 C 0.75905(16) 0.14767(11) 0.34741(9) 0.0380(4) Uani 1 1 d D . . . .
H46A H 0.8180 0.0990 0.3308 0.057 Uiso 1 1 calc R U . . .
H46B H 0.8027 0.1835 0.3696 0.057 Uiso 1 1 calc R U . . .
H46C H 0.7351 0.1777 0.3039 0.057 Uiso 1 1 calc R U . . .
C47 C 0.67273(17) 0.07485(10) 0.47430(9) 0.0360(4) Uani 1 1 d D . . . .
H47A H 0.5939 0.0572 0.5116 0.054 Uiso 1 1 calc R U . . .
H47B H 0.7147 0.1112 0.4970 0.054 Uiso 1 1 calc R U . . .
H47C H 0.7329 0.0265 0.4581 0.054 Uiso 1 1 calc R U . . .
C48 C 0.35406(12) 0.39519(7) 0.37240(7) 0.0167(2) Uani 1 1 d . . . . .
C50 C 0.24465(14) 0.52576(8) 0.34887(8) 0.0244(3) Uani 1 1 d . . . . .
H50 H 0.1704 0.5588 0.3410 0.029 Uiso 1 1 calc R U . . .
C51 C 0.35405(14) 0.56293(8) 0.34837(8) 0.0264(3) Uani 1 1 d . . . . .
H51 H 0.3535 0.6212 0.3409 0.032 Uiso 1 1 calc R U . . .
C52 C 0.46463(14) 0.51617(8) 0.35859(8) 0.0250(3) Uani 1 1 d . . . . .
H52 H 0.5396 0.5426 0.3569 0.030 Uiso 1 1 calc R U . . .
C49 C 0.24180(12) 0.44032(8) 0.36082(7) 0.0191(3) Uani 1 1 d D . . . .
C54 C 0.12090(13) 0.39990(8) 0.36253(8) 0.0226(3) Uani 1 1 d D . . . .
H54 H 0.1453 0.3395 0.3591 0.027 Uiso 1 1 calc R U . . .
C55 C 0.06910(15) 0.43256(10) 0.29513(9) 0.0303(3) Uani 1 1 d D . . . .
H55A H 0.1407 0.4309 0.2485 0.045 Uiso 1 1 calc R U . . .
H55B H 0.0312 0.4894 0.3016 0.045 Uiso 1 1 calc R U . . .
H55C H 0.0022 0.3983 0.2920 0.045 Uiso 1 1 calc R U . . .
C56 C 0.01432(14) 0.41200(10) 0.43654(9) 0.0311(3) Uani 1 1 d D . . . .
H56A H -0.0152 0.4706 0.4396 0.047 Uiso 1 1 calc R U . . .
H56B H 0.0491 0.3920 0.4794 0.047 Uiso 1 1 calc R U . . .
H56C H -0.0592 0.3811 0.4380 0.047 Uiso 1 1 calc R U . . .
C53 C 0.46685(13) 0.43075(8) 0.37137(7) 0.0205(3) Uani 1 1 d D . . . .
C57 C 0.58588(13) 0.37985(9) 0.38636(9) 0.0274(3) Uani 1 1 d D . . . .
H57 H 0.5790 0.3213 0.3787 0.033 Uiso 1 1 calc R U . . .
C58 C 0.5871(2) 0.38325(14) 0.46799(11) 0.0550(5) Uani 1 1 d D . . . .
H58A H 0.6601 0.3467 0.4778 0.083 Uiso 1 1 calc R U . . .
H58B H 0.5051 0.3655 0.5020 0.083 Uiso 1 1 calc R U . . .
H58C H 0.5967 0.4398 0.4767 0.083 Uiso 1 1 calc R U . . .
C59 C 0.71267(16) 0.40588(12) 0.33239(12) 0.0492(5) Uani 1 1 d D . . . .
H59A H 0.7846 0.3659 0.3386 0.074 Uiso 1 1 calc R U . . .
H59B H 0.7281 0.4603 0.3435 0.074 Uiso 1 1 calc R U . . .
H59C H 0.7071 0.4082 0.2803 0.074 Uiso 1 1 calc R U . . .
N60 N 0.12569(10) 0.23641(7) 0.63243(6) 0.0195(2) Uani 1 1 d . . . . .
S61 S 0.02576(3) 0.16853(2) 0.65427(2) 0.01806(7) Uani 1 1 d . . . . .
O62 O -0.05239(10) 0.16218(6) 0.73071(5) 0.0275(2) Uani 1 1 d . . . . .
