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

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

data_1a
_database_code_depnum_ccdc_archive 'CCDC 2096462'
loop_
_audit_author_name
_audit_author_address
'Rong Shang '
;Graduate School of Advanced Engineering and Science, Hiroshima University
Japan
;
_audit_update_record             
;
2021-07-14 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
#data_oishi_exp131_0m

_audit_creation_method           SHELXL-2014/5
_chemical_name_systematic        2014/7
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H74 B4 O8 P2'
_chemical_formula_weight         1028.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.9474(18)
_cell_length_b                   14.320(2)
_cell_length_c                   19.292(3)
_cell_angle_alpha                104.883(2)
_cell_angle_beta                 91.015(2)
_cell_angle_gamma                99.535(2)
_cell_volume                     2876.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8165
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      26.02

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.124
_exptl_absorpt_coefficient_mu    0.128
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34791
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.890
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             13873
_reflns_number_gt                9651
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0628P)²+1.0459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13873
_refine_ls_number_parameters     769
_refine_ls_number_restraints     432
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1481
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P -0.00072(4) 0.67751(4) 0.33436(2) 0.02764(12) Uani 1 1 d . . . . .
P2 P 0.41060(4) 0.31974(4) 0.16448(3) 0.02868(12) Uani 1 1 d . . . . .
O1 O 0.27855(13) 0.79346(10) 0.18620(7) 0.0375(3) Uani 1 1 d . . . . .
O2 O 0.12059(13) 0.67323(10) 0.19517(7) 0.0411(4) Uani 1 1 d . . . . .
O3 O -0.32555(15) 0.83753(12) 0.41574(8) 0.0512(4) Uani 1 1 d . . . . .
O4 O -0.20494(15) 0.79167(12) 0.32347(8) 0.0467(4) Uani 1 1 d . . . . .
O7 O 0.54856(13) 0.32599(10) 0.30457(7) 0.0392(3) Uani 1 1 d . . . . .
O8 O 0.62462(13) 0.19300(10) 0.31931(7) 0.0391(3) Uani 1 1 d . . . . .
B1 B 0.1865(2) 0.76382(16) 0.22699(11) 0.0293(4) Uani 1 1 d . . . . .
B2 B -0.2352(2) 0.78491(16) 0.38982(12) 0.0303(4) Uani 1 1 d . . . . .
B4 B 0.5572(2) 0.23056(17) 0.27555(12) 0.0327(5) Uani 1 1 d . . . . .
B3 B 0.1265(9) 0.2081(8) 0.1047(5) 0.0347(11) Uani 0.694(4) 1 d . U P A 1
O5 O 0.0126(3) 0.1597(3) 0.0794(2) 0.0628(9) Uani 0.694(4) 1 d . U P A 1
O6 O 0.1618(3) 0.2009(3) 0.1703(2) 0.0449(7) Uani 0.694(4) 1 d . U P A 1
C71 C -0.0433(4) 0.1219(4) 0.1375(3) 0.0611(10) Uani 0.694(4) 1 d . U P A 1
C72 C -0.1204(5) 0.1978(4) 0.1814(4) 0.1008(17) Uani 0.694(4) 1 d . U P A 1
H72A H -0.1688 0.1689 0.2153 0.151 Uiso 0.694(4) 1 calc R U P A 1
H72B H -0.1767 0.2147 0.1483 0.151 Uiso 0.694(4) 1 calc R U P A 1
H72C H -0.0638 0.2573 0.2079 0.151 Uiso 0.694(4) 1 calc R U P A 1
C73 C -0.1283(5) 0.0270(5) 0.1036(3) 0.0943(17) Uani 0.694(4) 1 d . U P A 1
H73A H -0.1627 -0.0025 0.1412 0.141 Uiso 0.694(4) 1 calc R U P A 1
H73B H -0.0817 -0.0180 0.0722 0.141 Uiso 0.694(4) 1 calc R U P A 1
H73C H -0.1960 0.0393 0.0751 0.141 Uiso 0.694(4) 1 calc R U P A 1
C74 C 0.0697(4) 0.1227(4) 0.1846(3) 0.0508(9) Uani 0.694(4) 1 d . U P A 1
C75 C 0.0607(6) 0.1460(4) 0.2649(3) 0.0843(15) Uani 0.694(4) 1 d . U P A 1
H75A H -0.0033 0.0968 0.2766 0.126 Uiso 0.694(4) 1 calc R U P A 1
H75B H 0.0386 0.2112 0.2823 0.126 Uiso 0.694(4) 1 calc R U P A 1
H75C H 0.1408 0.1451 0.2880 0.126 Uiso 0.694(4) 1 calc R U P A 1
C76 C 0.1228(5) 0.0279(4) 0.1615(3) 0.0776(14) Uani 0.694(4) 1 d . U P A 1
H76A H 0.0689 -0.0248 0.1759 0.116 Uiso 0.694(4) 1 calc R U P A 1
H76B H 0.2062 0.0380 0.1846 0.116 Uiso 0.694(4) 1 calc R U P A 1
H76C H 0.1274 0.0096 0.1092 0.116 Uiso 0.694(4) 1 calc R U P A 1
B3A B 0.138(3) 0.215(2) 0.0978(15) 0.0442(18) Uani 0.306(4) 1 d . U P A 2
O5A O 0.0482(7) 0.1256(6) 0.0613(4) 0.0544(14) Uani 0.306(4) 1 d . U P A 2
O6A O 0.1258(7) 0.2246(6) 0.1682(5) 0.0497(15) Uani 0.306(4) 1 d . U P A 2
C71A C -0.0293(11) 0.0911(9) 0.1123(7) 0.0638(16) Uani 0.306(4) 1 d . U P A 2
C72A C -0.1516(9) 0.1419(10) 0.1141(8) 0.087(2) Uani 0.306(4) 1 d . U P A 2
H72D H -0.2090 0.1193 0.1472 0.130 Uiso 0.306(4) 1 calc R U P A 2
H72E H -0.1926 0.1237 0.0658 0.130 Uiso 0.306(4) 1 calc R U P A 2
H72F H -0.1270 0.2134 0.1304 0.130 Uiso 0.306(4) 1 calc R U P A 2
C73A C -0.0637(14) -0.0126(9) 0.0936(7) 0.092(3) Uani 0.306(4) 1 d . U P A 2
H73D H -0.1077 -0.0351 0.0459 0.138 Uiso 0.306(4) 1 calc R U P A 2
H73E H -0.1182 -0.0321 0.1291 0.138 Uiso 0.306(4) 1 calc R U P A 2
H73F H 0.0109 -0.0423 0.0927 0.138 Uiso 0.306(4) 1 calc R U P A 2
C74A C 0.0372(12) 0.1466(10) 0.1866(8) 0.0602(16) Uani 0.306(4) 1 d . U P A 2
C75A C -0.0270(12) 0.1859(9) 0.2485(7) 0.092(3) Uani 0.306(4) 1 d . U P A 2
H75D H -0.0913 0.1342 0.2567 0.138 Uiso 0.306(4) 1 calc R U P A 2
H75E H -0.0655 0.2397 0.2406 0.138 Uiso 0.306(4) 1 calc R U P A 2
H75F H 0.0320 0.2106 0.2906 0.138 Uiso 0.306(4) 1 calc R U P A 2
C76A C 0.1263(12) 0.0831(11) 0.2100(8) 0.092(3) Uani 0.306(4) 1 d . U P A 2
H76D H 0.0783 0.0342 0.2309 0.138 Uiso 0.306(4) 1 calc R U P A 2
H76E H 0.1900 0.1259 0.2457 0.138 Uiso 0.306(4) 1 calc R U P A 2
H76F H 0.1661 0.0498 0.1679 0.138 Uiso 0.306(4) 1 calc R U P A 2
C1 C 0.11938(17) 0.60264(14) 0.33782(9) 0.0291(4) Uani 1 1 d . . . . .
C2 C 0.09064(19) 0.50354(14) 0.30146(11) 0.0354(4) Uani 1 1 d . . . . .
H2 H 0.0100 0.4770 0.2790 0.042 Uiso 1 1 calc R U . . .
C3 C 0.1786(2) 0.44287(16) 0.29766(11) 0.0406(5) Uani 1 1 d . . . . .
H3 H 0.1577 0.3753 0.2728 0.049 Uiso 1 1 calc R U . . .
C4 C 0.2965(2) 0.48054(16) 0.33001(11) 0.0411(5) Uani 1 1 d . . . . .
H4 H 0.3570 0.4394 0.3268 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3252(2) 0.57795(17) 0.36679(11) 0.0411(5) Uani 1 1 d . . . . .
H5 H 0.4057 0.6038 0.3896 0.049 Uiso 1 1 calc R U . . .
C6 C 0.23765(18) 0.63935(15) 0.37109(10) 0.0356(4) Uani 1 1 d . . . . .
H6 H 0.2588 0.7065 0.3968 0.043 Uiso 1 1 calc R U . . .
C11 C 0.09321(16) 0.80222(13) 0.35516(10) 0.0279(4) Uani 1 1 d . . . . .
C12 C 0.08984(19) 0.87052(15) 0.42107(10) 0.0369(4) Uani 1 1 d . . . . .
H12 H 0.0418 0.8512 0.4572 0.044 Uiso 1 1 calc R U . . .
C13 C 0.1548(2) 0.96602(16) 0.43524(12) 0.0442(5) Uani 1 1 d . . . . .
H13 H 0.1508 1.0113 0.4804 0.053 Uiso 1 1 calc R U . . .
C14 C 0.2255(2) 0.99464(16) 0.38311(12) 0.0450(5) Uani 1 1 d . . . . .
H14 H 0.2694 1.0600 0.3920 0.054 Uiso 1 1 calc R U . . .
C15 C 0.23182(19) 0.92765(15) 0.31798(11) 0.0364(4) Uani 1 1 d . . . . .
H15 H 0.2821 0.9476 0.2829 0.044 Uiso 1 1 calc R U . . .
C16 C 0.16641(17) 0.83135(13) 0.30216(10) 0.0290(4) Uani 1 1 d . . . . .
C21 C -0.07603(17) 0.67720(13) 0.41910(10) 0.0287(4) Uani 1 1 d . . . . .
C22 C -0.03911(18) 0.62545(15) 0.46575(10) 0.0339(4) Uani 1 1 d . . . . .
H22 H 0.0290 0.5920 0.4547 0.041 Uiso 1 1 calc R U . . .
