# Supplementary Information (SI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_compound_9a
_audit_block_doi                 10.5517/ccdc.csd.cc2f6qr4
_database_code_depnum_ccdc_archive 'CCDC 2240796'
loop_
_audit_author_name
_audit_author_address
'Yoichi Hoshimoto'
;Osaka University
Japan
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_audit_creation_date             2022-09-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C48 H46 B2 F10 N3 O2 P, C H2 Cl2'
_chemical_formula_sum            'C49 H48 B2 Cl2 F10 N3 O2 P'
_chemical_formula_weight         1024.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C98 H94 B4 F22 N6 O4 P4 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.5399(5)
_cell_length_b                   11.4428(6)
_cell_length_c                   21.6413(9)
_cell_angle_alpha                85.586(4)
_cell_angle_beta                 85.395(4)
_cell_angle_gamma                69.910(4)
_cell_volume                     2439.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3959
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      75.6860
_cell_measurement_theta_min      4.5060
_shelx_estimated_absorpt_T_max   0.937
_shelx_estimated_absorpt_T_min   0.809
_exptl_absorpt_coefficient_mu    2.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29927
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         4.104
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00  44.00   0.50    5.00    --   49.92-109.00 -81.00   56
  2  ω     18.00 102.00   0.50    5.00    --   66.50-109.00 -81.00  168
  3  ω     94.00 133.00   0.50    5.00    --   66.50  57.00   0.00   78
  4  ω     82.00 115.00   0.50    5.00    --   66.50 109.00  14.00   66
  5  ω    -61.00 -22.00   0.50    5.00    --  -53.17  37.00   0.00   78
  6  ω    -60.00  19.00   0.50    5.00    --  -53.17  37.00  30.00  158
  7  ω    -60.00 -20.00   0.50    5.00    --  -53.17 109.00  14.00   80
  8  ω    -69.00 -34.00   0.50    5.00    -- -105.75  57.00 120.00   70
  9  ω    -65.00 -40.00   0.50    5.00    -- -105.75 125.00  60.00   50
 10  ω    -64.00 -37.00   0.50    5.00    -- -105.75 125.00  90.00   54
 11  ω    -98.00 -70.00   0.50    5.00    -- -105.75 125.00  60.00   56
 12  ω   -111.00 -84.00   0.50    5.00    -- -105.75 109.00  14.00   54
 13  ω    -85.00 -58.00   0.50    5.00    -- -105.75  77.00 -30.00   54
 14  ω   -109.00 -36.00   0.50    5.00    -- -105.75  37.00  30.00  146
 15  ω   -117.00 -34.00   0.50    5.00    -- -105.75  57.00  30.00  166
 16  ω   -117.00 -72.00   0.50    5.00    -- -105.75  57.00-120.00   90
 17  ω    -68.00 -36.00   0.50    5.00    -- -105.75  57.00-120.00   64
 18  ω   -113.00 -35.00   0.50    5.00    -- -105.75  19.00-180.00  156
 19  ω   -114.00 -34.00   0.50    5.00    -- -105.75 125.00-150.00  160
 20  ω   -116.00 -84.00   0.50    5.00    -- -105.75 125.00-180.00   64
 21  ω   -123.00 -41.00   0.50    5.00    -- -105.75  77.00-120.00  164
 22  ω   -124.00 -46.00   0.50    5.00    --  -53.17 -19.00-150.00  156
 23  ω   -119.00 -80.00   0.50    5.00    --  -53.17-109.00 -81.00   78
 24  ω   -123.00 -84.00   0.50    5.00    --  -53.17-125.00 -30.00   78
 25  ω   -126.00 -81.00   0.50    5.00    -- -105.75-109.00 -81.00   90
 26  ω   -126.00-100.00   0.50    5.00    -- -105.75 -99.00-150.00   52
 27  ω   -146.00-119.00   0.50    5.00    -- -105.75 -19.00-180.00   54
 28  ω   -173.00-148.00   0.50    5.00    -- -105.75 -99.00-150.00   50
 29  ω   -160.00-133.00   0.50    5.00    -- -105.75-109.00 -81.00   54
 30  ω   -170.00-120.00   0.50    5.00    -- -105.75 -57.00   0.00  100
 31  ω   -159.00 -98.00   0.50    5.00    -- -105.75 -19.00  30.00  122
 32  ω   -117.00 -78.00   0.50    5.00    -- -105.75  57.00 120.00   78
 33  ω   -115.00 -88.00   0.50    5.00    -- -105.75 125.00  90.00   54
 34  ω   -116.00 -54.00   0.50    5.00    -- -105.75 125.00  30.00  124
 35  ω   -177.00-108.00   0.50    5.00    -- -105.75 -57.00  30.00  138
 36  ω   -117.00 -79.00   0.50    5.00    --  -53.17-125.00  60.00   76
 37  ω   -108.00 -83.00   0.50    5.00    -- -105.75 -99.00 150.00   50
 38  ω   -170.00-126.00   0.50    5.00    -- -105.75 -99.00 150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0876198000
_diffrn_orient_matrix_UB_12      -0.0564175000
_diffrn_orient_matrix_UB_13      -0.0579841000
_diffrn_orient_matrix_UB_21      0.1259998000
_diffrn_orient_matrix_UB_22      -0.0477778000
_diffrn_orient_matrix_UB_23      0.0387001000
_diffrn_orient_matrix_UB_31      -0.0273684000
_diffrn_orient_matrix_UB_32      -0.1230527000
_diffrn_orient_matrix_UB_33      0.0159606000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5774
_reflns_number_total             8887
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         8887
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0721
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0852P)²+1.3789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1892
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C68 \\sim Cl2A-C68
 with sigma of 0.02
3. Others
 Sof(H68C)=Sof(H68D)=Sof(Cl2A)=1-FVAR(1)
 Sof(Cl2)=Sof(H68A)=Sof(H68B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C53(H53), C56(H56), B23(H23)
4.b Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C68(H68C,H68D)
4.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C10(H10), C7(H7), C13(H13), C4(H4), C51(H51), C50(H50),
 C11(H11), C5(H5), C49(H49), C12(H12), C6(H6)
4.d Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C60(H60A,H60B,H60C), C66(H66A,H66B,
 H66C), C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C55(H55A,H55B,H55C), C54(H54A,
 H54B,H54C), C58(H58A,H58B,H58C), C57(H57A,H57B,H57C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P15 P 0.58653(9) 0.21460(9) 0.33261(4) 0.0373(2) Uani 1 1 d . . . . .
Cl1 Cl 0.40180(18) 0.72715(16) 0.40757(8) 0.1048(5) Uani 1 1 d . . . . .
Cl2 Cl 0.1146(9) 0.8614(7) 0.4181(4) 0.091(3) Uani 0.54(5) 1 d D . P A 1
F35 F 0.1394(2) 0.3151(2) 0.36662(10) 0.0492(5) Uani 1 1 d . . . . .
F34 F -0.0708(3) 0.7489(2) 0.32716(11) 0.0631(7) Uani 1 1 d . . . . .
F33 F -0.0235(3) 0.3260(2) 0.46777(11) 0.0606(6) Uani 1 1 d . . . . .
O25 O 0.2574(2) 0.4185(2) 0.27082(11) 0.0399(6) Uani 1 1 d . . . . .
F32 F -0.2152(3) 0.5443(3) 0.49966(11) 0.0677(7) Uani 1 1 d . . . . .
O24 O 0.3666(3) 0.4318(2) 0.35433(12) 0.0467(6) Uani 1 1 d . . . . .
F42 F -0.0142(3) 0.3841(3) 0.24842(12) 0.0704(7) Uani 1 1 d . . . . .
F31 F -0.2364(3) 0.7565(3) 0.42806(13) 0.0761(8) Uani 1 1 d . . . . .
F44 F 0.1188(3) 0.7248(3) 0.17134(12) 0.0783(8) Uani 1 1 d . . . . .
N16 N 0.6741(3) 0.1071(3) 0.27938(13) 0.0368(7) Uani 1 1 d . . . . .
N14 N 0.4549(3) 0.2713(3) 0.28986(13) 0.0364(7) Uani 1 1 d . . . . .
N19 N 0.6782(3) 0.0045(3) 0.19903(14) 0.0414(7) Uani 1 1 d . . . . .
F43 F -0.1377(3) 0.3948(4) 0.14386(14) 0.0989(11) Uani 1 1 d . . . . .
F46 F -0.1258(4) 0.5656(4) 0.05013(13) 0.1052(12) Uani 1 1 d . . . . .
F45 F 0.0039(4) 0.7275(3) 0.06514(14) 0.1092(12) Uani 1 1 d . . . . .
C20 C 0.6016(4) 0.1022(3) 0.23061(16) 0.0371(8) Uani 1 1 d . . . . .
C21 C 0.3551(4) 0.3816(3) 0.30797(16) 0.0391(8) Uani 1 1 d . . . . .
C25 C 0.0436(4) 0.5330(3) 0.34141(16) 0.0391(8) Uani 1 1 d . . . . .
C18 C 0.8012(4) -0.0520(4) 0.22726(18) 0.0481(9) Uani 1 1 d . . . . .
H18 H 0.8737 -0.1221 0.2130 0.058 Uiso 1 1 calc R U . . .
C26 C 0.0495(4) 0.4290(4) 0.37941(17) 0.0415(9) Uani 1 1 d . . . . .
C8 C 0.4378(4) 0.3019(4) 0.16460(17) 0.0475(9) Uani 1 1 d . . . . .
C17 C 0.7993(4) 0.0094(4) 0.27752(18) 0.0458(9) Uani 1 1 d . . . . .
H17 H 0.8683 -0.0090 0.3061 0.055 Uiso 1 1 calc R U . . .
C36 C 0.0584(4) 0.5542(4) 0.21516(18) 0.0487(10) Uani 1 1 d . . . . .
C1 C 0.3289(4) 0.1581(4) 0.22030(17) 0.0419(9) Uani 1 1 d . . . . .
C30 C -0.0562(4) 0.6410(4) 0.36071(17) 0.0476(9) Uani 1 1 d . . . . .
C27 C -0.0347(4) 0.4310(4) 0.43296(17) 0.0452(9) Uani 1 1 d . . . . .
C29 C -0.1414(4) 0.6470(4) 0.41257(19) 0.0519(10) Uani 1 1 d . . . . .
C3 C 0.3293(4) 0.2947(4) 0.13194(18) 0.0530(10) Uani 1 1 d . . . . .
C63 C 0.5607(4) 0.1215(4) 0.40280(17) 0.0481(9) Uani 1 1 d . . . . .
C28 C -0.1312(4) 0.5408(4) 0.44870(18) 0.0511(10) Uani 1 1 d . . . . .
C47 C 0.6466(4) -0.0397(4) 0.14269(18) 0.0477(9) Uani 1 1 d . . . . .
C2 C 0.2688(4) 0.2067(4) 0.16407(19) 0.0520(10) Uani 1 1 d . . . . .
C59 C 0.6878(4) 0.3148(4) 0.3422(2) 0.0510(10) Uani 1 1 d . . . . .
C37 C -0.0082(4) 0.4732(4) 0.20452(18) 0.0549(11) Uani 1 1 d . . . . .
C48 C 0.5854(4) -0.1320(4) 0.1501(2) 0.0558(11) Uani 1 1 d . . . . .
C10 C 0.2719(4) 0.0837(4) 0.2582(2) 0.0519(10) Uani 1 1 d . . . . .
H10 H 0.3107 0.0493 0.2965 0.062 Uiso 1 1 calc R U . . .
C64 C 0.6919(4) 0.0620(4) 0.43798(19) 0.0553(10) Uani 1 1 d . . . . .
H64A H 0.7644 0.0125 0.4097 0.083 Uiso 1 1 calc R U . . .
H64B H 0.6759 0.0079 0.4729 0.083 Uiso 1 1 calc R U . . .
H64C H 0.7185 0.1278 0.4537 0.083 Uiso 1 1 calc R U . . .
C41 C 0.0582(5) 0.6395(4) 0.1674(2) 0.0600(11) Uani 1 1 d . . . . .
C52 C 0.6880(5) 0.0043(4) 0.0862(2) 0.0606(12) Uani 1 1 d . . . . .
C40 C -0.0011(6) 0.6457(5) 0.1112(2) 0.0714(15) Uani 1 1 d . . . . .
C38 C -0.0724(5) 0.4772(5) 0.1502(2) 0.0697(14) Uani 1 1 d . . . . .
C65 C 0.4486(5) 0.2021(5) 0.44621(19) 0.0622(12) Uani 1 1 d . . . . .
H65A H 0.4719 0.2736 0.4569 0.093 Uiso 1 1 calc R U . . .
H65B H 0.4388 0.1526 0.4841 0.093 Uiso 1 1 calc R U . . .
H65C H 0.3631 0.2318 0.4254 0.093 Uiso 1 1 calc R U . . .
C60 C 0.8404(4) 0.2348(4) 0.3419(2) 0.0567(11) Uani 1 1 d . . . . .
H60A H 0.8545 0.1677 0.3744 0.085 Uiso 1 1 calc R U . . .
H60B H 0.8930 0.2875 0.3498 0.085 Uiso 1 1 calc R U . . .
H60C H 0.8701 0.1988 0.3014 0.085 Uiso 1 1 calc R U . . .
C7 C 0.4995(5) 0.3867(4) 0.1434(2) 0.0643(12) Uani 1 1 d . . . . .
H7 H 0.5725 0.3926 0.1645 0.077 Uiso 1 1 calc R U . . .
C39 C -0.0670(5) 0.5621(6) 0.1040(2) 0.0711(14) Uani 1 1 d . . . . .
C53 C 0.5442(5) -0.1795(4) 0.2133(2) 0.0621(12) Uani 1 1 d . . . . .
H53 H 0.5170 -0.1086 0.2414 0.075 Uiso 1 1 calc R U . . .
C13 C 0.1588(5) 0.1771(5) 0.1462(2) 0.0746(15) Uani 1 1 d . . . . .
H13 H 0.1205 0.2078 0.1074 0.090 Uiso 1 1 calc R U . . .
C4 C 0.2865(6) 0.3699(5) 0.0788(2) 0.0680(13) Uani 1 1 d . . . . .
H4 H 0.2157 0.3626 0.0565 0.082 Uiso 1 1 calc R U . . .
B9 B 0.4531(4) 0.2085(4) 0.22611(19) 0.0384(9) Uani 1 1 d . . . . .
C66 C 0.5157(5) 0.0171(5) 0.3818(2) 0.0634(12) Uani 1 1 d . . . . .
H66A H 0.4344 0.0539 0.3582 0.095 Uiso 1 1 calc R U . . .
H66B H 0.4958 -0.0313 0.4182 0.095 Uiso 1 1 calc R U . . .
H66C H 0.5884 -0.0376 0.3554 0.095 Uiso 1 1 calc R U . . .
C62 C 0.6657(5) 0.4075(4) 0.2870(3) 0.0715(14) Uani 1 1 d . . . . .
H62A H 0.6895 0.3628 0.2486 0.107 Uiso 1 1 calc R U . . .
H62B H 0.7228 0.4588 0.2891 0.107 Uiso 1 1 calc R U . . .
H62C H 0.5704 0.4611 0.2877 0.107 Uiso 1 1 calc R U . . .
C61 C 0.6467(5) 0.3834(5) 0.4035(3) 0.0739(15) Uani 1 1 d . . . . .
H61A H 0.5483 0.4246 0.4069 0.111 Uiso 1 1 calc R U . . .
H61B H 0.6911 0.4459 0.4036 0.111 Uiso 1 1 calc R U . . .
H61C H 0.6747 0.3231 0.4388 0.111 Uiso 1 1 calc R U . . .
C56 C 0.7572(6) 0.1010(5) 0.0801(2) 0.0744(15) Uani 1 1 d . . . . .
H56 H 0.7368 0.1461 0.1194 0.089 Uiso 1 1 calc R U . . .
C51 C 0.6683(6) -0.0491(5) 0.0332(2) 0.0740(14) Uani 1 1 d . . . . .
H51 H 0.6948 -0.0217 -0.0067 0.089 Uiso 1 1 calc R U . . .
C50 C 0.6108(6) -0.1411(5) 0.0387(3) 0.0801(16) Uani 1 1 d . . . . .
H50 H 0.5999 -0.1777 0.0024 0.096 Uiso 1 1 calc R U . . .
C11 C 0.1596(5) 0.0579(5) 0.2419(3) 0.0712(14) Uani 1 1 d . . . . .
H11 H 0.1202 0.0096 0.2696 0.085 Uiso 1 1 calc R U . . .
B23 B 0.1395(4) 0.5395(4) 0.2779(2) 0.0433(10) Uani 1 1 d . . . . .
H23 H 0.1742 0.6104 0.2791 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3487(7) 0.4549(5) 0.0592(2) 0.0835(17) Uani 1 1 d . . . . .
H5 H 0.3188 0.5081 0.0234 0.100 Uiso 1 1 calc R U . . .
C49 C 0.5690(6) -0.1810(5) 0.0957(3) 0.0733(14) Uani 1 1 d . . . . .
H49 H 0.5280 -0.2434 0.0980 0.088 Uiso 1 1 calc R U . . .
C12 C 0.1072(6) 0.1020(6) 0.1864(3) 0.0844(17) Uani 1 1 d . . . . .
H12 H 0.0331 0.0810 0.1746 0.101 Uiso 1 1 calc R U . . .
C55 C 0.6627(6) -0.2850(4) 0.2420(3) 0.0763(15) Uani 1 1 d . . . . .
H55A H 0.6915 -0.3563 0.2155 0.114 Uiso 1 1 calc R U . . .
H55B H 0.6333 -0.3106 0.2834 0.114 Uiso 1 1 calc R U . . .
H55C H 0.7385 -0.2552 0.2454 0.114 Uiso 1 1 calc R U . . .
C6 C 0.4544(7) 0.4647(5) 0.0904(3) 0.0837(17) Uani 1 1 d . . . . .
H6 H 0.4961 0.5240 0.0759 0.100 Uiso 1 1 calc R U . . .
C54 C 0.4224(6) -0.2241(5) 0.2118(3) 0.0858(17) Uani 1 1 d . . . . .
H54A H 0.3506 -0.1610 0.1893 0.129 Uiso 1 1 calc R U . . .
H54B H 0.3885 -0.2371 0.2543 0.129 Uiso 1 1 calc R U . . .
H54C H 0.4505 -0.3026 0.1907 0.129 Uiso 1 1 calc R U . . .
C68 C 0.2390(6) 0.7247(5) 0.3991(3) 0.0854(17) Uani 1 1 d D . . . .
H68A H 0.2312 0.7086 0.3555 0.102 Uiso 0.54(5) 1 calc R U P A 1
H68B H 0.2252 0.6554 0.4258 0.102 Uiso 0.54(5) 1 calc R U P A 1
H68C H 0.2165 0.6687 0.4319 0.102 Uiso 0.46(5) 1 calc R U P A 2
H68D H 0.2352 0.6927 0.3583 0.102 Uiso 0.46(5) 1 calc R U P A 2
C58 C 0.9130(6) 0.0315(7) 0.0733(3) 0.101(2) Uani 1 1 d . . . . .
H58A H 0.9423 -0.0233 0.1103 0.152 Uiso 1 1 calc R U . . .
H58B H 0.9599 0.0926 0.0687 0.152 Uiso 1 1 calc R U . . .
H58C H 0.9347 -0.0183 0.0365 0.152 Uiso 1 1 calc R U . . .
C57 C 0.7099(8) 0.1969(6) 0.0263(2) 0.101(2) Uani 1 1 d . . . . .
H57A H 0.7368 0.1558 -0.0130 0.152 Uiso 1 1 calc R U . . .
H57B H 0.7513 0.2614 0.0274 0.152 Uiso 1 1 calc R U . . .
H57C H 0.6112 0.2353 0.0302 0.152 Uiso 1 1 calc R U . . .
Cl2A Cl 0.1216(18) 0.8766(17) 0.4044(17) 0.166(5) Uani 0.46(5) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P15 N16 1.720(3) . ?
P15 N14 1.642(3) . ?
P15 C63 1.844(4) . ?
P15 C59 1.846(4) . ?
Cl1 C68 1.750(6) . ?
Cl2 C68 1.715(9) . ?
F35 C26 1.356(4) . ?
F34 C30 1.351(5) . ?
F33 C27 1.342(5) . ?
O25 C21 1.291(4) . ?
O25 B23 1.518(5) . ?
F32 C28 1.352(4) . ?
O24 C21 1.227(4) . ?
F42 C37 1.354(5) . ?
F31 C29 1.354(5) . ?
F44 C41 1.349(6) . ?
N16 C20 1.368(4) . ?
N16 C17 1.407(5) . ?
N14 C21 1.397(5) . ?
N14 B9 1.608(5) . ?
N19 C20 1.333(4) . ?
N19 C18 1.401(5) . ?
N19 C47 1.460(5) . ?
F43 C38 1.365(6) . ?
F46 C39 1.355(5) . ?
F45 C40 1.324(6) . ?
C20 B9 1.624(6) . ?
C25 C26 1.380(5) . ?
C25 C30 1.386(5) . ?
C25 B23 1.652(6) . ?
C18 H18 0.9500 . ?
C18 C17 1.335(5) . ?
C26 C27 1.398(5) . ?
C8 C3 1.420(6) . ?
C8 C7 1.377(6) . ?
C8 B9 1.624(6) . ?
C17 H17 0.9500 . ?
C36 C37 1.381(6) . ?
C36 C41 1.367(6) . ?
C36 B23 1.630(6) . ?
C1 C2 1.403(6) . ?
C1 C10 1.388(6) . ?
C1 B9 1.618(5) . ?
C30 C29 1.370(6) . ?
C27 C28 1.364(6) . ?
C29 C28 1.370(6) . ?
C3 C2 1.471(6) . ?
C3 C4 1.390(6) . ?
C63 C64 1.549(6) . ?
C63 C65 1.528(6) . ?
C63 C66 1.538(6) . ?
C47 C48 1.408(6) . ?
C47 C52 1.383(6) . ?
C2 C13 1.405(6) . ?
C59 C60 1.553(6) . ?
C59 C62 1.511(7) . ?
C59 C61 1.549(6) . ?
C37 C38 1.393(6) . ?
C48 C53 1.518(7) . ?
C48 C49 1.389(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.391(6) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C41 C40 1.398(7) . ?
C52 C56 1.513(7) . ?
C52 C51 1.401(6) . ?
C40 C39 1.384(8) . ?
C38 C39 1.352(7) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C7 H7 0.9500 . ?
C7 C6 1.406(7) . ?
C53 H53 1.0000 . ?
C53 C55 1.541(7) . ?
C53 C54 1.539(6) . ?
C13 H13 0.9500 . ?
C13 C12 1.386(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(8) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C56 H56 1.0000 . ?
C56 C58 1.559(8) . ?
C56 C57 1.526(8) . ?
C51 H51 0.9500 . ?
C51 C50 1.378(8) . ?
C50 H50 0.9500 . ?
C50 C49 1.375(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.351(8) . ?
B23 H23 1.0000 . ?
C5 H5 0.9500 . ?
C5 C6 1.388(9) . ?
C49 H49 0.9500 . ?
C12 H12 0.9500 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C6 H6 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 H68C 0.9900 . ?
C68 H68D 0.9900 . ?
C68 Cl2A 1.759(12) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 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
N16 P15 C63 105.08(17) . . ?
N16 P15 C59 107.49(17) . . ?
N14 P15 N16 92.67(14) . . ?
N14 P15 C63 114.76(17) . . ?
N14 P15 C59 117.73(17) . . ?
C63 P15 C59 115.26(19) . . ?
C21 O25 B23 122.6(3) . . ?
C20 N16 P15 114.7(2) . . ?
C20 N16 C17 109.9(3) . . ?
C17 N16 P15 134.8(3) . . ?
C21 N14 P15 117.1(2) . . ?
C21 N14 B9 122.8(3) . . ?
B9 N14 P15 119.8(2) . . ?
C20 N19 C18 109.6(3) . . ?
C20 N19 C47 127.7(3) . . ?
C18 N19 C47 122.8(3) . . ?
N16 C20 B9 116.2(3) . . ?
N19 C20 N16 106.3(3) . . ?
N19 C20 B9 137.5(3) . . ?
O25 C21 N14 111.9(3) . . ?
O24 C21 O25 127.7(3) . . ?
O24 C21 N14 120.5(3) . . ?
C26 C25 C30 113.5(3) . . ?
C26 C25 B23 127.1(3) . . ?
C30 C25 B23 119.3(3) . . ?
N19 C18 H18 125.8 . . ?
C17 C18 N19 108.5(3) . . ?
C17 C18 H18 125.8 . . ?
F35 C26 C25 121.3(3) . . ?
F35 C26 C27 114.8(3) . . ?
C25 C26 C27 123.9(3) . . ?
C3 C8 B9 107.8(3) . . ?
C7 C8 C3 118.9(4) . . ?
C7 C8 B9 133.1(4) . . ?
N16 C17 H17 127.1 . . ?
C18 C17 N16 105.7(3) . . ?
C18 C17 H17 127.1 . . ?
C37 C36 B23 121.5(4) . . ?
C41 C36 C37 114.6(4) . . ?
C41 C36 B23 123.8(4) . . ?
C2 C1 B9 108.5(3) . . ?
C10 C1 C2 117.2(4) . . ?
C10 C1 B9 134.3(3) . . ?
F34 C30 C25 118.7(3) . . ?
F34 C30 C29 116.8(4) . . ?
C29 C30 C25 124.5(4) . . ?
F33 C27 C26 120.7(4) . . ?
F33 C27 C28 120.1(4) . . ?
C28 C27 C26 119.2(4) . . ?
F31 C29 C30 120.7(4) . . ?
F31 C29 C28 119.7(4) . . ?
C30 C29 C28 119.6(4) . . ?
C8 C3 C2 111.2(4) . . ?
C4 C3 C8 121.3(4) . . ?
C4 C3 C2 127.4(4) . . ?
C64 C63 P15 112.1(3) . . ?
C65 C63 P15 110.3(3) . . ?
C65 C63 C64 109.6(3) . . ?
C65 C63 C66 108.5(4) . . ?
C66 C63 P15 107.3(3) . . ?
C66 C63 C64 108.9(4) . . ?
F32 C28 C27 120.1(4) . . ?
F32 C28 C29 120.6(4) . . ?
C27 C28 C29 119.3(4) . . ?
C48 C47 N19 117.1(4) . . ?
C52 C47 N19 118.0(4) . . ?
C52 C47 C48 124.6(4) . . ?
C1 C2 C3 111.4(3) . . ?
C1 C2 C13 121.0(4) . . ?
C13 C2 C3 127.4(4) . . ?
C60 C59 P15 109.9(3) . . ?
C62 C59 P15 107.2(3) . . ?
C62 C59 C60 108.6(4) . . ?
C62 C59 C61 110.4(4) . . ?
C61 C59 P15 111.9(3) . . ?
C61 C59 C60 108.8(3) . . ?
F42 C37 C36 120.0(3) . . ?
F42 C37 C38 116.2(4) . . ?
C36 C37 C38 123.8(4) . . ?
C47 C48 C53 122.8(4) . . ?
C49 C48 C47 115.7(4) . . ?
C49 C48 C53 121.5(4) . . ?
C1 C10 H10 119.0 . . ?
C1 C10 C11 122.0(4) . . ?
C11 C10 H10 119.0 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
F44 C41 C36 121.1(4) . . ?
F44 C41 C40 114.7(4) . . ?
C36 C41 C40 124.2(5) . . ?
C47 C52 C56 123.1(4) . . ?
C47 C52 C51 116.7(4) . . ?
C51 C52 C56 120.2(4) . . ?
F45 C40 C41 122.5(6) . . ?
F45 C40 C39 119.5(5) . . ?
C39 C40 C41 118.0(4) . . ?
F43 C38 C37 120.0(5) . . ?
C39 C38 F43 121.0(4) . . ?
C39 C38 C37 119.0(5) . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C8 C7 H7 120.1 . . ?
C8 C7 C6 119.9(5) . . ?
C6 C7 H7 120.1 . . ?
F46 C39 C40 119.5(5) . . ?
C38 C39 F46 120.0(5) . . ?
C38 C39 C40 120.4(4) . . ?
C48 C53 H53 107.5 . . ?
C48 C53 C55 111.9(4) . . ?
C48 C53 C54 113.0(4) . . ?
C55 C53 H53 107.5 . . ?
C54 C53 H53 107.5 . . ?
C54 C53 C55 109.3(4) . . ?
C2 C13 H13 120.7 . . ?
C12 C13 C2 118.5(5) . . ?
C12 C13 H13 120.7 . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.6(5) . . ?
C5 C4 H4 120.7 . . ?
N14 B9 C20 96.2(3) . . ?
N14 B9 C8 114.5(3) . . ?