O63 O 0.08967(9) 0.09495(6) 0.62075(5) 0.0238(2) Uani 1 1 d . . . . .
C64 C -0.08947(13) 0.20740(8) 0.59935(8) 0.0232(3) Uani 1 1 d . . . . .
F65 F -0.18947(9) 0.16136(6) 0.61708(6) 0.0381(2) Uani 1 1 d . . . . .
F66 F -0.03293(9) 0.20613(6) 0.52619(5) 0.0357(2) Uani 1 1 d . . . . .
F67 F -0.13610(9) 0.28440(5) 0.61334(5) 0.0336(2) Uani 1 1 d . . . . .
S68 S 0.10841(3) 0.31891(2) 0.67220(2) 0.01844(7) Uani 1 1 d . . . . .
O69 O -0.01307(10) 0.33660(6) 0.72650(5) 0.0250(2) Uani 1 1 d . . . . .
O70 O 0.16128(11) 0.38294(6) 0.61725(6) 0.0297(2) Uani 1 1 d . . . . .
C71 C 0.22632(17) 0.29677(9) 0.72690(10) 0.0352(4) Uani 1 1 d . . . . .
F72 F 0.19595(13) 0.23371(6) 0.77763(6) 0.0544(3) Uani 1 1 d . . . . .
F73 F 0.22842(11) 0.36275(6) 0.76278(6) 0.0493(3) Uani 1 1 d . . . . .
F74 F 0.34555(10) 0.27923(7) 0.68329(8) 0.0571(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
B0 C0 1.630(2) . ?
B0 H5B 1.260(11) . ?
B0 H0BA 1.120(13) . ?
B0 H0BB 1.088(13) . ?
C0 C1 1.4668(17) . ?
C0 H0A 0.9900 . ?
C0 H0B 0.9900 . ?
C1 N5 1.3432(16) . ?
C1 N2 1.3463(17) . ?
N2 C3 1.3888(16) . ?
N2 C6 1.4476(17) . ?
C3 C4 1.338(2) . ?
C3 H3 0.9500 . ?
C4 N5 1.3886(17) . ?
C4 H4 0.9500 . ?
N5 C18 1.4472(17) . ?
C6 C11 1.3969(19) . ?
C6 C7 1.400(2) . ?
C8 C9 1.380(2) . ?
C8 C7 1.389(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.378(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(2) . ?
C10 H10 0.9500 . ?
C7 C12' 1.519(2) . ?
C7 C12 1.519(2) . ?
C12 C13 1.503(6) . ?
C12 C14 1.547(5) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C12' C14' 1.510(7) . ?
C12' C13' 1.568(8) . ?
C12' H12' 1.0000 . ?
C13' H13X 0.9800 . ?
C13' H13Y 0.9800 . ?
C13' H13Z 0.9800 . ?
C14' H14X 0.9800 . ?
C14' H14Y 0.9800 . ?
C14' H14Z 0.9800 . ?
C11 C15 1.514(2) . ?
C15 C16 1.531(2) . ?
C15 C17 1.532(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 C23 1.3924(18) . ?
C18 C19 1.4041(18) . ?
C20 C21 1.377(2) . ?
C20 C19 1.392(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.380(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.398(2) . ?
C22 H22 0.9500 . ?
C19 C24' 1.517(2) . ?
C19 C24 1.517(2) . ?
C24 C25 1.472(5) . ?
C24 C26 1.563(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C24' C26' 1.454(6) . ?
C24' C25' 1.592(7) . ?
C24' H24' 1.0000 . ?
C25' H25X 0.9800 . ?
C25' H25Y 0.9800 . ?
C25' H25Z 0.9800 . ?
C26' H26X 0.9800 . ?
C26' H26Y 0.9800 . ?
C26' H26Z 0.9800 . ?
C23 C27 1.5202(18) . ?
C27 C29 1.527(2) . ?
C27 C28 1.5271(19) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
B30 C30 1.633(2) . ?
B30 H5B 1.268(11) . ?
B30 H3BA 1.102(12) . ?
B30 H3BB 1.101(12) . ?
C30 C31 1.4675(16) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 N35 1.3429(15) . ?
C31 N32 1.3479(15) . ?
N32 C33 1.3873(15) . ?
N32 C36 1.4466(15) . ?
C33 C34 1.3459(18) . ?
C33 H33 0.9500 . ?
C34 N35 1.3847(15) . ?
C34 H34 0.9500 . ?