C23 C -0.0996(2) 0.62178(16) 0.52798(11) 0.0389(5) Uani 1 1 d . . . . .
H23 H -0.0729 0.5859 0.5587 0.047 Uiso 1 1 calc R U . . .
C24 C -0.1983(2) 0.67009(16) 0.54518(11) 0.0412(5) Uani 1 1 d . . . . .
H24 H -0.2394 0.6685 0.5879 0.049 Uiso 1 1 calc R U . . .
C25 C -0.23655(19) 0.72095(16) 0.49931(11) 0.0378(5) Uani 1 1 d . . . . .
H25 H -0.3044 0.7544 0.5114 0.045 Uiso 1 1 calc R U . . .
C26 C -0.17924(17) 0.72512(14) 0.43569(10) 0.0296(4) Uani 1 1 d . . . . .
C31 C 0.33461(17) 0.31992(14) 0.07833(10) 0.0300(4) Uani 1 1 d . . . . .
C32 C 0.39401(19) 0.37280(15) 0.03326(10) 0.0344(4) Uani 1 1 d . . . . .
H32 H 0.4770 0.4063 0.0459 0.041 Uiso 1 1 calc R U . . .
C33 C 0.3349(2) 0.37769(16) -0.02967(11) 0.0402(5) Uani 1 1 d . . . . .
H33 H 0.3771 0.4150 -0.0590 0.048 Uiso 1 1 calc R U . . .
C34 C 0.2153(2) 0.32863(17) -0.04961(12) 0.0449(5) Uani 1 1 d . . . . .
H34 H 0.1749 0.3309 -0.0930 0.054 Uiso 1 1 calc R U . . .
C35 C 0.1548(2) 0.27601(17) -0.00552(12) 0.0455(5) Uani 1 1 d . . . . .
H35 H 0.0724 0.2419 -0.0195 0.055 Uiso 1 1 calc R U . . .
C36 C 0.21069(18) 0.27119(15) 0.05899(11) 0.0348(4) Uani 1 1 d . . . . .
C41 C 0.44318(17) 0.19375(14) 0.14615(10) 0.0300(4) Uani 1 1 d . . . . .
C42 C 0.4029(2) 0.12387(15) 0.08126(11) 0.0392(5) Uani 1 1 d . . . . .
H42 H 0.3653 0.1433 0.0437 0.047 Uiso 1 1 calc R U . . .
C43 C 0.4167(2) 0.02676(16) 0.07054(13) 0.0529(6) Uani 1 1 d . . . . .
H43 H 0.3871 -0.0196 0.0263 0.064 Uiso 1 1 calc R U . . .
C44 C 0.4728(3) -0.00272(17) 0.12342(15) 0.0649(8) Uani 1 1 d . . . . .
H44 H 0.4819 -0.0693 0.1162 0.078 Uiso 1 1 calc R U . . .
C45 C 0.5157(2) 0.06522(16) 0.18695(13) 0.0510(6) Uani 1 1 d . . . . .
H45 H 0.5565 0.0448 0.2229 0.061 Uiso 1 1 calc R U . . .
C46 C 0.50148(18) 0.16369(14) 0.20070(10) 0.0339(4) Uani 1 1 d . . . . .
C51 C 0.25956(19) 0.72234(15) 0.11586(10) 0.0351(4) Uani 1 1 d . . . . .
C52 C 0.1832(3) 0.7649(2) 0.06938(13) 0.0639(7) Uani 1 1 d . . . . .
H52A H 0.1726 0.7223 0.0202 0.096 Uiso 1 1 calc R U . . .
H52B H 0.2259 0.8305 0.0690 0.096 Uiso 1 1 calc R U . . .
H52C H 0.1016 0.7693 0.0888 0.096 Uiso 1 1 calc R U . . .
C53 C 0.3828(2) 0.7098(2) 0.08390(14) 0.0584(7) Uani 1 1 d . . . . .
H53A H 0.3701 0.6541 0.0410 0.088 Uiso 1 1 calc R U . . .
H53B H 0.4391 0.6975 0.1193 0.088 Uiso 1 1 calc R U . . .
H53C H 0.4190 0.7696 0.0707 0.088 Uiso 1 1 calc R U . . .
C54 C 0.1903(2) 0.63011(15) 0.13425(11) 0.0398(5) Uani 1 1 d . . . . .
C55 C 0.1004(3) 0.5630(2) 0.07478(14) 0.0691(9) Uani 1 1 d . . . . .
H55A H 0.1446 0.5435 0.0311 0.104 Uiso 1 1 calc R U . . .
H55B H 0.0345 0.5976 0.0652 0.104 Uiso 1 1 calc R U . . .
H55C H 0.0638 0.5044 0.0895 0.104 Uiso 1 1 calc R U . . .
C56 C 0.2773(3) 0.5743(2) 0.16233(14) 0.0705(9) Uani 1 1 d . . . . .
H56A H 0.3247 0.5431 0.1231 0.106 Uiso 1 1 calc R U . . .
H56B H 0.2289 0.5238 0.1817 0.106 Uiso 1 1 calc R U . . .
H56C H 0.3345 0.6198 0.2004 0.106 Uiso 1 1 calc R U . . .
C61 C -0.3736(2) 0.87033(17) 0.35647(13) 0.0458(5) Uani 1 1 d . . . . .
C62 C -0.4871(3) 0.7963(2) 0.3213(2) 0.0943(12) Uani 1 1 d . . . . .
H62A H -0.5222 0.8171 0.2819 0.141 Uiso 1 1 calc R U . . .
H62B H -0.5490 0.7919 0.3569 0.141 Uiso 1 1 calc R U . . .
H62C H -0.4634 0.7319 0.3024 0.141 Uiso 1 1 calc R U . . .
C63 C -0.4093(3) 0.9693(2) 0.38795(15) 0.0667(8) Uani 1 1 d . . . . .
H63A H -0.4346 0.9959 0.3490 0.100 Uiso 1 1 calc R U . . .
H63B H -0.3381 1.0142 0.4164 0.100 Uiso 1 1 calc R U . . .
H63C H -0.4784 0.9620 0.4189 0.100 Uiso 1 1 calc R U . . .
C64 C -0.2640(2) 0.86957(18) 0.30814(12) 0.0484(6) Uani 1 1 d . . . . .
C65 C -0.2968(4) 0.8426(3) 0.22810(15) 0.0963(13) Uani 1 1 d . . . . .
H65A H -0.3365 0.8936 0.2163 0.144 Uiso 1 1 calc R U . . .
H65B H -0.3540 0.7797 0.2140 0.144 Uiso 1 1 calc R U . . .
H65C H -0.2211 0.8372 0.2021 0.144 Uiso 1 1 calc R U . . .
C66 C -0.1685(3) 0.9631(2) 0.3299(2) 0.0815(10) Uani 1 1 d . . . . .
H66A H -0.2044 1.0176 0.3210 0.122 Uiso 1 1 calc R U . . .
H66B H -0.0956 0.9549 0.3017 0.122 Uiso 1 1 calc R U . . .
H66C H -0.1437 0.9774 0.3812 0.122 Uiso 1 1 calc R U . . .
C81 C 0.6383(2) 0.36203(16) 0.36766(11) 0.0399(5) Uani 1 1 d . . . . .
C82 C 0.7597(2) 0.4048(2) 0.34067(14) 0.0596(7) Uani 1 1 d . . . . .
H82A H 0.8228 0.4296 0.3808 0.089 Uiso 1 1 calc R U . . .
H82B H 0.7463 0.4587 0.3204 0.089 Uiso 1 1 calc R U . . .
H82C H 0.7879 0.3535 0.3035 0.089 Uiso 1 1 calc R U . . .
C83 C 0.5888(3) 0.43901(19) 0.42328(14) 0.0609(7) Uani 1 1 d . . . . .
H83A H 0.6419 0.4571 0.4678 0.091 Uiso 1 1 calc R U . . .
H83B H 0.5041 0.4128 0.4328 0.091 Uiso 1 1 calc R U . . .
H83C H 0.5883 0.4971 0.4054 0.091 Uiso 1 1 calc R U . . .
C84 C 0.64649(19) 0.26591(16) 0.38869(10) 0.0378(5) Uani 1 1 d . . . . .
C85 C 0.7704(2) 0.2621(2) 0.42261(13) 0.0539(6) Uani 1 1 d . . . . .
H85A H 0.7912 0.3171 0.4657 0.081 Uiso 1 1 calc R U . . .
H85B H 0.8345 0.2668 0.3883 0.081 Uiso 1 1 calc R U . . .
H85C H 0.7658 0.2001 0.4359 0.081 Uiso 1 1 calc R U . . .
C86 C 0.5425(2) 0.2375(2) 0.43438(13) 0.0548(6) Uani 1 1 d . . . . .
H86A H 0.5546 0.2833 0.4824 0.082 Uiso 1 1 calc R U . . .
H86B H 0.5430 0.1707 0.4384 0.082 Uiso 1 1 calc R U . . .
H86C H 0.4626 0.2402 0.4119 0.082 Uiso 1 1 calc R U . . .
C91 C 0.56570(17) 0.39119(14) 0.16238(10) 0.0297(4) Uani 1 1 d . . . . .
C92 C 0.58615(19) 0.48961(14) 0.20101(11) 0.0354(4) Uani 1 1 d . . . . .
H92 H 0.5199 0.5171 0.2247 0.042 Uiso 1 1 calc R U . . .
C93 C 0.7021(2) 0.54807(15) 0.20536(11) 0.0398(5) Uani 1 1 d . . . . .
H93 H 0.7147 0.6151 0.2319 0.048 Uiso 1 1 calc R U . . .
C94 C 0.7992(2) 0.50903(16) 0.17123(11) 0.0395(5) Uani 1 1 d . . . . .
H94 H 0.8787 0.5488 0.1744 0.047 Uiso 1 1 calc R U . . .
C95 C 0.77995(19) 0.41202(17) 0.13255(11) 0.0425(5) Uani 1 1 d . . . . .
H95 H 0.8465 0.3851 0.1088 0.051 Uiso 1 1 calc R U . . .
C96 C 0.66402(18) 0.35323(15) 0.12790(11) 0.0365(4) Uani 1 1 d . . . . .
H96 H 0.6519 0.2865 0.1009 0.044 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 C1 1.8394(19) . ?
P1 C21 1.8447(19) . ?