N14 B9 C1 116.3(3) . . ?
C20 B9 C8 114.1(3) . . ?
C1 B9 C20 115.7(3) . . ?
C1 B9 C8 100.8(3) . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C52 C56 H56 108.1 . . ?
C52 C56 C58 108.1(5) . . ?
C52 C56 C57 113.4(5) . . ?
C58 C56 H56 108.1 . . ?
C57 C56 H56 108.1 . . ?
C57 C56 C58 111.0(5) . . ?
C52 C51 H51 119.8 . . ?
C50 C51 C52 120.4(5) . . ?
C50 C51 H51 119.8 . . ?
C51 C50 H50 119.4 . . ?
C49 C50 C51 121.2(5) . . ?
C49 C50 H50 119.4 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.4(5) . . ?
C12 C11 H11 120.3 . . ?
O25 B23 C25 111.3(3) . . ?
O25 B23 C36 103.8(3) . . ?
O25 B23 H23 109.9 . . ?
C25 B23 H23 109.9 . . ?
C36 B23 C25 112.0(3) . . ?
C36 B23 H23 109.9 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.4(5) . . ?
C6 C5 H5 119.3 . . ?
C48 C49 H49 119.3 . . ?
C50 C49 C48 121.5(5) . . ?
C50 C49 H49 119.3 . . ?
C13 C12 H12 119.2 . . ?
C11 C12 C13 121.7(4) . . ?
C11 C12 H12 119.2 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 C7 119.9(5) . . ?
C5 C6 H6 120.0 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
Cl1 C68 H68A 109.0 . . ?
Cl1 C68 H68B 109.0 . . ?
Cl1 C68 H68C 109.8 . . ?
Cl1 C68 H68D 109.8 . . ?
Cl1 C68 Cl2A 109.3(7) . . ?
Cl2 C68 Cl1 112.8(4) . . ?
Cl2 C68 H68A 109.0 . . ?
Cl2 C68 H68B 109.0 . . ?
H68A C68 H68B 107.8 . . ?
H68C C68 H68D 108.3 . . ?
Cl2A C68 H68C 109.8 . . ?
Cl2A C68 H68D 109.8 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P15 N16 C20 N19 -172.2(2) . . . . ?
P15 N16 C20 B9 7.3(4) . . . . ?
P15 N16 C17 C18 170.9(3) . . . . ?
P15 N14 C21 O25 179.3(2) . . . . ?
P15 N14 C21 O24 -0.8(5) . . . . ?
P15 N14 B9 C20 -0.5(3) . . . . ?
P15 N14 B9 C8 -120.6(3) . . . . ?
P15 N14 B9 C1 122.3(3) . . . . ?
F35 C26 C27 F33 0.2(5) . . . . ?
F35 C26 C27 C28 -178.1(3) . . . . ?
F34 C30 C29 F31 1.0(6) . . . . ?
F34 C30 C29 C28 -179.7(3) . . . . ?
F33 C27 C28 F32 0.5(5) . . . . ?
F33 C27 C28 C29 -179.9(3) . . . . ?
F42 C37 C38 F43 0.6(6) . . . . ?
F42 C37 C38 C39 -178.3(4) . . . . ?
F31 C29 C28 F32 0.0(6) . . . . ?
F31 C29 C28 C27 -179.6(3) . . . . ?
F44 C41 C40 F45 1.1(7) . . . . ?
F44 C41 C40 C39 -179.1(4) . . . . ?
N16 P15 N14 C21 -169.6(3) . . . . ?
N16 P15 N14 B9 3.7(3) . . . . ?
N16 P15 C63 C64 75.1(3) . . . . ?
N16 P15 C63 C65 -162.5(3) . . . . ?
N16 P15 C63 C66 -44.4(3) . . . . ?
N16 P15 C59 C60 -39.4(3) . . . . ?
N16 P15 C59 C62 78.5(3) . . . . ?
N16 P15 C59 C61 -160.3(3) . . . . ?
N16 C20 B9 N14 -4.2(4) . . . . ?
N16 C20 B9 C8 116.3(3) . . . . ?
N16 C20 B9 C1 -127.3(3) . . . . ?
N14 P15 N16 C20 -6.3(3) . . . . ?
N14 P15 N16 C17 -176.0(3) . . . . ?
N14 P15 C63 C64 175.3(3) . . . . ?
N14 P15 C63 C65 -62.2(3) . . . . ?
N14 P15 C63 C66 55.8(3) . . . . ?
N14 P15 C59 C60 -142.1(3) . . . . ?
N14 P15 C59 C62 -24.2(4) . . . . ?
N14 P15 C59 C61 96.9(3) . . . . ?
N19 C20 B9 N14 175.1(4) . . . . ?
N19 C20 B9 C8 -64.5(5) . . . . ?
N19 C20 B9 C1 51.9(6) . . . . ?
N19 C18 C17 N16 -1.3(4) . . . . ?
N19 C47 C48 C53 3.9(6) . . . . ?
N19 C47 C48 C49 -173.8(4) . . . . ?
N19 C47 C52 C56 -3.5(7) . . . . ?
N19 C47 C52 C51 173.8(4) . . . . ?
F43 C38 C39 F46 -0.6(7) . . . . ?
F43 C38 C39 C40 179.6(4) . . . . ?
F45 C40 C39 F46 -0.3(7) . . . . ?
F45 C40 C39 C38 179.5(4) . . . . ?
C20 N16 C17 C18 0.8(4) . . . . ?
C20 N19 C18 C17 1.5(4) . . . . ?
C20 N19 C47 C48 -92.9(5) . . . . ?
C20 N19 C47 C52 92.0(5) . . . . ?
C21 O25 B23 C25 -67.8(4) . . . . ?
C21 O25 B23 C36 171.5(3) . . . . ?
C21 N14 B9 C20 172.3(3) . . . . ?
C21 N14 B9 C8 52.2(4) . . . . ?
C21 N14 B9 C1 -64.9(5) . . . . ?
C25 C26 C27 F33 179.9(3) . . . . ?
C25 C26 C27 C28 1.6(6) . . . . ?
C25 C30 C29 F31 -179.9(3) . . . . ?
C25 C30 C29 C28 -0.7(6) . . . . ?
C18 N19 C20 N16 -0.9(4) . . . . ?
C18 N19 C20 B9 179.7(4) . . . . ?
C18 N19 C47 C48 88.7(5) . . . . ?
C18 N19 C47 C52 -86.4(5) . . . . ?
C26 C25 C30 F34 179.6(3) . . . . ?
C26 C25 C30 C29 0.6(6) . . . . ?
C26 C25 B23 O25 -10.5(5) . . . . ?
C26 C25 B23 C36 105.2(4) . . . . ?
C26 C27 C28 F32 178.8(3) . . . . ?
C26 C27 C28 C29 -1.6(6) . . . . ?
C8 C3 C2 C1 3.3(5) . . . . ?
C8 C3 C2 C13 178.9(4) . . . . ?
C8 C3 C4 C5 -2.0(7) . . . . ?
C8 C7 C6 C5 -0.7(8) . . . . ?
C17 N16 C20 N19 0.1(4) . . . . ?
C17 N16 C20 B9 179.6(3) . . . . ?
C36 C37 C38 F43 -179.0(4) . . . . ?
C36 C37 C38 C39 2.0(7) . . . . ?
C36 C41 C40 F45 -178.1(4) . . . . ?
C36 C41 C40 C39 1.8(7) . . . . ?
C1 C2 C13 C12 2.3(7) . . . . ?
C1 C10 C11 C12 2.8(8) . . . . ?
C30 C25 C26 F35 178.6(3) . . . . ?
C30 C25 C26 C27 -1.1(5) . . . . ?
C30 C25 B23 O25 170.0(3) . . . . ?
C30 C25 B23 C36 -74.3(4) . . . . ?
C30 C29 C28 F32 -179.2(4) . . . . ?
C30 C29 C28 C27 1.1(6) . . . . ?
C3 C8 C7 C6 0.3(6) . . . . ?
C3 C8 B9 N14 -128.2(3) . . . . ?
C3 C8 B9 C20 122.2(3) . . . . ?
C3 C8 B9 C1 -2.5(4) . . . . ?
C3 C2 C13 C12 -172.9(5) . . . . ?
C3 C4 C5 C6 1.5(8) . . . . ?
C63 P15 N16 C20 110.2(3) . . . . ?
C63 P15 N16 C17 -59.5(4) . . . . ?
C63 P15 N14 C21 82.5(3) . . . . ?
C63 P15 N14 B9 -104.3(3) . . . . ?
C63 P15 C59 C60 77.4(4) . . . . ?
C63 P15 C59 C62 -164.7(3) . . . . ?
C63 P15 C59 C61 -43.6(4) . . . . ?
C47 N19 C20 N16 -179.4(3) . . . . ?
C47 N19 C20 B9 1.2(7) . . . . ?
C47 N19 C18 C17 -179.9(3) . . . . ?
C47 C48 C53 C55 -85.4(5) . . . . ?
C47 C48 C53 C54 150.8(4) . . . . ?
C47 C48 C49 C50 0.2(7) . . . . ?
C47 C52 C56 C58 96.7(5) . . . . ?
C47 C52 C56 C57 -139.8(5) . . . . ?
C47 C52 C51 C50 -0.3(8) . . . . ?
C2 C1 C10 C11 -0.2(6) . . . . ?
C2 C1 B9 N14 129.0(4) . . . . ?
C2 C1 B9 C20 -119.1(4) . . . . ?
C2 C1 B9 C8 4.5(4) . . . . ?
C2 C3 C4 C5 173.8(4) . . . . ?
C2 C13 C12 C11 0.3(9) . . . . ?
C59 P15 N16 C20 -126.5(3) . . . . ?
C59 P15 N16 C17 63.8(4) . . . . ?
C59 P15 N14 C21 -58.2(3) . . . . ?
C59 P15 N14 B9 115.1(3) . . . . ?
C59 P15 C63 C64 -43.1(4) . . . . ?
C59 P15 C63 C65 79.4(3) . . . . ?
C59 P15 C63 C66 -162.5(3) . . . . ?
C37 C36 C41 F44 179.7(4) . . . . ?
C37 C36 C41 C40 -1.2(6) . . . . ?
C37 C36 B23 O25 67.4(4) . . . . ?
C37 C36 B23 C25 -52.8(5) . . . . ?
C37 C38 C39 F46 178.3(4) . . . . ?
C37 C38 C39 C40 -1.4(7) . . . . ?
C48 C47 C52 C56 -178.2(5) . . . . ?
C48 C47 C52 C51 -0.9(7) . . . . ?
C10 C1 C2 C3 173.6(3) . . . . ?
C10 C1 C2 C13 -2.3(6) . . . . ?
C10 C1 B9 N14 -49.3(6) . . . . ?
C10 C1 B9 C20 62.6(6) . . . . ?
C10 C1 B9 C8 -173.7(4) . . . . ?
C10 C11 C12 C13 -2.8(9) . . . . ?
C41 C36 C37 F42 179.7(4) . . . . ?
C41 C36 C37 C38 -0.7(6) . . . . ?
C41 C36 B23 O25 -107.7(4) . . . . ?
C41 C36 B23 C25 132.2(4) . . . . ?
C41 C40 C39 F46 179.9(4) . . . . ?
C41 C40 C39 C38 -0.3(7) . . . . ?
C52 C47 C48 C53 178.7(4) . . . . ?
C52 C47 C48 C49 0.9(7) . . . . ?
C52 C51 C50 C49 1.3(9) . . . . ?
C7 C8 C3 C2 -175.3(4) . . . . ?
C7 C8 C3 C4 1.1(6) . . . . ?
C7 C8 B9 N14 46.0(6) . . . . ?
C7 C8 B9 C20 -63.5(6) . . . . ?
C7 C8 B9 C1 171.7(4) . . . . ?
C53 C48 C49 C50 -177.6(5) . . . . ?
C4 C3 C2 C1 -172.8(4) . . . . ?
C4 C3 C2 C13 2.7(7) . . . . ?
C4 C5 C6 C7 -0.2(8) . . . . ?
B9 N14 C21 O25 6.2(5) . . . . ?
B9 N14 C21 O24 -173.8(3) . . . . ?
B9 C8 C3 C2 -0.1(4) . . . . ?
B9 C8 C3 C4 176.3(4) . . . . ?
B9 C8 C7 C6 -173.5(4) . . . . ?
B9 C1 C2 C3 -5.0(4) . . . . ?
B9 C1 C2 C13 179.1(4) . . . . ?
B9 C1 C10 C11 177.9(4) . . . . ?
C56 C52 C51 C50 177.1(5) . . . . ?
C51 C52 C56 C58 -80.5(6) . . . . ?
C51 C52 C56 C57 43.0(7) . . . . ?
C51 C50 C49 C48 -1.3(9) . . . . ?
B23 O25 C21 O24 3.4(6) . . . . ?
B23 O25 C21 N14 -176.7(3) . . . . ?
B23 C25 C26 F35 -0.9(5) . . . . ?
B23 C25 C26 C27 179.4(3) . . . . ?
B23 C25 C30 F34 -0.8(5) . . . . ?
B23 C25 C30 C29 -179.8(4) . . . . ?
B23 C36 C37 F42 4.2(6) . . . . ?
B23 C36 C37 C38 -176.2(4) . . . . ?
B23 C36 C41 F44 -4.9(6) . . . . ?
B23 C36 C41 C40 174.2(4) . . . . ?
C49 C48 C53 C55 92.3(5) . . . . ?
C49 C48 C53 C54 -31.6(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.412
_oxdiff_exptl_absorpt_empirical_full_min 0.462
####################################################################### 
# 
# 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_SN2024_compound_6b
_audit_block_doi                 10.5517/ccdc.csd.cc2kv6k6
_database_code_depnum_ccdc_archive 'CCDC 2378678'
loop_
_audit_author_name
_audit_author_address
'Yoichi Hoshimoto'
;Osaka University
Japan
;
_audit_update_record             
;
2024-08-20 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_audit_creation_date             2022-03-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H50 B N4 O P, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H54 B Cl4 N4 O P'
_chemical_formula_weight         838.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42 H51 B1  N4 O1 P1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.90590(10)
_cell_length_b                   19.1588(2)
_cell_length_c                   23.6340(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.5180(10)
_cell_angle_gamma                90
_cell_volume                     4476.93(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18949
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      74.0100
_cell_measurement_theta_min      3.7470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34450
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.748
_diffrn_ambient_temperature      193.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -90.00   0.50    0.20    --  -42.93-134.00  -8.00   50
  2  ω     42.00  67.00   0.50    0.20    --   42.93-135.00 172.00   50
  3  ω     66.00  91.00   0.50    0.20    --   42.93 135.00-121.00   50
  4  ω     66.00 114.00   0.50    0.20    --   42.93 134.00  59.00   96
  5  ω     44.00  70.00   0.50    0.20    --   42.93-134.00  -8.00   52
  6  ω     19.00  98.00   0.50    1.00    --   76.50-135.00 172.00  158
  7  ω     77.00 147.00   0.50    1.00    --   76.50 134.00  59.00  140
  8  ω   -123.00 -37.00   0.50    1.00    -- -106.00 135.00-121.00  172
  9  ω   -145.00-120.00   0.50    1.00    -- -106.00-135.00 172.00   50
 10  ω    -57.00 -32.00   0.50    1.00    -- -106.00 134.00  59.00   50
 11  ω   -103.00 -77.00   0.50    1.00    -- -106.00 134.00  59.00   52
 12  ω   -113.00 -14.00   0.50    0.20    --  -42.93 -77.00-120.00  198
 13  ω   -113.00 -78.00   0.50    0.20    --  -42.93-125.00  60.00   70
 14  ω     73.00 116.00   0.50    0.20    --   42.93 125.00   0.00   86
 15  ω     71.00 116.00   0.50    0.20    --   42.93 125.00-150.00   90
 16  ω     83.00 108.00   0.50    1.00    --   76.50 135.00-121.00   50
 17  ω   -117.00 -36.00   0.50    1.00    -- -106.00 125.00-150.00  162
 18  ω   -176.00 -83.00   0.50    1.00    -- -106.00 -19.00  60.00  186
 19  ω   -134.00-108.00   0.50    1.00    -- -106.00 -77.00 -90.00   52
 20  ω   -134.00 -86.00   0.50    1.00    -- -106.00 -37.00-120.00   96
 21  ω   -167.00-141.00   0.50    1.00    -- -106.00 -37.00-120.00   52
 22  ω   -134.00 -80.00   0.50    1.00    -- -106.00  77.00 -90.00  108
 23  ω   -117.00 -38.00   0.50    1.00    -- -106.00 125.00  60.00  158
 24  ω   -122.00 -33.00   0.50    1.00    -- -106.00  57.00  90.00  178
 25  ω   -122.00 -30.00   0.50    1.00    -- -106.00  37.00 120.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0660497000
_diffrn_orient_matrix_UB_12      0.0724489000
_diffrn_orient_matrix_UB_13      -0.0042374000
_diffrn_orient_matrix_UB_21      -0.1368154000
_diffrn_orient_matrix_UB_22      0.0348495000
_diffrn_orient_matrix_UB_23      0.0097518000
_diffrn_orient_matrix_UB_31      0.0348095000
_diffrn_orient_matrix_UB_32      -0.0004036000
_diffrn_orient_matrix_UB_33      0.0644292000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7328
_reflns_number_total             8160
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0548
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0822P)²+2.6552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1545
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C44(H44), C47(H47)
2.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C51(H51A,H51B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C40(H40), C18(H18), C12(H12), C4(H4), C7(H7), C10(H10), C41(H41),
 C19(H19), C42(H42), C11(H11), C25(H25), C6(H6), C29(H29), C5(H5), C28(H28),
 C27(H27), C26(H26)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C46(H46A,H46B,H46C), C31(H31A,H31B,
 H31C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C33(H33A,H33B,H33C), C32(H32A,
 H32B,H32C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P14 P 0.25047(6) 0.13366(2) 0.57099(2) 0.03750(15) Uani 1 1 d . . . . .
Cl4 Cl -0.06767(9) 0.32122(4) 0.34295(4) 0.0785(2) Uani 1 1 d . . . . .
Cl1 Cl 0.62046(13) 0.17409(5) 0.35996(5) 0.1046(3) Uani 1 1 d . . . . .
Cl2 Cl 0.53260(15) 0.30222(6) 0.30463(4) 0.1150(4) Uani 1 1 d . . . . .
Cl3 Cl 0.14906(13) 0.39012(7) 0.29029(6) 0.1212(4) Uani 1 1 d . . . . .
O21 O 0.20665(17) 0.10081(7) 0.50013(6) 0.0437(4) Uani 1 1 d . . . . .
N17 N 0.39182(17) 0.29969(8) 0.65458(6) 0.0330(3) Uani 1 1 d . . . . .
N15 N 0.29542(17) 0.19659(8) 0.52682(6) 0.0318(3) Uani 1 1 d . . . . .
N20 N 0.31021(19) 0.19801(8) 0.62885(7) 0.0379(4) Uani 1 1 d . . . . .
N23 N 0.24728(19) 0.18143(9) 0.42726(7) 0.0382(4) Uani 1 1 d . . . . .
C38 C 0.4457(2) 0.37018(10) 0.65422(7) 0.0330(4) Uani 1 1 d . . . . .
C1 C 0.26766(19) 0.33688(9) 0.51640(7) 0.0290(4) Uani 1 1 d . . . . .
C8 C 0.50057(19) 0.28855(11) 0.51695(7) 0.0333(4) Uani 1 1 d . . . . .
C16 C 0.35490(19) 0.25973(9) 0.60912(8) 0.0299(4) Uani 1 1 d . . . . .
C22 C 0.2506(2) 0.16177(10) 0.47820(8) 0.0337(4) Uani 1 1 d . . . . .
C2 C 0.3572(2) 0.38459(10) 0.49304(8) 0.0332(4) Uani 1 1 d . . . . .
C3 C 0.4943(2) 0.35603(11) 0.49292(8) 0.0356(4) Uani 1 1 d . . . . .
C39 C 0.3545(2) 0.42593(10) 0.65554(8) 0.0366(4) Uani 1 1 d . . . . .
C13 C 0.1317(2) 0.35364(11) 0.51296(9) 0.0375(4) Uani 1 1 d . . . . .
H13 H 0.0700 0.3231 0.5278 0.045 Uiso 1 1 calc R U . . .
C43 C 0.5860(2) 0.37900(12) 0.65598(8) 0.0404(5) Uani 1 1 d . . . . .
C40 C 0.4105(3) 0.49306(11) 0.65714(9) 0.0463(5) Uani 1 1 d . . . . .
H40 H 0.3534 0.5316 0.6578 0.056 Uiso 1 1 calc R U . . .
C24 C 0.1843(3) 0.13594(11) 0.38609(8) 0.0426(5) Uani 1 1 d . . . . .
C44 C 0.2034(2) 0.41583(12) 0.65768(9) 0.0439(5) Uani 1 1 d . . . . .
H44 H 0.1794 0.3720 0.6382 0.053 Uiso 1 1 calc R U . . .
C18 C 0.3716(3) 0.26239(11) 0.70365(8) 0.0461(5) Uani 1 1 d . . . . .
H18 H 0.3892 0.2779 0.7407 0.055 Uiso 1 1 calc R U . . .
C12 C 0.0854(2) 0.41575(12) 0.48750(10) 0.0494(5) Uani 1 1 d . . . . .
H12 H -0.0068 0.4255 0.4845 0.059 Uiso 1 1 calc R U . . .
C4 C 0.6048(2) 0.38602(14) 0.46809(10) 0.0489(5) Uani 1 1 d . . . . .
H4 H 0.5995 0.4313 0.4540 0.059 Uiso 1 1 calc R U . . .
C7 C 0.6206(2) 0.25165(14) 0.51315(9) 0.0472(5) Uani 1 1 d . . . . .
H7 H 0.6287 0.2072 0.5287 0.057 Uiso 1 1 calc R U . . .
C10 C 0.3122(3) 0.44786(11) 0.46945(9) 0.0437(5) Uani 1 1 d . . . . .
H10 H 0.3734 0.4795 0.4557 0.052 Uiso 1 1 calc R U . . .
C41 C 0.5470(3) 0.50320(12) 0.65773(10) 0.0525(6) Uani 1 1 d . . . . .
H41 H 0.5814 0.5484 0.6585 0.063 Uiso 1 1 calc R U . . .
C19 C 0.3220(3) 0.20013(11) 0.68787(9) 0.0480(6) Uani 1 1 d . . . . .
H19 H 0.2993 0.1643 0.7121 0.058 Uiso 1 1 calc R U . . .
C42 C 0.6340(3) 0.44730(14) 0.65725(10) 0.0505(6) Uani 1 1 d . . . . .
H42 H 0.7266 0.4553 0.6578 0.061 Uiso 1 1 calc R U . . .
C34 C 0.0713(3) 0.12261(12) 0.59136(10) 0.0508(6) Uani 1 1 d . . . . .
C11 C 0.1760(3) 0.46283(12) 0.46676(10) 0.0500(6) Uani 1 1 d . . . . .
H11 H 0.1448 0.5047 0.4509 0.060 Uiso 1 1 calc R U . . .
C30 C 0.3725(3) 0.06165(12) 0.59190(10) 0.0541(6) Uani 1 1 d . . . . .
B9 B 0.3540(2) 0.26982(10) 0.54118(8) 0.0282(4) Uani 1 1 d . . . . .
C25 C 0.2576(3) 0.08780(13) 0.35786(10) 0.0588(7) Uani 1 1 d . . . . .
H25 H 0.3496 0.0822 0.3669 0.071 Uiso 1 1 calc R U . . .
C6 C 0.7294(2) 0.28058(18) 0.48616(11) 0.0611(7) Uani 1 1 d . . . . .
H6 H 0.8076 0.2545 0.4826 0.073 Uiso 1 1 calc R U . . .
C29 C 0.0463(3) 0.14325(14) 0.37173(11) 0.0559(6) Uani 1 1 d . . . . .
H29 H -0.0038 0.1757 0.3908 0.067 Uiso 1 1 calc R U . . .
C5 C 0.7213(3) 0.34777(18) 0.46476(11) 0.0611(7) Uani 1 1 d . . . . .
H5 H 0.7952 0.3671 0.4480 0.073 Uiso 1 1 calc R U . . .
C47 C 0.6834(3) 0.31777(15) 0.65846(11) 0.0549(6) Uani 1 1 d . . . . .
H47 H 0.6374 0.2780 0.6397 0.066 Uiso 1 1 calc R U . . .
C35 C 0.0461(3) 0.13459(16) 0.65402(12) 0.0663(8) Uani 1 1 d . . . . .
H35A H 0.1012 0.1031 0.6771 0.099 Uiso 1 1 calc R U . . .
H35B H -0.0476 0.1263 0.6600 0.099 Uiso 1 1 calc R U . . .
H35C H 0.0688 0.1818 0.6642 0.099 Uiso 1 1 calc R U . . .
C36 C -0.0121(3) 0.17576(17) 0.55584(14) 0.0677(8) Uani 1 1 d . . . . .
H36A H 0.0183 0.2221 0.5655 0.102 Uiso 1 1 calc R U . . .
H36B H -0.1058 0.1712 0.5634 0.102 Uiso 1 1 calc R U . . .
H36C H -0.0011 0.1674 0.5163 0.102 Uiso 1 1 calc R U . . .
C54 C 0.5164(3) 0.24741(15) 0.36264(13) 0.0641(7) Uani 1 1 d . . . . .
H54A H 0.4230 0.2325 0.3635 0.077 Uiso 1 1 calc R U . . .
H54B H 0.5395 0.2731 0.3973 0.077 Uiso 1 1 calc R U . . .
C46 C 0.1219(3) 0.47428(15) 0.62782(13) 0.0646(7) Uani 1 1 d . . . . .
H46A H 0.1318 0.5164 0.6497 0.097 Uiso 1 1 calc R U . . .
H46B H 0.0282 0.4613 0.6241 0.097 Uiso 1 1 calc R U . . .
H46C H 0.1546 0.4819 0.5909 0.097 Uiso 1 1 calc R U . . .
C31 C 0.3623(4) 0.03782(15) 0.65359(11) 0.0725(9) Uani 1 1 d . . . . .
H31A H 0.3965 0.0739 0.6788 0.109 Uiso 1 1 calc R U . . .
H31B H 0.4147 -0.0039 0.6601 0.109 Uiso 1 1 calc R U . . .
H31C H 0.2695 0.0286 0.6604 0.109 Uiso 1 1 calc R U . . .
C28 C -0.0167(4) 0.10284(16) 0.32955(12) 0.0695(8) Uani 1 1 d . . . . .
H28 H -0.1088 0.1082 0.3203 0.083 Uiso 1 1 calc R U . . .
C27 C 0.0552(4) 0.05550(18) 0.30172(11) 0.0771(10) Uani 1 1 d . . . . .
H27 H 0.0121 0.0284 0.2734 0.093 Uiso 1 1 calc R U . . .
C37 C 0.0205(4) 0.04893(16) 0.57555(13) 0.0754(9) Uani 1 1 d . . . . .
H37A H 0.0348 0.0400 0.5364 0.113 Uiso 1 1 calc R U . . .
H37B H -0.0743 0.0456 0.5815 0.113 Uiso 1 1 calc R U . . .
H37C H 0.0692 0.0152 0.5989 0.113 Uiso 1 1 calc R U . . .
C45 C 0.1639(3) 0.4093(2) 0.71905(11) 0.0687(8) Uani 1 1 d . . . . .
H45A H 0.2087 0.3697 0.7365 0.103 Uiso 1 1 calc R U . . .
H45B H 0.0678 0.4034 0.7196 0.103 Uiso 1 1 calc R U . . .
H45C H 0.1906 0.4508 0.7396 0.103 Uiso 1 1 calc R U . . .
C26 C 0.1912(5) 0.04668(16) 0.31458(12) 0.0788(10) Uani 1 1 d . . . . .
H26 H 0.2396 0.0139 0.2950 0.095 Uiso 1 1 calc R U . . .
C33 C 0.5145(4) 0.08986(16) 0.58382(16) 0.0777(9) Uani 1 1 d . . . . .
H33A H 0.5215 0.1030 0.5449 0.117 Uiso 1 1 calc R U . . .
H33B H 0.5801 0.0544 0.5938 0.117 Uiso 1 1 calc R U . . .
H33C H 0.5310 0.1299 0.6077 0.117 Uiso 1 1 calc R U . . .
C32 C 0.3493(4) -0.00320(14) 0.55409(13) 0.0833(11) Uani 1 1 d . . . . .
H32A H 0.2624 -0.0230 0.5602 0.125 Uiso 1 1 calc R U . . .
H32B H 0.4186 -0.0371 0.5634 0.125 Uiso 1 1 calc R U . . .