N35 C48 1.4485(15) . ?
C36 C37 1.3986(17) . ?
C36 C41 1.3998(17) . ?
C38 C39 1.387(2) . ?
C38 C37 1.3945(18) . ?
C38 H38 0.9500 . ?
C39 C40 1.383(2) . ?
C39 H39 0.9500 . ?
C40 C41 1.3973(18) . ?
C40 H40 0.9500 . ?
C37 C42 1.5217(18) . ?
C42 C44 1.5231(19) . ?
C42 C43 1.5313(19) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C41 C45 1.5183(18) . ?
C45 C47 1.5202(19) . ?
C45 C46 1.5251(19) . ?
C45 H45 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C53 1.3996(18) . ?
C48 C49 1.3998(18) . ?
C50 C51 1.383(2) . ?
C50 C49 1.3977(18) . ?
C50 H50 0.9500 . ?
C51 C52 1.388(2) . ?
C51 H51 0.9500 . ?
C52 C53 1.3944(19) . ?
C52 H52 0.9500 . ?
C49 C54 1.5169(18) . ?
C54 C55 1.5284(19) . ?
C54 C56 1.5307(19) . ?
C54 H54 1.0000 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C53 C57 1.5231(19) . ?
C57 C59 1.518(2) . ?
C57 C58 1.522(2) . ?
C57 H57 1.0000 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
N60 S61 1.5775(11) . ?
N60 S68 1.5777(11) . ?
S61 O62 1.4250(10) . ?
S61 O63 1.4295(9) . ?
S61 C64 1.8358(14) . ?
C64 F66 1.3186(16) . ?
C64 F67 1.3290(15) . ?
C64 F65 1.3292(16) . ?
S68 O69 1.4248(10) . ?
S68 O70 1.4276(10) . ?
S68 C71 1.8194(16) . ?
C71 F72 1.323(2) . ?
C71 F74 1.325(2) . ?
C71 F73 1.3354(17) . ?

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
C0 B0 H5B 101.2(8) . . ?
C0 B0 H0BA 111.8(9) . . ?
H5B B0 H0BA 110.6(12) . . ?
C0 B0 H0BB 114.7(9) . . ?
H5B B0 H0BB 103.0(12) . . ?
H0BA B0 H0BB 114.3(13) . . ?
C1 C0 B0 111.08(11) . . ?
C1 C0 H0A 109.4 . . ?
B0 C0 H0A 109.4 . . ?
C1 C0 H0B 109.4 . . ?
B0 C0 H0B 109.4 . . ?
H0A C0 H0B 108.0 . . ?
N5 C1 N2 106.52(11) . . ?
N5 C1 C0 126.37(12) . . ?
N2 C1 C0 127.09(12) . . ?
C1 N2 C3 109.58(11) . . ?
C1 N2 C6 127.66(11) . . ?
C3 N2 C6 122.55(11) . . ?
C4 C3 N2 107.10(12) . . ?
C4 C3 H3 126.5 . . ?
N2 C3 H3 126.5 . . ?
C3 C4 N5 107.14(11) . . ?
C3 C4 H4 126.4 . . ?
N5 C4 H4 126.4 . . ?
C1 N5 C4 109.67(11) . . ?
C1 N5 C18 126.63(11) . . ?
C4 N5 C18 123.70(11) . . ?
C11 C6 C7 124.02(13) . . ?
C11 C6 N2 118.18(12) . . ?
C7 C6 N2 117.62(12) . . ?
C9 C8 C7 121.38(15) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C8 120.61(14) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 121.03(14) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C8 C7 C6 116.40(13) . . ?
C8 C7 C12' 120.42(13) . . ?
C6 C7 C12' 123.17(13) . . ?
C8 C7 C12 120.42(13) . . ?
C6 C7 C12 123.17(13) . . ?
C13 C12 C7 114.3(4) . . ?
C13 C12 C14 110.2(4) . . ?
C7 C12 C14 110.0(3) . . ?
C13 C12 H12 107.4 . . ?
C7 C12 H12 107.4 . . ?
C14 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C14' C12' C7 112.8(4) . . ?
C14' C12' C13' 108.9(5) . . ?
C7 C12' C13' 109.6(4) . . ?
C14' C12' H12' 108.5 . . ?
C7 C12' H12' 108.5 . . ?
C13' C12' H12' 108.5 . . ?
C12' C13' H13X 109.5 . . ?
C12' C13' H13Y 109.5 . . ?
H13X C13' H13Y 109.5 . . ?