P1 C11 1.8483(19) . ?
P2 C91 1.8384(19) . ?
P2 C41 1.843(2) . ?
P2 C31 1.8460(19) . ?
O1 B1 1.368(2) . ?
O1 C51 1.460(2) . ?
O2 B1 1.358(3) . ?
O2 C54 1.470(2) . ?
O3 B2 1.366(3) . ?
O3 C61 1.463(3) . ?
O4 B2 1.351(3) . ?
O4 C64 1.467(2) . ?
O7 B4 1.357(3) . ?
O7 C81 1.477(2) . ?
O8 B4 1.374(3) . ?
O8 C84 1.458(2) . ?
B1 C16 1.565(3) . ?
B2 C26 1.560(3) . ?
B4 C46 1.562(3) . ?
B3 O5 1.338(10) . ?
B3 O6 1.351(11) . ?
B3 C36 1.615(7) . ?
O5 C71 1.465(5) . ?
O6 C74 1.464(5) . ?
C71 C73 1.497(7) . ?
C71 C74 1.520(7) . ?
C71 C72 1.571(7) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C75 1.507(7) . ?
C74 C76 1.530(6) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
B3A O6A 1.34(3) . ?
B3A C36 1.40(2) . ?
B3A O5A 1.48(3) . ?
O5A C71A 1.440(13) . ?
O6A C74A 1.474(14) . ?
C71A C73A 1.418(16) . ?
C71A C74A 1.550(19) . ?
C71A C72A 1.623(17) . ?
C72A H72D 0.9800 . ?
C72A H72E 0.9800 . ?
C72A H72F 0.9800 . ?
C73A H73D 0.9800 . ?
C73A H73E 0.9800 . ?
C73A H73F 0.9800 . ?
C74A C75A 1.432(16) . ?
C74A C76A 1.572(17) . ?
C75A H75D 0.9800 . ?
C75A H75E 0.9800 . ?
C75A H75F 0.9800 . ?
C76A H76D 0.9800 . ?
C76A H76E 0.9800 . ?
C76A H76F 0.9800 . ?
C1 C6 1.392(3) . ?
C1 C2 1.392(3) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C11 C12 1.396(3) . ?
C11 C16 1.414(3) . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.399(3) . ?
C15 H15 0.9500 . ?
C21 C22 1.397(3) . ?
C21 C26 1.417(3) . ?
C22 C23 1.390(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.398(3) . ?
C25 H25 0.9500 . ?
C31 C32 1.395(3) . ?
C31 C36 1.415(3) . ?
C32 C33 1.389(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.376(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.400(3) . ?
C35 H35 0.9500 . ?
C41 C42 1.398(3) . ?
C41 C46 1.414(3) . ?
C42 C43 1.386(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.372(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.373(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.402(3) . ?
C45 H45 0.9500 . ?
C51 C53 1.511(3) . ?
C51 C52 1.516(3) . ?
C51 C54 1.537(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.513(3) . ?
C54 C56 1.515(3) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C61 C63 1.510(3) . ?
C61 C62 1.514(4) . ?
C61 C64 1.533(3) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C65 1.513(3) . ?
C64 C66 1.515(4) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C81 C83 1.507(3) . ?
C81 C82 1.527(3) . ?
C81 C84 1.547(3) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 C85 1.510(3) . ?
C84 C86 1.518(3) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C91 C96 1.389(3) . ?
C91 C92 1.394(3) . ?
C92 C93 1.388(3) . ?
C92 H92 0.9500 . ?
C93 C94 1.381(3) . ?
C93 H93 0.9500 . ?
C94 C95 1.377(3) . ?
C94 H94 0.9500 . ?
C95 C96 1.390(3) . ?
C95 H95 0.9500 . ?
C96 H96 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
C1 P1 C21 101.94(8) . . ?
C1 P1 C11 101.42(8) . . ?
C21 P1 C11 102.34(8) . . ?
C91 P2 C41 101.82(9) . . ?
C91 P2 C31 102.18(8) . . ?
C41 P2 C31 102.34(8) . . ?
B1 O1 C51 106.70(15) . . ?
B1 O2 C54 106.48(15) . . ?
B2 O3 C61 107.19(16) . . ?
B2 O4 C64 107.11(16) . . ?
B4 O7 C81 106.52(15) . . ?
B4 O8 C84 106.71(16) . . ?
O2 B1 O1 112.85(17) . . ?
O2 B1 C16 126.54(18) . . ?
O1 B1 C16 120.61(18) . . ?
O4 B2 O3 112.62(18) . . ?
O4 B2 C26 127.05(18) . . ?
O3 B2 C26 120.32(18) . . ?
O7 B4 O8 113.13(18) . . ?
O7 B4 C46 127.41(18) . . ?
O8 B4 C46 119.46(18) . . ?
O5 B3 O6 114.9(5) . . ?
O5 B3 C36 120.9(7) . . ?
O6 B3 C36 124.2(7) . . ?
B3 O5 C71 106.6(5) . . ?
B3 O6 C74 105.3(5) . . ?
O5 C71 C73 107.6(4) . . ?
O5 C71 C74 102.3(4) . . ?
C73 C71 C74 119.8(5) . . ?
O5 C71 C72 108.8(4) . . ?
C73 C71 C72 109.6(4) . . ?
C74 C71 C72 108.2(5) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
O6 C74 C75 106.9(4) . . ?
O6 C74 C71 103.2(4) . . ?
C75 C74 C71 118.9(4) . . ?
O6 C74 C76 106.9(3) . . ?
C75 C74 C76 107.6(4) . . ?
C71 C74 C76 112.6(5) . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C74 C76 H76A 109.5 . . ?
C74 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C74 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
O6A B3A C36 133(2) . . ?
O6A B3A O5A 104.9(15) . . ?
C36 B3A O5A 121.7(19) . . ?
C71A O5A B3A 110.7(11) . . ?
B3A O6A C74A 115.8(14) . . ?
C73A C71A O5A 112.7(10) . . ?
C73A C71A C74A 120.4(12) . . ?
O5A C71A C74A 104.6(9) . . ?
C73A C71A C72A 110.3(11) . . ?
O5A C71A C72A 106.1(9) . . ?
C74A C71A C72A 101.4(10) . . ?
C71A C72A H72D 109.5 . . ?
C71A C72A H72E 109.5 . . ?
H72D C72A H72E 109.5 . . ?
C71A C72A H72F 109.5 . . ?
H72D C72A H72F 109.5 . . ?
H72E C72A H72F 109.5 . . ?
C71A C73A H73D 109.5 . . ?
C71A C73A H73E 109.5 . . ?
H73D C73A H73E 109.5 . . ?
C71A C73A H73F 109.5 . . ?
H73D C73A H73F 109.5 . . ?
H73E C73A H73F 109.5 . . ?
C75A C74A O6A 110.9(10) . . ?
C75A C74A C71A 123.5(12) . . ?
O6A C74A C71A 101.7(10) . . ?
C75A C74A C76A 106.9(12) . . ?
O6A C74A C76A 101.9(9) . . ?
C71A C74A C76A 109.8(12) . . ?
C74A C75A H75D 109.5 . . ?
C74A C75A H75E 109.5 . . ?
H75D C75A H75E 109.5 . . ?
C74A C75A H75F 109.5 . . ?
H75D C75A H75F 109.5 . . ?
H75E C75A H75F 109.5 . . ?
C74A C76A H76D 109.5 . . ?
C74A C76A H76E 109.5 . . ?
H76D C76A H76E 109.5 . . ?
C74A C76A H76F 109.5 . . ?
H76D C76A H76F 109.5 . . ?
H76E C76A H76F 109.5 . . ?
C6 C1 C2 118.48(18) . . ?
C6 C1 P1 124.46(15) . . ?
C2 C1 P1 116.99(15) . . ?
C3 C2 C1 120.8(2) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 119.40(19) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.9(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 120.26(19) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C12 C11 C16 118.67(17) . . ?
C12 C11 P1 121.70(15) . . ?
C16 C11 P1 119.56(13) . . ?
C13 C12 C11 121.75(19) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C14 C13 C12 119.50(19) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 C13 119.6(2) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 122.0(2) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C15 C16 C11 118.46(17) . . ?
C15 C16 B1 115.65(17) . . ?
C11 C16 B1 125.83(17) . . ?
C22 C21 C26 118.48(17) . . ?
C22 C21 P1 121.70(14) . . ?
C26 C21 P1 119.69(14) . . ?
C23 C22 C21 121.57(18) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C24 C23 C22 120.16(19) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 118.97(19) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C24 C25 C26 122.54(19) . . ?
C24 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
C25 C26 C21 118.24(17) . . ?
C25 C26 B2 115.80(17) . . ?
C21 C26 B2 125.94(17) . . ?
C32 C31 C36 118.45(18) . . ?
C32 C31 P2 121.35(15) . . ?
C36 C31 P2 120.07(14) . . ?
C33 C32 C31 121.66(19) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 119.0(2) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C34 C35 C36 122.3(2) . . ?
C34 C35 H35 118.8 . . ?
C36 C35 H35 118.8 . . ?
B3A C36 C35 115.7(12) . . ?
B3A C36 C31 125.9(12) . . ?
C35 C36 C31 118.38(18) . . ?
C35 C36 B3 116.0(4) . . ?
C31 C36 B3 125.6(4) . . ?
C42 C41 C46 118.37(18) . . ?
C42 C41 P2 121.67(15) . . ?
C46 C41 P2 119.77(14) . . ?
C43 C42 C41 121.4(2) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C44 C43 C42 120.4(2) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 119.2(2) . . ?
C43 C44 H44 120.4 . . ?
C45 C44 H44 120.4 . . ?
C44 C45 C46 122.4(2) . . ?
C44 C45 H45 118.8 . . ?
C46 C45 H45 118.8 . . ?
C45 C46 C41 118.28(18) . . ?
C45 C46 B4 115.23(18) . . ?
C41 C46 B4 126.46(18) . . ?
O1 C51 C53 110.33(17) . . ?
O1 C51 C52 105.86(17) . . ?
C53 C51 C52 109.9(2) . . ?
O1 C51 C54 101.92(15) . . ?
C53 C51 C54 113.89(19) . . ?
C52 C51 C54 114.4(2) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O2 C54 C55 109.30(18) . . ?
O2 C54 C56 106.67(17) . . ?
C55 C54 C56 111.6(2) . . ?
O2 C54 C51 101.58(15) . . ?