H32C H 0.3526 0.0100 0.5150 0.125 Uiso 1 1 calc R U . . .
C49 C 0.8117(3) 0.3320(2) 0.62820(15) 0.0832(11) Uani 1 1 d . . . . .
H49A H 0.7882 0.3496 0.5908 0.125 Uiso 1 1 calc R U . . .
H49B H 0.8622 0.2895 0.6255 0.125 Uiso 1 1 calc R U . . .
H49C H 0.8656 0.3660 0.6492 0.125 Uiso 1 1 calc R U . . .
C48 C 0.7199(4) 0.2971(2) 0.72036(14) 0.0840(10) Uani 1 1 d . . . . .
H48A H 0.7695 0.3343 0.7392 0.126 Uiso 1 1 calc R U . . .
H48B H 0.7745 0.2556 0.7213 0.126 Uiso 1 1 calc R U . . .
H48C H 0.6386 0.2884 0.7393 0.126 Uiso 1 1 calc R U . . .
C51 C 0.1079(4) 0.3359(2) 0.34628(17) 0.0842(10) Uani 1 1 d . . . . .
H51A H 0.1360 0.3577 0.3821 0.101 Uiso 1 1 calc R U . . .
H51B H 0.1552 0.2918 0.3439 0.101 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
P14 O21 1.8165(14) . ?
P14 N15 1.6730(16) . ?
P14 N20 1.9081(17) . ?
P14 C22 2.258(2) . ?
P14 C34 1.879(3) . ?
P14 C30 1.880(2) . ?
Cl4 C51 1.759(4) . ?
Cl1 C54 1.746(3) . ?
Cl2 C54 1.742(3) . ?
Cl3 C51 1.750(4) . ?
O21 C22 1.360(2) . ?
N17 C38 1.452(2) . ?
N17 C16 1.351(2) . ?
N17 C18 1.387(3) . ?
N15 C22 1.378(2) . ?
N15 B9 1.548(3) . ?
N20 C16 1.355(2) . ?
N20 C19 1.393(3) . ?
N23 C22 1.260(3) . ?
N23 C24 1.421(3) . ?
C38 C39 1.400(3) . ?
C38 C43 1.398(3) . ?
C1 C2 1.410(3) . ?
C1 C13 1.382(3) . ?
C1 B9 1.632(3) . ?
C8 C3 1.412(3) . ?
C8 C7 1.391(3) . ?
C8 B9 1.633(3) . ?
C16 B9 1.617(3) . ?
C2 C3 1.464(3) . ?
C2 C10 1.396(3) . ?
C3 C4 1.397(3) . ?
C39 C40 1.400(3) . ?
C39 C44 1.514(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.398(3) . ?
C43 C42 1.392(3) . ?
C43 C47 1.518(3) . ?
C40 H40 0.9300 . ?
C40 C41 1.365(4) . ?
C24 C25 1.372(4) . ?
C24 C29 1.396(4) . ?
C44 H44 0.9800 . ?
C44 C46 1.527(3) . ?
C44 C45 1.530(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.334(3) . ?
C12 H12 0.9300 . ?
C12 C11 1.384(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.374(4) . ?
C7 H7 0.9300 . ?
C7 C6 1.400(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.377(4) . ?
C41 H41 0.9300 . ?
C41 C42 1.375(4) . ?
C19 H19 0.9300 . ?
C42 H42 0.9300 . ?
C34 C35 1.534(3) . ?
C34 C36 1.529(4) . ?
C34 C37 1.537(3) . ?
C11 H11 0.9300 . ?
C30 C31 1.537(3) . ?
C30 C33 1.530(5) . ?
C30 C32 1.539(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.420(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.384(4) . ?
C29 H29 0.9300 . ?
C29 C28 1.381(4) . ?
C5 H5 0.9300 . ?
C47 H47 0.9800 . ?
C47 C49 1.520(4) . ?
C47 C48 1.537(4) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C28 H28 0.9300 . ?
C28 C27 1.350(5) . ?
C27 H27 0.9300 . ?
C27 C26 1.373(5) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C26 H26 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?

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
O21 P14 N20 158.52(7) . . ?
O21 P14 C22 37.02(7) . . ?
O21 P14 C34 91.21(9) . . ?
O21 P14 C30 95.83(9) . . ?
N15 P14 O21 74.46(7) . . ?
N15 P14 N20 84.19(7) . . ?
N15 P14 C22 37.46(7) . . ?
N15 P14 C34 122.19(10) . . ?
N15 P14 C30 120.09(11) . . ?
N20 P14 C22 121.55(7) . . ?
C34 P14 N20 98.36(9) . . ?
C34 P14 C22 109.41(9) . . ?
C34 P14 C30 116.87(12) . . ?
C30 P14 N20 96.87(10) . . ?
C30 P14 C22 113.06(9) . . ?
C22 O21 P14 89.42(11) . . ?
C16 N17 C38 127.14(15) . . ?
C16 N17 C18 109.08(16) . . ?
C18 N17 C38 123.77(16) . . ?
C22 N15 P14 94.97(12) . . ?
C22 N15 B9 135.95(15) . . ?
B9 N15 P14 128.83(12) . . ?
C16 N20 P14 114.25(12) . . ?
C16 N20 C19 108.05(16) . . ?
C19 N20 P14 137.70(14) . . ?
C22 N23 C24 117.08(17) . . ?
C39 C38 N17 118.12(18) . . ?
C43 C38 N17 118.50(18) . . ?
C43 C38 C39 123.27(19) . . ?
C2 C1 B9 108.82(16) . . ?
C13 C1 C2 117.44(17) . . ?
C13 C1 B9 133.72(17) . . ?
C3 C8 B9 108.91(16) . . ?
C7 C8 C3 117.13(19) . . ?
C7 C8 B9 133.86(19) . . ?
N17 C16 N20 107.39(16) . . ?
N17 C16 B9 134.97(17) . . ?
N20 C16 B9 117.64(16) . . ?
O21 C22 P14 53.55(9) . . ?
O21 C22 N15 101.09(15) . . ?
N15 C22 P14 47.57(9) . . ?
N23 C22 P14 176.10(16) . . ?
N23 C22 O21 129.10(18) . . ?
N23 C22 N15 129.78(18) . . ?
C1 C2 C3 111.37(17) . . ?
C10 C2 C1 121.73(19) . . ?
C10 C2 C3 126.70(19) . . ?
C8 C3 C2 111.06(17) . . ?
C4 C3 C8 122.0(2) . . ?
C4 C3 C2 126.7(2) . . ?
C38 C39 C44 122.95(19) . . ?
C40 C39 C38 116.5(2) . . ?
C40 C39 C44 120.5(2) . . ?
C1 C13 H13 119.5 . . ?
C1 C13 C12 121.1(2) . . ?
C12 C13 H13 119.5 . . ?
C38 C43 C47 122.4(2) . . ?
C42 C43 C38 116.9(2) . . ?
C42 C43 C47 120.7(2) . . ?
C39 C40 H40 119.3 . . ?
C41 C40 C39 121.4(2) . . ?
C41 C40 H40 119.3 . . ?
C25 C24 N23 121.5(2) . . ?
C25 C24 C29 119.3(2) . . ?
C29 C24 N23 119.1(2) . . ?
C39 C44 H44 107.8 . . ?
C39 C44 C46 112.7(2) . . ?
C39 C44 C45 110.65(18) . . ?
C46 C44 H44 107.8 . . ?
C46 C44 C45 109.8(2) . . ?
C45 C44 H44 107.8 . . ?
N17 C18 H18 126.4 . . ?
C19 C18 N17 107.24(17) . . ?
C19 C18 H18 126.4 . . ?
C13 C12 H12 119.9 . . ?
C11 C12 C13 120.3(2) . . ?
C11 C12 H12 119.9 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(2) . . ?
C5 C4 H4 120.4 . . ?
C8 C7 H7 119.6 . . ?
C8 C7 C6 120.9(2) . . ?
C6 C7 H7 119.6 . . ?
C2 C10 H10 120.4 . . ?
C11 C10 C2 119.2(2) . . ?
C11 C10 H10 120.4 . . ?
C40 C41 H41 119.7 . . ?
C40 C41 C42 120.6(2) . . ?
C42 C41 H41 119.7 . . ?
N20 C19 H19 125.9 . . ?
C18 C19 N20 108.22(18) . . ?
C18 C19 H19 125.9 . . ?
C43 C42 H42 119.4 . . ?
C41 C42 C43 121.3(2) . . ?
C41 C42 H42 119.4 . . ?
C35 C34 P14 116.28(19) . . ?
C35 C34 C37 107.6(2) . . ?
C36 C34 P14 105.73(16) . . ?
C36 C34 C35 108.4(2) . . ?
C36 C34 C37 108.7(2) . . ?
C37 C34 P14 110.0(2) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C31 C30 P14 112.89(19) . . ?
C31 C30 C32 107.1(2) . . ?
C33 C30 P14 106.82(16) . . ?
C33 C30 C31 109.7(3) . . ?
C33 C30 C32 108.5(3) . . ?
C32 C30 P14 111.7(2) . . ?
N15 B9 C1 117.00(15) . . ?
N15 B9 C8 116.84(15) . . ?
N15 B9 C16 95.09(14) . . ?
C1 B9 C8 99.13(14) . . ?
C16 B9 C1 114.93(15) . . ?
C16 B9 C8 115.05(15) . . ?
C24 C25 H25 120.4 . . ?
C24 C25 C26 119.2(3) . . ?
C26 C25 H25 120.4 . . ?
C7 C6 H6 119.8 . . ?
C5 C6 C7 120.4(2) . . ?
C5 C6 H6 119.8 . . ?
C24 C29 H29 119.6 . . ?
C28 C29 C24 120.8(3) . . ?
C28 C29 H29 119.6 . . ?
C4 C5 C6 120.4(2) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C43 C47 H47 107.8 . . ?
C43 C47 C49 113.0(3) . . ?
C43 C47 C48 110.3(2) . . ?
C49 C47 H47 107.8 . . ?
C49 C47 C48 109.8(3) . . ?
C48 C47 H47 107.8 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Cl1 C54 H54A 109.2 . . ?
Cl1 C54 H54B 109.2 . . ?
Cl2 C54 Cl1 111.92(17) . . ?
Cl2 C54 H54A 109.2 . . ?
Cl2 C54 H54B 109.2 . . ?
H54A C54 H54B 107.9 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 C29 120.0(3) . . ?
C27 C28 H28 120.0 . . ?
C28 C27 H27 119.5 . . ?
C28 C27 C26 121.0(3) . . ?
C26 C27 H27 119.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.7(3) . . ?
C27 C26 H26 120.1 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Cl4 C51 H51A 109.7 . . ?
Cl4 C51 H51B 109.7 . . ?
Cl3 C51 Cl4 109.7(2) . . ?
Cl3 C51 H51A 109.7 . . ?
Cl3 C51 H51B 109.7 . . ?
H51A C51 H51B 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P14 O21 C22 N15 1.88(14) . . . . ?
P14 O21 C22 N23 -176.4(2) . . . . ?
P14 N15 C22 O21 -2.05(15) . . . . ?
P14 N15 C22 N23 176.2(2) . . . . ?
P14 N15 B9 C1 -120.58(17) . . . . ?
P14 N15 B9 C8 122.20(17) . . . . ?
P14 N15 B9 C16 0.8(2) . . . . ?
P14 N20 C16 N17 179.28(13) . . . . ?
P14 N20 C16 B9 -1.0(2) . . . . ?
P14 N20 C19 C18 -179.44(19) . . . . ?
O21 P14 N15 C22 1.56(12) . . . . ?
O21 P14 N15 B9 176.56(18) . . . . ?
O21 P14 C34 C35 172.4(2) . . . . ?
O21 P14 C34 C36 -67.28(19) . . . . ?
O21 P14 C34 C37 49.87(19) . . . . ?
O21 P14 C30 C31 -140.4(2) . . . . ?
O21 P14 C30 C33 98.91(19) . . . . ?
O21 P14 C30 C32 -19.6(2) . . . . ?
N17 C38 C39 C40 177.86(16) . . . . ?
N17 C38 C39 C44 0.4(3) . . . . ?
N17 C38 C43 C42 -178.18(17) . . . . ?
N17 C38 C43 C47 -0.2(3) . . . . ?
N17 C16 B9 N15 179.9(2) . . . . ?
N17 C16 B9 C1 -57.1(3) . . . . ?
N17 C16 B9 C8 57.1(3) . . . . ?
N17 C18 C19 N20 -0.3(3) . . . . ?
N15 P14 O21 C22 -1.58(12) . . . . ?
N15 P14 C34 C35 -115.26(19) . . . . ?
N15 P14 C34 C36 5.1(2) . . . . ?
N15 P14 C34 C37 122.22(18) . . . . ?
N15 P14 C30 C31 144.2(2) . . . . ?
N15 P14 C30 C33 23.5(2) . . . . ?
N15 P14 C30 C32 -95.0(2) . . . . ?
N20 P14 O21 C22 4.8(3) . . . . ?
N20 P14 N15 C22 -176.10(13) . . . . ?
N20 P14 N15 B9 -1.11(17) . . . . ?
N20 P14 C34 C35 -26.9(2) . . . . ?
N20 P14 C34 C36 93.43(19) . . . . ?
N20 P14 C34 C37 -149.41(18) . . . . ?
N20 P14 C30 C31 57.0(2) . . . . ?
N20 P14 C30 C33 -63.7(2) . . . . ?
N20 P14 C30 C32 177.7(2) . . . . ?
N20 C16 B9 N15 0.2(2) . . . . ?
N20 C16 B9 C1 123.20(18) . . . . ?
N20 C16 B9 C8 -122.58(19) . . . . ?
N23 C24 C25 C26 -176.0(2) . . . . ?
N23 C24 C29 C28 176.1(2) . . . . ?
C38 N17 C16 N20 -179.91(18) . . . . ?
C38 N17 C16 B9 0.4(3) . . . . ?
C38 N17 C18 C19 -179.7(2) . . . . ?
C38 C39 C40 C41 -0.4(3) . . . . ?
C38 C39 C44 C46 -148.8(2) . . . . ?
C38 C39 C44 C45 87.8(3) . . . . ?
C38 C43 C42 C41 1.1(3) . . . . ?
C38 C43 C47 C49 147.6(2) . . . . ?
C38 C43 C47 C48 -89.0(3) . . . . ?
C1 C2 C3 C8 -0.8(2) . . . . ?
C1 C2 C3 C4 173.32(19) . . . . ?
C1 C2 C10 C11 -2.8(3) . . . . ?
C1 C13 C12 C11 -2.0(3) . . . . ?
C8 C3 C4 C5 2.8(3) . . . . ?
C8 C7 C6 C5 2.7(4) . . . . ?
C16 N17 C38 C39 91.8(2) . . . . ?
C16 N17 C38 C43 -92.0(2) . . . . ?
C16 N17 C18 C19 -0.2(3) . . . . ?
C16 N20 C19 C18 0.7(3) . . . . ?
C22 P14 N15 B9 175.0(2) . . . . ?
C22 P14 C34 C35 -154.67(18) . . . . ?
C22 P14 C34 C36 -34.3(2) . . . . ?
C22 P14 C34 C37 82.82(19) . . . . ?
C22 P14 C30 C31 -174.4(2) . . . . ?
C22 P14 C30 C33 64.9(2) . . . . ?
C22 P14 C30 C32 -53.6(2) . . . . ?
C22 N15 B9 C1 52.2(3) . . . . ?
C22 N15 B9 C8 -65.0(3) . . . . ?
C22 N15 B9 C16 173.6(2) . . . . ?
C22 N23 C24 C25 -93.2(3) . . . . ?
C22 N23 C24 C29 90.6(2) . . . . ?
C2 C1 C13 C12 -0.3(3) . . . . ?
C2 C1 B9 N15 -134.56(16) . . . . ?
C2 C1 B9 C8 -8.04(18) . . . . ?
C2 C1 B9 C16 115.17(18) . . . . ?
C2 C3 C4 C5 -170.7(2) . . . . ?
C2 C10 C11 C12 0.3(3) . . . . ?
C3 C8 C7 C6 -0.5(3) . . . . ?
C3 C8 B9 N15 134.23(17) . . . . ?
C3 C8 B9 C1 7.60(18) . . . . ?
C3 C8 B9 C16 -115.51(17) . . . . ?
C3 C2 C10 C11 171.6(2) . . . . ?
C3 C4 C5 C6 -0.5(4) . . . . ?
C39 C38 C43 C42 -2.1(3) . . . . ?
C39 C38 C43 C47 175.82(19) . . . . ?
C39 C40 C41 C42 -0.5(3) . . . . ?
C13 C1 C2 C3 -172.45(16) . . . . ?
C13 C1 C2 C10 2.7(3) . . . . ?
C13 C1 B9 N15 43.6(3) . . . . ?
C13 C1 B9 C8 170.1(2) . . . . ?
C13 C1 B9 C16 -66.7(3) . . . . ?
C13 C12 C11 C10 2.0(4) . . . . ?
C43 C38 C39 C40 1.8(3) . . . . ?
C43 C38 C39 C44 -175.68(18) . . . . ?
C40 C39 C44 C46 33.9(3) . . . . ?
C40 C39 C44 C45 -89.6(3) . . . . ?
C40 C41 C42 C43 0.2(3) . . . . ?
C24 N23 C22 O21 3.0(3) . . . . ?
C24 N23 C22 N15 -174.8(2) . . . . ?
C24 C25 C26 C27 -0.1(4) . . . . ?
C24 C29 C28 C27 0.1(4) . . . . ?
C44 C39 C40 C41 177.13(19) . . . . ?
C18 N17 C38 C39 -88.9(2) . . . . ?
C18 N17 C38 C43 87.4(2) . . . . ?
C18 N17 C16 N20 0.7(2) . . . . ?
C18 N17 C16 B9 -179.0(2) . . . . ?
C7 C8 C3 C2 172.17(17) . . . . ?
C7 C8 C3 C4 -2.2(3) . . . . ?
C7 C8 B9 N15 -42.1(3) . . . . ?
C7 C8 B9 C1 -168.7(2) . . . . ?
C7 C8 B9 C16 68.2(3) . . . . ?
C7 C6 C5 C4 -2.2(4) . . . . ?
C10 C2 C3 C8 -175.62(19) . . . . ?
C10 C2 C3 C4 -1.5(3) . . . . ?
C19 N20 C16 N17 -0.8(2) . . . . ?
C19 N20 C16 B9 178.93(18) . . . . ?
C42 C43 C47 C49 -34.5(3) . . . . ?
C42 C43 C47 C48 88.9(3) . . . . ?
C34 P14 O21 C22 121.60(13) . . . . ?
C34 P14 N15 C22 -79.87(15) . . . . ?
C34 P14 N15 B9 95.13(18) . . . . ?
C34 P14 C30 C31 -46.1(3) . . . . ?
C34 P14 C30 C33 -166.76(19) . . . . ?
C34 P14 C30 C32 74.7(2) . . . . ?
C30 P14 O21 C22 -121.23(14) . . . . ?
C30 P14 N15 C22 89.31(15) . . . . ?
C30 P14 N15 B9 -95.69(18) . . . . ?
C30 P14 C34 C35 75.2(2) . . . . ?
C30 P14 C34 C36 -164.45(18) . . . . ?
C30 P14 C34 C37 -47.3(2) . . . . ?
B9 N15 C22 P14 -174.4(3) . . . . ?
B9 N15 C22 O21 -176.4(2) . . . . ?
B9 N15 C22 N23 1.8(4) . . . . ?
B9 C1 C2 C3 6.0(2) . . . . ?
B9 C1 C2 C10 -178.82(17) . . . . ?
B9 C1 C13 C12 -178.3(2) . . . . ?
B9 C8 C3 C2 -4.8(2) . . . . ?
B9 C8 C3 C4 -179.26(18) . . . . ?
B9 C8 C7 C6 175.6(2) . . . . ?
C25 C24 C29 C28 -0.1(3) . . . . ?
C29 C24 C25 C26 0.2(4) . . . . ?
C29 C28 C27 C26 -0.1(4) . . . . ?
C47 C43 C42 C41 -176.9(2) . . . . ?
C28 C27 C26 C25 0.1(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.602
_oxdiff_exptl_absorpt_empirical_full_min 0.638
# start Validation Reply Form
_vrf_PLAT196_SN2024_compound_6b  
;
PROBLEM: No TEMP record and _measurement_temperature .NE. 293 Degree
RESPONSE: As shown in this cif., this experiment was carried out at 193.15 K
;
# end Validation Reply Form
####################################################################### 
# 
# 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_SN2024_compound_8b
_audit_block_doi                 10.5517/ccdc.csd.cc2kv6l7
_database_code_depnum_ccdc_archive 'CCDC 2378679'
loop_
_audit_author_name
_audit_author_address
'Yoichi Hoshimoto'
;Osaka University
Japan
;
_audit_update_record             
;
2024-08-20 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_audit_creation_date             2022-09-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H50 B N4 O P, 1.5[H2O]'
_chemical_formula_sum            'C42 H50 B N4 O P'
_chemical_formula_weight         668.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C88 H108 B2 N6 O2 P2 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.9881(3)
_cell_length_b                   13.2977(5)
_cell_length_c                   15.5488(6)
_cell_angle_alpha                102.478(3)
_cell_angle_beta                 94.349(3)
_cell_angle_gamma                100.379(3)
_cell_volume                     1969.19(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5911
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      72.6020
_cell_measurement_theta_min      3.4810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22010
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         3.476
_diffrn_ambient_temperature      193.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  34.00   0.50    5.00    --  -42.93  39.00  84.00   80
  2  ω     67.00 120.00   0.50    5.00    --   42.93  39.00  84.00  106
  3  ω     80.00 105.00   0.50   10.00    --   76.50  39.00  84.00   50
  4  ω     67.00  97.00   0.50   10.00    --   76.50 -39.00 -69.00   60
  5  ω     51.00  94.00   0.50   10.00    --   76.50 -99.00 -90.00   86
  6  ω     21.00  60.00   0.50    5.00    --   42.93  39.00  84.00   78
  7  ω    -34.00  46.00   0.50    5.00    --   42.93 -39.00 -69.00  160
  8  ω    110.00 149.00   0.50   10.00    --   76.50 125.00 -90.00   78
  9  ω    -60.00 -32.00   0.50   10.00    -- -106.00 125.00  30.00   56
 10  ω    -94.00 -17.00   0.50    5.00    --  -42.93 125.00 150.00  154
 11  ω    -99.00 -64.00   0.50   10.00    -- -106.00  77.00   0.00   70
 12  ω   -106.00 -80.00   0.50   10.00    -- -106.00 125.00  30.00   52
 13  ω   -112.00 -36.00   0.50   10.00    -- -106.00 125.00  60.00  152
 14  ω   -106.00 -35.00   0.50   10.00    -- -106.00  57.00  90.00  142
 15  ω   -114.00 -32.00   0.50   10.00    -- -106.00 125.00 -60.00  164
 16  ω   -114.00 -68.00   0.50   10.00    -- -106.00 125.00  90.00   92
 17  ω   -124.00 -29.00   0.50   10.00    -- -106.00  39.00  84.00  190
 18  ω   -108.00 -83.00   0.50   10.00    -- -106.00 -37.00  60.00   50
 19  ω   -123.00 -97.00   0.50   10.00    -- -106.00 -37.00   0.00   52
 20  ω   -134.00 -25.00   0.50   10.00    -- -106.00  19.00 -60.00  218
 21  ω   -107.00 -65.00   0.50   10.00    -- -106.00  77.00 -90.00   84
 22  ω   -117.00 -41.00   0.50   10.00    -- -106.00 125.00-120.00  152
 23  ω   -124.00 -33.00   0.50   10.00    -- -106.00  57.00 -90.00  182
 24  ω   -119.00 -23.00   0.50    5.00    --  -42.93 -39.00 -69.00  192
 25  ω   -115.00 -84.00   0.50    5.00    --  -42.93-125.00  90.00   62
 26  ω   -142.00 -85.00   0.50   10.00    -- -106.00 -57.00 120.00  114
 27  ω   -150.00-123.00   0.50   10.00    -- -106.00 -37.00  60.00   54
 28  ω   -174.00-149.00   0.50   10.00    -- -106.00 -57.00 120.00   50
 29  ω   -175.00 -86.00   0.50   10.00    -- -106.00 -99.00 150.00  178
 30  ω   -174.00-134.00   0.50   10.00    -- -106.00 -37.00   0.00   80
 31  ω   -163.00 -84.00   0.50   10.00    -- -106.00 -39.00 -69.00  158
 32  ω   -127.00 -34.00   0.50   10.00    -- -106.00  37.00 -90.00  186
 33  ω   -116.00 -72.00   0.50    5.00    --  -42.93-125.00 -90.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1336442000
_diffrn_orient_matrix_UB_12      -0.0720355000
_diffrn_orient_matrix_UB_13      -0.0506388000
_diffrn_orient_matrix_UB_21      0.0680474000
_diffrn_orient_matrix_UB_22      -0.0961338000
_diffrn_orient_matrix_UB_23      -0.0066744000
_diffrn_orient_matrix_UB_31      -0.0495269000
_diffrn_orient_matrix_UB_32      -0.0156916000
_diffrn_orient_matrix_UB_33      0.0885308000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5767
_reflns_number_total             7179
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0500
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0543P)²+0.6522P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1236
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C33(H33), C36(H36)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C10(H10), C29(H29), C7(H7), C31(H31), C13(H13), C4(H4),
 C30(H30), C11(H11), C5(H5), C12(H12), C6(H6), C24(H24), C26(H26), C22(H22),
 C25(H25), C23(H23)
2.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C37(H37A,H37B,
 H37C), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C42(H42A,H42B,H42C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P40 P 0.52959(5) 0.71341(4) 0.75397(3) 0.03179(13) Uani 1 1 d . . . . .
O49 O 0.55109(16) 0.70422(11) 0.65906(9) 0.0428(4) Uani 1 1 d . . . . .
N16 N 0.24134(15) 0.33661(11) 0.56076(9) 0.0268(3) Uani 1 1 d . . . . .
N19 N 0.32064(15) 0.48052(11) 0.65826(10) 0.0274(3) Uani 1 1 d . . . . .
N14 N 0.23292(16) 0.49037(12) 0.78618(10) 0.0294(3) Uani 1 1 d . . . . .
N39 N 0.39785(17) 0.63711(12) 0.77827(10) 0.0341(4) Uani 1 1 d . . . . .
C15 C 0.23620(18) 0.38544(14) 0.64441(12) 0.0267(4) Uani 1 1 d . . . . .
C21 C 0.2094(2) 0.53589(15) 0.87479(12) 0.0326(4) Uani 1 1 d . . . . .
C27 C 0.16403(19) 0.23494(14) 0.51072(12) 0.0289(4) Uani 1 1 d . . . . .
C8 C 0.2379(2) 0.28803(15) 0.77957(12) 0.0327(4) Uani 1 1 d . . . . .
C20 C 0.32396(19) 0.54588(14) 0.74633(11) 0.0282(4) Uani 1 1 d . . . . .
C17 C 0.33060(19) 0.40157(15) 0.52133(12) 0.0331(4) Uani 1 1 d . . . . .
H17 H 0.3525 0.3848 0.4622 0.040 Uiso 1 1 calc R U . . .
C18 C 0.3800(2) 0.49230(15) 0.58225(12) 0.0329(4) Uani 1 1 d . . . . .
H18 H 0.4424 0.5518 0.5747 0.039 Uiso 1 1 calc R U . . .
C28 C 0.2252(2) 0.14762(15) 0.50665(12) 0.0320(4) Uani 1 1 d . . . . .
C33 C 0.3608(2) 0.15289(15) 0.56022(13) 0.0353(4) Uani 1 1 d . . . . .
H33 H 0.3863 0.2235 0.6025 0.042 Uiso 1 1 calc R U . . .
C2 C -0.0036(2) 0.22964(15) 0.75956(12) 0.0350(4) Uani 1 1 d . . . . .
C1 C 0.01265(19) 0.32499(14) 0.73151(12) 0.0308(4) Uani 1 1 d . . . . .
C32 C 0.03923(19) 0.23229(15) 0.46218(13) 0.0333(4) Uani 1 1 d . . . . .
C10 C -0.1033(2) 0.35934(16) 0.70618(13) 0.0366(4) Uani 1 1 d . . . . .
H10 H -0.0942 0.4238 0.6881 0.044 Uiso 1 1 calc R U . . .
C29 C 0.1562(2) 0.05415(16) 0.44890(14) 0.0402(5) Uani 1 1 d . . . . .
H29 H 0.1937 -0.0073 0.4440 0.048 Uiso 1 1 calc R U . . .
C3 C 0.1301(2) 0.20952(15) 0.79041(13) 0.0358(4) Uani 1 1 d . . . . .