C12' C13' H13Z 109.5 . . ?
H13X C13' H13Z 109.5 . . ?
H13Y C13' H13Z 109.5 . . ?
C12' C14' H14X 109.5 . . ?
C12' C14' H14Y 109.5 . . ?
H14X C14' H14Y 109.5 . . ?
C12' C14' H14Z 109.5 . . ?
H14X C14' H14Z 109.5 . . ?
H14Y C14' H14Z 109.5 . . ?
C6 C11 C10 116.46(14) . . ?
C6 C11 C15 123.08(13) . . ?
C10 C11 C15 120.44(13) . . ?
C11 C15 C16 110.14(14) . . ?
C11 C15 C17 112.22(13) . . ?
C16 C15 C17 110.26(14) . . ?
C11 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 . . ?
C23 C18 C19 123.64(13) . . ?
C23 C18 N5 117.67(11) . . ?
C19 C18 N5 118.60(12) . . ?
C21 C20 C19 121.02(14) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 120.74(14) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C23 121.03(14) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C20 C19 C18 116.81(13) . . ?
C20 C19 C24' 121.22(13) . . ?
C18 C19 C24' 121.93(13) . . ?
C20 C19 C24 121.22(13) . . ?
C18 C19 C24 121.93(13) . . ?
C25 C24 C19 110.9(3) . . ?
C25 C24 C26 112.2(3) . . ?
C19 C24 C26 108.9(2) . . ?
C25 C24 H24 108.2 . . ?
C19 C24 H24 108.2 . . ?
C26 C24 H24 108.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C26' C24' C19 118.3(4) . . ?
C26' C24' C25' 110.2(4) . . ?
C19 C24' C25' 111.8(3) . . ?
C26' C24' H24' 105.1 . . ?
C19 C24' H24' 105.1 . . ?
C25' C24' H24' 105.1 . . ?
C24' C25' H25X 109.5 . . ?
C24' C25' H25Y 109.5 . . ?
H25X C25' H25Y 109.5 . . ?
C24' C25' H25Z 109.5 . . ?
H25X C25' H25Z 109.5 . . ?
H25Y C25' H25Z 109.5 . . ?
C24' C26' H26X 109.5 . . ?
C24' C26' H26Y 109.5 . . ?
H26X C26' H26Y 109.5 . . ?
C24' C26' H26Z 109.5 . . ?
H26X C26' H26Z 109.5 . . ?
H26Y C26' H26Z 109.5 . . ?
C18 C23 C22 116.72(12) . . ?
C18 C23 C27 122.52(12) . . ?
C22 C23 C27 120.75(12) . . ?
C23 C27 C29 110.97(12) . . ?
C23 C27 C28 111.18(11) . . ?
C29 C27 C28 111.17(12) . . ?
C23 C27 H27 107.8 . . ?
C29 C27 H27 107.8 . . ?
C28 C27 H27 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 B30 H5B 110.3(8) . . ?
C30 B30 H3BA 114.1(8) . . ?
H5B B30 H3BA 108.0(11) . . ?
C30 B30 H3BB 113.7(8) . . ?
H5B B30 H3BB 95.8(11) . . ?
H3BA B30 H3BB 113.3(12) . . ?
C31 C30 B30 110.16(10) . . ?
C31 C30 H30A 109.6 . . ?
B30 C30 H30A 109.6 . . ?
C31 C30 H30B 109.6 . . ?
B30 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
N35 C31 N32 106.68(10) . . ?
N35 C31 C30 127.06(11) . . ?
N32 C31 C30 126.23(11) . . ?
C31 N32 C33 109.53(10) . . ?
C31 N32 C36 124.91(10) . . ?
C33 N32 C36 124.94(10) . . ?
C34 C33 N32 106.94(11) . . ?
C34 C33 H33 126.5 . . ?
N32 C33 H33 126.5 . . ?
C33 C34 N35 107.16(11) . . ?
C33 C34 H34 126.4 . . ?
N35 C34 H34 126.4 . . ?
C31 N35 C34 109.69(10) . . ?
C31 N35 C48 127.59(10) . . ?
C34 N35 C48 122.63(10) . . ?
C37 C36 C41 124.19(11) . . ?
C37 C36 N32 118.56(11) . . ?
C41 C36 N32 117.25(11) . . ?
C39 C38 C37 121.17(12) . . ?
C39 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
C40 C39 C38 120.82(12) . . ?
C40 C39 H39 119.6 . . ?
C38 C39 H39 119.6 . . ?