C55 C54 C51 114.4(2) . . ?
C56 C54 C51 112.5(2) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O3 C61 C63 107.7(2) . . ?
O3 C61 C62 107.7(2) . . ?
C63 C61 C62 110.1(2) . . ?
O3 C61 C64 101.84(16) . . ?
C63 C61 C64 115.9(2) . . ?
C62 C61 C64 112.8(2) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
O4 C64 C65 107.76(19) . . ?
O4 C64 C66 106.7(2) . . ?
C65 C64 C66 110.2(3) . . ?
O4 C64 C61 102.15(16) . . ?
C65 C64 C61 116.1(2) . . ?
C66 C64 C61 113.2(2) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O7 C81 C83 108.75(18) . . ?
O7 C81 C82 106.31(17) . . ?
C83 C81 C82 111.5(2) . . ?
O7 C81 C84 101.49(15) . . ?
C83 C81 C84 115.5(2) . . ?
C82 C81 C84 112.35(19) . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
O8 C84 C85 109.08(17) . . ?
O8 C84 C86 106.32(17) . . ?
C85 C84 C86 110.19(19) . . ?
O8 C84 C81 102.10(15) . . ?
C85 C84 C81 115.26(19) . . ?
C86 C84 C81 113.14(19) . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C84 C86 H86A 109.5 . . ?
C84 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C84 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C96 C91 C92 118.33(18) . . ?
C96 C91 P2 124.83(15) . . ?
C92 C91 P2 116.78(14) . . ?
C93 C92 C91 120.83(19) . . ?
C93 C92 H92 119.6 . . ?
C91 C92 H92 119.6 . . ?
C94 C93 C92 120.14(19) . . ?
C94 C93 H93 119.9 . . ?
C92 C93 H93 119.9 . . ?
C95 C94 C93 119.57(19) . . ?
C95 C94 H94 120.2 . . ?
C93 C94 H94 120.2 . . ?
C94 C95 C96 120.5(2) . . ?
C94 C95 H95 119.7 . . ?
C96 C95 H95 119.7 . . ?
C91 C96 C95 120.60(19) . . ?
C91 C96 H96 119.7 . . ?
C95 C96 H96 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C54 O2 B1 O1 12.1(2) . . . . ?
C54 O2 B1 C16 -167.30(18) . . . . ?
C51 O1 B1 O2 9.5(2) . . . . ?
C51 O1 B1 C16 -171.00(16) . . . . ?
C64 O4 B2 O3 10.8(2) . . . . ?
C64 O4 B2 C26 -169.6(2) . . . . ?
C61 O3 B2 O4 9.4(2) . . . . ?
C61 O3 B2 C26 -170.18(18) . . . . ?
C81 O7 B4 O8 11.7(2) . . . . ?
C81 O7 B4 C46 -167.7(2) . . . . ?
C84 O8 B4 O7 9.5(2) . . . . ?
C84 O8 B4 C46 -170.96(18) . . . . ?
O6 B3 O5 C71 6.2(10) . . . . ?
C36 B3 O5 C71 -172.6(7) . . . . ?
O5 B3 O6 C74 12.1(10) . . . . ?
C36 B3 O6 C74 -169.1(8) . . . . ?
B3 O5 C71 C73 -147.9(7) . . . . ?
B3 O5 C71 C74 -20.8(7) . . . . ?
B3 O5 C71 C72 93.5(7) . . . . ?
B3 O6 C74 C75 -150.3(7) . . . . ?
B3 O6 C74 C71 -24.2(7) . . . . ?
B3 O6 C74 C76 94.8(7) . . . . ?
O5 C71 C74 O6 27.1(4) . . . . ?
C73 C71 C74 O6 145.9(4) . . . . ?
C72 C71 C74 O6 -87.7(4) . . . . ?
O5 C71 C74 C75 145.1(4) . . . . ?
C73 C71 C74 C75 -96.1(6) . . . . ?
C72 C71 C74 C75 30.4(6) . . . . ?
O5 C71 C74 C76 -87.8(4) . . . . ?
C73 C71 C74 C76 31.0(6) . . . . ?
C72 C71 C74 C76 157.5(4) . . . . ?
O6A B3A O5A C71A 8(3) . . . . ?
C36 B3A O5A C71A -170(2) . . . . ?
C36 B3A O6A C74A -179(3) . . . . ?
O5A B3A O6A C74A 2(3) . . . . ?
B3A O5A C71A C73A -147.1(17) . . . . ?
B3A O5A C71A C74A -14.6(18) . . . . ?
B3A O5A C71A C72A 92.1(17) . . . . ?
B3A O6A C74A C75A -143.7(19) . . . . ?
B3A O6A C74A C71A -11(2) . . . . ?
B3A O6A C74A C76A 102.8(19) . . . . ?
C73A C71A C74A C75A -92.4(17) . . . . ?
O5A C71A C74A C75A 139.7(12) . . . . ?
C72A C71A C74A C75A 29.5(15) . . . . ?
C73A C71A C74A O6A 142.4(11) . . . . ?
O5A C71A C74A O6A 14.5(12) . . . . ?
C72A C71A C74A O6A -95.6(9) . . . . ?
C73A C71A C74A C76A 35.1(16) . . . . ?
O5A C71A C74A C76A -92.8(11) . . . . ?
C72A C71A C74A C76A 157.1(9) . . . . ?
C21 P1 C1 C6 -87.10(17) . . . . ?
C11 P1 C1 C6 18.29(18) . . . . ?
C21 P1 C1 C2 96.16(15) . . . . ?
C11 P1 C1 C2 -158.45(15) . . . . ?
C6 C1 C2 C3 -0.8(3) . . . . ?
P1 C1 C2 C3 176.11(15) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C3 C4 C5 1.0(3) . . . . ?
C3 C4 C5 C6 -0.8(3) . . . . ?
C2 C1 C6 C5 1.0(3) . . . . ?
P1 C1 C6 C5 -175.71(15) . . . . ?
C4 C5 C6 C1 -0.2(3) . . . . ?
C1 P1 C11 C12 -107.97(16) . . . . ?
C21 P1 C11 C12 -2.88(18) . . . . ?
C1 P1 C11 C16 74.90(15) . . . . ?
C21 P1 C11 C16 179.99(14) . . . . ?
C16 C11 C12 C13 0.9(3) . . . . ?
P1 C11 C12 C13 -176.24(16) . . . . ?
C11 C12 C13 C14 -0.3(3) . . . . ?
C12 C13 C14 C15 -0.8(3) . . . . ?
C13 C14 C15 C16 1.4(3) . . . . ?
C14 C15 C16 C11 -0.8(3) . . . . ?
C14 C15 C16 B1 -178.29(19) . . . . ?
C12 C11 C16 C15 -0.3(3) . . . . ?
P1 C11 C16 C15 176.88(14) . . . . ?
C12 C11 C16 B1 176.85(18) . . . . ?
P1 C11 C16 B1 -5.9(3) . . . . ?
O2 B1 C16 C15 -169.63(19) . . . . ?
O1 B1 C16 C15 11.0(3) . . . . ?
O2 B1 C16 C11 13.1(3) . . . . ?
O1 B1 C16 C11 -166.30(17) . . . . ?
C1 P1 C21 C22 -1.72(18) . . . . ?
C11 P1 C21 C22 -106.40(16) . . . . ?
C1 P1 C21 C26 -177.56(15) . . . . ?
C11 P1 C21 C26 77.76(16) . . . . ?
C26 C21 C22 C23 -1.2(3) . . . . ?
P1 C21 C22 C23 -177.10(16) . . . . ?
C21 C22 C23 C24 -0.2(3) . . . . ?
C22 C23 C24 C25 0.7(3) . . . . ?
C23 C24 C25 C26 0.2(3) . . . . ?
C24 C25 C26 C21 -1.7(3) . . . . ?
C24 C25 C26 B2 179.4(2) . . . . ?
C22 C21 C26 C25 2.1(3) . . . . ?
P1 C21 C26 C25 178.07(15) . . . . ?
C22 C21 C26 B2 -179.06(18) . . . . ?
P1 C21 C26 B2 -3.1(3) . . . . ?
O4 B2 C26 C25 -172.8(2) . . . . ?
O3 B2 C26 C25 6.7(3) . . . . ?
O4 B2 C26 C21 8.3(3) . . . . ?
O3 B2 C26 C21 -172.15(19) . . . . ?
C91 P2 C31 C32 -4.32(18) . . . . ?
C41 P2 C31 C32 -109.48(16) . . . . ?
C91 P2 C31 C36 179.93(15) . . . . ?
C41 P2 C31 C36 74.76(17) . . . . ?
C36 C31 C32 C33 -0.6(3) . . . . ?
P2 C31 C32 C33 -176.38(15) . . . . ?
C31 C32 C33 C34 -0.9(3) . . . . ?
C32 C33 C34 C35 1.0(3) . . . . ?
C33 C34 C35 C36 0.3(4) . . . . ?
O6A B3A C36 C35 -144(3) . . . . ?
O5A B3A C36 C35 34(3) . . . . ?
O6A B3A C36 C31 38(4) . . . . ?
O5A B3A C36 C31 -143.9(17) . . . . ?
C34 C35 C36 B3A 179.9(15) . . . . ?
C34 C35 C36 C31 -1.7(3) . . . . ?
C34 C35 C36 B3 179.0(5) . . . . ?
C32 C31 C36 B3A -180.0(17) . . . . ?
P2 C31 C36 B3A -4.1(17) . . . . ?
C32 C31 C36 C35 1.8(3) . . . . ?
P2 C31 C36 C35 177.70(16) . . . . ?
C32 C31 C36 B3 -179.0(5) . . . . ?
P2 C31 C36 B3 -3.2(6) . . . . ?
O5 B3 C36 C35 3.3(11) . . . . ?
O6 B3 C36 C35 -175.3(8) . . . . ?
O5 B3 C36 C31 -175.8(6) . . . . ?
O6 B3 C36 C31 5.5(13) . . . . ?
C91 P2 C41 C42 -110.04(17) . . . . ?
C31 P2 C41 C42 -4.58(18) . . . . ?
C91 P2 C41 C46 75.16(16) . . . . ?
C31 P2 C41 C46 -179.39(15) . . . . ?
C46 C41 C42 C43 1.4(3) . . . . ?
P2 C41 C42 C43 -173.44(18) . . . . ?
C41 C42 C43 C44 -1.2(4) . . . . ?