C36 C -0.0252(2) 0.32863(17) 0.46846(14) 0.0412(5) Uani 1 1 d . . . . .
H36 H 0.0226 0.3829 0.5221 0.049 Uiso 1 1 calc R U . . .
C7 C 0.3717(2) 0.28465(18) 0.80915(14) 0.0417(5) Uani 1 1 d . . . . .
H7 H 0.4454 0.3367 0.8014 0.050 Uiso 1 1 calc R U . . .
C41 C 0.4965(2) 0.84519(16) 0.80194(14) 0.0412(5) Uani 1 1 d . . . . .
C31 C -0.0251(2) 0.13644(17) 0.40593(14) 0.0417(5) Uani 1 1 d . . . . .
H31 H -0.1105 0.1310 0.3722 0.050 Uiso 1 1 calc R U . . .
C13 C -0.1333(2) 0.16998(17) 0.75851(15) 0.0440(5) Uani 1 1 d . . . . .
H13 H -0.1433 0.1051 0.7760 0.053 Uiso 1 1 calc R U . . .
C35 C 0.3488(2) 0.06938(17) 0.61481(14) 0.0406(5) Uani 1 1 d . . . . .
H35A H 0.2789 0.0796 0.6550 0.061 Uiso 1 1 calc R U . . .
H35B H 0.4373 0.0758 0.6496 0.061 Uiso 1 1 calc R U . . .
H35C H 0.3227 -0.0007 0.5749 0.061 Uiso 1 1 calc R U . . .
C4 C 0.1574(3) 0.12905(17) 0.82978(15) 0.0473(5) Uani 1 1 d . . . . .
H4 H 0.0845 0.0752 0.8358 0.057 Uiso 1 1 calc R U . . .
C30 C 0.0341(2) 0.04941(16) 0.39873(14) 0.0439(5) Uani 1 1 d . . . . .
H30 H -0.0098 -0.0148 0.3587 0.053 Uiso 1 1 calc R U . . .
C11 C -0.2342(2) 0.30032(19) 0.70686(15) 0.0457(5) Uani 1 1 d . . . . .
H11 H -0.3134 0.3252 0.6902 0.055 Uiso 1 1 calc R U . . .
C34 C 0.4731(2) 0.1433(2) 0.49958(16) 0.0482(5) Uani 1 1 d . . . . .
H34A H 0.4499 0.0750 0.4568 0.072 Uiso 1 1 calc R U . . .
H34B H 0.5605 0.1490 0.5352 0.072 Uiso 1 1 calc R U . . .
H34C H 0.4811 0.1997 0.4677 0.072 Uiso 1 1 calc R U . . .
C5 C 0.2909(3) 0.12846(19) 0.85981(15) 0.0538(6) Uani 1 1 d . . . . .
H5 H 0.3092 0.0745 0.8875 0.065 Uiso 1 1 calc R U . . .
C12 C -0.2476(2) 0.20559(19) 0.73185(15) 0.0499(6) Uani 1 1 d . . . . .
H12 H -0.3364 0.1646 0.7307 0.060 Uiso 1 1 calc R U . . .
C6 C 0.3989(3) 0.2057(2) 0.85012(15) 0.0515(6) Uani 1 1 d . . . . .
H6 H 0.4903 0.2047 0.8712 0.062 Uiso 1 1 calc R U . . .
C43 C 0.6781(2) 0.68052(18) 0.81215(15) 0.0452(5) Uani 1 1 d . . . . .
B9 B 0.1747(2) 0.37204(16) 0.73552(14) 0.0287(4) Uani 1 1 d . . . . .
C38 C -0.1769(2) 0.3047(2) 0.47965(16) 0.0553(6) Uani 1 1 d . . . . .
H38A H -0.2289 0.2630 0.4234 0.083 Uiso 1 1 calc R U . . .
H38B H -0.2091 0.3707 0.4972 0.083 Uiso 1 1 calc R U . . .
H38C H -0.1904 0.2649 0.5256 0.083 Uiso 1 1 calc R U . . .
C37 C -0.0050(3) 0.3755(2) 0.38759(19) 0.0610(7) Uani 1 1 d . . . . .
H37A H 0.0932 0.3978 0.3847 0.091 Uiso 1 1 calc R U . . .
H37B H -0.0491 0.4363 0.3928 0.091 Uiso 1 1 calc R U . . .
H37C H -0.0462 0.3224 0.3336 0.091 Uiso 1 1 calc R U . . .
C24 C 0.1582(3) 0.6242(2) 1.04386(17) 0.0673(8) Uani 1 1 d . . . . .
H24 H 0.1384 0.6527 1.1018 0.081 Uiso 1 1 calc R U . . .
C47 C 0.3666(3) 0.8521(2) 0.74748(17) 0.0570(6) Uani 1 1 d . . . . .
H47A H 0.3805 0.8401 0.6846 0.085 Uiso 1 1 calc R U . . .
H47B H 0.3455 0.9220 0.7674 0.085 Uiso 1 1 calc R U . . .
H47C H 0.2903 0.7985 0.7553 0.085 Uiso 1 1 calc R U . . .
C46 C 0.6789(3) 0.5662(2) 0.76616(18) 0.0567(6) Uani 1 1 d . . . . .
H46A H 0.5960 0.5201 0.7758 0.085 Uiso 1 1 calc R U . . .
H46B H 0.7600 0.5454 0.7909 0.085 Uiso 1 1 calc R U . . .
H46C H 0.6812 0.5602 0.7024 0.085 Uiso 1 1 calc R U . . .
C42 C 0.4747(4) 0.8629(2) 0.89981(16) 0.0685(8) Uani 1 1 d . . . . .
H42A H 0.4073 0.8037 0.9086 0.103 Uiso 1 1 calc R U . . .
H42B H 0.4410 0.9282 0.9180 0.103 Uiso 1 1 calc R U . . .
H42C H 0.5618 0.8681 0.9357 0.103 Uiso 1 1 calc R U . . .
C45 C 0.6722(3) 0.6883(3) 0.91109(17) 0.0734(9) Uani 1 1 d . . . . .
H45A H 0.6828 0.7622 0.9421 0.110 Uiso 1 1 calc R U . . .
H45B H 0.7463 0.6589 0.9346 0.110 Uiso 1 1 calc R U . . .
H45C H 0.5836 0.6488 0.9200 0.110 Uiso 1 1 calc R U . . .
C26 C 0.2891(4) 0.5262(2) 0.94709(16) 0.0696(8) Uani 1 1 d . . . . .
H26 H 0.3607 0.4880 0.9391 0.083 Uiso 1 1 calc R U . . .
C22 C 0.1073(3) 0.5894(3) 0.88759(17) 0.0780(10) Uani 1 1 d . . . . .
H22 H 0.0517 0.5967 0.8378 0.094 Uiso 1 1 calc R U . . .
C48 C 0.6128(3) 0.9308(2) 0.7881(2) 0.0777(9) Uani 1 1 d . . . . .
H48A H 0.6952 0.9339 0.8278 0.116 Uiso 1 1 calc R U . . .
H48B H 0.5849 0.9990 0.8013 0.116 Uiso 1 1 calc R U . . .
H48C H 0.6324 0.9142 0.7264 0.116 Uiso 1 1 calc R U . . .
C25 C 0.2652(4) 0.5721(3) 1.03205(17) 0.0803(10) Uani 1 1 d . . . . .
H25 H 0.3226 0.5676 1.0821 0.096 Uiso 1 1 calc R U . . .
C44 C 0.8106(3) 0.7500(2) 0.7970(3) 0.0781(9) Uani 1 1 d . . . . .
H44A H 0.8060 0.7537 0.7346 0.117 Uiso 1 1 calc R U . . .
H44B H 0.8893 0.7198 0.8120 0.117 Uiso 1 1 calc R U . . .
H44C H 0.8209 0.8209 0.8347 0.117 Uiso 1 1 calc R U . . .
C23 C 0.0826(4) 0.6339(4) 0.9724(2) 0.0991(13) Uani 1 1 d . . . . .
H23 H 0.0108 0.6720 0.9800 0.119 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
P40 O49 1.4894(14) . ?
P40 N39 1.6320(16) . ?
P40 C41 1.849(2) . ?
P40 C43 1.847(2) . ?
N16 C15 1.332(2) . ?
N16 C27 1.452(2) . ?
N16 C17 1.397(2) . ?
N19 C15 1.352(2) . ?
N19 C20 1.449(2) . ?
N19 C18 1.388(2) . ?
N14 C21 1.435(2) . ?
N14 C20 1.340(2) . ?
N14 B9 1.581(2) . ?
N39 C20 1.275(2) . ?
C15 B9 1.618(3) . ?
C21 C26 1.370(3) . ?
C21 C22 1.348(3) . ?
C27 C28 1.398(3) . ?
C27 C32 1.398(3) . ?
C8 C3 1.406(3) . ?
C8 C7 1.392(3) . ?
C8 B9 1.623(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.348(3) . ?
C18 H18 0.9500 . ?
C28 C33 1.517(3) . ?
C28 C29 1.393(3) . ?
C33 H33 1.0000 . ?
C33 C35 1.531(3) . ?
C33 C34 1.525(3) . ?
C2 C1 1.414(3) . ?
C2 C3 1.474(3) . ?
C2 C13 1.389(3) . ?
C1 C10 1.380(3) . ?
C1 B9 1.618(3) . ?
C32 C36 1.522(3) . ?
C32 C31 1.393(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.401(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.381(3) . ?
C3 C4 1.399(3) . ?
C36 H36 1.0000 . ?
C36 C38 1.523(3) . ?
C36 C37 1.530(3) . ?
C7 H7 0.9500 . ?
C7 C6 1.395(3) . ?
C41 C47 1.523(3) . ?
C41 C42 1.527(3) . ?
C41 C48 1.536(3) . ?
C31 H31 0.9500 . ?
C31 C30 1.379(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.381(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C4 H4 0.9500 . ?
C4 C5 1.381(4) . ?
C30 H30 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.384(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C5 H5 0.9500 . ?
C5 C6 1.391(4) . ?
C12 H12 0.9500 . ?
C6 H6 0.9500 . ?
C43 C46 1.535(3) . ?
C43 C45 1.526(3) . ?
C43 C44 1.536(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C24 H24 0.9500 . ?
C24 C25 1.376(4) . ?
C24 C23 1.339(5) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C25 1.388(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.383(4) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C25 H25 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C23 H23 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O49 P40 N39 118.85(8) . . ?
O49 P40 C41 109.77(9) . . ?
O49 P40 C43 108.60(10) . . ?
N39 P40 C41 101.52(9) . . ?
N39 P40 C43 103.77(10) . . ?
C43 P40 C41 114.37(10) . . ?
C15 N16 C27 128.75(15) . . ?
C15 N16 C17 109.66(15) . . ?
C17 N16 C27 121.49(14) . . ?
C15 N19 C20 113.45(14) . . ?
C15 N19 C18 110.80(15) . . ?
C18 N19 C20 135.71(15) . . ?
C21 N14 B9 124.53(15) . . ?
C20 N14 C21 119.01(15) . . ?
C20 N14 B9 115.88(14) . . ?
C20 N39 P40 138.32(14) . . ?
N16 C15 N19 106.23(15) . . ?
N16 C15 B9 144.14(16) . . ?
N19 C15 B9 109.51(15) . . ?
C26 C21 N14 121.3(2) . . ?
C22 C21 N14 119.69(19) . . ?
C22 C21 C26 119.1(2) . . ?
C28 C27 N16 118.02(16) . . ?
C28 C27 C32 123.90(17) . . ?
C32 C27 N16 117.73(16) . . ?
C3 C8 B9 109.13(17) . . ?
C7 C8 C3 118.91(19) . . ?
C7 C8 B9 131.90(18) . . ?
N14 C20 N19 105.48(15) . . ?
N39 C20 N19 126.79(16) . . ?
N39 C20 N14 127.73(17) . . ?
N16 C17 H17 126.1 . . ?
C18 C17 N16 107.71(16) . . ?
C18 C17 H17 126.1 . . ?
N19 C18 H18 127.2 . . ?
C17 C18 N19 105.61(16) . . ?
C17 C18 H18 127.2 . . ?
C27 C28 C33 122.70(17) . . ?
C29 C28 C27 116.46(18) . . ?
C29 C28 C33 120.83(17) . . ?
C28 C33 H33 107.8 . . ?
C28 C33 C35 111.41(16) . . ?
C28 C33 C34 110.38(17) . . ?
C35 C33 H33 107.8 . . ?
C34 C33 H33 107.8 . . ?
C34 C33 C35 111.46(17) . . ?
C1 C2 C3 111.01(17) . . ?
C13 C2 C1 120.7(2) . . ?
C13 C2 C3 128.24(19) . . ?
C2 C1 B9 108.74(17) . . ?
C10 C1 C2 118.52(18) . . ?
C10 C1 B9 132.73(17) . . ?
C27 C32 C36 122.66(17) . . ?
C31 C32 C27 116.90(18) . . ?
C31 C32 C36 120.43(18) . . ?
C1 C10 H10 119.6 . . ?
C1 C10 C11 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
C28 C29 H29 119.5 . . ?
C30 C29 C28 121.08(19) . . ?
C30 C29 H29 119.5 . . ?
C8 C3 C2 110.87(17) . . ?
C4 C3 C8 120.4(2) . . ?
C4 C3 C2 128.7(2) . . ?
C32 C36 H36 107.7 . . ?
C32 C36 C38 112.18(19) . . ?
C32 C36 C37 111.25(18) . . ?
C38 C36 H36 107.7 . . ?
C38 C36 C37 110.02(19) . . ?
C37 C36 H36 107.7 . . ?
C8 C7 H7 119.6 . . ?
C8 C7 C6 120.8(2) . . ?
C6 C7 H7 119.6 . . ?
C47 C41 P40 105.03(14) . . ?
C47 C41 C42 109.5(2) . . ?
C47 C41 C48 107.6(2) . . ?
C42 C41 P40 113.77(15) . . ?
C42 C41 C48 110.4(2) . . ?
C48 C41 P40 110.19(18) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 C32 120.67(19) . . ?
C30 C31 H31 119.7 . . ?
C2 C13 H13 120.2 . . ?
C12 C13 C2 119.6(2) . . ?
C12 C13 H13 120.2 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.5(2) . . ?
C5 C4 H4 120.2 . . ?
C29 C30 H30 119.5 . . ?
C31 C30 C29 120.96(19) . . ?
C31 C30 H30 119.5 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.7(2) . . ?
C12 C11 H11 120.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.0(2) . . ?
C6 C5 H5 119.5 . . ?
C13 C12 C11 120.7(2) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C7 C6 H6 120.3 . . ?
C5 C6 C7 119.4(2) . . ?
C5 C6 H6 120.3 . . ?
C46 C43 P40 105.24(16) . . ?
C46 C43 C44 108.0(2) . . ?
C45 C43 P40 114.81(17) . . ?
C45 C43 C46 108.9(2) . . ?
C45 C43 C44 110.4(2) . . ?
C44 C43 P40 109.25(18) . . ?
N14 B9 C15 94.36(14) . . ?
N14 B9 C8 113.53(15) . . ?
N14 B9 C1 118.55(15) . . ?
C15 B9 C8 112.66(15) . . ?
C15 B9 C1 118.66(16) . . ?
C1 B9 C8 99.98(15) . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C23 C24 C25 119.0(2) . . ?
C41 C47 H47A 109.5 . . ?
C41 C47 H47B 109.5 . . ?
C41 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C21 C26 H26 120.0 . . ?
C21 C26 C25 120.1(3) . . ?
C25 C26 H26 120.0 . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.7(3) . . ?
C23 C22 H22 119.6 . . ?
C41 C48 H48A 109.5 . . ?
C41 C48 H48B 109.5 . . ?
C41 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C24 C25 C26 120.0(3) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C24 C23 C22 121.1(3) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P40 N39 C20 N19 -13.1(3) . . . . ?
P40 N39 C20 N14 167.29(16) . . . . ?
O49 P40 N39 C20 29.4(3) . . . . ?
O49 P40 C41 C47 60.91(18) . . . . ?
O49 P40 C41 C42 -179.34(19) . . . . ?
O49 P40 C41 C48 -54.7(2) . . . . ?
O49 P40 C43 C46 -61.35(18) . . . . ?
O49 P40 C43 C45 179.0(2) . . . . ?
O49 P40 C43 C44 54.4(2) . . . . ?
N16 C15 B9 N14 -175.8(2) . . . . ?
N16 C15 B9 C8 66.4(3) . . . . ?
N16 C15 B9 C1 -49.8(3) . . . . ?
N16 C27 C28 C33 6.9(3) . . . . ?
N16 C27 C28 C29 -171.87(17) . . . . ?
N16 C27 C32 C36 -7.2(3) . . . . ?
N16 C27 C32 C31 172.16(17) . . . . ?
N16 C17 C18 N19 0.5(2) . . . . ?
N19 C15 B9 N14 8.98(18) . . . . ?
N19 C15 B9 C8 -108.77(17) . . . . ?
N19 C15 B9 C1 134.99(17) . . . . ?
N14 C21 C26 C25 179.2(3) . . . . ?
N14 C21 C22 C23 179.9(3) . . . . ?
N39 P40 C41 C47 -65.71(17) . . . . ?
N39 P40 C41 C42 54.0(2) . . . . ?
N39 P40 C41 C48 178.67(18) . . . . ?
N39 P40 C43 C46 65.99(17) . . . . ?
N39 P40 C43 C45 -53.7(2) . . . . ?
N39 P40 C43 C44 -178.29(18) . . . . ?
C15 N16 C27 C28 -95.7(2) . . . . ?
C15 N16 C27 C32 90.8(2) . . . . ?
C15 N16 C17 C18 -0.5(2) . . . . ?
C15 N19 C20 N14 -3.0(2) . . . . ?
C15 N19 C20 N39 177.31(18) . . . . ?
C15 N19 C18 C17 -0.4(2) . . . . ?
C21 N14 C20 N19 -178.26(15) . . . . ?
C21 N14 C20 N39 1.4(3) . . . . ?
C21 N14 B9 C15 177.11(17) . . . . ?
C21 N14 B9 C8 -65.8(2) . . . . ?
C21 N14 B9 C1 51.0(3) . . . . ?
C21 C26 C25 C24 2.4(5) . . . . ?
C21 C22 C23 C24 -0.7(6) . . . . ?
C27 N16 C15 N19 -176.08(16) . . . . ?
C27 N16 C15 B9 8.7(4) . . . . ?
C27 N16 C17 C18 176.12(16) . . . . ?
C27 C28 C33 C35 126.45(19) . . . . ?
C27 C28 C33 C34 -109.1(2) . . . . ?
C27 C28 C29 C30 0.1(3) . . . . ?
C27 C32 C36 C38 -133.1(2) . . . . ?
C27 C32 C36 C37 103.2(2) . . . . ?
C27 C32 C31 C30 -0.7(3) . . . . ?
C8 C3 C4 C5 1.4(3) . . . . ?
C8 C7 C6 C5 1.3(3) . . . . ?
C20 N19 C15 N16 178.23(14) . . . . ?
C20 N19 C15 B9 -4.7(2) . . . . ?
C20 N19 C18 C17 -177.93(19) . . . . ?
C20 N14 C21 C26 -87.0(3) . . . . ?
C20 N14 C21 C22 92.9(3) . . . . ?
C20 N14 B9 C15 -11.73(19) . . . . ?
C20 N14 B9 C8 105.31(18) . . . . ?
C20 N14 B9 C1 -137.82(17) . . . . ?
C17 N16 C15 N19 0.2(2) . . . . ?
C17 N16 C15 B9 -175.1(2) . . . . ?
C17 N16 C27 C28 88.4(2) . . . . ?
C17 N16 C27 C32 -85.2(2) . . . . ?
C18 N19 C15 N16 0.1(2) . . . . ?
C18 N19 C15 B9 177.19(15) . . . . ?
C18 N19 C20 N14 174.43(19) . . . . ?
C18 N19 C20 N39 -5.2(3) . . . . ?
C28 C27 C32 C36 179.63(18) . . . . ?
C28 C27 C32 C31 -1.0(3) . . . . ?
C28 C29 C30 C31 -1.7(3) . . . . ?
C33 C28 C29 C30 -178.74(19) . . . . ?
C2 C1 C10 C11 -1.0(3) . . . . ?
C2 C1 B9 N14 -128.82(17) . . . . ?
C2 C1 B9 C15 117.85(18) . . . . ?
C2 C1 B9 C8 -4.96(18) . . . . ?
C2 C3 C4 C5 -175.4(2) . . . . ?
C2 C13 C12 C11 -0.5(3) . . . . ?
C1 C2 C3 C8 -2.8(2) . . . . ?
C1 C2 C3 C4 174.27(19) . . . . ?
C1 C2 C13 C12 -1.6(3) . . . . ?
C1 C10 C11 C12 -1.0(3) . . . . ?
C32 C27 C28 C33 -179.95(17) . . . . ?
C32 C27 C28 C29 1.2(3) . . . . ?
C32 C31 C30 C29 2.0(3) . . . . ?
C10 C1 B9 N14 52.0(3) . . . . ?
C10 C1 B9 C15 -61.3(3) . . . . ?
C10 C1 B9 C8 175.87(19) . . . . ?
C10 C11 C12 C13 1.8(3) . . . . ?
C29 C28 C33 C35 -54.8(2) . . . . ?
C29 C28 C33 C34 69.6(2) . . . . ?
C3 C8 C7 C6 -0.9(3) . . . . ?
C3 C8 B9 N14 130.61(17) . . . . ?
C3 C8 B9 C15 -123.63(17) . . . . ?
C3 C8 B9 C1 3.32(19) . . . . ?
C3 C2 C1 C10 -175.67(17) . . . . ?
C3 C2 C1 B9 5.0(2) . . . . ?
C3 C2 C13 C12 176.02(19) . . . . ?
C3 C4 C5 C6 -1.1(3) . . . . ?
C36 C32 C31 C30 178.8(2) . . . . ?
C7 C8 C3 C2 176.96(17) . . . . ?
C7 C8 C3 C4 -0.4(3) . . . . ?
C7 C8 B9 N14 -46.6(3) . . . . ?
C7 C8 B9 C15 59.2(3) . . . . ?
C7 C8 B9 C1 -173.89(19) . . . . ?
C41 P40 N39 C20 149.9(2) . . . . ?
C41 P40 C43 C46 175.67(16) . . . . ?
C41 P40 C43 C45 56.0(2) . . . . ?
C41 P40 C43 C44 -68.6(2) . . . . ?
C31 C32 C36 C38 47.5(3) . . . . ?
C31 C32 C36 C37 -76.2(3) . . . . ?
C13 C2 C1 C10 2.3(3) . . . . ?
C13 C2 C1 B9 -176.96(17) . . . . ?
C13 C2 C3 C8 179.34(19) . . . . ?
C13 C2 C3 C4 -3.6(3) . . . . ?
C4 C5 C6 C7 -0.2(3) . . . . ?
C43 P40 N39 C20 -91.2(2) . . . . ?
C43 P40 C41 C47 -176.74(16) . . . . ?
C43 P40 C41 C42 -57.0(2) . . . . ?
C43 P40 C41 C48 67.6(2) . . . . ?
B9 N14 C21 C26 83.9(3) . . . . ?
B9 N14 C21 C22 -96.2(3) . . . . ?
B9 N14 C20 N19 10.1(2) . . . . ?
B9 N14 C20 N39 -170.27(18) . . . . ?
B9 C8 C3 C2 -0.7(2) . . . . ?
B9 C8 C3 C4 -178.05(17) . . . . ?
B9 C8 C7 C6 176.1(2) . . . . ?
B9 C1 C10 C11 178.10(19) . . . . ?
C26 C21 C22 C23 -0.1(5) . . . . ?
C22 C21 C26 C25 -0.7(5) . . . . ?
C25 C24 C23 C22 2.4(6) . . . . ?
C23 C24 C25 C26 -3.2(5) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 28 electrons were 
found in a volume of 177Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[H2O] per Asymmetric Unit 
which account for 30 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 177.3 28.3 '3 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.002
_oxdiff_exptl_absorpt_empirical_full_min 0.668
####################################################################### 
# 
# 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_compound_6a
_audit_block_doi                 10.5517/ccdc.csd.cc2f6qt6
_database_code_depnum_ccdc_archive 'CCDC 2240798'
loop_
_audit_author_name
_audit_author_address
'Yoichi Hoshimoto'
;Osaka University
Japan
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_audit_creation_date             2021-12-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H45 B N3 O2 P, C H2 Cl2'
_chemical_formula_sum            'C37 H47 B Cl2 N3 O2 P'
_chemical_formula_weight         678.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 H50 B1 N3 O2 P1 Cl4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.6693(3)
_cell_length_b                   19.5252(3)
_cell_length_c                   16.0002(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.512(2)
_cell_angle_gamma                90
_cell_volume                     3774.54(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9489
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      75.8490
_cell_measurement_theta_min      3.6860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.213
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28175
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         3.676
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     56.00 123.00   0.50    2.96    --   49.96  31.00-140.00  134
  2  ω     74.00  99.00   0.50    2.96    --   66.50  31.00-140.00   50
  3  ω     77.00 121.00   0.50    2.96    --   49.96 125.00-120.00   88
  4  ω      5.00  45.00   0.50    2.96    --   66.50 -31.00  59.00   80
  5  ω     -5.00  79.00   0.50    2.96    --   66.50 -57.00   0.00  168
  6  ω    -19.00  11.00   0.50    2.96    --   49.96 -31.00  59.00   60
  7  ω    -21.00  58.00   0.50    2.96    --   49.96 -37.00 -60.00  158
  8  ω    -45.00  20.00   0.50    2.96    --  -53.21  31.00-140.00  130
  9  ω    -89.00 -51.00   0.50    2.96    --  -53.21 -31.00  59.00   76
 10  ω    -98.00 -53.00   0.50    2.96    -- -105.75  37.00  30.00   90
 11  ω   -111.00 -52.00   0.50    2.96    -- -105.75  77.00  60.00  118
 12  ω   -112.00 -53.00   0.50    2.96    -- -105.75  19.00 -30.00  118
 13  ω   -110.00 -72.00   0.50    2.96    -- -105.75  31.00-140.00   76
 14  ω   -109.00 -32.00   0.50    2.96    -- -105.75  19.00-120.00  154
 15  ω   -112.00 -33.00   0.50    2.96    -- -105.75  19.00  30.00  158
 16  ω   -112.00 -34.00   0.50    2.96    -- -105.75  57.00  60.00  156
 17  ω   -161.00-136.00   0.50    2.96    -- -105.75 -31.00  59.00   50
 18  ω   -167.00-110.00   0.50    2.96    -- -105.75 -19.00   0.00  114
 19  ω   -175.00-122.00   0.50    2.96    -- -105.75 -19.00  90.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0186268000
_diffrn_orient_matrix_UB_12      -0.0242063000
_diffrn_orient_matrix_UB_13      -0.0861562000
_diffrn_orient_matrix_UB_21      0.1226971000
_diffrn_orient_matrix_UB_22      0.0209788000
_diffrn_orient_matrix_UB_23      0.0352584000
_diffrn_orient_matrix_UB_31      0.0294245000
_diffrn_orient_matrix_UB_32      -0.0720750000
_diffrn_orient_matrix_UB_33      0.0390802000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5733
_reflns_number_total             6898
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6898
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0716
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1048P)²+3.9052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.1998
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C38(H38), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C7(H7), C13(H13), C4(H4), C6(H6), C34(H34), C36(H36),
 C12(H12), C10(H10), C11(H11), C5(H5), C35(H35)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C24(H24A,H24B,H24C), C39(H39A,H39B,H39C), C26(H26A,H26B,
 H26C), C43(H43A,H43B,H43C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C42(H42A,H42B,H42C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P14 P 0.17161(6) 0.30734(3) 0.80814(4) 0.0278(2) Uani 1 1 d . . . . .
O21 O 0.18988(18) 0.21426(9) 0.81445(14) 0.0417(5) Uani 1 1 d . . . . .
N17 N 0.26699(18) 0.47313(10) 0.71175(14) 0.0283(5) Uani 1 1 d . . . . .
N20 N 0.18681(18) 0.39896(10) 0.77363(14) 0.0281(5) Uani 1 1 d . . . . .
N15 N 0.24369(18) 0.28735(10) 0.73947(14) 0.0282(5) Uani 1 1 d . . . . .
O31 O 0.2937(2) 0.17255(10) 0.73120(17) 0.0546(6) Uani 1 1 d . . . . .
C16 C 0.2535(2) 0.40609(12) 0.72306(15) 0.0248(5) Uani 1 1 d . . . . .
C8 C 0.2449(2) 0.32922(12) 0.57820(17) 0.0305(6) Uani 1 1 d . . . . .
C3 C 0.3330(3) 0.32638(13) 0.54310(19) 0.0357(6) Uani 1 1 d . . . . .