C39 C40 C41 120.65(13) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C38 C37 C36 116.35(12) . . ?
C38 C37 C42 121.82(12) . . ?
C36 C37 C42 121.79(11) . . ?
C37 C42 C44 112.97(12) . . ?
C37 C42 C43 110.92(11) . . ?
C44 C42 C43 109.86(11) . . ?
C37 C42 H42 107.6 . . ?
C44 C42 H42 107.6 . . ?
C43 C42 H42 107.6 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C40 C41 C36 116.80(12) . . ?
C40 C41 C45 120.57(12) . . ?
C36 C41 C45 122.62(11) . . ?
C41 C45 C47 110.79(11) . . ?
C41 C45 C46 112.01(12) . . ?
C47 C45 C46 109.85(12) . . ?
C41 C45 H45 108.0 . . ?
C47 C45 H45 108.0 . . ?
C46 C45 H45 108.0 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C53 C48 C49 123.74(12) . . ?
C53 C48 N35 117.91(11) . . ?
C49 C48 N35 118.17(11) . . ?
C51 C50 C49 120.95(13) . . ?
C51 C50 H50 119.5 . . ?
C49 C50 H50 119.5 . . ?
C50 C51 C52 120.79(13) . . ?
C50 C51 H51 119.6 . . ?
C52 C51 H51 119.6 . . ?
C51 C52 C53 120.69(13) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 H52 119.7 . . ?
C50 C49 C48 116.75(12) . . ?
C50 C49 C54 120.79(12) . . ?
C48 C49 C54 122.45(11) . . ?
C49 C54 C55 111.24(11) . . ?
C49 C54 C56 111.34(11) . . ?
C55 C54 C56 110.12(11) . . ?
C49 C54 H54 108.0 . . ?
C55 C54 H54 108.0 . . ?
C56 C54 H54 108.0 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C52 C53 C48 117.05(12) . . ?
C52 C53 C57 120.66(12) . . ?
C48 C53 C57 122.25(12) . . ?
C59 C57 C58 110.59(15) . . ?
C59 C57 C53 112.65(13) . . ?
C58 C57 C53 110.51(13) . . ?
C59 C57 H57 107.6 . . ?
C58 C57 H57 107.6 . . ?
C53 C57 H57 107.6 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
S61 N60 S68 125.05(7) . . ?
O62 S61 O63 118.58(6) . . ?
O62 S61 N60 116.61(6) . . ?
O63 S61 N60 108.27(6) . . ?
O62 S61 C64 104.53(6) . . ?
O63 S61 C64 104.54(6) . . ?
N60 S61 C64 102.14(6) . . ?
F66 C64 F67 107.96(12) . . ?
F66 C64 F65 108.34(11) . . ?
F67 C64 F65 107.97(11) . . ?
F66 C64 S61 111.00(9) . . ?
F67 C64 S61 111.15(9) . . ?
F65 C64 S61 110.31(10) . . ?
O69 S68 O70 118.67(6) . . ?
O69 S68 N60 116.71(6) . . ?
O70 S68 N60 109.20(6) . . ?
O69 S68 C71 104.96(7) . . ?
O70 S68 C71 103.56(7) . . ?
N60 S68 C71 101.14(7) . . ?
F72 C71 F74 108.00(13) . . ?
F72 C71 F73 108.71(14) . . ?
F74 C71 F73 107.72(13) . . ?
F72 C71 S68 111.17(11) . . ?
F74 C71 S68 111.82(12) . . ?
F73 C71 S68 109.31(10) . . ?

_refine_diff_density_max         0.334
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.046

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1401734'
_audit_update_record             
;
2015-07-06 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H43 B N2'
_chemical_formula_sum            'C28 H43 B N2'
_chemical_formula_weight         418.45

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'

_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                   11.624(2)
_cell_length_b                   15.921(3)
_cell_length_c                   14.028(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.23(2)
_cell_angle_gamma                90
_cell_volume                     2562.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5414
_cell_measurement_theta_min      2.188
_cell_measurement_theta_max      27.8465

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.062
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7110
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS-2015/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC Microsource'
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23574
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.775
_diffrn_reflns_theta_max         27.887
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6095
_reflns_number_gt                4688
_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 v2012.2'
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_reduction        'SAINT V8.30C'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_refine_special_details          '3 SADI constraints on the B-H distances.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0462P)²+1.0321P] 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         6095
_refine_ls_number_parameters     300
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1078
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.038
_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
B1 B 0.69867(14) 0.35305(10) 0.30926(10) 0.0193(3) Uani 1 1 d D . . . .