C42 C43 C44 C45 -0.3(4) . . . . ?
C43 C44 C45 C46 1.7(4) . . . . ?
C44 C45 C46 C41 -1.4(4) . . . . ?
C44 C45 C46 B4 -179.4(2) . . . . ?
C42 C41 C46 C45 -0.1(3) . . . . ?
P2 C41 C46 C45 174.85(17) . . . . ?
C42 C41 C46 B4 177.60(19) . . . . ?
P2 C41 C46 B4 -7.4(3) . . . . ?
O7 B4 C46 C45 -174.7(2) . . . . ?
O8 B4 C46 C45 5.9(3) . . . . ?
O7 B4 C46 C41 7.5(3) . . . . ?
O8 B4 C46 C41 -171.92(19) . . . . ?
B1 O1 C51 C53 -146.96(19) . . . . ?
B1 O1 C51 C52 94.2(2) . . . . ?
B1 O1 C51 C54 -25.65(19) . . . . ?
B1 O2 C54 C55 -148.3(2) . . . . ?
B1 O2 C54 C56 90.9(2) . . . . ?
B1 O2 C54 C51 -27.1(2) . . . . ?
O1 C51 C54 O2 31.54(19) . . . . ?
C53 C51 C54 O2 150.35(18) . . . . ?
C52 C51 C54 O2 -82.2(2) . . . . ?
O1 C51 C54 C55 149.17(18) . . . . ?
C53 C51 C54 C55 -92.0(2) . . . . ?
C52 C51 C54 C55 35.5(3) . . . . ?
O1 C51 C54 C56 -82.15(19) . . . . ?
C53 C51 C54 C56 36.7(2) . . . . ?
C52 C51 C54 C56 164.13(19) . . . . ?
B2 O3 C61 C63 -146.7(2) . . . . ?
B2 O3 C61 C62 94.6(2) . . . . ?
B2 O3 C61 C64 -24.2(2) . . . . ?
B2 O4 C64 C65 -147.9(2) . . . . ?
B2 O4 C64 C66 93.8(2) . . . . ?
B2 O4 C64 C61 -25.1(2) . . . . ?
O3 C61 C64 O4 29.4(2) . . . . ?
C63 C61 C64 O4 145.9(2) . . . . ?
C62 C61 C64 O4 -85.8(2) . . . . ?
O3 C61 C64 C65 146.3(2) . . . . ?
C63 C61 C64 C65 -97.2(3) . . . . ?
C62 C61 C64 C65 31.1(3) . . . . ?
O3 C61 C64 C66 -84.9(2) . . . . ?
C63 C61 C64 C66 31.7(3) . . . . ?
C62 C61 C64 C66 159.9(2) . . . . ?
B4 O7 C81 C83 -148.5(2) . . . . ?
B4 O7 C81 C82 91.3(2) . . . . ?
B4 O7 C81 C84 -26.3(2) . . . . ?
B4 O8 C84 C85 -147.66(19) . . . . ?
B4 O8 C84 C86 93.5(2) . . . . ?
B4 O8 C84 C81 -25.3(2) . . . . ?
O7 C81 C84 O8 30.90(18) . . . . ?
C83 C81 C84 O8 148.32(18) . . . . ?
C82 C81 C84 O8 -82.3(2) . . . . ?
O7 C81 C84 C85 148.99(18) . . . . ?
C83 C81 C84 C85 -93.6(2) . . . . ?
C82 C81 C84 C85 35.8(3) . . . . ?
O7 C81 C84 C86 -82.9(2) . . . . ?
C83 C81 C84 C86 34.5(3) . . . . ?
C82 C81 C84 C86 163.90(19) . . . . ?
C41 P2 C91 C96 22.07(19) . . . . ?
C31 P2 C91 C96 -83.50(18) . . . . ?
C41 P2 C91 C92 -155.11(15) . . . . ?
C31 P2 C91 C92 99.32(16) . . . . ?
C96 C91 C92 C93 -0.5(3) . . . . ?
P2 C91 C92 C93 176.90(15) . . . . ?
C91 C92 C93 C94 0.0(3) . . . . ?
C92 C93 C94 C95 0.4(3) . . . . ?
C93 C94 C95 C96 -0.3(3) . . . . ?
C92 C91 C96 C95 0.6(3) . . . . ?
P2 C91 C96 C95 -176.55(16) . . . . ?
C94 C95 C96 C91 -0.2(3) . . . . ?

_refine_diff_density_max         0.455
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.048

_shelxl_version_number           2014/5


####################################################################### 
# 
# 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_3_H2O
_database_code_depnum_ccdc_archive 'CCDC 2109052'
loop_
_audit_author_name
_audit_author_address
'Rong Shang'
;Hiroshima University
Japan
;
_audit_update_record             
;
2021-09-10 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
#data_20210806oishiexp651_0m_a

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H59 B2 O4 P'
_chemical_formula_weight         680.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.542(8)
_cell_length_b                   10.722(8)
_cell_length_c                   17.445(14)
_cell_angle_alpha                96.766(7)
_cell_angle_beta                 96.231(14)
_cell_angle_gamma                104.461(9)
_cell_volume                     1877(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7333
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.93

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_F_000             736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.097
_exptl_absorpt_coefficient_mu    0.114
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22543
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.984
_diffrn_reflns_theta_max         28.044
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             8919
_reflns_number_gt                7177
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0450P)²+0.8169P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8919
_refine_ls_number_parameters     504
_refine_ls_number_restraints     216
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1103
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.44792(3) 0.40811(3) 0.76230(2) 0.01272(8) Uani 1 1 d . . . . .
C1 C 0.38927(13) 0.37140(13) 0.85182(8) 0.0156(3) Uani 1 1 d . . . . .
O1 O 0.55372(9) 0.33708(9) 0.74173(5) 0.0151(2) Uani 1 1 d . . . . .
B1 B 0.70569(15) 0.43522(15) 0.74859(9) 0.0164(3) Uani 1 1 d . . . . .
O2 O 0.41532(10) 0.12255(10) 0.64024(6) 0.0177(2) Uani 1 1 d . . . . .
H2A H 0.4711(13) 0.1847(18) 0.6721(10) 0.027 Uiso 1 1 calc R U . . .
C2 C 0.26981(15) 0.39280(16) 0.86888(9) 0.0237(3) Uani 1 1 d . . . . .
H2 H 0.2135 0.4176 0.8307 0.028 Uiso 1 1 calc R U . . .
B2 B 0.26673(15) 0.11205(15) 0.66107(10) 0.0165(3) Uani 1 1 d . . . . .
O3 O 0.45240(12) 0.17580(11) 0.50361(6) 0.0301(3) Uani 1 1 d . . . . .
C3 C 0.23345(17) 0.37757(18) 0.94233(10) 0.0306(4) Uani 1 1 d . . . . .
H3 H 0.1523 0.3926 0.9544 0.037 Uiso 1 1 calc R U . . .
C5 C 0.43362(15) 0.31814(15) 0.98056(9) 0.0246(3) Uani 1 1 d . . . . .
H5 H 0.4887 0.2912 1.0185 0.029 Uiso 1 1 calc R U . . .
C4 C 0.31526(17) 0.34067(16) 0.99763(9) 0.0282(3) Uani 1 1 d . . . . .
H4 H 0.2901 0.3307 1.0477 0.034 Uiso 1 1 calc R U . . .
C6 C 0.47152(14) 0.33498(14) 0.90805(8) 0.0202(3) Uani 1 1 d . . . . .
H6 H 0.5537 0.3217 0.8967 0.024 Uiso 1 1 calc R U . . .
C12 C 0.50446(14) 0.68208(14) 0.81051(8) 0.0185(3) Uani 1 1 d . . . . .
H12 H 0.4144 0.6744 0.8163 0.022 Uiso 1 1 calc R U . . .
C11 C 0.54567(13) 0.57278(13) 0.78307(8) 0.0151(3) Uani 1 1 d . . . . .
C13 C 0.59764(16) 0.80161(14) 0.82911(8) 0.0221(3) Uani 1 1 d . . . . .
H13 H 0.5721 0.8777 0.8469 0.027 Uiso 1 1 calc R U . . .
C14 C 0.72912(16) 0.80894(14) 0.82137(9) 0.0235(3) Uani 1 1 d . . . . .
H14 H 0.7931 0.8910 0.8337 0.028 Uiso 1 1 calc R U . . .
C16 C 0.67805(13) 0.57504(14) 0.77600(8) 0.0164(3) Uani 1 1 d . . . . .
C15 C 0.76888(14) 0.69893(14) 0.79605(8) 0.0208(3) Uani 1 1 d . . . . .
H15 H 0.8597 0.7074 0.7921 0.025 Uiso 1 1 calc R U . . .
C21 C 0.31549(13) 0.37924(13) 0.68231(8) 0.0137(3) Uani 1 1 d . . . . .
C22 C 0.29752(14) 0.49292(13) 0.65520(8) 0.0167(3) Uani 1 1 d . . . . .
H22 H 0.3497 0.5755 0.6814 0.020 Uiso 1 1 calc R U . . .
C23 C 0.20498(14) 0.48676(14) 0.59098(8) 0.0197(3) Uani 1 1 d . . . . .
H23 H 0.1934 0.5641 0.5731 0.024 Uiso 1 1 calc R U . . .
C24 C 0.13006(14) 0.36604(14) 0.55358(9) 0.0205(3) Uani 1 1 d . . . . .
H24 H 0.0655 0.3598 0.5099 0.025 Uiso 1 1 calc R U . . .
C25 C 0.14890(14) 0.25356(14) 0.57976(8) 0.0184(3) Uani 1 1 d . . . . .
H25 H 0.0961 0.1720 0.5525 0.022 Uiso 1 1 calc R U . . .
C26 C 0.24137(13) 0.25298(13) 0.64421(8) 0.0149(3) Uani 1 1 d . . . . .
C31 C 0.75883(14) 0.41769(14) 0.66573(8) 0.0189(3) Uani 1 1 d . . . . .
H31 H 0.6991 0.4438 0.6258 0.023 Uiso 1 1 calc R U . . .
C32 C 0.75788(15) 0.27507(15) 0.63961(9) 0.0244(3) Uani 1 1 d . . . . .
H32A H 0.6648 0.2231 0.6242 0.029 Uiso 1 1 calc R U . . .