C1 C 0.4251(2) 0.33058(12) 0.69628(19) 0.0322(6) Uani 1 1 d . . . . .
C32 C 0.3443(2) 0.50247(12) 0.67062(18) 0.0318(6) Uani 1 1 d . . . . .
C22 C 0.2478(3) 0.21856(13) 0.7575(2) 0.0376(6) Uani 1 1 d . . . . .
C19 C 0.1561(3) 0.46440(13) 0.79295(19) 0.0368(6) Uani 1 1 d . . . . .
H19 H 0.1093 0.4744 0.8263 0.044 Uiso 1 1 calc R U . . .
C33 C 0.3071(3) 0.51805(13) 0.58097(19) 0.0376(6) Uani 1 1 d . . . . .
C18 C 0.2058(3) 0.51009(13) 0.75508(19) 0.0378(7) Uani 1 1 d . . . . .
H18 H 0.2004 0.5575 0.7574 0.045 Uiso 1 1 calc R U . . .
C7 C 0.1382(3) 0.32415(14) 0.52018(19) 0.0387(7) Uani 1 1 d . . . . .
H7 H 0.0779 0.3256 0.5418 0.046 Uiso 1 1 calc R U . . .
C13 C 0.5185(2) 0.32722(14) 0.7687(2) 0.0412(7) Uani 1 1 d . . . . .
H13 H 0.5110 0.3272 0.8248 0.049 Uiso 1 1 calc R U . . .
C37 C 0.4535(3) 0.51442(14) 0.7236(2) 0.0427(7) Uani 1 1 d . . . . .
C2 C 0.4402(3) 0.32854(13) 0.6127(2) 0.0373(7) Uani 1 1 d . . . . .
C38 C 0.1863(3) 0.51181(15) 0.5285(2) 0.0440(7) Uani 1 1 d . . . . .
H38 H 0.1549 0.4738 0.5532 0.053 Uiso 1 1 calc R U . . .
C27 C 0.0167(2) 0.30406(15) 0.77225(19) 0.0364(6) Uani 1 1 d . . . . .
C23 C 0.2430(3) 0.31727(16) 0.92866(19) 0.0409(7) Uani 1 1 d . . . . .
C4 C 0.3157(3) 0.31896(16) 0.4530(2) 0.0498(8) Uani 1 1 d . . . . .
H4 H 0.3755 0.3168 0.4308 0.060 Uiso 1 1 calc R U . . .
C6 C 0.1205(3) 0.31699(17) 0.4305(2) 0.0504(8) Uani 1 1 d . . . . .
H6 H 0.0486 0.3137 0.3929 0.061 Uiso 1 1 calc R U . . .
C34 C 0.3846(3) 0.54315(16) 0.5440(2) 0.0526(9) Uani 1 1 d . . . . .
H34 H 0.3630 0.5539 0.4846 0.063 Uiso 1 1 calc R U . . .
C36 C 0.5266(3) 0.53950(16) 0.6821(3) 0.0556(9) Uani 1 1 d . . . . .
H36 H 0.5997 0.5477 0.7147 0.067 Uiso 1 1 calc R U . . .
C12 C 0.6241(3) 0.32378(17) 0.7581(3) 0.0526(8) Uani 1 1 d . . . . .
H12 H 0.6860 0.3209 0.8072 0.063 Uiso 1 1 calc R U . . .
C10 C 0.5449(3) 0.32662(16) 0.6022(3) 0.0504(8) Uani 1 1 d . . . . .
H10 H 0.5533 0.3267 0.5464 0.060 Uiso 1 1 calc R U . . .
C11 C 0.6371(3) 0.32460(18) 0.6761(3) 0.0582(10) Uani 1 1 d . . . . .
H11 H 0.7077 0.3238 0.6699 0.070 Uiso 1 1 calc R U . . .
C5 C 0.2084(4) 0.31480(18) 0.3973(2) 0.0573(10) Uani 1 1 d . . . . .
H5 H 0.1959 0.3105 0.3372 0.069 Uiso 1 1 calc R U . . .
C35 C 0.4933(3) 0.55255(18) 0.5934(3) 0.0644(11) Uani 1 1 d . . . . .
H35 H 0.5447 0.5678 0.5665 0.077 Uiso 1 1 calc R U . . .
C40 C 0.1236(3) 0.57713(18) 0.5386(3) 0.0605(9) Uani 1 1 d . . . . .
H40A H 0.1331 0.5852 0.5996 0.091 Uiso 1 1 calc R U . . .
H40B H 0.0463 0.5716 0.5080 0.091 Uiso 1 1 calc R U . . .
H40C H 0.1523 0.6154 0.5145 0.091 Uiso 1 1 calc R U . . .
C41 C 0.4875(3) 0.50413(17) 0.8222(2) 0.0571(9) Uani 1 1 d . . . . .
H41 H 0.4433 0.4665 0.8347 0.068 Uiso 1 1 calc R U . . .
C24 C 0.2359(3) 0.38820(19) 0.9664(2) 0.0584(9) Uani 1 1 d . . . . .
H24A H 0.2733 0.4208 0.9403 0.088 Uiso 1 1 calc R U . . .
H24B H 0.2703 0.3874 1.0287 0.088 Uiso 1 1 calc R U . . .
H24C H 0.1596 0.4012 0.9541 0.088 Uiso 1 1 calc R U . . .
B9 B 0.2934(2) 0.33683(13) 0.68492(19) 0.0264(6) Uani 1 1 d . . . . .
C39 C 0.1669(4) 0.4966(2) 0.4315(2) 0.0687(11) Uani 1 1 d . . . . .
H39A H 0.1892 0.5353 0.4040 0.103 Uiso 1 1 calc R U . . .
H39B H 0.0897 0.4876 0.4039 0.103 Uiso 1 1 calc R U . . .
H39C H 0.2095 0.4572 0.4256 0.103 Uiso 1 1 calc R U . . .
C26 C 0.3657(3) 0.3006(2) 0.9417(2) 0.0608(10) Uani 1 1 d . . . . .
H26A H 0.3717 0.2557 0.9190 0.091 Uiso 1 1 calc R U . . .
H26B H 0.4056 0.3019 1.0031 0.091 Uiso 1 1 calc R U . . .
H26C H 0.3962 0.3338 0.9112 0.091 Uiso 1 1 calc R U . . .
C43 C 0.4633(4) 0.5683(2) 0.8674(3) 0.0715(11) Uani 1 1 d . . . . .
H43A H 0.5089 0.6052 0.8586 0.107 Uiso 1 1 calc R U . . .
H43B H 0.4791 0.5596 0.9290 0.107 Uiso 1 1 calc R U . . .
H43C H 0.3868 0.5804 0.8430 0.107 Uiso 1 1 calc R U . . .
C25 C 0.1960(3) 0.2659(2) 0.9806(2) 0.0595(10) Uani 1 1 d . . . . .
H25A H 0.1200 0.2768 0.9738 0.089 Uiso 1 1 calc R U . . .
H25B H 0.2379 0.2682 1.0415 0.089 Uiso 1 1 calc R U . . .
H25C H 0.2007 0.2205 0.9590 0.089 Uiso 1 1 calc R U . . .
C28 C -0.0208(3) 0.3107(3) 0.6730(2) 0.0669(11) Uani 1 1 d . . . . .
H28A H 0.0053 0.3533 0.6567 0.100 Uiso 1 1 calc R U . . .
H28B H -0.1002 0.3096 0.6517 0.100 Uiso 1 1 calc R U . . .
H28C H 0.0087 0.2734 0.6479 0.100 Uiso 1 1 calc R U . . .
C29 C -0.0350(3) 0.3604(3) 0.8112(3) 0.0836(15) Uani 1 1 d . . . . .
H29A H 0.0017 0.3633 0.8730 0.125 Uiso 1 1 calc R U . . .
H29B H -0.1120 0.3506 0.8013 0.125 Uiso 1 1 calc R U . . .
H29C H -0.0276 0.4032 0.7840 0.125 Uiso 1 1 calc R U . . .
C42 C 0.6105(4) 0.4857(2) 0.8617(4) 0.0887(16) Uani 1 1 d . . . . .
H42A H 0.6284 0.4479 0.8301 0.133 Uiso 1 1 calc R U . . .
H42B H 0.6248 0.4732 0.9221 0.133 Uiso 1 1 calc R U . . .
H42C H 0.6553 0.5245 0.8576 0.133 Uiso 1 1 calc R U . . .
C30 C -0.0263(4) 0.2352(2) 0.7944(4) 0.0862(15) Uani 1 1 d . . . . .
H30A H 0.0044 0.1988 0.7687 0.129 Uiso 1 1 calc R U . . .
H30B H -0.1055 0.2342 0.7715 0.129 Uiso 1 1 calc R U . . .
H30C H -0.0046 0.2294 0.8569 0.129 Uiso 1 1 calc R U . . .
Cl1 Cl 0.8709(4) 0.39939(18) 1.02291(17) 0.2250(15) Uani 1 1 d . . . . .
Cl2 Cl 1.0628(3) 0.40539(16) 1.1691(3) 0.2159(13) Uani 1 1 d . . . . .
C44 C 0.9491(8) 0.3536(3) 1.1082(7) 0.161(4) Uani 1 1 d . . . . .
H44A H 0.9765 0.3127 1.0872 0.193 Uiso 1 1 calc R U . . .
H44B H 0.9051 0.3397 1.1456 0.193 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
P14 O21 1.8310(19) . ?
P14 N20 1.899(2) . ?
P14 N15 1.673(2) . ?
P14 C22 2.250(3) . ?
P14 C27 1.873(3) . ?
P14 C23 1.877(3) . ?
O21 C22 1.333(3) . ?
N17 C16 1.339(3) . ?
N17 C32 1.452(3) . ?
N17 C18 1.387(3) . ?
N20 C16 1.342(3) . ?
N20 C19 1.397(3) . ?
N15 C22 1.372(3) . ?
N15 B9 1.556(3) . ?
O31 C22 1.212(3) . ?
C16 B9 1.625(3) . ?
C8 C3 1.393(4) . ?
C8 C7 1.394(4) . ?
C8 B9 1.638(4) . ?
C3 C2 1.475(5) . ?
C3 C4 1.399(4) . ?
C1 C13 1.387(4) . ?
C1 C2 1.407(4) . ?
C1 B9 1.628(4) . ?
C32 C33 1.402(4) . ?
C32 C37 1.407(4) . ?
C19 H19 0.9300 . ?
C19 C18 1.338(4) . ?
C33 C38 1.513(4) . ?
C33 C34 1.379(4) . ?
C18 H18 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.391(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.400(4) . ?
C37 C36 1.382(5) . ?
C37 C41 1.518(5) . ?
C2 C10 1.387(4) . ?
C38 H38 0.9800 . ?
C38 C40 1.536(5) . ?
C38 C39 1.526(5) . ?
C27 C28 1.520(4) . ?
C27 C29 1.508(5) . ?
C27 C30 1.532(5) . ?
C23 C24 1.525(5) . ?
C23 C26 1.539(5) . ?
C23 C25 1.532(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.386(5) . ?
C6 H6 0.9300 . ?
C6 C5 1.371(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.379(6) . ?
C36 H36 0.9300 . ?
C36 C35 1.378(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.370(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.391(5) . ?
C11 H11 0.9300 . ?
C5 H5 0.9300 . ?
C35 H35 0.9300 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41 0.9800 . ?
C41 C43 1.522(5) . ?
C41 C42 1.539(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
Cl1 C44 1.683(10) . ?
Cl2 C44 1.789(10) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?

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
O21 P14 N20 158.26(9) . . ?
O21 P14 C22 36.33(9) . . ?
O21 P14 C27 94.96(12) . . ?
O21 P14 C23 91.84(12) . . ?
N20 P14 C22 121.94(10) . . ?
N15 P14 O21 73.72(9) . . ?
N15 P14 N20 84.59(9) . . ?
N15 P14 C22 37.40(10) . . ?
N15 P14 C27 121.30(12) . . ?
N15 P14 C23 120.62(13) . . ?
C27 P14 N20 97.57(11) . . ?
C27 P14 C22 112.76(12) . . ?
C27 P14 C23 117.06(13) . . ?
C23 P14 N20 98.15(12) . . ?
C23 P14 C22 108.84(13) . . ?
C22 O21 P14 89.22(15) . . ?
C16 N17 C32 125.3(2) . . ?
C16 N17 C18 109.1(2) . . ?
C18 N17 C32 125.1(2) . . ?
C16 N20 P14 114.24(16) . . ?
C16 N20 C19 107.8(2) . . ?
C19 N20 P14 137.55(18) . . ?
C22 N15 P14 94.82(17) . . ?
C22 N15 B9 136.9(2) . . ?
B9 N15 P14 128.06(16) . . ?
N17 C16 N20 108.2(2) . . ?
N17 C16 B9 134.1(2) . . ?
N20 C16 B9 117.6(2) . . ?
C3 C8 C7 117.5(3) . . ?
C3 C8 B9 109.2(2) . . ?
C7 C8 B9 133.2(2) . . ?
C8 C3 C2 111.2(2) . . ?
C8 C3 C4 121.6(3) . . ?
C4 C3 C2 127.2(3) . . ?
C13 C1 C2 117.8(3) . . ?
C13 C1 B9 133.3(3) . . ?
C2 C1 B9 108.9(2) . . ?
C33 C32 N17 119.0(2) . . ?
C33 C32 C37 123.2(3) . . ?
C37 C32 N17 117.9(2) . . ?
O21 C22 P14 54.45(13) . . ?
O21 C22 N15 102.2(2) . . ?
N15 C22 P14 47.79(12) . . ?
O31 C22 P14 176.8(2) . . ?
O31 C22 O21 127.6(2) . . ?
O31 C22 N15 130.1(3) . . ?
N20 C19 H19 126.0 . . ?
C18 C19 N20 108.0(2) . . ?
C18 C19 H19 126.0 . . ?
C32 C33 C38 121.5(3) . . ?
C34 C33 C32 116.9(3) . . ?
C34 C33 C38 121.5(3) . . ?
N17 C18 H18 126.6 . . ?
C19 C18 N17 106.8(2) . . ?
C19 C18 H18 126.6 . . ?
C8 C7 H7 119.4 . . ?
C6 C7 C8 121.2(3) . . ?
C6 C7 H7 119.4 . . ?
C1 C13 H13 119.8 . . ?
C1 C13 C12 120.5(3) . . ?
C12 C13 H13 119.8 . . ?
C32 C37 C41 121.6(3) . . ?
C36 C37 C32 116.7(3) . . ?
C36 C37 C41 121.7(3) . . ?
C1 C2 C3 111.2(2) . . ?
C10 C2 C3 127.2(3) . . ?
C10 C2 C1 121.6(3) . . ?
C33 C38 H38 107.6 . . ?
C33 C38 C40 110.1(3) . . ?
C33 C38 C39 114.0(3) . . ?
C40 C38 H38 107.6 . . ?
C39 C38 H38 107.6 . . ?
C39 C38 C40 109.8(3) . . ?
C28 C27 P14 106.7(2) . . ?
C28 C27 C30 107.2(3) . . ?
C29 C27 P14 113.2(2) . . ?
C29 C27 C28 109.3(3) . . ?
C29 C27 C30 108.4(3) . . ?
C30 C27 P14 111.8(2) . . ?
C24 C23 P14 115.7(2) . . ?
C24 C23 C26 108.4(3) . . ?
C24 C23 C25 107.5(3) . . ?
C26 C23 P14 105.8(2) . . ?
C25 C23 P14 110.1(2) . . ?
C25 C23 C26 109.2(3) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C7 C6 H6 119.8 . . ?
C5 C6 C7 120.3(3) . . ?
C5 C6 H6 119.8 . . ?
C33 C34 H34 119.4 . . ?
C35 C34 C33 121.3(3) . . ?
C35 C34 H34 119.4 . . ?
C37 C36 H36 119.3 . . ?
C35 C36 C37 121.3(3) . . ?
C35 C36 H36 119.3 . . ?
C13 C12 H12 119.7 . . ?
C11 C12 C13 120.7(3) . . ?
C11 C12 H12 119.7 . . ?
C2 C10 H10 120.4 . . ?
C2 C10 C11 119.2(3) . . ?
C11 C10 H10 120.4 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 120.6(3) . . ?
C36 C35 H35 119.7 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C41 H41 108.1 . . ?
C37 C41 C43 110.5(3) . . ?
C37 C41 C42 113.2(4) . . ?
C43 C41 H41 108.1 . . ?
C43 C41 C42 108.7(3) . . ?
C42 C41 H41 108.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N15 B9 C16 94.72(19) . . ?
N15 B9 C8 116.1(2) . . ?
N15 B9 C1 117.7(2) . . ?
C16 B9 C8 113.9(2) . . ?
C16 B9 C1 116.4(2) . . ?
C1 B9 C8 99.2(2) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Cl1 C44 Cl2 108.8(3) . . ?
Cl1 C44 H44A 109.9 . . ?
Cl1 C44 H44B 109.9 . . ?
Cl2 C44 H44A 109.9 . . ?
Cl2 C44 H44B 109.9 . . ?
H44A C44 H44B 108.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P14 O21 C22 N15 -1.6(2) . . . . ?
P14 O21 C22 O31 177.0(3) . . . . ?
P14 N20 C16 N17 -173.11(16) . . . . ?
P14 N20 C16 B9 10.4(3) . . . . ?
P14 N20 C19 C18 171.3(2) . . . . ?
P14 N15 C22 O21 1.7(2) . . . . ?
P14 N15 C22 O31 -176.8(3) . . . . ?
P14 N15 B9 C16 2.0(3) . . . . ?
P14 N15 B9 C8 -117.6(2) . . . . ?
P14 N15 B9 C1 125.2(2) . . . . ?
O21 P14 N20 C16 -3.4(4) . . . . ?
O21 P14 N20 C19 -175.3(3) . . . . ?
O21 P14 N15 C22 -1.30(17) . . . . ?
O21 P14 N15 B9 -176.3(2) . . . . ?
O21 P14 C27 C28 -96.8(2) . . . . ?
O21 P14 C27 C29 142.9(3) . . . . ?
O21 P14 C27 C30 20.1(3) . . . . ?
O21 P14 C23 C24 -170.2(3) . . . . ?
O21 P14 C23 C26 69.8(2) . . . . ?
O21 P14 C23 C25 -48.1(2) . . . . ?
N17 C16 B9 N15 177.0(3) . . . . ?
N17 C16 B9 C8 -61.7(4) . . . . ?
N17 C16 B9 C1 52.8(4) . . . . ?
N17 C32 C33 C38 6.3(4) . . . . ?
N17 C32 C33 C34 -177.4(2) . . . . ?
N17 C32 C37 C36 177.2(2) . . . . ?
N17 C32 C37 C41 -6.2(4) . . . . ?
N20 P14 O21 C22 -2.5(4) . . . . ?
N20 P14 N15 C22 177.27(18) . . . . ?
N20 P14 N15 B9 2.3(2) . . . . ?
N20 P14 C27 C28 65.4(3) . . . . ?
N20 P14 C27 C29 -54.9(3) . . . . ?
N20 P14 C27 C30 -177.7(3) . . . . ?
N20 P14 C23 C24 29.2(3) . . . . ?
N20 P14 C23 C26 -90.8(2) . . . . ?
N20 P14 C23 C25 151.3(2) . . . . ?
N20 C16 B9 N15 -7.7(3) . . . . ?
N20 C16 B9 C8 113.6(2) . . . . ?
N20 C16 B9 C1 -131.8(2) . . . . ?
N20 C19 C18 N17 0.3(3) . . . . ?
N15 P14 O21 C22 1.33(17) . . . . ?
N15 P14 N20 C16 -7.10(19) . . . . ?
N15 P14 N20 C19 -179.0(3) . . . . ?
N15 P14 C27 C28 -22.8(3) . . . . ?
N15 P14 C27 C29 -143.1(3) . . . . ?
N15 P14 C27 C30 94.1(3) . . . . ?
N15 P14 C23 C24 117.7(3) . . . . ?
N15 P14 C23 C26 -2.3(3) . . . . ?
N15 P14 C23 C25 -120.2(2) . . . . ?
C16 N17 C32 C33 94.3(3) . . . . ?
C16 N17 C32 C37 -86.3(3) . . . . ?
C16 N17 C18 C19 0.4(3) . . . . ?
C16 N20 C19 C18 -0.9(3) . . . . ?
C8 C3 C2 C1 2.0(3) . . . . ?
C8 C3 C2 C10 179.9(3) . . . . ?
C8 C3 C4 C5 0.4(4) . . . . ?
C8 C7 C6 C5 0.0(5) . . . . ?
C3 C8 C7 C6 -0.4(4) . . . . ?
C3 C8 B9 N15 -131.7(2) . . . . ?
C3 C8 B9 C16 119.7(2) . . . . ?
C3 C8 B9 C1 -4.6(2) . . . . ?
C3 C2 C10 C11 -175.8(3) . . . . ?
C3 C4 C5 C6 -0.9(5) . . . . ?
C1 C13 C12 C11 0.9(5) . . . . ?
C1 C2 C10 C11 1.9(4) . . . . ?
C32 N17 C16 N20 171.6(2) . . . . ?
C32 N17 C16 B9 -12.7(4) . . . . ?
C32 N17 C18 C19 -172.2(3) . . . . ?
C32 C33 C38 C40 84.1(3) . . . . ?
C32 C33 C38 C39 -152.0(3) . . . . ?
C32 C33 C34 C35 -0.2(4) . . . . ?
C32 C37 C36 C35 0.5(5) . . . . ?
C32 C37 C41 C43 -85.5(4) . . . . ?
C32 C37 C41 C42 152.3(3) . . . . ?
C22 P14 N20 C16 -5.1(2) . . . . ?
C22 P14 N20 C19 -177.1(3) . . . . ?
C22 P14 N15 B9 -175.0(3) . . . . ?
C22 P14 C27 C28 -64.0(3) . . . . ?
C22 P14 C27 C29 175.8(3) . . . . ?
C22 P14 C27 C30 52.9(3) . . . . ?
C22 P14 C23 C24 157.0(2) . . . . ?
C22 P14 C23 C26 37.0(3) . . . . ?
C22 P14 C23 C25 -80.8(2) . . . . ?
C22 N15 B9 C16 -170.6(3) . . . . ?
C22 N15 B9 C8 69.8(4) . . . . ?
C22 N15 B9 C1 -47.5(4) . . . . ?
C19 N20 C16 N17 1.2(3) . . . . ?
C19 N20 C16 B9 -175.3(2) . . . . ?
C33 C32 C37 C36 -3.4(4) . . . . ?
C33 C32 C37 C41 173.2(3) . . . . ?
C33 C34 C35 C36 -2.5(5) . . . . ?
C18 N17 C16 N20 -1.0(3) . . . . ?
C18 N17 C16 B9 174.7(3) . . . . ?
C18 N17 C32 C33 -94.3(3) . . . . ?
C18 N17 C32 C37 85.2(3) . . . . ?
C7 C8 C3 C2 -176.9(2) . . . . ?
C7 C8 C3 C4 0.2(4) . . . . ?
C7 C8 B9 N15 47.0(4) . . . . ?
C7 C8 B9 C16 -61.6(4) . . . . ?
C7 C8 B9 C1 174.1(3) . . . . ?
C7 C6 C5 C4 0.7(5) . . . . ?
C13 C1 C2 C3 174.9(2) . . . . ?
C13 C1 C2 C10 -3.1(4) . . . . ?
C13 C1 B9 N15 -48.3(4) . . . . ?
C13 C1 B9 C16 63.1(4) . . . . ?
C13 C1 B9 C8 -174.3(3) . . . . ?
C13 C12 C11 C10 -2.1(5) . . . . ?
C37 C32 C33 C38 -173.1(3) . . . . ?
C37 C32 C33 C34 3.2(4) . . . . ?
C37 C36 C35 C34 2.3(5) . . . . ?
C2 C3 C4 C5 177.0(3) . . . . ?
C2 C1 C13 C12 1.7(4) . . . . ?
C2 C1 B9 N15 131.8(2) . . . . ?
C2 C1 B9 C16 -116.9(2) . . . . ?
C2 C1 B9 C8 5.7(2) . . . . ?
C2 C10 C11 C12 0.7(5) . . . . ?
C38 C33 C34 C35 176.1(3) . . . . ?
C27 P14 O21 C22 122.52(19) . . . . ?
C27 P14 N20 C16 -128.02(19) . . . . ?
C27 P14 N20 C19 60.1(3) . . . . ?
C27 P14 N15 C22 -87.2(2) . . . . ?
C27 P14 N15 B9 97.9(2) . . . . ?
C27 P14 C23 C24 -73.7(3) . . . . ?
C27 P14 C23 C26 166.3(2) . . . . ?
C27 P14 C23 C25 48.5(3) . . . . ?
C23 P14 O21 C22 -120.11(19) . . . . ?
C23 P14 N20 C16 113.1(2) . . . . ?
C23 P14 N20 C19 -58.8(3) . . . . ?
C23 P14 N15 C22 81.0(2) . . . . ?
C23 P14 N15 B9 -94.0(2) . . . . ?
C23 P14 C27 C28 168.6(2) . . . . ?
C23 P14 C27 C29 48.3(3) . . . . ?
C23 P14 C27 C30 -74.5(3) . . . . ?
C4 C3 C2 C1 -174.9(3) . . . . ?
C4 C3 C2 C10 3.0(5) . . . . ?
C34 C33 C38 C40 -92.0(4) . . . . ?
C34 C33 C38 C39 31.9(4) . . . . ?
C36 C37 C41 C43 90.9(4) . . . . ?
C36 C37 C41 C42 -31.3(4) . . . . ?
C41 C37 C36 C35 -176.1(3) . . . . ?
B9 N15 C22 P14 174.2(4) . . . . ?
B9 N15 C22 O21 175.9(3) . . . . ?
B9 N15 C22 O31 -2.6(6) . . . . ?
B9 C8 C3 C2 2.1(3) . . . . ?
B9 C8 C3 C4 179.1(2) . . . . ?
B9 C8 C7 C6 -179.0(3) . . . . ?
B9 C1 C13 C12 -178.2(3) . . . . ?
B9 C1 C2 C3 -5.1(3) . . . . ?
B9 C1 C2 C10 176.8(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.145
_oxdiff_exptl_absorpt_empirical_full_min 0.358
####################################################################### 
# 
# 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_SN2024_compound_6a
_audit_block_doi                 10.5517/ccdc.csd.cc2kv6j5
_database_code_depnum_ccdc_archive 'CCDC 2378677'
loop_
_audit_author_name
_audit_author_address
'Yoichi Hoshimoto'
;Osaka University
Japan
;
_audit_update_record             
;
2024-08-20 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_audit_creation_date             2023-03-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C43 H52 B N4 O3 P S, C H2 Cl2'
_chemical_formula_sum            'C44 H54 B Cl2 N4 O3 P S'
_chemical_formula_weight         831.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C43 H52 B1 N4 O3 P1 S1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.24486(14)
_cell_length_b                   19.6073(3)
_cell_length_c                   24.3636(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.1494(14)
_cell_angle_gamma                90
_cell_volume                     4409.64(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17683
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      76.7910
_cell_measurement_theta_min      3.6430
_shelx_estimated_absorpt_T_max   0.792
_shelx_estimated_absorpt_T_min   0.527
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28396
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.634
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     77.00 156.00   0.50    1.00    --   96.50  32.00 173.00  158
  2  ω     55.00 122.00   0.50    0.20    --   43.05  32.00 173.00  134
  3  ω    114.00 140.00   0.50    1.00    --   96.50   0.00  90.00   52
  4  ω     71.00  97.00   0.50    1.00    --   96.50   0.00  90.00   52
  5  ω     24.00  64.00   0.50    1.00    --   96.50   0.00  90.00   80
  6  ω     22.00  49.00   0.50    1.00    --   96.50 -61.00 -90.00   54
  7  ω    -36.00   4.00   0.50    0.20    --   43.05 -19.00-150.00   80
  8  ω    -33.00  20.00   0.50    0.20    --   43.05 -37.00 -90.00  106
  9  ω    -34.00  -9.00   0.50    0.20    --   43.05 -32.00  14.00   50
 10  ω     22.00  49.00   0.50    1.00    --   96.50 -61.00 -60.00   54
 11  ω     77.00 106.00   0.50    1.00    --   96.50 -94.00 -90.00   58
 12  ω     36.00  66.00   0.50    1.00    --   96.50 -94.00 -90.00   60
 13  ω     74.00 100.00   0.50    1.00    --   96.50 -94.00  30.00   52
 14  ω     40.00  67.00   0.50    1.00    --   96.50 -94.00  30.00   54
 15  ω   -108.00 -36.00   0.50    0.20    --  -43.05 -32.00  14.00  144
 16  ω    -83.00 -38.00   0.50    1.00    -- -111.75  61.00 150.00   90
 17  ω   -124.00 -38.00   0.50    1.00    -- -111.75  77.00  30.00  172
 18  ω    -81.00 -37.00   0.50    1.00    -- -111.75  61.00  30.00   88
 19  ω    -79.00 -52.00   0.50    1.00    -- -111.75  61.00 -30.00   54
 20  ω    -72.00 -38.00   0.50    1.00    -- -111.75  45.00  30.00   68
 21  ω    -93.00 -40.00   0.50    1.00    -- -111.75  61.00 120.00  106
 22  ω    -72.00 -41.00   0.50    1.00    -- -111.75  45.00 120.00   62
 23  ω   -131.00 -88.00   0.50    1.00    -- -111.75 -32.00  14.00   86
 24  ω    -58.00  17.00   0.50    0.20    --  -43.05  32.00 173.00  150
 25  ω    -59.00 -32.00   0.50    1.00    -- -111.75  32.00 173.00   54
 26  ω    -66.00 -41.00   0.50    1.00    -- -111.75  45.00   0.00   50
 27  ω    -72.00 -37.00   0.50    1.00    -- -111.75  61.00 -60.00   70
 28  ω    -89.00 -38.00   0.50    1.00    -- -111.75  61.00-180.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0571786000
_diffrn_orient_matrix_UB_12      0.0022283000
_diffrn_orient_matrix_UB_13      -0.0581749000
_diffrn_orient_matrix_UB_21      -0.1418028000
_diffrn_orient_matrix_UB_22      -0.0327622000
_diffrn_orient_matrix_UB_23      -0.0233717000
_diffrn_orient_matrix_UB_31      -0.0667616000
_diffrn_orient_matrix_UB_32      0.0714201000
_diffrn_orient_matrix_UB_33      -0.0088805000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7360
_reflns_number_total             8046
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8046
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0409
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1318
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C15(H15), C26(H26), C24(H24), C3(H3), C32(H32), C48(H48), C33(H33),
 C31(H31), C25(H25), C27(H27), C14(H14), C30(H30), C13(H13), C52(H52), C51(H51),
  C49(H49)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C22(H22A,H22B,
 H22C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C41(H41A,
 H41B,H41C), C53(H53A,H53B,H53C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.26160(4) 0.33144(2) 0.78100(2) 0.01821(12) Uani 1 1 d . . . . .