H1 H 0.6935(14) 0.4167(8) 0.3443(11) 0.030(4) Uiso 1 1 d D . . . .
H2 H 0.7482(13) 0.3584(10) 0.2451(10) 0.026(4) Uiso 1 1 d D . . . .
H3 H 0.6082(11) 0.3263(9) 0.2839(11) 0.027(4) Uiso 1 1 d D . . . .
C2 C 0.77371(11) 0.28700(8) 0.38924(9) 0.0159(3) Uani 1 1 d . . . . .
H2A H 0.7802 0.2315 0.3587 0.019 Uiso 1 1 calc R U . . .
H2B H 0.8534 0.3091 0.4102 0.019 Uiso 1 1 calc R U . . .
C3 C 0.71456(10) 0.27794(8) 0.47231(8) 0.0134(2) Uani 1 1 d . . . . .
N4 N 0.62918(9) 0.22307(7) 0.47881(7) 0.0143(2) Uani 1 1 d . . . . .
C5 C 0.59356(11) 0.15120(8) 0.41863(9) 0.0156(3) Uani 1 1 d . . . . .
C6 C 0.48032(11) 0.15015(8) 0.36539(9) 0.0176(3) Uani 1 1 d . . . . .
C8 C 0.29484(12) 0.21069(9) 0.40729(10) 0.0239(3) Uani 1 1 d . . . . .
H8A H 0.2467 0.2615 0.4037 0.036 Uiso 1 1 calc R U . . .
H8B H 0.3219 0.1964 0.4751 0.036 Uiso 1 1 calc R U . . .
H8C H 0.2485 0.1641 0.3755 0.036 Uiso 1 1 calc R U . . .
C7 C 0.40020(11) 0.22636(8) 0.35651(9) 0.0187(3) Uani 1 1 d . . . . .
H7 H 0.4450 0.2751 0.3886 0.022 Uiso 1 1 calc R U . . .
C9 C 0.35964(12) 0.24892(9) 0.24976(10) 0.0243(3) Uani 1 1 d . . . . .
H9A H 0.4276 0.2620 0.2191 0.037 Uiso 1 1 calc R U . . .
H9B H 0.3081 0.2979 0.2456 0.037 Uiso 1 1 calc R U . . .
H9C H 0.3174 0.2012 0.2166 0.037 Uiso 1 1 calc R U . . .
C10 C 0.44041(12) 0.07509(9) 0.32008(10) 0.0227(3) Uani 1 1 d . . . . .
H10 H 0.3639 0.0728 0.2842 0.027 Uiso 1 1 calc R U . . .
C11 C 0.50947(13) 0.00413(9) 0.32623(10) 0.0255(3) Uani 1 1 d . . . . .
H11 H 0.4799 -0.0467 0.2963 0.031 Uiso 1 1 calc R U . . .
C12 C 0.62197(13) 0.00759(9) 0.37623(11) 0.0246(3) Uani 1 1 d . . . . .
H12 H 0.6699 -0.0410 0.3787 0.029 Uiso 1 1 calc R U . . .
C13 C 0.66691(12) 0.08067(8) 0.42315(10) 0.0199(3) Uani 1 1 d . . . . .
C14 C 0.79134(12) 0.08060(8) 0.47638(10) 0.0225(3) Uani 1 1 d . . . . .
H14 H 0.8103 0.1391 0.4998 0.027 Uiso 1 1 calc R U . . .
C15 C 0.87728(13) 0.05675(10) 0.40853(12) 0.0313(3) Uani 1 1 d . . . . .
H15A H 0.8657 -0.0022 0.3893 0.047 Uiso 1 1 calc R U . . .
H15B H 0.9573 0.0647 0.4420 0.047 Uiso 1 1 calc R U . . .
H15C H 0.8638 0.0925 0.3510 0.047 Uiso 1 1 calc R U . . .
C16 C 0.80491(14) 0.02320(10) 0.56460(11) 0.0309(3) Uani 1 1 d . . . . .
H16A H 0.7905 -0.0351 0.5436 0.046 Uiso 1 1 calc R U . . .
H16B H 0.7487 0.0396 0.6064 0.046 Uiso 1 1 calc R U . . .
H16C H 0.8842 0.0283 0.6005 0.046 Uiso 1 1 calc R U . . .
C17 C 0.58443(11) 0.23212(8) 0.57110(9) 0.0180(3) Uani 1 1 d . . . . .