H32B H 0.8027 0.2714 0.5927 0.029 Uiso 1 1 calc R U . . .
H80 H 0.425(2) 0.142(2) 0.5892(14) 0.056(7) Uiso 1 1 d . . . . .
C33 C 0.82449(16) 0.21090(16) 0.70072(10) 0.0300(4) Uani 1 1 d . . . . .
H33A H 0.9216 0.2408 0.7022 0.036 Uiso 1 1 calc R U . . .
H33B H 0.7974 0.1154 0.6842 0.036 Uiso 1 1 calc R U . . .
C34 C 0.79115(16) 0.24032(16) 0.78342(10) 0.0280(4) Uani 1 1 d . . . . .
H34A H 0.7004 0.1875 0.7857 0.034 Uiso 1 1 calc R U . . .
H34B H 0.8526 0.2125 0.8206 0.034 Uiso 1 1 calc R U . . .
C35 C 0.79942(14) 0.38417(15) 0.81015(9) 0.0205(3) Uani 1 1 d . . . . .
H35 H 0.7671 0.3918 0.8619 0.025 Uiso 1 1 calc R U . . .
C36 C 0.94108(14) 0.47419(17) 0.81866(9) 0.0262(3) Uani 1 1 d . . . . .
H36A H 1.0010 0.4371 0.8511 0.031 Uiso 1 1 calc R U . . .
H36B H 0.9422 0.5600 0.8472 0.031 Uiso 1 1 calc R U . . .
C37 C 0.99742(15) 0.49617(17) 0.74167(10) 0.0276(3) Uani 1 1 d . . . . .
H37A H 1.0729 0.5752 0.7523 0.033 Uiso 1 1 calc R U . . .
H37B H 1.0323 0.4215 0.7245 0.033 Uiso 1 1 calc R U . . .
C38 C 0.89847(14) 0.51194(16) 0.67395(9) 0.0234(3) Uani 1 1 d . . . . .
H38A H 0.9349 0.4985 0.6246 0.028 Uiso 1 1 calc R U . . .
H38B H 0.8905 0.6025 0.6816 0.028 Uiso 1 1 calc R U . . .
C41 C 0.16922(14) -0.01525(13) 0.60516(9) 0.0204(3) Uani 1 1 d . . . . .
H41 H 0.1629 0.0035 0.5503 0.025 Uiso 1 1 calc R U . . .
C42 C 0.22824(17) -0.13280(15) 0.60878(10) 0.0294(4) Uani 1 1 d . . . . .
H42A H 0.1653 -0.2105 0.5768 0.035 Uiso 1 1 calc R U . . .
H42B H 0.3109 -0.1155 0.5851 0.035 Uiso 1 1 calc R U . . .
C43 C 0.25893(19) -0.16387(15) 0.69108(11) 0.0336(4) Uani 1 1 d . . . . .
H43A H 0.3183 -0.2223 0.6895 0.040 Uiso 1 1 calc R U . . .
H43B H 0.1754 -0.2121 0.7071 0.040 Uiso 1 1 calc R U . . .
C44 C 0.32389(17) -0.04437(15) 0.75342(10) 0.0269(3) Uani 1 1 d . . . . .
H44A H 0.4199 -0.0183 0.7502 0.032 Uiso 1 1 calc R U . . .
H44B H 0.3137 -0.0709 0.8054 0.032 Uiso 1 1 calc R U . . .
C45 C 0.26977(14) 0.07632(14) 0.74829(9) 0.0197(3) Uani 1 1 d . . . . .
H45 H 0.3313 0.1516 0.7844 0.024 Uiso 1 1 calc R U . . .
C46 C 0.12973(16) 0.05992(16) 0.77051(10) 0.0271(3) Uani 1 1 d . . . . .
H46A H 0.1306 0.0395 0.8244 0.033 Uiso 1 1 calc R U . . .
H46B H 0.1065 0.1438 0.7701 0.033 Uiso 1 1 calc R U . . .
C47 C 0.02235(16) -0.04661(17) 0.71655(10) 0.0321(4) Uani 1 1 d . . . . .
H47A H -0.0655 -0.0383 0.7278 0.038 Uiso 1 1 calc R U . . .
H47B H 0.0303 -0.1327 0.7283 0.038 Uiso 1 1 calc R U . . .
C48 C 0.02915(15) -0.04198(15) 0.62946(10) 0.0267(3) Uani 1 1 d . . . . .
H48A H -0.0118 0.0265 0.6138 0.032 Uiso 1 1 calc R U . . .
H48B H -0.0251 -0.1263 0.5997 0.032 Uiso 1 1 calc R U . . .
C51 C 0.4675(2) 0.30809(17) 0.48826(10) 0.0379(4) Uani 1 1 d . . . . .
H51A H 0.5612 0.3505 0.4850 0.045 Uiso 1 1 calc R U . . .
H51B H 0.4379 0.3598 0.5302 0.045 Uiso 1 1 calc R U . . .
C52 C 0.3824(2) 0.29767(19) 0.41148(11) 0.0413(5) Uani 1 1 d . . . . .
H52A H 0.4219 0.3669 0.3816 0.050 Uiso 1 1 calc R U . A 1
H52B H 0.2921 0.3030 0.4192 0.050 Uiso 1 1 calc R U . A 1
C53 C 0.3803(2) 0.1641(2) 0.37069(12) 0.0376(6) Uani 0.918(6) 1 d . U P B 1
H53A H 0.3010 0.1282 0.3309 0.045 Uiso 0.918(6) 1 calc R U P B 1
H53B H 0.4607 0.1670 0.3456 0.045 Uiso 0.918(6) 1 calc R U P B 1
C54 C 0.316(3) 0.173(2) 0.3985(14) 0.038(5) Uani 0.082(6) 1 d . U P B 2
H54A H 0.3016 0.1434 0.3416 0.046 Uiso 0.082(6) 1 calc R U P B 2
H54B H 0.2279 0.1660 0.4151 0.046 Uiso 0.082(6) 1 calc R U P B 2
C55 C 0.37674(19) 0.08611(17) 0.43671(9) 0.0324(4) Uani 1 1 d . . . . .
H55A H 0.2845 0.0505 0.4459 0.039 Uiso 1 1 calc R U . B 1
H55B H 0.4167 0.0129 0.4252 0.039 Uiso 1 1 calc R U . B 1
O61 O 0.6747(13) 0.1767(13) 1.0441(6) 0.0614(19) Uani 0.561(8) 1 d . U P C 1
C62 C 0.7976(8) 0.2580(8) 1.0769(4) 0.0518(15) Uani 0.561(8) 1 d . U P C 1
H62A H 0.8029 0.2784 1.1341 0.062 Uiso 0.561(8) 1 calc R U P C 1
H62B H 0.8155 0.3404 1.0547 0.062 Uiso 0.561(8) 1 calc R U P C 1
C63 C 0.8943(4) 0.1806(4) 1.0559(3) 0.0460(11) Uani 0.561(8) 1 d . U P C 1
H63A H 0.9355 0.1540 1.1029 0.055 Uiso 0.561(8) 1 calc R U P C 1
H63B H 0.9648 0.2318 1.0303 0.055 Uiso 0.561(8) 1 calc R U P C 1
C64 C 0.8063(8) 0.0590(8) 0.9984(7) 0.0669(17) Uani 0.561(8) 1 d . U P C 1
H64A H 0.8083 0.0738 0.9436 0.080 Uiso 0.561(8) 1 calc R U P C 1
H64B H 0.8364 -0.0198 1.0056 0.080 Uiso 0.561(8) 1 calc R U P C 1
C65 C 0.6805(7) 0.0469(7) 1.0187(4) 0.0681(16) Uani 0.561(8) 1 d . U P C 1
H65A H 0.6665 -0.0067 1.0611 0.082 Uiso 0.561(8) 1 calc R U P C 1
H65B H 0.6120 0.0055 0.9732 0.082 Uiso 0.561(8) 1 calc R U P C 1
O71 O 0.6677(16) 0.1662(14) 1.0579(7) 0.0401(13) Uani 0.439(8) 1 d . U P C 2
C72 C 0.7953(12) 0.2635(10) 1.0495(5) 0.0538(18) Uani 0.439(8) 1 d . U P C 2
H72A H 0.7711 0.3259 1.0168 0.065 Uiso 0.439(8) 1 calc R U P C 2
H72B H 0.8327 0.3134 1.1020 0.065 Uiso 0.439(8) 1 calc R U P C 2
C73 C 0.8864(7) 0.2266(8) 1.0220(5) 0.0616(17) Uani 0.439(8) 1 d . U P C 2
H73A H 0.9664 0.2495 1.0616 0.074 Uiso 0.439(8) 1 calc R U P C 2
H73B H 0.9087 0.2696 0.9762 0.074 Uiso 0.439(8) 1 calc R U P C 2
C74 C 0.8411(10) 0.0860(11) 0.9991(9) 0.0646(19) Uani 0.439(8) 1 d . U P C 2
H74A H 0.8660 0.0379 1.0408 0.078 Uiso 0.439(8) 1 calc R U P C 2
H74B H 0.8717 0.0564 0.9502 0.078 Uiso 0.439(8) 1 calc R U P C 2
C75 C 0.6857(8) 0.0784(7) 0.9874(5) 0.0569(16) Uani 0.439(8) 1 d . U P C 2
H75A H 0.6600 0.1100 0.9385 0.068 Uiso 0.439(8) 1 calc R U P C 2
H75B H 0.6318 -0.0121 0.9857 0.068 Uiso 0.439(8) 1 calc R U P C 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
P1 O1 1.5491(13) . ?
P1 C11 1.7805(18) . ?
P1 C1 1.7913(18) . ?
P1 C21 1.8033(17) . ?
C1 C2 1.392(2) . ?
C1 C6 1.393(2) . ?
O1 B1 1.666(2) . ?
B1 C31 1.613(2) . ?
B1 C35 1.615(2) . ?
B1 C16 1.625(2) . ?
O2 B2 1.626(2) . ?
C2 C3 1.393(2) . ?
B2 C45 1.611(2) . ?
B2 C41 1.624(2) . ?
B2 C26 1.653(2) . ?
O3 C55 1.440(2) . ?
O3 C51 1.447(2) . ?
C3 C4 1.382(2) . ?
C5 C4 1.385(2) . ?
C5 C6 1.386(2) . ?
C12 C13 1.385(2) . ?
C12 C11 1.400(2) . ?
C11 C16 1.409(2) . ?