S36 S 0.07260(4) 0.53640(2) 0.84039(2) 0.02254(12) Uani 1 1 d . . . . .
Cl1 Cl 0.13842(6) 0.92706(3) 0.23771(2) 0.05016(15) Uani 1 1 d . . . . .
Cl2 Cl 0.32759(7) 0.87207(3) 0.15734(2) 0.05324(16) Uani 1 1 d . . . . .
O6 O 0.20440(11) 0.39962(5) 0.83050(4) 0.0232(2) Uani 1 1 d . . . . .
O38 O -0.00482(12) 0.59740(5) 0.82354(4) 0.0284(2) Uani 1 1 d . . . . .
O37 O 0.21494(13) 0.54483(6) 0.86670(5) 0.0326(3) Uani 1 1 d . . . . .
N1 N 0.20718(12) 0.27358(6) 0.62849(5) 0.0180(2) Uani 1 1 d . . . . .
N4 N 0.28105(12) 0.28844(6) 0.71401(5) 0.0199(2) Uani 1 1 d . . . . .
N9 N 0.07508(13) 0.49021(6) 0.78523(5) 0.0210(2) Uani 1 1 d . . . . .
N8 N 0.16839(12) 0.39147(6) 0.74423(4) 0.0178(2) Uani 1 1 d . . . . .
C23 C -0.04677(15) 0.44532(7) 0.61520(6) 0.0204(3) Uani 1 1 d . . . . .
C20 C 0.34420(16) 0.33653(7) 0.53613(6) 0.0239(3) Uani 1 1 d . . . . .
H20 H 0.3716 0.3477 0.5754 0.029 Uiso 1 1 calc R U . . .
C2 C 0.29577(16) 0.21849(7) 0.64336(6) 0.0237(3) Uani 1 1 d . . . . .
H2 H 0.3193 0.1814 0.6204 0.028 Uiso 1 1 calc R U . . .
C15 C 0.10187(17) 0.32029(8) 0.48411(6) 0.0260(3) Uani 1 1 d . . . . .
H15 H 0.1406 0.3428 0.4537 0.031 Uiso 1 1 calc R U . . .
C56 C 0.20091(14) 0.31621(7) 0.67158(5) 0.0173(3) Uani 1 1 d . . . . .
C26 C -0.29896(16) 0.38608(8) 0.64805(7) 0.0284(3) Uani 1 1 d . . . . .
H26 H -0.3862 0.3668 0.6599 0.034 Uiso 1 1 calc R U . . .
C24 C -0.17720(17) 0.45970(8) 0.58644(6) 0.0271(3) Uani 1 1 d . . . . .
H24 H -0.1798 0.4896 0.5557 0.033 Uiso 1 1 calc R U . . .
C29 C 0.09523(15) 0.47687(7) 0.60711(5) 0.0204(3) Uani 1 1 d . . . . .
C3 C 0.34175(16) 0.22749(7) 0.69601(6) 0.0232(3) Uani 1 1 d . . . . .
H3 H 0.4041 0.1979 0.7172 0.028 Uiso 1 1 calc R U . . .
C16 C 0.18736(15) 0.31279(7) 0.53289(6) 0.0214(3) Uani 1 1 d . . . . .
C32 C 0.37105(17) 0.53185(7) 0.60858(6) 0.0259(3) Uani 1 1 d . . . . .
H32 H 0.4654 0.5511 0.6095 0.031 Uiso 1 1 calc R U . . .
C40 C 0.47695(18) 0.33694(9) 0.86668(6) 0.0325(4) Uani 1 1 d . . . . .
H40A H 0.4065 0.3655 0.8846 0.049 Uiso 1 1 calc R U . . .
H40B H 0.5753 0.3510 0.8788 0.049 Uiso 1 1 calc R U . . .
H40C H 0.4623 0.2891 0.8766 0.049 Uiso 1 1 calc R U . . .
C48 C 0.02722(19) 0.45281(8) 0.92839(6) 0.0308(3) Uani 1 1 d . . . . .
H48 H 0.1293 0.4468 0.9317 0.037 Uiso 1 1 calc R U . . .
C11 C 0.12376(15) 0.28019(7) 0.57657(6) 0.0193(3) Uani 1 1 d . . . . .
C28 C -0.03836(14) 0.39893(7) 0.65965(5) 0.0194(3) Uani 1 1 d . . . . .
C39 C 0.45615(16) 0.34513(8) 0.80387(6) 0.0254(3) Uani 1 1 d . . . . .
C33 C 0.34041(15) 0.47838(7) 0.64428(6) 0.0216(3) Uani 1 1 d . . . . .
H33 H 0.4151 0.4610 0.6687 0.026 Uiso 1 1 calc R U . . .
C43 C 0.16018(16) 0.26165(7) 0.81534(6) 0.0251(3) Uani 1 1 d . . . . .
C31 C 0.26382(17) 0.55670(8) 0.57186(6) 0.0272(3) Uani 1 1 d . . . . .
H31 H 0.2854 0.5925 0.5473 0.033 Uiso 1 1 calc R U . . .
C57 C 0.14416(14) 0.43230(7) 0.78772(5) 0.0195(3) Uani 1 1 d . . . . .
C25 C -0.30343(16) 0.42987(8) 0.60315(6) 0.0297(3) Uani 1 1 d . . . . .
H25 H -0.3932 0.4394 0.5839 0.036 Uiso 1 1 calc R U . . .
C27 C -0.16672(15) 0.37019(7) 0.67590(6) 0.0238(3) Uani 1 1 d . . . . .
H27 H -0.1647 0.3395 0.7061 0.029 Uiso 1 1 calc R U . . .
C34 C 0.20245(14) 0.45035(7) 0.64445(5) 0.0186(3) Uani 1 1 d . . . . .
C14 C -0.03825(18) 0.29537(8) 0.47947(6) 0.0295(3) Uani 1 1 d . . . . .
H14 H -0.0953 0.3020 0.4463 0.035 Uiso 1 1 calc R U . . .
C47 C -0.03602(17) 0.49368(7) 0.88701(6) 0.0247(3) Uani 1 1 d . . . . .
C30 C 0.12516(17) 0.52954(8) 0.57076(6) 0.0253(3) Uani 1 1 d . . . . .
H30 H 0.0515 0.5465 0.5456 0.030 Uiso 1 1 calc R U . . .
C50 C -0.2112(2) 0.42904(8) 0.96062(6) 0.0329(4) Uani 1 1 d . . . . .
C44 C 0.13388(19) 0.27690(9) 0.87593(7) 0.0331(4) Uani 1 1 d . . . . .
H44A H 0.2271 0.2823 0.8966 0.050 Uiso 1 1 calc R U . . .
H44B H 0.0803 0.2390 0.8915 0.050 Uiso 1 1 calc R U . . .
H44C H 0.0775 0.3190 0.8783 0.050 Uiso 1 1 calc R U . . .
C12 C -0.01678(15) 0.25188(7) 0.57232(6) 0.0226(3) Uani 1 1 d . . . . .
C13 C -0.09611(16) 0.26091(8) 0.52262(6) 0.0278(3) Uani 1 1 d . . . . .
H13 H -0.1916 0.2431 0.5183 0.033 Uiso 1 1 calc R U . . .
C52 C -0.18455(19) 0.50296(8) 0.88206(6) 0.0301(3) Uani 1 1 d . . . . .
H52 H -0.2269 0.5310 0.8537 0.036 Uiso 1 1 calc R U . . .
C51 C -0.2712(2) 0.47067(9) 0.91913(7) 0.0344(4) Uani 1 1 d . . . . .
H51 H -0.3731 0.4772 0.9160 0.041 Uiso 1 1 calc R U . . .
C17 C -0.07766(16) 0.21080(8) 0.61885(6) 0.0267(3) Uani 1 1 d . . . . .
H17 H -0.0416 0.2318 0.6544 0.032 Uiso 1 1 calc R U . . .
C46 C 0.0106(2) 0.25751(11) 0.78465(8) 0.0449(5) Uani 1 1 d . . . . .
H46A H -0.0384 0.3017 0.7868 0.067 Uiso 1 1 calc R U . . .
H46B H -0.0477 0.2223 0.8016 0.067 Uiso 1 1 calc R U . . .
H46C H 0.0225 0.2459 0.7460 0.067 Uiso 1 1 calc R U . . .
C22 C 0.44360(19) 0.27890(9) 0.51829(8) 0.0389(4) Uani 1 1 d . . . . .
H22A H 0.4351 0.2398 0.5430 0.058 Uiso 1 1 calc R U . . .
H22B H 0.5441 0.2950 0.5200 0.058 Uiso 1 1 calc R U . . .
H22C H 0.4150 0.2652 0.4806 0.058 Uiso 1 1 calc R U . . .
C55 C 0.3045(2) 0.93667(9) 0.20648(7) 0.0375(4) Uani 1 1 d . . . . .
H55A H 0.3850 0.9347 0.2350 0.045 Uiso 1 1 calc R U . . .
H55B H 0.3073 0.9818 0.1884 0.045 Uiso 1 1 calc R U . . .
C21 C 0.36794(18) 0.40034(8) 0.50177(6) 0.0296(3) Uani 1 1 d . . . . .
H21A H 0.3488 0.3897 0.4627 0.044 Uiso 1 1 calc R U . . .
H21B H 0.4683 0.4158 0.5079 0.044 Uiso 1 1 calc R U . . .
H21C H 0.3019 0.4364 0.5126 0.044 Uiso 1 1 calc R U . . .
C19 C -0.24389(18) 0.21006(9) 0.61748(8) 0.0362(4) Uani 1 1 d . . . . .
H19A H -0.2807 0.2565 0.6113 0.054 Uiso 1 1 calc R U . . .
H19B H -0.2758 0.1929 0.6526 0.054 Uiso 1 1 calc R U . . .
H19C H -0.2813 0.1803 0.5876 0.054 Uiso 1 1 calc R U . . .
C49 C -0.0620(2) 0.42077(9) 0.96503(6) 0.0344(4) Uani 1 1 d . . . . .
H49 H -0.0197 0.3928 0.9935 0.041 Uiso 1 1 calc R U . . .
C18 C -0.02362(18) 0.13690(8) 0.61798(8) 0.0352(4) Uani 1 1 d . . . . .
H18A H -0.0586 0.1150 0.5836 0.053 Uiso 1 1 calc R U . . .
H18B H -0.0603 0.1120 0.6492 0.053 Uiso 1 1 calc R U . . .
H18C H 0.0825 0.1365 0.6206 0.053 Uiso 1 1 calc R U . . .
C41 C 0.49539(18) 0.41850(8) 0.78844(7) 0.0325(4) Uani 1 1 d . . . . .
H41A H 0.4810 0.4245 0.7486 0.049 Uiso 1 1 calc R U . . .
H41B H 0.5970 0.4274 0.7998 0.049 Uiso 1 1 calc R U . . .
H41C H 0.4332 0.4505 0.8071 0.049 Uiso 1 1 calc R U . . .
B1 B 0.13066(15) 0.39063(8) 0.68090(6) 0.0173(3) Uani 1 1 d . . . . .
C53 C -0.3066(2) 0.39448(11) 1.00055(7) 0.0451(5) Uani 1 1 d . . . . .
H53A H -0.2744 0.4069 1.0382 0.068 Uiso 1 1 calc R U . . .
H53B H -0.3004 0.3449 0.9961 0.068 Uiso 1 1 calc R U . . .
H53C H -0.4072 0.4092 0.9933 0.068 Uiso 1 1 calc R U . . .
C42 C 0.56200(16) 0.29655(9) 0.77749(7) 0.0337(4) Uani 1 1 d . . . . .
H42A H 0.5401 0.2495 0.7877 0.051 Uiso 1 1 calc R U . . .
H42B H 0.6614 0.3078 0.7905 0.051 Uiso 1 1 calc R U . . .
H42C H 0.5522 0.3013 0.7374 0.051 Uiso 1 1 calc R U . . .
C45 C 0.2377(2) 0.19271(9) 0.81293(8) 0.0420(4) Uani 1 1 d . . . . .
H45A H 0.2323 0.1759 0.7750 0.063 Uiso 1 1 calc R U . . .
H45B H 0.1910 0.1599 0.8366 0.063 Uiso 1 1 calc R U . . .
H45C H 0.3395 0.1982 0.8256 0.063 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
P1 O6 1.8950(10) . ?
P1 N4 1.8545(12) . ?
P1 N8 1.6871(11) . ?
P1 C39 1.8728(15) . ?
P1 C43 1.8808(15) . ?
P1 C57 2.2663(14) . ?
S36 O38 1.4419(11) . ?
S36 O37 1.4412(12) . ?
S36 N9 1.6218(12) . ?
S36 C47 1.7678(15) . ?
Cl1 C55 1.7606(19) . ?
Cl2 C55 1.7638(18) . ?
O6 C57 1.3202(17) . ?
N1 C2 1.3915(18) . ?
N1 C56 1.3456(18) . ?
N1 C11 1.4507(17) . ?
N4 C56 1.3528(17) . ?
N4 C3 1.4009(18) . ?
N9 C57 1.3027(19) . ?
N8 C57 1.3563(18) . ?
N8 B1 1.5631(17) . ?
C23 C24 1.390(2) . ?
C23 C29 1.474(2) . ?
C23 C28 1.413(2) . ?
C20 H20 1.0000 . ?
C20 C16 1.521(2) . ?
C20 C22 1.534(2) . ?
C20 C21 1.528(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.341(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.398(2) . ?
C15 C14 1.383(2) . ?
C56 B1 1.6182(19) . ?
C26 H26 0.9500 . ?
C26 C25 1.389(2) . ?
C26 C27 1.400(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(2) . ?
C29 C34 1.4077(19) . ?
C29 C30 1.398(2) . ?
C3 H3 0.9500 . ?
C16 C11 1.398(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.401(2) . ?
C32 C31 1.387(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C40 C39 1.540(2) . ?
C48 H48 0.9500 . ?
C48 C47 1.391(2) . ?
C48 C49 1.397(2) . ?
C11 C12 1.412(2) . ?
C28 C27 1.391(2) . ?
C28 B1 1.6271(19) . ?
C39 C41 1.535(2) . ?
C39 C42 1.532(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.389(2) . ?
C43 C44 1.539(2) . ?
C43 C46 1.538(2) . ?
C43 C45 1.533(2) . ?
C31 H31 0.9500 . ?
C31 C30 1.387(2) . ?
C25 H25 0.9500 . ?
C27 H27 0.9500 . ?
C34 B1 1.6325(19) . ?
C14 H14 0.9500 . ?
C14 C13 1.382(2) . ?
C47 C52 1.384(2) . ?
C30 H30 0.9500 . ?
C50 C51 1.391(3) . ?
C50 C49 1.387(3) . ?
C50 C53 1.510(2) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C12 C13 1.392(2) . ?
C12 C17 1.523(2) . ?
C13 H13 0.9500 . ?
C52 H52 0.9500 . ?
C52 C51 1.392(2) . ?
C51 H51 0.9500 . ?
C17 H17 1.0000 . ?
C17 C19 1.535(2) . ?
C17 C18 1.533(2) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C49 H49 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 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
O6 P1 C57 35.60(5) . . ?
N4 P1 O6 157.62(5) . . ?
N4 P1 C39 100.90(6) . . ?
N4 P1 C43 97.79(6) . . ?
N4 P1 C57 122.02(5) . . ?
N8 P1 O6 72.14(5) . . ?
N8 P1 N4 85.48(5) . . ?
N8 P1 C39 120.81(6) . . ?
N8 P1 C43 119.42(6) . . ?
N8 P1 C57 36.55(5) . . ?
C39 P1 O6 90.38(6) . . ?
C39 P1 C43 117.78(7) . . ?
C39 P1 C57 108.03(6) . . ?
C43 P1 O6 93.83(6) . . ?
C43 P1 C57 110.50(6) . . ?
O38 S36 N9 104.87(6) . . ?
O38 S36 C47 106.58(7) . . ?
O37 S36 O38 117.28(7) . . ?
O37 S36 N9 112.25(7) . . ?
O37 S36 C47 107.79(7) . . ?
N9 S36 C47 107.59(6) . . ?
C57 O6 P1 87.73(8) . . ?
C2 N1 C11 124.98(12) . . ?
C56 N1 C2 109.22(11) . . ?
C56 N1 C11 125.54(11) . . ?
C56 N4 P1 114.46(9) . . ?
C56 N4 C3 108.43(11) . . ?
C3 N4 P1 136.32(10) . . ?
C57 N9 S36 118.52(10) . . ?
C57 N8 P1 95.65(8) . . ?
C57 N8 B1 137.72(11) . . ?
B1 N8 P1 126.62(9) . . ?
C24 C23 C29 127.00(13) . . ?
C24 C23 C28 121.78(14) . . ?
C28 C23 C29 111.14(12) . . ?
C16 C20 H20 107.9 . . ?
C16 C20 C22 110.13(13) . . ?
C16 C20 C21 112.80(12) . . ?
C22 C20 H20 107.9 . . ?
C21 C20 H20 107.9 . . ?
C21 C20 C22 109.96(13) . . ?
N1 C2 H2 126.3 . . ?
C3 C2 N1 107.34(12) . . ?
C3 C2 H2 126.3 . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.02(14) . . ?
N1 C56 N4 107.51(11) . . ?
N1 C56 B1 134.78(12) . . ?
N4 C56 B1 117.57(11) . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.42(14) . . ?
C27 C26 H26 119.8 . . ?
C23 C24 H24 120.4 . . ?
C25 C24 C23 119.16(14) . . ?
C25 C24 H24 120.4 . . ?
C34 C29 C23 111.05(12) . . ?
C30 C29 C23 127.11(13) . . ?
C30 C29 C34 121.70(13) . . ?
N4 C3 H3 126.3 . . ?
C2 C3 N4 107.48(12) . . ?
C2 C3 H3 126.3 . . ?
C15 C16 C20 120.31(13) . . ?
C11 C16 C20 122.68(12) . . ?
C11 C16 C15 116.95(13) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C31 C32 C33 120.11(14) . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
C47 C48 H48 120.6 . . ?
C47 C48 C49 118.86(16) . . ?
C49 C48 H48 120.6 . . ?
C16 C11 N1 118.61(12) . . ?
C16 C11 C12 123.22(13) . . ?
C12 C11 N1 118.16(12) . . ?
C23 C28 B1 108.64(12) . . ?
C27 C28 C23 117.84(12) . . ?
C27 C28 B1 133.51(12) . . ?
C40 C39 P1 110.25(11) . . ?
C41 C39 P1 107.30(10) . . ?
C41 C39 C40 108.83(13) . . ?
C42 C39 P1 114.28(11) . . ?
C42 C39 C40 107.71(13) . . ?
C42 C39 C41 108.35(13) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 C32 120.99(13) . . ?
C34 C33 H33 119.5 . . ?
C44 C43 P1 113.22(10) . . ?
C46 C43 P1 106.22(10) . . ?
C46 C43 C44 106.94(14) . . ?
C45 C43 P1 112.27(11) . . ?
C45 C43 C44 107.88(13) . . ?
C45 C43 C46 110.17(15) . . ?
C32 C31 H31 119.8 . . ?
C32 C31 C30 120.32(13) . . ?
C30 C31 H31 119.8 . . ?
O6 C57 P1 56.67(7) . . ?
O6 C57 N8 104.46(11) . . ?
N9 C57 P1 173.20(10) . . ?
N9 C57 O6 130.11(12) . . ?
N9 C57 N8 125.43(12) . . ?
N8 C57 P1 47.80(6) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 C26 120.19(13) . . ?
C24 C25 H25 119.9 . . ?
C26 C27 H27 119.7 . . ?
C28 C27 C26 120.52(14) . . ?
C28 C27 H27 119.7 . . ?
C29 C34 B1 108.89(12) . . ?
C33 C34 C29 117.77(13) . . ?
C33 C34 B1 133.34(12) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 C15 120.69(14) . . ?
C13 C14 H14 119.7 . . ?
C48 C47 S36 120.51(13) . . ?
C52 C47 S36 118.54(12) . . ?
C52 C47 C48 120.94(14) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 C29 119.09(13) . . ?
C31 C30 H30 120.5 . . ?
C51 C50 C53 120.51(17) . . ?
C49 C50 C51 118.70(15) . . ?
C49 C50 C53 120.78(16) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C11 C12 C17 121.98(13) . . ?
C13 C12 C11 116.90(13) . . ?
C13 C12 C17 121.07(13) . . ?
C14 C13 C12 121.10(14) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C47 C52 H52 120.4 . . ?
C47 C52 C51 119.17(15) . . ?
C51 C52 H52 120.4 . . ?
C50 C51 C52 121.17(17) . . ?
C50 C51 H51 119.4 . . ?
C52 C51 H51 119.4 . . ?
C12 C17 H17 107.9 . . ?
C12 C17 C19 113.52(13) . . ?
C12 C17 C18 110.81(12) . . ?
C19 C17 H17 107.9 . . ?
C18 C17 H17 107.9 . . ?
C18 C17 C19 108.50(13) . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Cl1 C55 Cl2 110.95(10) . . ?
Cl1 C55 H55A 109.4 . . ?
Cl1 C55 H55B 109.4 . . ?
Cl2 C55 H55A 109.4 . . ?
Cl2 C55 H55B 109.4 . . ?
H55A C55 H55B 108.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C48 C49 H49 119.4 . . ?
C50 C49 C48 121.15(15) . . ?
C50 C49 H49 119.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N8 B1 C56 94.51(10) . . ?
N8 B1 C28 118.12(11) . . ?
N8 B1 C34 117.00(11) . . ?
C56 B1 C28 115.55(11) . . ?
C56 B1 C34 113.09(10) . . ?
C28 B1 C34 99.62(10) . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 O6 C57 N9 -179.32(14) . . . . ?
P1 O6 C57 N8 1.11(10) . . . . ?
P1 N4 C56 N1 -169.97(9) . . . . ?
P1 N4 C56 B1 13.63(15) . . . . ?
P1 N4 C3 C2 167.73(11) . . . . ?
P1 N8 C57 O6 -1.26(11) . . . . ?
P1 N8 C57 N9 179.15(12) . . . . ?
P1 N8 B1 C56 3.33(13) . . . . ?
P1 N8 B1 C28 125.52(11) . . . . ?
P1 N8 B1 C34 -115.46(12) . . . . ?
S36 N9 C57 O6 7.5(2) . . . . ?
S36 N9 C57 N8 -172.97(10) . . . . ?
S36 C47 C52 C51 -178.80(12) . . . . ?
O6 P1 N4 C56 -10.4(2) . . . . ?
O6 P1 N4 C3 -178.74(13) . . . . ?
O6 P1 N8 C57 0.89(8) . . . . ?
O6 P1 N8 B1 -178.19(12) . . . . ?
O6 P1 C39 C40 55.09(11) . . . . ?
O6 P1 C39 C41 -63.28(11) . . . . ?
O6 P1 C39 C42 176.56(11) . . . . ?
O6 P1 C43 C44 -23.90(12) . . . . ?
O6 P1 C43 C46 93.16(12) . . . . ?
O6 P1 C43 C45 -146.36(12) . . . . ?
O38 S36 N9 C57 177.27(11) . . . . ?
O38 S36 C47 C48 -150.90(12) . . . . ?
O38 S36 C47 C52 27.80(13) . . . . ?
O37 S36 N9 C57 48.88(13) . . . . ?
O37 S36 C47 C48 -24.18(14) . . . . ?
O37 S36 C47 C52 154.51(12) . . . . ?
N1 C2 C3 N4 0.16(16) . . . . ?
N1 C56 B1 N8 174.58(14) . . . . ?
N1 C56 B1 C28 50.4(2) . . . . ?
N1 C56 B1 C34 -63.50(19) . . . . ?
N1 C11 C12 C13 177.96(12) . . . . ?
N1 C11 C12 C17 -4.43(19) . . . . ?
N4 P1 O6 C57 0.67(17) . . . . ?
N4 P1 N8 C57 -178.51(9) . . . . ?
N4 P1 N8 B1 2.41(11) . . . . ?
N4 P1 C39 C40 -144.36(11) . . . . ?
N4 P1 C39 C41 97.27(11) . . . . ?
N4 P1 C39 C42 -22.89(12) . . . . ?
N4 P1 C43 C44 175.28(11) . . . . ?
N4 P1 C43 C46 -67.66(13) . . . . ?
N4 P1 C43 C45 52.82(12) . . . . ?
N4 C56 B1 N8 -10.26(14) . . . . ?
N4 C56 B1 C28 -134.43(12) . . . . ?
N4 C56 B1 C34 111.66(13) . . . . ?
N9 S36 C47 C48 97.07(13) . . . . ?
N9 S36 C47 C52 -84.24(13) . . . . ?
N8 P1 O6 C57 -0.91(8) . . . . ?
N8 P1 N4 C56 -8.93(10) . . . . ?
N8 P1 N4 C3 -177.24(14) . . . . ?
N8 P1 C39 C40 124.41(11) . . . . ?
N8 P1 C39 C41 6.04(14) . . . . ?
N8 P1 C39 C42 -114.11(11) . . . . ?
N8 P1 C43 C44 -95.53(12) . . . . ?
N8 P1 C43 C46 21.53(14) . . . . ?
N8 P1 C43 C45 142.00(12) . . . . ?
C23 C24 C25 C26 -0.1(2) . . . . ?
C23 C29 C34 C33 -175.88(12) . . . . ?
C23 C29 C34 B1 3.27(15) . . . . ?
C23 C29 C30 C31 174.80(13) . . . . ?
C23 C28 C27 C26 1.3(2) . . . . ?
C23 C28 B1 N8 135.77(12) . . . . ?
C23 C28 B1 C56 -113.48(13) . . . . ?
C23 C28 B1 C34 7.98(13) . . . . ?
C20 C16 C11 N1 5.01(19) . . . . ?
C20 C16 C11 C12 -173.47(13) . . . . ?
C2 N1 C56 N4 -1.46(15) . . . . ?
C2 N1 C56 B1 174.05(14) . . . . ?
C2 N1 C11 C16 -90.98(16) . . . . ?
C2 N1 C11 C12 87.58(16) . . . . ?
C15 C16 C11 N1 -177.84(12) . . . . ?
C15 C16 C11 C12 3.7(2) . . . . ?
C15 C14 C13 C12 1.7(2) . . . . ?
C56 N1 C2 C3 0.80(16) . . . . ?
C56 N1 C11 C16 95.58(16) . . . . ?
C56 N1 C11 C12 -85.86(16) . . . . ?