H17A H 0.5936 0.1792 0.6087 0.022 Uiso 1 1 calc R U . . .
H17B H 0.5012 0.2484 0.5600 0.022 Uiso 1 1 calc R U . . .
C18 C 0.66042(11) 0.30185(8) 0.62289(9) 0.0180(3) Uani 1 1 d . . . . .
H18A H 0.6124 0.3495 0.6392 0.022 Uiso 1 1 calc R U . . .
H18B H 0.7086 0.2807 0.6827 0.022 Uiso 1 1 calc R U . . .
N19 N 0.73368(9) 0.32667(7) 0.55093(7) 0.0141(2) Uani 1 1 d . . . . .
C20 C 0.82852(11) 0.38503(8) 0.57592(9) 0.0158(3) Uani 1 1 d . . . . .
C21 C 0.80532(12) 0.47156(8) 0.56735(9) 0.0183(3) Uani 1 1 d . . . . .
C22 C 0.68335(12) 0.50510(8) 0.53311(10) 0.0209(3) Uani 1 1 d . . . . .
H22 H 0.6338 0.4572 0.5046 0.025 Uiso 1 1 calc R U . . .
C23 C 0.63189(14) 0.53834(10) 0.61967(11) 0.0291(3) Uani 1 1 d . . . . .
H23A H 0.6788 0.5857 0.6487 0.044 Uiso 1 1 calc R U . . .
H23B H 0.6323 0.4935 0.6676 0.044 Uiso 1 1 calc R U . . .
H23C H 0.5517 0.5571 0.5981 0.044 Uiso 1 1 calc R U . . .
C24 C 0.67980(14) 0.57320(9) 0.45555(11) 0.0278(3) Uani 1 1 d . . . . .
H24A H 0.7129 0.5510 0.4007 0.042 Uiso 1 1 calc R U . . .
H24B H 0.7253 0.6219 0.4826 0.042 Uiso 1 1 calc R U . . .
H24C H 0.5989 0.5903 0.4337 0.042 Uiso 1 1 calc R U . . .
C25 C 0.89742(13) 0.52670(9) 0.59695(10) 0.0238(3) Uani 1 1 d . . . . .
H25 H 0.8841 0.5855 0.5914 0.029 Uiso 1 1 calc R U . . .
C26 C 1.00751(13) 0.49772(9) 0.63414(10) 0.0267(3) Uani 1 1 d . . . . .
H26 H 1.0690 0.5364 0.6538 0.032 Uiso 1 1 calc R U . . .
C27 C 1.02791(12) 0.41221(9) 0.64270(10) 0.0237(3) Uani 1 1 d . . . . .
H27 H 1.1039 0.3928 0.6684 0.028 Uiso 1 1 calc R U . . .
C28 C 0.93946(11) 0.35372(9) 0.61444(9) 0.0183(3) Uani 1 1 d . . . . .
C29 C 0.96524(12) 0.26040(9) 0.62731(10) 0.0224(3) Uani 1 1 d . . . . .
H29 H 0.8909 0.2292 0.6060 0.027 Uiso 1 1 calc R U . . .
C30 C 1.05396(13) 0.23100(10) 0.56441(11) 0.0308(3) Uani 1 1 d . . . . .
H30A H 1.0672 0.1705 0.5733 0.046 Uiso 1 1 calc R U . . .
H30B H 1.1276 0.2611 0.5834 0.046 Uiso 1 1 calc R U . . .
H30C H 1.0237 0.2426 0.4964 0.046 Uiso 1 1 calc R U . . .
C31 C 1.00778(13) 0.23840(10) 0.73346(11) 0.0299(3) Uani 1 1 d . . . . .
H31A H 1.0192 0.1775 0.7399 0.045 Uiso 1 1 calc R U . . .
H31B H 0.9496 0.2564 0.7726 0.045 Uiso 1 1 calc R U . . .
H31C H 1.0818 0.2671 0.7558 0.045 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
B1 C2 1.6767(19) . ?
B1 H1 1.132(13) . ?
B1 H2 1.147(12) . ?
B1 H3 1.138(12) . ?
C2 C3 1.4522(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.3361(16) . ?
C3 N19 1.3376(16) . ?
N4 C5 1.4427(16) . ?
N4 C17 1.4777(16) . ?
C5 C13 1.4051(18) . ?
C5 C6 1.4055(18) . ?
C6 C10 1.3974(19) . ?
C6 C7 1.5224(19) . ?
C8 C7 1.5328(19) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C7 C9 1.5385(18) . ?