C13 C14 1.391(2) . ?
C14 C15 1.388(2) . ?
C16 C15 1.409(2) . ?
C21 C22 1.406(2) . ?
C21 C26 1.425(2) . ?
C22 C23 1.387(2) . ?
C23 C24 1.380(2) . ?
C24 C25 1.390(2) . ?
C25 C26 1.408(2) . ?
C31 C32 1.541(2) . ?
C31 C38 1.545(2) . ?
C32 C33 1.534(2) . ?
C33 C34 1.537(3) . ?
C34 C35 1.536(2) . ?
C35 C36 1.543(2) . ?
C36 C37 1.546(2) . ?
C37 C38 1.543(2) . ?
C41 C42 1.543(2) . ?
C41 C48 1.548(2) . ?
C42 C43 1.531(3) . ?
C43 C44 1.538(2) . ?
C44 C45 1.547(2) . ?
C45 C46 1.540(2) . ?
C46 C47 1.530(2) . ?
C47 C48 1.535(3) . ?
C51 C52 1.505(3) . ?
C52 C54 1.32(2) . ?
C52 C53 1.516(3) . ?
C53 C55 1.499(3) . ?
C54 C55 1.44(3) . ?
O61 C62 1.387(16) . ?
O61 C65 1.429(16) . ?
C62 C63 1.514(10) . ?
C63 C64 1.566(8) . ?
C64 C65 1.388(11) . ?
O71 C72 1.52(2) . ?
O71 C75 1.518(18) . ?
C72 C73 1.247(13) . ?
C73 C74 1.455(12) . ?
C74 C75 1.609(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 C11 100.82(8) . . ?
O1 P1 C1 112.19(6) . . ?
C11 P1 C1 105.48(7) . . ?
O1 P1 C21 111.50(7) . . ?
C11 P1 C21 113.52(7) . . ?
C1 P1 C21 112.65(8) . . ?
C2 C1 C6 119.98(14) . . ?
C2 C1 P1 120.62(11) . . ?
C6 C1 P1 119.02(12) . . ?
P1 O1 B1 114.19(10) . . ?
C31 B1 C35 106.79(12) . . ?
C31 B1 C16 116.47(12) . . ?
C35 B1 C16 116.74(12) . . ?
C31 B1 O1 109.13(11) . . ?
C35 B1 O1 106.63(12) . . ?
C16 B1 O1 100.32(11) . . ?
C1 C2 C3 119.55(14) . . ?
C45 B2 C41 105.69(12) . . ?
C45 B2 O2 105.29(11) . . ?
C41 B2 O2 106.88(12) . . ?
C45 B2 C26 119.52(12) . . ?
C41 B2 C26 115.10(13) . . ?
O2 B2 C26 103.28(10) . . ?
C55 O3 C51 109.50(13) . . ?
C4 C3 C2 120.11(15) . . ?
C4 C5 C6 119.81(14) . . ?
C3 C4 C5 120.46(15) . . ?
C5 C6 C1 120.08(14) . . ?
C13 C12 C11 118.66(14) . . ?
C12 C11 C16 124.10(13) . . ?
C12 C11 P1 126.97(12) . . ?
C16 C11 P1 108.56(10) . . ?
C12 C13 C14 119.17(14) . . ?
C15 C14 C13 121.41(14) . . ?
C11 C16 C15 114.86(13) . . ?
C11 C16 B1 116.06(12) . . ?
C15 C16 B1 129.04(13) . . ?
C14 C15 C16 121.75(15) . . ?
C22 C21 C26 121.52(13) . . ?
C22 C21 P1 114.22(10) . . ?
C26 C21 P1 124.05(10) . . ?
C23 C22 C21 121.25(13) . . ?
C24 C23 C22 118.65(13) . . ?
C23 C24 C25 120.14(14) . . ?
C24 C25 C26 124.07(13) . . ?
C25 C26 C21 114.36(12) . . ?
C25 C26 B2 118.38(12) . . ?
C21 C26 B2 126.76(13) . . ?
C32 C31 C38 112.42(13) . . ?
C32 C31 B1 111.46(12) . . ?
C38 C31 B1 107.58(12) . . ?
C33 C32 C31 115.48(13) . . ?
C32 C33 C34 114.19(13) . . ?
C35 C34 C33 114.58(13) . . ?
C34 C35 C36 113.23(13) . . ?
C34 C35 B1 110.07(12) . . ?
C36 C35 B1 108.00(13) . . ?
C35 C36 C37 115.87(13) . . ?
C38 C37 C36 115.50(13) . . ?
C37 C38 C31 114.56(13) . . ?
C42 C41 C48 112.25(13) . . ?
C42 C41 B2 109.72(13) . . ?
C48 C41 B2 109.64(12) . . ?
C43 C42 C41 114.57(14) . . ?
C42 C43 C44 114.89(14) . . ?
C43 C44 C45 116.27(14) . . ?
C46 C45 C44 114.31(13) . . ?
C46 C45 B2 107.87(12) . . ?
C44 C45 B2 110.10(12) . . ?
C47 C46 C45 114.20(14) . . ?
C46 C47 C48 113.82(13) . . ?
C47 C48 C41 115.99(13) . . ?
O3 C51 C52 105.92(14) . . ?
C54 C52 C51 102.3(10) . . ?
C51 C52 C53 102.73(15) . . ?
C55 C53 C52 102.32(17) . . ?
C52 C54 C55 116.3(17) . . ?
O3 C55 C54 99.3(9) . . ?
O3 C55 C53 105.45(16) . . ?
C62 O61 C65 112.4(11) . . ?
O61 C62 C63 104.2(8) . . ?
C62 C63 C64 103.7(5) . . ?
C65 C64 C63 103.7(6) . . ?
C64 C65 O61 105.5(8) . . ?
C72 O71 C75 89.1(9) . . ?
C73 C72 O71 120.8(11) . . ?
C72 C73 C74 107.9(8) . . ?
C73 C74 C75 95.8(8) . . ?
O71 C75 C74 104.6(10) . . ?

_refine_diff_density_max         0.372
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.046




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

data_2
_database_code_depnum_ccdc_archive 'CCDC 2096464'
loop_
_audit_author_name
_audit_author_address
'Rong Shang '
;Graduate School of Advanced Engineering and Science, Hiroshima University
Japan
;
_audit_update_record             
;
2021-07-14 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
#data_exp494oishiBPB9bbnBuNc_0m_a

_audit_creation_method           SHELXL-2014/5
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H59 B2 N2 P'
_chemical_formula_weight         668.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   15.557(18)
_cell_length_b                   14.394(16)
_cell_length_c                   17.425(19)
_cell_angle_alpha                90
_cell_angle_beta                 97.347(8)
_cell_angle_gamma                90
_cell_volume                     3870(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6259
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      24.56

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.057
_exptl_absorpt_coefficient_mu    0.104
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36660
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.841
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             6880
_reflns_number_gt                5380
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0337P)²+1.9111P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6880
_refine_ls_number_parameters     448
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1018
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.65391(3) 0.52942(3) 0.34225(3) 0.01907(11) Uani 1 1 d . . . . .
B1 B 0.75108(13) 0.70759(13) 0.44110(11) 0.0211(4) Uani 1 1 d . . . . .
B2 B 0.77964(13) 0.39828(14) 0.24115(12) 0.0246(4) Uani 1 1 d . . . . .
N1 N 0.77276(9) 0.55827(10) 0.54049(8) 0.0251(3) Uani 1 1 d . . . . .
N2 N 0.71859(10) 0.26264(11) 0.33092(9) 0.0301(4) Uani 1 1 d . . . . .
C1 C 0.56066(11) 0.45055(11) 0.34560(10) 0.0207(4) Uani 1 1 d . . . . .
C2 C 0.53316(12) 0.43546(12) 0.41780(10) 0.0249(4) Uani 1 1 d . . . . .
H2 H 0.5638 0.4640 0.4623 0.030 Uiso 1 1 calc R U . . .
C3 C 0.46232(12) 0.37993(12) 0.42583(11) 0.0300(4) Uani 1 1 d . . . . .
H3 H 0.4448 0.3706 0.4755 0.036 Uiso 1 1 calc R U . . .
C4 C 0.41693(13) 0.33787(13) 0.36162(12) 0.0340(5) Uani 1 1 d . . . . .
H4 H 0.3676 0.3006 0.3668 0.041 Uiso 1 1 calc R U . . .
C5 C 0.44396(12) 0.35064(13) 0.28995(12) 0.0331(5) Uani 1 1 d . . . . .
H5 H 0.4136 0.3212 0.2458 0.040 Uiso 1 1 calc R U . . .
C6 C 0.51516(12) 0.40616(12) 0.28173(10) 0.0266(4) Uani 1 1 d . . . . .
H6 H 0.5331 0.4140 0.2320 0.032 Uiso 1 1 calc R U . . .
C21 C 0.60031(10) 0.63990(11) 0.36616(9) 0.0184(4) Uani 1 1 d . . . . .
C22 C 0.64751(11) 0.71054(11) 0.40975(9) 0.0184(4) Uani 1 1 d . . . . .
C23 C 0.59857(11) 0.78659(12) 0.42995(10) 0.0235(4) Uani 1 1 d . . . . .
H23 H 0.6278 0.8345 0.4605 0.028 Uiso 1 1 calc R U . . .
C24 C 0.51046(12) 0.79594(12) 0.40812(10) 0.0261(4) Uani 1 1 d . . . . .
H24 H 0.4808 0.8496 0.4226 0.031 Uiso 1 1 calc R U . . .
C25 C 0.46593(11) 0.72679(12) 0.36520(10) 0.0260(4) Uani 1 1 d . . . . .
H25 H 0.4055 0.7324 0.3492 0.031 Uiso 1 1 calc R U . . .
C26 C 0.51071(11) 0.64901(12) 0.34578(10) 0.0219(4) Uani 1 1 d . . . . .
H26 H 0.4797 0.6003 0.3178 0.026 Uiso 1 1 calc R U . . .
C31 C 0.65512(11) 0.53327(11) 0.23593(10) 0.0204(4) Uani 1 1 d . . . . .
C32 C 0.70192(10) 0.46510(11) 0.19919(10) 0.0201(4) Uani 1 1 d . . . . .
C33 C 0.68069(11) 0.45873(12) 0.11867(10) 0.0245(4) Uani 1 1 d . . . . .