C56 N4 C3 C2 -1.06(16) . . . . ?
C24 C23 C29 C34 178.97(14) . . . . ?
C24 C23 C29 C30 3.2(2) . . . . ?
C24 C23 C28 C27 -3.2(2) . . . . ?
C24 C23 C28 B1 176.31(13) . . . . ?
C29 C23 C24 C25 -173.68(14) . . . . ?
C29 C23 C28 C27 173.66(12) . . . . ?
C29 C23 C28 B1 -6.84(15) . . . . ?
C29 C34 B1 N8 -135.19(12) . . . . ?
C29 C34 B1 C56 116.56(12) . . . . ?
C29 C34 B1 C28 -6.66(13) . . . . ?
C3 N4 C56 N1 1.54(15) . . . . ?
C3 N4 C56 B1 -174.86(11) . . . . ?
C16 C15 C14 C13 -1.6(2) . . . . ?
C16 C11 C12 C13 -3.5(2) . . . . ?
C16 C11 C12 C17 174.05(13) . . . . ?
C32 C33 C34 C29 0.8(2) . . . . ?
C32 C33 C34 B1 -178.09(14) . . . . ?
C32 C31 C30 C29 0.0(2) . . . . ?
C48 C47 C52 C51 -0.1(2) . . . . ?
C11 N1 C2 C3 -173.55(13) . . . . ?
C11 N1 C56 N4 172.86(12) . . . . ?
C11 N1 C56 B1 -11.6(2) . . . . ?
C11 C12 C13 C14 0.8(2) . . . . ?
C11 C12 C17 C19 155.93(13) . . . . ?
C11 C12 C17 C18 -81.67(17) . . . . ?
C28 C23 C24 C25 2.6(2) . . . . ?
C28 C23 C29 C34 2.32(16) . . . . ?
C28 C23 C29 C30 -173.44(13) . . . . ?
C39 P1 O6 C57 121.50(8) . . . . ?
C39 P1 N4 C56 -129.46(10) . . . . ?
C39 P1 N4 C3 62.23(15) . . . . ?
C39 P1 N8 C57 -78.51(10) . . . . ?
C39 P1 N8 B1 102.41(12) . . . . ?
C39 P1 C43 C44 68.56(13) . . . . ?
C39 P1 C43 C46 -174.38(12) . . . . ?
C39 P1 C43 C45 -53.91(14) . . . . ?
C33 C32 C31 C30 0.9(2) . . . . ?
C33 C34 B1 N8 43.8(2) . . . . ?
C33 C34 B1 C56 -64.47(19) . . . . ?
C33 C34 B1 C28 172.32(14) . . . . ?
C43 P1 O6 C57 -120.62(8) . . . . ?
C43 P1 N4 C56 110.18(10) . . . . ?
C43 P1 N4 C3 -58.13(15) . . . . ?
C43 P1 N8 C57 85.09(10) . . . . ?
C43 P1 N8 B1 -93.99(12) . . . . ?
C43 P1 C39 C40 -39.45(14) . . . . ?
C43 P1 C39 C41 -157.82(10) . . . . ?
C43 P1 C39 C42 82.03(13) . . . . ?
C31 C32 C33 C34 -1.4(2) . . . . ?
C57 P1 N4 C56 -9.98(12) . . . . ?
C57 P1 N4 C3 -178.29(13) . . . . ?
C57 P1 N8 B1 -179.08(16) . . . . ?
C57 P1 C39 C40 86.55(11) . . . . ?
C57 P1 C39 C41 -31.82(12) . . . . ?
C57 P1 C39 C42 -151.97(10) . . . . ?
C57 P1 C43 C44 -56.23(12) . . . . ?
C57 P1 C43 C46 60.83(13) . . . . ?
C57 P1 C43 C45 -178.69(11) . . . . ?
C57 N8 B1 C56 -175.31(15) . . . . ?
C57 N8 B1 C28 -53.1(2) . . . . ?
C57 N8 B1 C34 65.9(2) . . . . ?
C25 C26 C27 C28 1.1(2) . . . . ?
C27 C26 C25 C24 -1.7(2) . . . . ?
C27 C28 B1 N8 -44.8(2) . . . . ?
C27 C28 B1 C56 65.91(19) . . . . ?
C27 C28 B1 C34 -172.63(15) . . . . ?
C34 C29 C30 C31 -0.5(2) . . . . ?
C14 C15 C16 C20 176.18(13) . . . . ?
C14 C15 C16 C11 -1.0(2) . . . . ?
C47 S36 N9 C57 -69.53(13) . . . . ?
C47 C48 C49 C50 0.1(2) . . . . ?
C47 C52 C51 C50 -0.5(2) . . . . ?
C30 C29 C34 C33 0.1(2) . . . . ?
C30 C29 C34 B1 179.29(12) . . . . ?
C13 C12 C17 C19 -26.6(2) . . . . ?
C13 C12 C17 C18 95.83(16) . . . . ?
C51 C50 C49 C48 -0.6(2) . . . . ?
C17 C12 C13 C14 -176.86(14) . . . . ?
C22 C20 C16 C15 -88.75(17) . . . . ?
C22 C20 C16 C11 88.31(17) . . . . ?
C21 C20 C16 C15 34.51(18) . . . . ?
C21 C20 C16 C11 -148.43(13) . . . . ?
C49 C48 C47 S36 178.94(12) . . . . ?
C49 C48 C47 C52 0.3(2) . . . . ?
C49 C50 C51 C52 0.8(2) . . . . ?
B1 N8 C57 P1 178.90(19) . . . . ?
B1 N8 C57 O6 177.65(14) . . . . ?
B1 N8 C57 N9 -2.0(2) . . . . ?
B1 C28 C27 C26 -178.07(14) . . . . ?
C53 C50 C51 C52 179.90(16) . . . . ?
C53 C50 C49 C48 -179.72(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.562
_oxdiff_exptl_absorpt_empirical_full_min 0.627
####################################################################### 
# 
# 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_compound_8a
_audit_block_doi                 10.5517/ccdc.csd.cc2f6qs5
_database_code_depnum_ccdc_archive 'CCDC 2240797'
loop_
_audit_author_name
_audit_author_address
'Yoichi Hoshimoto'
;Osaka University
Japan
;
_audit_update_record             
;
2023-02-09 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_audit_creation_date             2023-02-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C4 H8 O), C54 H54 B2 N4'
_chemical_formula_sum            'C62 H70 B2 N4 O2'
_chemical_formula_weight         924.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C244 H292 B12 N24 O1 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.7952(3)
_cell_length_b                   19.5207(4)
_cell_length_c                   20.9941(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.160(2)
_cell_angle_gamma                90
_cell_volume                     5222.47(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29121
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      77.3120
_cell_measurement_theta_min      3.4890
_shelx_estimated_absorpt_T_max   0.974
_shelx_estimated_absorpt_T_min   0.948
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9444
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         4.143
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     42.00 124.00   0.50    1.44    --   50.04  23.00 -26.00  164
  2  ω     13.00  58.00   0.50    1.44    --   50.04 -23.00 167.00   90
  3  ω    -55.00 -29.00   0.50    1.44    --  -53.16  23.00 -26.00   52
  4  ω   -100.00 -48.00   0.50    1.44    --  -53.16 -23.00 167.00  104
  5  ω     75.00 100.00   0.50    1.44    --   66.50  23.00 -26.00   50
  6  ω     34.00  59.00   0.50    1.44    --   66.50 -23.00 167.00   50
  7  ω   -163.00-137.00   0.50    1.44    -- -105.75 -23.00 167.00   52
  8  ω   -113.00 -38.00   0.50    1.44    -- -105.75  23.00 -26.00  150
  9  ω     90.00 120.00   0.50    1.44    --   50.04 125.00-150.00   60
 10  ω   -124.00 -74.00   0.50    1.44    --  -53.16-125.00 -30.00  100
 11  ω     -5.00  72.00   0.50    1.44    --   66.50 -37.00 -30.00  154
 12  ω   -100.00 -34.00   0.50    1.44    -- -105.75  37.00 150.00  132
 13  ω   -118.00 -41.00   0.50    1.44    -- -105.75  57.00-120.00  154
 14  ω   -173.00 -99.00   0.50    1.44    -- -105.75 -19.00  90.00  148
 15  ω   -138.00-105.00   0.50    1.44    -- -105.75 -19.00-180.00   66
 16  ω    -68.00 -42.00   0.50    1.44    -- -105.75 125.00   0.00   52
 17  ω   -106.00 -79.00   0.50    1.44    -- -105.75 125.00   0.00   54
 18  ω   -105.00 -35.00   0.50    1.44    -- -105.75  19.00  60.00  140
 19  ω   -112.00 -60.00   0.50    1.44    -- -105.75  57.00 150.00  104
 20  ω    -99.00 -62.00   0.50    1.44    -- -105.75 125.00 -30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1104253000
_diffrn_orient_matrix_UB_12      0.0078792000
_diffrn_orient_matrix_UB_13      0.0229013000
_diffrn_orient_matrix_UB_21      0.0491048000
_diffrn_orient_matrix_UB_22      0.0223683000
_diffrn_orient_matrix_UB_23      0.0664665000
_diffrn_orient_matrix_UB_31      -0.0029878000
_diffrn_orient_matrix_UB_32      0.0752665000
_diffrn_orient_matrix_UB_33      -0.0220764000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8419
_reflns_number_total             9444
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         9444
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0793
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1113P)²+9.7025P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2191
_refine_ls_wR_factor_ref         0.2258
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9919(5)
 0.0081(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C5-C4 \\sim C5-C4A
 with sigma of 0.02
 C3-C4 \\sim C3-C4A
 with sigma of 0.02
 C70-C69 \\sim C70-C69A
 with sigma of 0.02
 C68-C69 \\sim C68-C69A
 with sigma of 0.02
4. Others
 Sof(H5BC)=Sof(H5BD)=Sof(H3BC)=Sof(H3BD)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(1)
 Sof(H5AA)=Sof(H5AB)=Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(1)
 Sof(H70C)=Sof(H70D)=Sof(H68C)=Sof(H68D)=Sof(C69A)=Sof(H69C)=Sof(H69D)=1-FVAR(2)
 Sof(H70A)=Sof(H70B)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=Sof(H69B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C27(H27), C39(H39), C36(H36), C24(H24)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C67(H67A,H67B), C5(H5AA,H5AB), C5(H5BC,H5BD), C70(H70A,H70B),
 C70(H70C,H70D), C3(H3AA,H3AB), C3(H3BC,H3BD), C68(H68A,H68B), C68(H68C,H68D),
 C69(H69A,H69B), C4(H4A,H4B), C4A(H4AA,H4AB), C69A(H69C,H69D)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C7(H7), C58(H58), C13(H13), C22(H22), C62(H62), C61(H61),
 C55(H55), C64(H64), C63(H63), C20(H20), C34(H34), C33(H33), C56(H56), C21(H21),
  C32(H32), C57(H57), C49(H49), C43(H43), C50(H50), C52(H52), C45(H45),
 C46(H46), C51(H51), C44(H44)
5.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C41(H41A,H41B,
 H41C), C40(H40A,H40B,H40C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C), C25(H25A,
 H25B,H25C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.78032(15) 0.10539(10) 0.29894(10) 0.0319(5) Uani 1 1 d . . . . .
N6 N 0.74580(16) 0.29959(11) 0.62699(10) 0.0191(4) Uani 1 1 d . . . . .
N9 N 0.59449(16) 0.28972(11) 0.57222(10) 0.0197(4) Uani 1 1 d . . . . .
O66 O 0.46241(17) 0.40079(11) 0.73836(11) 0.0381(5) Uani 1 1 d . . . . .
N15 N 0.65413(16) 0.22256(10) 0.46091(10) 0.0191(4) Uani 1 1 d . . . . .
N12 N 0.50147(16) 0.20148(11) 0.41112(10) 0.0202(4) Uani 1 1 d . . . . .
C17 C 0.69718(19) 0.27787(12) 0.57007(12) 0.0179(5) Uani 1 1 d . . . . .
C11 C 0.55090(19) 0.23150(12) 0.46441(12) 0.0188(5) Uani 1 1 d . . . . .
C59 C 0.9297(2) 0.21109(13) 0.49292(12) 0.0218(5) Uani 1 1 d . . . . .
C54 C 0.83722(19) 0.18999(13) 0.51896(12) 0.0196(5) Uani 1 1 d . . . . .
C31 C 0.3374(2) 0.13662(14) 0.40850(13) 0.0239(5) Uani 1 1 d . . . . .
C60 C 0.9162(2) 0.27930(13) 0.46295(12) 0.0217(5) Uani 1 1 d . . . . .
C30 C 0.38982(19) 0.19681(13) 0.39327(12) 0.0205(5) Uani 1 1 d . . . . .
C8 C 0.5781(2) 0.31977(14) 0.63003(13) 0.0243(6) Uani 1 1 d . . . . .
H8 H 0.5122 0.3335 0.6433 0.029 Uiso 1 1 calc R U . . .
C65 C 0.8153(2) 0.30523(13) 0.47057(12) 0.0208(5) Uani 1 1 d . . . . .
C23 C 0.92456(19) 0.34520(13) 0.63847(12) 0.0208(5) Uani 1 1 d . . . . .
C14 C 0.6703(2) 0.18768(14) 0.40516(13) 0.0241(6) Uani 1 1 d . . . . .
H14 H 0.7364 0.1754 0.3913 0.029 Uiso 1 1 calc R U . . .
C7 C 0.6714(2) 0.32631(13) 0.66437(12) 0.0228(5) Uani 1 1 d . . . . .
H7 H 0.6840 0.3454 0.7060 0.027 Uiso 1 1 calc R U . . .
C18 C 0.85512(19) 0.29233(13) 0.64989(12) 0.0199(5) Uani 1 1 d . . . . .
C58 C 1.0175(2) 0.16849(15) 0.49443(14) 0.0286(6) Uani 1 1 d . . . . .
H58 H 1.0801 0.1838 0.4778 0.034 Uiso 1 1 calc R U . . .
C13 C 0.5756(2) 0.17418(14) 0.37404(13) 0.0241(6) Uani 1 1 d . . . . .
H13 H 0.5624 0.1506 0.3345 0.029 Uiso 1 1 calc R U . . .
C22 C 1.0290(2) 0.33682(15) 0.66233(13) 0.0273(6) Uani 1 1 d . . . . .
H22 H 1.0786 0.3714 0.6547 0.033 Uiso 1 1 calc R U . . .
C35 C 0.3403(2) 0.25060(14) 0.35805(12) 0.0243(6) Uani 1 1 d . . . . .
C27 C 0.8879(2) 0.41152(13) 0.60589(13) 0.0236(5) Uani 1 1 d . . . . .
H27 H 0.8223 0.4015 0.5779 0.028 Uiso 1 1 calc R U . . .
C19 C 0.8853(2) 0.23380(14) 0.68658(13) 0.0256(6) Uani 1 1 d . . . . .
C62 C 0.9560(2) 0.37750(15) 0.40108(14) 0.0326(7) Uani 1 1 d . . . . .
H62 H 1.0033 0.4024 0.3775 0.039 Uiso 1 1 calc R U . . .
C61 C 0.9867(2) 0.31510(15) 0.42882(14) 0.0299(6) Uani 1 1 d . . . . .
H61 H 1.0548 0.2973 0.4245 0.036 Uiso 1 1 calc R U . . .
C42 C 0.4270(2) 0.33617(16) 0.50458(14) 0.0315(7) Uani 1 1 d . . . . .
C48 C 0.4177(2) 0.22358(16) 0.55821(13) 0.0312(7) Uani 1 1 d . . . . .
C55 C 0.8339(2) 0.12449(14) 0.54459(13) 0.0265(6) Uani 1 1 d . . . . .
H55 H 0.7719 0.1090 0.5617 0.032 Uiso 1 1 calc R U . . .
C64 C 0.7869(2) 0.36788(14) 0.44217(13) 0.0256(6) Uani 1 1 d . . . . .
H64 H 0.7192 0.3863 0.4465 0.031 Uiso 1 1 calc R U . . .
C63 C 0.8568(2) 0.40362(15) 0.40767(14) 0.0316(6) Uani 1 1 d . . . . .
H63 H 0.8365 0.4462 0.3885 0.038 Uiso 1 1 calc R U . . .
C20 C 0.9908(2) 0.22875(15) 0.70911(13) 0.0307(6) Uani 1 1 d . . . . .
H20 H 1.0144 0.1898 0.7334 0.037 Uiso 1 1 calc R U . . .
C34 C 0.2329(2) 0.24417(15) 0.34088(14) 0.0302(6) Uani 1 1 d . . . . .
H34 H 0.1964 0.2804 0.3182 0.036 Uiso 1 1 calc R U . . .
C29 C 0.8614(2) 0.46445(15) 0.65581(15) 0.0338(7) Uani 1 1 d . . . . .
H29A H 0.8092 0.4453 0.6822 0.051 Uiso 1 1 calc R U . . .
H29B H 0.8330 0.5058 0.6341 0.051 Uiso 1 1 calc R U . . .
H29C H 0.9251 0.4762 0.6831 0.051 Uiso 1 1 calc R U . . .
C33 C 0.1787(2) 0.18633(17) 0.35614(15) 0.0330(7) Uani 1 1 d . . . . .
H33 H 0.1055 0.1830 0.3440 0.040 Uiso 1 1 calc R U . . .
C56 C 0.9209(2) 0.08120(15) 0.54539(15) 0.0333(7) Uani 1 1 d . . . . .
H56 H 0.9176 0.0365 0.5629 0.040 Uiso 1 1 calc R U . . .
C21 C 1.0618(2) 0.27927(16) 0.69678(13) 0.0312(6) Uani 1 1 d . . . . .
H21 H 1.1336 0.2744 0.7121 0.037 Uiso 1 1 calc R U . . .
C32 C 0.2303(2) 0.13303(16) 0.38897(14) 0.0307(6) Uani 1 1 d . . . . .
H32 H 0.1921 0.0931 0.3984 0.037 Uiso 1 1 calc R U . . .
C39 C 0.4017(2) 0.31103(15) 0.33485(14) 0.0322(6) Uani 1 1 d . . . . .
H39 H 0.4608 0.3212 0.3680 0.039 Uiso 1 1 calc R U . . .
C36 C 0.3927(2) 0.07553(14) 0.44110(14) 0.0297(6) Uani 1 1 d . . . . .
H36 H 0.4575 0.0925 0.4664 0.036 Uiso 1 1 calc R U . . .
C28 C 0.9680(2) 0.44074(15) 0.56387(14) 0.0288(6) Uani 1 1 d . . . . .
H28A H 1.0308 0.4551 0.5907 0.043 Uiso 1 1 calc R U . . .
H28B H 0.9376 0.4803 0.5401 0.043 Uiso 1 1 calc R U . . .
H28C H 0.9871 0.4056 0.5337 0.043 Uiso 1 1 calc R U . . .
C24 C 0.8064(3) 0.18082(15) 0.70484(15) 0.0349(7) Uani 1 1 d . . . . .
H24 H 0.7466 0.1804 0.6707 0.042 Uiso 1 1 calc R U . . .
C2 C 0.8891(2) 0.12200(16) 0.31479(14) 0.0322(6) Uani 1 1 d . . . . .
H2A H 0.8961 0.1595 0.3466 0.039 Uiso 1 1 calc R U . . .
H2B H 0.9220 0.1367 0.2761 0.039 Uiso 1 1 calc R U . . .
C57 C 1.0120(2) 0.10322(16) 0.52067(14) 0.0339(7) Uani 1 1 d . . . . .
H57 H 1.0711 0.0736 0.5217 0.041 Uiso 1 1 calc R U . . .
C53 C 0.3204(2) 0.2589(2) 0.55613(16) 0.0456(10) Uani 1 1 d . . . . .
C38 C 0.3259(3) 0.03833(17) 0.48663(16) 0.0419(8) Uani 1 1 d . . . . .
H38A H 0.2984 0.0715 0.5159 0.063 Uiso 1 1 calc R U . . .
H38B H 0.3690 0.0043 0.5112 0.063 Uiso 1 1 calc R U . . .
H38C H 0.2674 0.0153 0.4620 0.063 Uiso 1 1 calc R U . . .
C41 C 0.4487(3) 0.29238(19) 0.27241(16) 0.0434(8) Uani 1 1 d . . . . .
H41A H 0.4959 0.2531 0.2798 0.065 Uiso 1 1 calc R U . . .
H41B H 0.4880 0.3316 0.2578 0.065 Uiso 1 1 calc R U . . .
H41C H 0.3920 0.2805 0.2397 0.065 Uiso 1 1 calc R U . . .
C49 C 0.4297(3) 0.16329(18) 0.59221(16) 0.0439(8) Uani 1 1 d . . . . .
H49 H 0.4947 0.1395 0.5948 0.053 Uiso 1 1 calc R U . . .
C67 C 0.3532(3) 0.38666(18) 0.72176(17) 0.0423(8) Uani 1 1 d . . . . .
H67A H 0.3178 0.3758 0.7605 0.051 Uiso 1 1 calc R U . . .
H67B H 0.3449 0.3472 0.6921 0.051 Uiso 1 1 calc R U . . .
B16 B 0.7487(2) 0.24929(14) 0.50799(13) 0.0187(6) Uani 1 1 d . . . . .
C40 C 0.3348(3) 0.37550(17) 0.32470(18) 0.0466(9) Uani 1 1 d . . . . .
H40A H 0.2840 0.3693 0.2874 0.070 Uiso 1 1 calc R U . . .
H40B H 0.3802 0.4147 0.3176 0.070 Uiso 1 1 calc R U . . .
H40C H 0.2974 0.3839 0.3627 0.070 Uiso 1 1 calc R U . . .
C37 C 0.4263(3) 0.02524(16) 0.39055(18) 0.0436(8) Uani 1 1 d . . . . .
H37A H 0.3639 0.0078 0.3652 0.065 Uiso 1 1 calc R U . . .
H37B H 0.4648 -0.0130 0.4118 0.065 Uiso 1 1 calc R U . . .
H37C H 0.4715 0.0489 0.3624 0.065 Uiso 1 1 calc R U . . .
C5 C 0.7592(3) 0.04004(17) 0.32513(18) 0.0420(8) Uani 1 1 d D . . . .
H5AA H 0.7535 0.0047 0.2911 0.050 Uiso 0.670(11) 1 calc R U P A 1
H5AB H 0.6925 0.0412 0.3457 0.050 Uiso 0.670(11) 1 calc R U P A 1
H5BC H 0.7043 0.0159 0.2975 0.050 Uiso 0.330(11) 1 calc R U P A 2
H5BD H 0.7348 0.0452 0.3683 0.050 Uiso 0.330(11) 1 calc R U P A 2
C70 C 0.4886(3) 0.46582(17) 0.71245(17) 0.0437(8) Uani 1 1 d D . . . .
H70A H 0.5563 0.4631 0.6932 0.052 Uiso 0.873(14) 1 calc R U P B 1
H70B H 0.4943 0.5012 0.7463 0.052 Uiso 0.873(14) 1 calc R U P B 1
H70C H 0.5204 0.4596 0.6716 0.052 Uiso 0.127(14) 1 calc R U P B 2
H70D H 0.5393 0.4904 0.7427 0.052 Uiso 0.127(14) 1 calc R U P B 2
B10 B 0.4999(2) 0.26922(15) 0.52236(14) 0.0218(6) Uani 1 1 d . . . . .
C43 C 0.4503(3) 0.39976(17) 0.47974(16) 0.0465(9) Uani 1 1 d . . . . .
H43 H 0.5180 0.4076 0.4660 0.056 Uiso 1 1 calc R U . . .
C47 C 0.3270(2) 0.3260(2) 0.52479(16) 0.0455(9) Uani 1 1 d . . . . .
C26 C 0.8523(3) 0.10802(17) 0.71045(18) 0.0499(9) Uani 1 1 d . . . . .
H26A H 0.8903 0.0982 0.6730 0.075 Uiso 1 1 calc R U . . .
H26B H 0.7953 0.0748 0.7127 0.075 Uiso 1 1 calc R U . . .
H26C H 0.9006 0.1047 0.7493 0.075 Uiso 1 1 calc R U . . .
C25 C 0.7629(3) 0.20091(18) 0.76813(17) 0.0443(8) Uani 1 1 d . . . . .
H25A H 0.8202 0.2014 0.8024 0.067 Uiso 1 1 calc R U . . .
H25B H 0.7097 0.1676 0.7784 0.067 Uiso 1 1 calc R U . . .
H25C H 0.7312 0.2466 0.7639 0.067 Uiso 1 1 calc R U . . .
C3 C 0.9407(3) 0.05793(19) 0.34202(19) 0.0493(9) Uani 1 1 d D . . . .
H3AA H 0.9994 0.0684 0.3746 0.059 Uiso 0.670(11) 1 calc R U P A 1
H3AB H 0.9663 0.0286 0.3082 0.059 Uiso 0.670(11) 1 calc R U P A 1
H3BC H 0.9581 0.0631 0.3887 0.059 Uiso 0.330(11) 1 calc R U P A 2
H3BD H 1.0064 0.0491 0.3219 0.059 Uiso 0.330(11) 1 calc R U P A 2
C50 C 0.3448(4) 0.1370(2) 0.62313(19) 0.0679(15) Uani 1 1 d . . . . .
H50 H 0.3528 0.0957 0.6470 0.081 Uiso 1 1 calc R U . . .
C52 C 0.2372(3) 0.2318(3) 0.5855(2) 0.0699(15) Uani 1 1 d . . . . .
H52 H 0.1717 0.2550 0.5826 0.084 Uiso 1 1 calc R U . . .
C68 C 0.3067(3) 0.4504(2) 0.6901(2) 0.0566(10) Uani 1 1 d D . . . .
H68A H 0.2775 0.4811 0.7215 0.068 Uiso 0.873(14) 1 calc R U P B 1
H68B H 0.2510 0.4390 0.6559 0.068 Uiso 0.873(14) 1 calc R U P B 1
H68C H 0.2908 0.4427 0.6436 0.068 Uiso 0.127(14) 1 calc R U P B 2
H68D H 0.2410 0.4631 0.7087 0.068 Uiso 0.127(14) 1 calc R U P B 2
C69 C 0.4013(4) 0.4828(2) 0.6625(2) 0.0489(16) Uani 0.873(14) 1 d D . P B 1
H69A H 0.4136 0.4623 0.6206 0.059 Uiso 0.873(14) 1 calc R U P B 1
H69B H 0.3925 0.5329 0.6574 0.059 Uiso 0.873(14) 1 calc R U P B 1
C45 C 0.2783(5) 0.4417(3) 0.4935(2) 0.088(2) Uani 1 1 d . . . . .
H45 H 0.2282 0.4777 0.4898 0.105 Uiso 1 1 calc R U . . .
C46 C 0.2506(3) 0.3787(3) 0.5182(2) 0.0754(17) Uani 1 1 d . . . . .
H46 H 0.1818 0.3712 0.5304 0.090 Uiso 1 1 calc R U . . .
C51 C 0.2494(4) 0.1717(3) 0.6186(2) 0.089(2) Uani 1 1 d . . . . .
H51 H 0.1921 0.1533 0.6389 0.107 Uiso 1 1 calc R U . . .
C44 C 0.3761(5) 0.4523(2) 0.4747(2) 0.0747(16) Uani 1 1 d . . . . .
H44 H 0.3938 0.4956 0.4580 0.090 Uiso 1 1 calc R U . . .
C4 C 0.8469(4) 0.0247(3) 0.3723(3) 0.0471(19) Uani 0.670(11) 1 d D . P A 1
H4A H 0.8568 -0.0253 0.3777 0.057 Uiso 0.670(11) 1 calc R U P A 1
H4B H 0.8365 0.0456 0.4143 0.057 Uiso 0.670(11) 1 calc R U P A 1
C4A C 0.8652(8) -0.0009(5) 0.3288(5) 0.042(3) Uani 0.330(11) 1 d D . P A 2
H4AA H 0.8701 -0.0348 0.3640 0.051 Uiso 0.330(11) 1 calc R U P A 2
H4AB H 0.8756 -0.0241 0.2879 0.051 Uiso 0.330(11) 1 calc R U P A 2
C69A C 0.3869(14) 0.5060(10) 0.7017(19) 0.066(14) Uani 0.127(14) 1 d D . P B 2
H69C H 0.3740 0.5335 0.7399 0.079 Uiso 0.127(14) 1 calc R U P B 2
H69D H 0.3875 0.5367 0.6643 0.079 Uiso 0.127(14) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.439(3) . ?
O1 C5 1.425(4) . ?
N6 C17 1.364(3) . ?
N6 C7 1.388(3) . ?
N6 C18 1.445(3) . ?
N9 C17 1.339(3) . ?
N9 C8 1.381(3) . ?
N9 B10 1.579(3) . ?