C7 H7 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.381(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.3962(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.5176(19) . ?
C14 C16 1.526(2) . ?
C14 C15 1.534(2) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.5280(18) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 N19 1.4752(16) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
N19 C20 1.4414(16) . ?
C20 C21 1.4052(19) . ?
C20 C28 1.4071(18) . ?
C21 C25 1.3953(19) . ?
C21 C22 1.5190(19) . ?
C22 C23 1.532(2) . ?
C22 C24 1.5319(19) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.381(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.3967(19) . ?
C27 H27 0.9500 . ?
C28 C29 1.5206(19) . ?
C29 C31 1.5325(19) . ?
C29 C30 1.534(2) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
C2 B1 H1 109.2(8) . . ?
C2 B1 H2 107.4(8) . . ?
H1 B1 H2 110.0(11) . . ?
C2 B1 H3 109.3(8) . . ?
H1 B1 H3 111.1(11) . . ?
H2 B1 H3 109.7(11) . . ?
C3 C2 B1 109.68(10) . . ?
C3 C2 H2A 109.7 . . ?
B1 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
B1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N4 C3 N19 110.49(11) . . ?
N4 C3 C2 124.90(11) . . ?
N19 C3 C2 124.51(11) . . ?
C3 N4 C5 128.70(10) . . ?
C3 N4 C17 111.45(10) . . ?
C5 N4 C17 118.79(10) . . ?
C13 C5 C6 121.62(12) . . ?
C13 C5 N4 119.50(11) . . ?
C6 C5 N4 118.47(11) . . ?
C10 C6 C5 117.78(12) . . ?
C10 C6 C7 119.36(12) . . ?
C5 C6 C7 122.86(11) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C7 C8 110.87(11) . . ?
C6 C7 C9 110.71(11) . . ?
C8 C7 C9 110.33(11) . . ?
C6 C7 H7 108.3 . . ?
C8 C7 H7 108.3 . . ?
C9 C7 H7 108.3 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C6 121.61(13) . . ?
C11 C10 H10 119.2 . . ?
C6 C10 H10 119.2 . . ?
C10 C11 C12 119.50(13) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C13 121.62(13) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C5 117.79(12) . . ?
C12 C13 C14 119.09(12) . . ?
C5 C13 C14 123.11(12) . . ?
C13 C14 C16 111.46(12) . . ?
C13 C14 C15 111.05(12) . . ?
C16 C14 C15 111.22(12) . . ?
C13 C14 H14 107.6 . . ?
C16 C14 H14 107.6 . . ?
C15 C14 H14 107.6 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 103.27(10) . . ?
N4 C17 H17A 111.1 . . ?
C18 C17 H17A 111.1 . . ?
N4 C17 H17B 111.1 . . ?
C18 C17 H17B 111.1 . . ?
H17A C17 H17B 109.1 . . ?
N19 C18 C17 102.85(10) . . ?
N19 C18 H18A 111.2 . . ?
C17 C18 H18A 111.2 . . ?
N19 C18 H18B 111.2 . . ?
C17 C18 H18B 111.2 . . ?
H18A C18 H18B 109.1 . . ?
C3 N19 C20 126.44(10) . . ?
C3 N19 C18 111.78(10) . . ?
C20 N19 C18 120.61(10) . . ?
C21 C20 C28 122.12(12) . . ?
C21 C20 N19 118.84(11) . . ?
C28 C20 N19 118.89(12) . . ?
C25 C21 C20 117.64(12) . . ?
C25 C21 C22 120.37(12) . . ?
C20 C21 C22 121.89(12) . . ?
C21 C22 C23 109.52(11) . . ?
C21 C22 C24 113.01(12) . . ?
C23 C22 C24 110.43(12) . . ?
C21 C22 H22 107.9 . . ?
C23 C22 H22 107.9 . . ?
C24 C22 H22 107.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C21 121.48(13) . . ?
C26 C25 H25 119.3 . . ?
C21 C25 H25 119.3 . . ?
C25 C26 C27 119.79(13) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C26 C27 C28 121.55(13) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C20 117.41(13) . . ?
C27 C28 C29 119.71(12) . . ?
C20 C28 C29 122.87(12) . . ?
C28 C29 C31 111.43(12) . . ?
C28 C29 C30 111.58(12) . . ?
C31 C29 C30 110.32(12) . . ?
C28 C29 H29 107.8 . . ?
C31 C29 H29 107.8 . . ?
C30 C29 H29 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

_refine_diff_density_max         0.280
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.042