O66 C67 1.436(4) . ?
O66 C70 1.433(4) . ?
N15 C11 1.341(3) . ?
N15 C14 1.385(3) . ?
N15 B16 1.581(3) . ?
N12 C11 1.367(3) . ?
N12 C30 1.447(3) . ?
N12 C13 1.387(3) . ?
C17 B16 1.612(4) . ?
C11 B10 1.610(4) . ?
C59 C54 1.409(4) . ?
C59 C60 1.476(4) . ?
C59 C58 1.396(4) . ?
C54 C55 1.389(4) . ?
C54 B16 1.621(4) . ?
C31 C30 1.404(4) . ?
C31 C32 1.396(4) . ?
C31 C36 1.518(4) . ?
C60 C65 1.410(4) . ?
C60 C61 1.390(4) . ?
C30 C35 1.402(4) . ?
C8 H8 0.9500 . ?
C8 C7 1.345(4) . ?
C65 C64 1.394(4) . ?
C65 B16 1.630(4) . ?
C23 C18 1.397(4) . ?
C23 C22 1.394(4) . ?
C23 C27 1.518(4) . ?
C14 H14 0.9500 . ?
C14 C13 1.349(4) . ?
C7 H7 0.9500 . ?
C18 C19 1.412(4) . ?
C58 H58 0.9500 . ?
C58 C57 1.393(4) . ?
C13 H13 0.9500 . ?
C22 H22 0.9500 . ?
C22 C21 1.381(4) . ?
C35 C34 1.395(4) . ?
C35 C39 1.522(4) . ?
C27 H27 1.0000 . ?
C27 C29 1.531(4) . ?
C27 C28 1.522(4) . ?
C19 C20 1.393(4) . ?
C19 C24 1.519(4) . ?
C62 H62 0.9500 . ?
C62 C61 1.392(4) . ?
C62 C63 1.387(4) . ?
C61 H61 0.9500 . ?
C42 B10 1.629(4) . ?
C42 C43 1.389(5) . ?
C42 C47 1.399(5) . ?
C48 C53 1.420(5) . ?
C48 C49 1.378(5) . ?
C48 B10 1.615(4) . ?
C55 H55 0.9500 . ?
C55 C56 1.396(4) . ?
C64 H64 0.9500 . ?
C64 C63 1.388(4) . ?
C63 H63 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.381(4) . ?
C34 H34 0.9500 . ?
C34 C33 1.378(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C33 H33 0.9500 . ?
C33 C32 1.383(4) . ?
C56 H56 0.9500 . ?
C56 C57 1.387(4) . ?
C21 H21 0.9500 . ?
C32 H32 0.9500 . ?
C39 H39 1.0000 . ?
C39 C41 1.534(5) . ?
C39 C40 1.526(4) . ?
C36 H36 1.0000 . ?
C36 C38 1.523(4) . ?
C36 C37 1.535(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C24 H24 1.0000 . ?
C24 C26 1.538(4) . ?
C24 C25 1.536(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.503(5) . ?
C57 H57 0.9500 . ?
C53 C47 1.472(6) . ?
C53 C52 1.381(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C49 H49 0.9500 . ?
C49 C50 1.411(5) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.508(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C5 H5AA 0.9900 . ?
C5 H5AB 0.9900 . ?
C5 H5BC 0.9900 . ?
C5 H5BD 0.9900 . ?
C5 C4 1.459(6) . ?
C5 C4A 1.570(10) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 H70C 0.9900 . ?
C70 H70D 0.9900 . ?
C70 C69 1.499(5) . ?
C70 C69A 1.519(17) . ?
C43 H43 0.9500 . ?
C43 C44 1.396(5) . ?
C47 C46 1.418(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.550(7) . ?
C3 C4A 1.511(10) . ?
C50 H50 0.9500 . ?
C50 C51 1.391(8) . ?
C52 H52 0.9500 . ?
C52 C51 1.367(8) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 H68C 0.9900 . ?
C68 H68D 0.9900 . ?
C68 C69 1.525(6) . ?
C68 C69A 1.498(19) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C45 H45 0.9500 . ?
C45 C46 1.392(8) . ?
C45 C44 1.362(8) . ?
C46 H46 0.9500 . ?
C51 H51 0.9500 . ?
C44 H44 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C69A H69C 0.9900 . ?
C69A H69D 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
C5 O1 C2 109.0(2) . . ?
C17 N6 C7 109.3(2) . . ?
C17 N6 C18 127.8(2) . . ?
C7 N6 C18 122.7(2) . . ?
C17 N9 C8 109.3(2) . . ?
C17 N9 B10 129.1(2) . . ?
C8 N9 B10 121.5(2) . . ?
C70 O66 C67 109.5(2) . . ?
C11 N15 C14 109.4(2) . . ?
C11 N15 B16 128.7(2) . . ?
C14 N15 B16 121.8(2) . . ?
C11 N12 C30 127.8(2) . . ?
C11 N12 C13 109.6(2) . . ?
C13 N12 C30 122.7(2) . . ?
N6 C17 B16 128.9(2) . . ?
N9 C17 N6 106.8(2) . . ?
N9 C17 B16 124.1(2) . . ?
N15 C11 N12 106.6(2) . . ?
N15 C11 B10 124.7(2) . . ?
N12 C11 B10 128.7(2) . . ?
C54 C59 C60 111.1(2) . . ?
C58 C59 C54 121.3(2) . . ?
C58 C59 C60 127.6(2) . . ?
C59 C54 B16 109.7(2) . . ?
C55 C54 C59 118.4(2) . . ?
C55 C54 B16 131.8(2) . . ?
C30 C31 C36 123.1(2) . . ?
C32 C31 C30 116.8(3) . . ?
C32 C31 C36 119.9(2) . . ?
C65 C60 C59 110.4(2) . . ?
C61 C60 C59 128.1(2) . . ?
C61 C60 C65 121.4(3) . . ?
C31 C30 N12 118.3(2) . . ?
C35 C30 N12 118.6(2) . . ?
C35 C30 C31 123.0(2) . . ?
N9 C8 H8 125.9 . . ?
C7 C8 N9 108.3(2) . . ?
C7 C8 H8 125.9 . . ?
C60 C65 B16 109.8(2) . . ?
C64 C65 C60 118.2(2) . . ?
C64 C65 B16 131.8(2) . . ?
C18 C23 C27 122.1(2) . . ?
C22 C23 C18 117.1(2) . . ?
C22 C23 C27 120.6(2) . . ?
N15 C14 H14 126.0 . . ?
C13 C14 N15 108.0(2) . . ?
C13 C14 H14 126.0 . . ?
N6 C7 H7 126.8 . . ?
C8 C7 N6 106.4(2) . . ?
C8 C7 H7 126.8 . . ?
C23 C18 N6 118.8(2) . . ?
C23 C18 C19 123.0(2) . . ?
C19 C18 N6 118.1(2) . . ?
C59 C58 H58 120.5 . . ?
C57 C58 C59 119.0(3) . . ?
C57 C58 H58 120.5 . . ?
N12 C13 H13 126.8 . . ?
C14 C13 N12 106.4(2) . . ?
C14 C13 H13 126.8 . . ?
C23 C22 H22 119.3 . . ?
C21 C22 C23 121.4(3) . . ?
C21 C22 H22 119.3 . . ?
C30 C35 C39 121.8(2) . . ?
C34 C35 C30 117.2(3) . . ?
C34 C35 C39 120.8(3) . . ?
C23 C27 H27 107.9 . . ?
C23 C27 C29 110.2(2) . . ?
C23 C27 C28 112.6(2) . . ?
C29 C27 H27 107.9 . . ?
C28 C27 H27 107.9 . . ?
C28 C27 C29 110.2(2) . . ?
C18 C19 C24 122.2(2) . . ?
C20 C19 C18 116.9(2) . . ?
C20 C19 C24 120.8(3) . . ?
C61 C62 H62 119.8 . . ?
C63 C62 H62 119.8 . . ?
C63 C62 C61 120.5(3) . . ?
C60 C61 C62 118.9(3) . . ?
C60 C61 H61 120.5 . . ?
C62 C61 H61 120.5 . . ?
C43 C42 B10 131.7(3) . . ?
C43 C42 C47 118.3(3) . . ?
C47 C42 B10 109.7(3) . . ?
C53 C48 B10 108.9(3) . . ?
C49 C48 C53 119.1(3) . . ?
C49 C48 B10 131.7(3) . . ?
C54 C55 H55 119.7 . . ?
C54 C55 C56 120.7(3) . . ?
C56 C55 H55 119.7 . . ?
C65 C64 H64 119.7 . . ?
C63 C64 C65 120.6(3) . . ?
C63 C64 H64 119.7 . . ?
C62 C63 C64 120.4(3) . . ?
C62 C63 H63 119.8 . . ?
C64 C63 H63 119.8 . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.3(3) . . ?
C21 C20 H20 119.3 . . ?
C35 C34 H34 119.4 . . ?
C33 C34 C35 121.2(3) . . ?
C33 C34 H34 119.4 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C34 C33 H33 119.8 . . ?
C34 C33 C32 120.3(3) . . ?
C32 C33 H33 119.8 . . ?
C55 C56 H56 119.9 . . ?
C57 C56 C55 120.3(3) . . ?
C57 C56 H56 119.9 . . ?
C22 C21 C20 120.3(2) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.4(3) . . ?
C33 C32 H32 119.3 . . ?
C35 C39 H39 108.2 . . ?
C35 C39 C41 110.0(2) . . ?
C35 C39 C40 112.6(3) . . ?
C41 C39 H39 108.2 . . ?
C40 C39 H39 108.2 . . ?
C40 C39 C41 109.5(3) . . ?
C31 C36 H36 108.0 . . ?
C31 C36 C38 113.1(3) . . ?
C31 C36 C37 109.8(2) . . ?
C38 C36 H36 108.0 . . ?
C38 C36 C37 109.7(3) . . ?
C37 C36 H36 108.0 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C19 C24 H24 108.0 . . ?
C19 C24 C26 112.9(3) . . ?
C19 C24 C25 110.2(3) . . ?
C26 C24 H24 108.0 . . ?
C25 C24 H24 108.0 . . ?
C25 C24 C26 109.6(3) . . ?
O1 C2 H2A 110.4 . . ?
O1 C2 H2B 110.4 . . ?
O1 C2 C3 106.4(2) . . ?
H2A C2 H2B 108.6 . . ?
C3 C2 H2A 110.4 . . ?
C3 C2 H2B 110.4 . . ?
C58 C57 H57 119.8 . . ?
C56 C57 C58 120.4(3) . . ?
C56 C57 H57 119.8 . . ?
C48 C53 C47 111.1(3) . . ?
C52 C53 C48 120.6(4) . . ?
C52 C53 C47 128.1(4) . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C48 C49 H49 120.2 . . ?
C48 C49 C50 119.6(4) . . ?
C50 C49 H49 120.2 . . ?
O66 C67 H67A 110.4 . . ?
O66 C67 H67B 110.4 . . ?
O66 C67 C68 106.6(3) . . ?
H67A C67 H67B 108.6 . . ?
C68 C67 H67A 110.4 . . ?
C68 C67 H67B 110.4 . . ?
N15 B16 C17 105.88(19) . . ?
N15 B16 C54 109.8(2) . . ?
N15 B16 C65 108.9(2) . . ?
C17 B16 C54 117.6(2) . . ?
C17 B16 C65 115.3(2) . . ?
C54 B16 C65 99.11(19) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O1 C5 H5AA 110.4 . . ?
O1 C5 H5AB 110.4 . . ?
O1 C5 H5BC 110.5 . . ?
O1 C5 H5BD 110.5 . . ?
O1 C5 C4 106.5(3) . . ?
O1 C5 C4A 106.4(4) . . ?
H5AA C5 H5AB 108.6 . . ?
H5BC C5 H5BD 108.6 . . ?
C4 C5 H5AA 110.4 . . ?
C4 C5 H5AB 110.4 . . ?
C4A C5 H5BC 110.5 . . ?
C4A C5 H5BD 110.5 . . ?
O66 C70 H70A 110.5 . . ?
O66 C70 H70B 110.5 . . ?
O66 C70 H70C 110.4 . . ?
O66 C70 H70D 110.4 . . ?
O66 C70 C69 106.1(3) . . ?
O66 C70 C69A 106.7(9) . . ?
H70A C70 H70B 108.7 . . ?
H70C C70 H70D 108.6 . . ?
C69 C70 H70A 110.5 . . ?
C69 C70 H70B 110.5 . . ?
C69A C70 H70C 110.4 . . ?
C69A C70 H70D 110.4 . . ?
N9 B10 C11 106.1(2) . . ?
N9 B10 C42 109.7(2) . . ?
N9 B10 C48 108.9(2) . . ?
C11 B10 C42 117.2(2) . . ?
C11 B10 C48 115.2(2) . . ?
C48 B10 C42 99.6(2) . . ?
C42 C43 H43 119.4 . . ?
C42 C43 C44 121.2(4) . . ?
C44 C43 H43 119.4 . . ?
C42 C47 C53 110.7(3) . . ?
C42 C47 C46 120.6(4) . . ?
C46 C47 C53 128.6(4) . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C2 C3 H3AA 111.8 . . ?
C2 C3 H3AB 111.8 . . ?
C2 C3 H3BC 110.1 . . ?
C2 C3 H3BD 110.1 . . ?
C2 C3 C4 100.1(3) . . ?
C2 C3 C4A 108.1(4) . . ?
H3AA C3 H3AB 109.5 . . ?
H3BC C3 H3BD 108.4 . . ?
C4 C3 H3AA 111.8 . . ?
C4 C3 H3AB 111.8 . . ?
C4A C3 H3BC 110.1 . . ?
C4A C3 H3BD 110.1 . . ?
C49 C50 H50 120.0 . . ?
C51 C50 C49 120.0(5) . . ?
C51 C50 H50 120.0 . . ?
C53 C52 H52 120.0 . . ?
C51 C52 C53 119.9(5) . . ?
C51 C52 H52 120.0 . . ?
C67 C68 H68A 111.3 . . ?
C67 C68 H68B 111.3 . . ?
C67 C68 H68C 110.4 . . ?
C67 C68 H68D 110.4 . . ?
C67 C68 C69 102.4(3) . . ?
H68A C68 H68B 109.2 . . ?
H68C C68 H68D 108.6 . . ?
C69 C68 H68A 111.3 . . ?
C69 C68 H68B 111.3 . . ?
C69A C68 C67 106.8(9) . . ?
C69A C68 H68C 110.4 . . ?
C69A C68 H68D 110.4 . . ?
C70 C69 C68 102.1(3) . . ?
C70 C69 H69A 111.4 . . ?
C70 C69 H69B 111.4 . . ?
C68 C69 H69A 111.4 . . ?
C68 C69 H69B 111.4 . . ?
H69A C69 H69B 109.2 . . ?
C46 C45 H45 119.5 . . ?
C44 C45 H45 119.5 . . ?
C44 C45 C46 121.0(4) . . ?
C47 C46 H46 120.6 . . ?
C45 C46 C47 118.8(4) . . ?
C45 C46 H46 120.6 . . ?
C50 C51 H51 119.6 . . ?
C52 C51 C50 120.7(4) . . ?
C52 C51 H51 119.6 . . ?
C43 C44 H44 119.9 . . ?
C45 C44 C43 120.1(5) . . ?
C45 C44 H44 119.9 . . ?
C5 C4 C3 102.3(4) . . ?
C5 C4 H4A 111.3 . . ?
C5 C4 H4B 111.3 . . ?
C3 C4 H4A 111.3 . . ?
C3 C4 H4B 111.3 . . ?
H4A C4 H4B 109.2 . . ?
C5 C4A H4AA 112.0 . . ?
C5 C4A H4AB 112.0 . . ?
C3 C4A C5 99.0(6) . . ?
C3 C4A H4AA 112.0 . . ?
C3 C4A H4AB 112.0 . . ?
H4AA C4A H4AB 109.6 . . ?
C70 C69A H69C 111.3 . . ?
C70 C69A H69D 111.3 . . ?
C68 C69A C70 102.4(11) . . ?
C68 C69A H69C 111.3 . . ?
C68 C69A H69D 111.3 . . ?
H69C C69A H69D 109.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 -30.0(4) . . . . ?
O1 C2 C3 C4A 12.1(6) . . . . ?
O1 C5 C4 C3 -34.3(5) . . . . ?
O1 C5 C4A C3 33.0(7) . . . . ?
N6 C17 B16 N15 172.2(2) . . . . ?
N6 C17 B16 C54 49.1(3) . . . . ?
N6 C17 B16 C65 -67.3(3) . . . . ?
N6 C18 C19 C20 -178.8(2) . . . . ?
N6 C18 C19 C24 -2.8(4) . . . . ?
N9 C17 B16 N15 -13.5(3) . . . . ?
N9 C17 B16 C54 -136.7(2) . . . . ?
N9 C17 B16 C65 106.9(3) . . . . ?
N9 C8 C7 N6 -0.2(3) . . . . ?
O66 C67 C68 C69 26.7(4) . . . . ?
O66 C67 C68 C69A -11.9(16) . . . . ?
O66 C70 C69 C68 32.8(5) . . . . ?
O66 C70 C69A C68 -29(2) . . . . ?
N15 C11 B10 N9 -1.8(3) . . . . ?
N15 C11 B10 C42 121.1(3) . . . . ?
N15 C11 B10 C48 -122.3(3) . . . . ?
N15 C14 C13 N12 0.3(3) . . . . ?
N12 C11 B10 N9 176.6(2) . . . . ?
N12 C11 B10 C42 -60.5(4) . . . . ?
N12 C11 B10 C48 56.1(4) . . . . ?
N12 C30 C35 C34 179.2(2) . . . . ?
N12 C30 C35 C39 3.8(4) . . . . ?
C17 N6 C7 C8 0.7(3) . . . . ?
C17 N6 C18 C23 92.6(3) . . . . ?
C17 N6 C18 C19 -91.6(3) . . . . ?
C17 N9 C8 C7 -0.4(3) . . . . ?
C17 N9 B10 C11 -1.7(3) . . . . ?
C17 N9 B10 C42 -129.1(3) . . . . ?
C17 N9 B10 C48 122.9(3) . . . . ?
C11 N15 C14 C13 -0.7(3) . . . . ?
C11 N15 B16 C17 10.8(3) . . . . ?
C11 N15 B16 C54 138.8(2) . . . . ?
C11 N15 B16 C65 -113.7(3) . . . . ?
C11 N12 C30 C31 -96.4(3) . . . . ?
C11 N12 C30 C35 87.7(3) . . . . ?
C11 N12 C13 C14 0.1(3) . . . . ?
C59 C54 C55 C56 1.0(4) . . . . ?
C59 C54 B16 N15 114.1(2) . . . . ?
C59 C54 B16 C17 -124.7(2) . . . . ?
C59 C54 B16 C65 0.2(3) . . . . ?
C59 C60 C65 C64 -176.7(2) . . . . ?
C59 C60 C65 B16 -1.7(3) . . . . ?
C59 C60 C61 C62 176.2(3) . . . . ?
C59 C58 C57 C56 -0.5(4) . . . . ?
C54 C59 C60 C65 1.8(3) . . . . ?
C54 C59 C60 C61 -175.4(3) . . . . ?
C54 C59 C58 C57 1.8(4) . . . . ?
C54 C55 C56 C57 0.2(4) . . . . ?
C31 C30 C35 C34 3.4(4) . . . . ?
C31 C30 C35 C39 -171.9(2) . . . . ?
C60 C59 C54 C55 175.0(2) . . . . ?
C60 C59 C54 B16 -1.2(3) . . . . ?
C60 C59 C58 C57 -174.8(3) . . . . ?
C60 C65 C64 C63 -0.3(4) . . . . ?
C60 C65 B16 N15 -113.8(2) . . . . ?
C60 C65 B16 C17 127.4(2) . . . . ?
C60 C65 B16 C54 0.9(3) . . . . ?
C30 N12 C11 N15 179.3(2) . . . . ?
C30 N12 C11 B10 0.7(4) . . . . ?
C30 N12 C13 C14 -179.7(2) . . . . ?
C30 C31 C32 C33 0.1(4) . . . . ?
C30 C31 C36 C38 145.4(3) . . . . ?
C30 C31 C36 C37 -91.7(3) . . . . ?
C30 C35 C34 C33 -2.1(4) . . . . ?
C30 C35 C39 C41 82.8(3) . . . . ?
C30 C35 C39 C40 -154.8(3) . . . . ?
C8 N9 C17 N6 0.8(3) . . . . ?
C8 N9 C17 B16 -174.5(2) . . . . ?
C8 N9 B10 C11 -176.2(2) . . . . ?
C8 N9 B10 C42 56.4(3) . . . . ?
C8 N9 B10 C48 -51.6(3) . . . . ?
C65 C60 C61 C62 -0.7(4) . . . . ?
C65 C64 C63 C62 -0.1(4) . . . . ?
C23 C18 C19 C20 -3.1(4) . . . . ?
C23 C18 C19 C24 172.9(3) . . . . ?
C23 C22 C21 C20 -0.9(4) . . . . ?
C14 N15 C11 N12 0.7(3) . . . . ?
C14 N15 C11 B10 179.4(2) . . . . ?
C14 N15 B16 C17 -173.0(2) . . . . ?
C14 N15 B16 C54 -45.1(3) . . . . ?
C14 N15 B16 C65 62.4(3) . . . . ?
C7 N6 C17 N9 -1.0(3) . . . . ?
C7 N6 C17 B16 174.1(2) . . . . ?
C7 N6 C18 C23 -92.9(3) . . . . ?
C7 N6 C18 C19 83.0(3) . . . . ?
C18 N6 C17 N9 174.2(2) . . . . ?
C18 N6 C17 B16 -10.8(4) . . . . ?
C18 N6 C7 C8 -174.7(2) . . . . ?
C18 C23 C22 C21 -1.2(4) . . . . ?
C18 C23 C27 C29 91.0(3) . . . . ?
C18 C23 C27 C28 -145.5(2) . . . . ?
C18 C19 C20 C21 0.9(4) . . . . ?
C18 C19 C24 C26 148.6(3) . . . . ?
C18 C19 C24 C25 -88.5(3) . . . . ?
C58 C59 C54 C55 -2.0(4) . . . . ?
C58 C59 C54 B16 -178.2(2) . . . . ?
C58 C59 C60 C65 178.7(3) . . . . ?
C58 C59 C60 C61 1.4(4) . . . . ?
C13 N12 C11 N15 -0.5(3) . . . . ?
C13 N12 C11 B10 -179.1(2) . . . . ?
C13 N12 C30 C31 83.4(3) . . . . ?
C13 N12 C30 C35 -92.6(3) . . . . ?
C22 C23 C18 N6 178.9(2) . . . . ?
C22 C23 C18 C19 3.2(4) . . . . ?
C22 C23 C27 C29 -84.4(3) . . . . ?
C22 C23 C27 C28 39.1(3) . . . . ?
C35 C34 C33 C32 -0.1(4) . . . . ?
C27 C23 C18 N6 3.3(4) . . . . ?
C27 C23 C18 C19 -172.4(2) . . . . ?
C27 C23 C22 C21 174.5(2) . . . . ?
C19 C20 C21 C22 1.0(4) . . . . ?
C61 C60 C65 C64 0.8(4) . . . . ?
C61 C60 C65 B16 175.8(2) . . . . ?
C61 C62 C63 C64 0.2(4) . . . . ?
C42 C43 C44 C45 -0.7(6) . . . . ?
C42 C47 C46 C45 -2.4(5) . . . . ?
C48 C53 C47 C42 1.0(3) . . . . ?
C48 C53 C47 C46 -174.0(3) . . . . ?
C48 C53 C52 C51 2.2(5) . . . . ?
C48 C49 C50 C51 0.6(5) . . . . ?
C55 C54 B16 N15 -61.4(3) . . . . ?
C55 C54 B16 C17 59.7(4) . . . . ?
C55 C54 B16 C65 -175.3(3) . . . . ?
C55 C56 C57 C58 -0.5(4) . . . . ?
C64 C65 B16 N15 60.3(3) . . . . ?
C64 C65 B16 C17 -58.5(4) . . . . ?
C64 C65 B16 C54 175.0(3) . . . . ?
C63 C62 C61 C60 0.3(4) . . . . ?
C20 C19 C24 C26 -35.6(4) . . . . ?
C20 C19 C24 C25 87.3(3) . . . . ?
C34 C35 C39 C41 -92.5(3) . . . . ?
C34 C35 C39 C40 30.0(4) . . . . ?
C34 C33 C32 C31 1.2(4) . . . . ?
C32 C31 C30 N12 -178.2(2) . . . . ?
C32 C31 C30 C35 -2.4(4) . . . . ?
C32 C31 C36 C38 -38.2(4) . . . . ?
C32 C31 C36 C37 84.6(3) . . . . ?
C39 C35 C34 C33 173.3(3) . . . . ?
C36 C31 C30 N12 -1.8(4) . . . . ?
C36 C31 C30 C35 174.0(2) . . . . ?
C36 C31 C32 C33 -176.5(3) . . . . ?
C24 C19 C20 C21 -175.1(3) . . . . ?
C2 O1 C5 C4 15.8(4) . . . . ?
C2 O1 C5 C4A -27.9(5) . . . . ?
C2 C3 C4 C5 38.8(4) . . . . ?
C2 C3 C4A C5 -26.7(7) . . . . ?
C53 C48 C49 C50 1.3(4) . . . . ?
C53 C48 B10 N9 117.3(2) . . . . ?
C53 C48 B10 C11 -123.7(2) . . . . ?
C53 C48 B10 C42 2.5(3) . . . . ?
C53 C47 C46 C45 172.2(3) . . . . ?
C53 C52 C51 C50 -0.2(6) . . . . ?
C49 C48 C53 C47 172.7(3) . . . . ?
C49 C48 C53 C52 -2.7(4) . . . . ?
C49 C48 B10 N9 -56.9(4) . . . . ?
C49 C48 B10 C11 62.1(4) . . . . ?
C49 C48 B10 C42 -171.7(3) . . . . ?
C49 C50 C51 C52 -1.2(6) . . . . ?
C67 O66 C70 C69 -16.8(4) . . . . ?
C67 O66 C70 C69A 22.4(16) . . . . ?
C67 C68 C69 C70 -35.7(5) . . . . ?
C67 C68 C69A C70 24(2) . . . . ?
B16 N15 C11 N12 177.2(2) . . . . ?
B16 N15 C11 B10 -4.1(4) . . . . ?
B16 N15 C14 C13 -177.5(2) . . . . ?
B16 C54 C55 C56 176.2(3) . . . . ?
B16 C65 C64 C63 -174.0(3) . . . . ?
C5 O1 C2 C3 10.3(3) . . . . ?
C70 O66 C67 C68 -6.6(4) . . . . ?
B10 N9 C17 N6 -174.2(2) . . . . ?
B10 N9 C17 B16 10.5(4) . . . . ?
B10 N9 C8 C7 175.1(2) . . . . ?
B10 C42 C43 C44 -173.2(3) . . . . ?
B10 C42 C47 C53 0.8(3) . . . . ?
B10 C42 C47 C46 176.2(3) . . . . ?
B10 C48 C53 C47 -2.3(3) . . . . ?
B10 C48 C53 C52 -177.8(3) . . . . ?
B10 C48 C49 C50 175.0(3) . . . . ?
C43 C42 B10 N9 57.3(4) . . . . ?
C43 C42 B10 C11 -63.7(4) . . . . ?
C43 C42 B10 C48 171.4(3) . . . . ?
C43 C42 C47 C53 -173.6(3) . . . . ?
C43 C42 C47 C46 1.8(4) . . . . ?
C47 C42 B10 N9 -116.1(3) . . . . ?
C47 C42 B10 C11 122.9(3) . . . . ?
C47 C42 B10 C48 -1.9(3) . . . . ?
C47 C42 C43 C44 -0.3(5) . . . . ?
C47 C53 C52 C51 -172.4(3) . . . . ?
C52 C53 C47 C42 176.1(3) . . . . ?
C52 C53 C47 C46 1.0(6) . . . . ?
C69 C70 C69A C68 66.3(16) . . . . ?
C69 C68 C69A C70 -64.3(13) . . . . ?
C46 C45 C44 C43 0.1(6) . . . . ?
C44 C45 C46 C47 1.4(6) . . . . ?
C4 C5 C4A C3 -63.6(6) . . . . ?
C4 C3 C4A C5 58.0(5) . . . . ?
C4A C5 C4 C3 62.0(6) . . . . ?
C4A C3 C4 C5 -67.3(6) . . . . ?
C69A C70 C69 C68 -63.9(12) . . . . ?
C69A C68 C69 C70 65.8(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.562
_oxdiff_exptl_absorpt_empirical_full_min 0.648
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9919(5)
2 0.0081(5)