H33 H 0.7068 0.4106 0.0924 0.029 Uiso 1 1 calc R U . . .
C34 C 0.62412(12) 0.51808(13) 0.07529(10) 0.0271(4) Uani 1 1 d . . . . .
H34 H 0.6116 0.5099 0.0209 0.033 Uiso 1 1 calc R U . . .
C35 C 0.58605(12) 0.58925(13) 0.11155(10) 0.0293(4) Uani 1 1 d . . . . .
H35 H 0.5502 0.6333 0.0822 0.035 Uiso 1 1 calc R U . . .
C36 C 0.60085(11) 0.59562(12) 0.19135(10) 0.0256(4) Uani 1 1 d . . . . .
H36 H 0.5734 0.6437 0.2166 0.031 Uiso 1 1 calc R U . . .
C41 C 0.81714(11) 0.69631(12) 0.37613(10) 0.0245(4) Uani 1 1 d . . . . .
H41 H 0.7972 0.6424 0.3423 0.029 Uiso 1 1 calc R U . . .
C42 C 0.81037(13) 0.78454(14) 0.32583(11) 0.0354(5) Uani 1 1 d . . . . .
H42A H 0.8492 0.7777 0.2854 0.043 Uiso 1 1 calc R U . . .
H42B H 0.7503 0.7898 0.2994 0.043 Uiso 1 1 calc R U . . .
C43 C 0.83357(15) 0.87445(14) 0.37038(13) 0.0442(6) Uani 1 1 d . . . . .
H43A H 0.8151 0.9277 0.3363 0.053 Uiso 1 1 calc R U . . .
H43B H 0.8974 0.8778 0.3830 0.053 Uiso 1 1 calc R U . . .
C44 C 0.79267(13) 0.88425(13) 0.44529(12) 0.0343(5) Uani 1 1 d . . . . .
H44A H 0.7325 0.9066 0.4318 0.041 Uiso 1 1 calc R U . . .
H44B H 0.8248 0.9328 0.4774 0.041 Uiso 1 1 calc R U . . .
C45 C 0.79038(12) 0.79587(12) 0.49490(11) 0.0263(4) Uani 1 1 d . . . . .
H45 H 0.7516 0.8075 0.5354 0.032 Uiso 1 1 calc R U . . .
C46 C 0.88150(12) 0.77124(14) 0.53553(12) 0.0355(5) Uani 1 1 d . . . . .
H46A H 0.9053 0.8259 0.5655 0.043 Uiso 1 1 calc R U . . .
H46B H 0.8760 0.7202 0.5727 0.043 Uiso 1 1 calc R U . . .
C47 C 0.94597(12) 0.74162(15) 0.48091(13) 0.0392(5) Uani 1 1 d . . . . .
H47A H 0.9956 0.7106 0.5118 0.047 Uiso 1 1 calc R U . . .
H47B H 0.9684 0.7982 0.4579 0.047 Uiso 1 1 calc R U . . .
C48 C 0.90985(12) 0.67593(14) 0.41473(12) 0.0328(5) Uani 1 1 d . . . . .
H48A H 0.9492 0.6781 0.3744 0.039 Uiso 1 1 calc R U . . .
H48B H 0.9113 0.6117 0.4353 0.039 Uiso 1 1 calc R U . . .
C51 C 0.85715(11) 0.45151(12) 0.29770(10) 0.0267(4) Uani 1 1 d . . . . .
H51 H 0.8295 0.4889 0.3362 0.032 Uiso 1 1 calc R U . . .
C52 C 0.90264(12) 0.51932(14) 0.24781(12) 0.0356(5) Uani 1 1 d . . . . .
H52A H 0.8598 0.5658 0.2252 0.043 Uiso 1 1 calc R U . . .
H52B H 0.9482 0.5530 0.2818 0.043 Uiso 1 1 calc R U . . .
C53 C 0.94415(13) 0.47382(16) 0.18207(12) 0.0428(5) Uani 1 1 d . . . . .
H53A H 0.9977 0.4413 0.2042 0.051 Uiso 1 1 calc R U . . .
H53B H 0.9608 0.5229 0.1470 0.051 Uiso 1 1 calc R U . . .
C54 C 0.88418(13) 0.40437(15) 0.13495(12) 0.0395(5) Uani 1 1 d . . . . .
H54A H 0.9196 0.3665 0.1034 0.047 Uiso 1 1 calc R U . . .
H54B H 0.8421 0.4398 0.0988 0.047 Uiso 1 1 calc R U . . .
C55 C 0.83309(12) 0.33785(14) 0.18194(11) 0.0309(4) Uani 1 1 d . . . . .
H55 H 0.7899 0.3037 0.1449 0.037 Uiso 1 1 calc R U . . .
C56 C 0.89278(13) 0.26572(15) 0.22725(12) 0.0395(5) Uani 1 1 d . . . . .
H56A H 0.8561 0.2184 0.2485 0.047 Uiso 1 1 calc R U . . .
H56B H 0.9266 0.2338 0.1906 0.047 Uiso 1 1 calc R U . . .
C57 C 0.95629(13) 0.30526(15) 0.29404(12) 0.0409(5) Uani 1 1 d . . . . .
H57A H 1.0068 0.3316 0.2723 0.049 Uiso 1 1 calc R U . . .
H57B H 0.9777 0.2535 0.3288 0.049 Uiso 1 1 calc R U . . .
C58 C 0.91849(12) 0.38069(14) 0.34257(11) 0.0332(5) Uani 1 1 d . . . . .
H58A H 0.9673 0.4152 0.3716 0.040 Uiso 1 1 calc R U . . .
H58B H 0.8867 0.3496 0.3810 0.040 Uiso 1 1 calc R U . . .
C61 C 0.76231(11) 0.61851(12) 0.49710(10) 0.0220(4) Uani 1 1 d . . . . .
C62 C 0.79463(12) 0.47838(12) 0.59131(10) 0.0275(4) Uani 1 1 d . . . . .
C63 C 0.85676(18) 0.41930(17) 0.55208(15) 0.0657(8) Uani 1 1 d . . . . .
H63A H 0.8286 0.3997 0.5011 0.099 Uiso 1 1 calc R U . . .
H63B H 0.8732 0.3644 0.5838 0.099 Uiso 1 1 calc R U . . .
H63C H 0.9087 0.4556 0.5459 0.099 Uiso 1 1 calc R U . . .
C64 C 0.71163(14) 0.42726(16) 0.60048(15) 0.0516(6) Uani 1 1 d . . . . .
H64A H 0.6841 0.4065 0.5496 0.077 Uiso 1 1 calc R U . . .
H64B H 0.6722 0.4689 0.6235 0.077 Uiso 1 1 calc R U . . .
H64C H 0.7248 0.3733 0.6342 0.077 Uiso 1 1 calc R U . . .
C65 C 0.83666(17) 0.51593(17) 0.66784(13) 0.0554(7) Uani 1 1 d . . . . .
H65A H 0.8872 0.5534 0.6596 0.083 Uiso 1 1 calc R U . . .
H65B H 0.8551 0.4641 0.7026 0.083 Uiso 1 1 calc R U . . .
H65C H 0.7950 0.5546 0.6910 0.083 Uiso 1 1 calc R U . . .
C66 C 0.73928(11) 0.32247(13) 0.29347(11) 0.0264(4) Uani 1 1 d . . . . .
C67 C 0.70286(13) 0.18333(13) 0.38017(11) 0.0312(4) Uani 1 1 d . . . . .
C68 C 0.79002(15) 0.15441(17) 0.42261(15) 0.0592(7) Uani 1 1 d . . . . .
H68A H 0.8295 0.1389 0.3849 0.089 Uiso 1 1 calc R U . . .
H68B H 0.7824 0.1000 0.4549 0.089 Uiso 1 1 calc R U . . .
H68C H 0.8144 0.2057 0.4554 0.089 Uiso 1 1 calc R U . . .
C69 C 0.66335(19) 0.10688(16) 0.32767(14) 0.0611(7) Uani 1 1 d . . . . .
H69A H 0.6091 0.1290 0.2986 0.092 Uiso 1 1 calc R U . . .
H69B H 0.6514 0.0529 0.3589 0.092 Uiso 1 1 calc R U . . .
H69C H 0.7039 0.0892 0.2915 0.092 Uiso 1 1 calc R U . . .
C70 C 0.64145(18) 0.21472(17) 0.43537(15) 0.0601(7) Uani 1 1 d . . . . .
H70A H 0.5884 0.2391 0.4059 0.090 Uiso 1 1 calc R U . . .
H70B H 0.6691 0.2635 0.4692 0.090 Uiso 1 1 calc R U . . .
H70C H 0.6270 0.1619 0.4669 0.090 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 C1 1.849(2) . ?
P1 C31 1.856(3) . ?
P1 C21 1.867(2) . ?
B1 C61 1.607(3) . ?
B1 C41 1.631(3) . ?
B1 C22 1.634(3) . ?
B1 C45 1.649(3) . ?
B2 C66 1.601(3) . ?
B2 C32 1.642(3) . ?
B2 C51 1.646(3) . ?
B2 C55 1.653(3) . ?
N1 C61 1.148(2) . ?
N1 C62 1.465(2) . ?
N2 C66 1.151(2) . ?
N2 C67 1.467(3) . ?
C1 C6 1.395(3) . ?
C1 C2 1.397(3) . ?
C2 C3 1.383(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C21 C26 1.400(3) . ?
C21 C22 1.417(2) . ?
C22 C23 1.404(3) . ?
C23 C24 1.381(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.383(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.398(3) . ?
C31 C32 1.422(2) . ?
C32 C33 1.403(3) . ?
C33 C34 1.380(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.539(3) . ?
C41 C48 1.540(3) . ?
C41 H41 1.0000 . ?
C42 C43 1.528(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.530(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.541(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.543(3) . ?
C45 H45 1.0000 . ?
C46 C47 1.529(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.541(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C51 C52 1.538(3) . ?
C51 C58 1.540(3) . ?
C51 H51 1.0000 . ?
C52 C53 1.532(3) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.532(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.545(3) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.541(3) . ?
C55 H55 1.0000 . ?
C56 C57 1.536(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.539(3) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C62 C65 1.508(3) . ?
C62 C64 1.512(3) . ?
C62 C63 1.515(3) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C67 C70 1.509(3) . ?
C67 C69 1.511(3) . ?
C67 C68 1.517(3) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 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
C1 P1 C31 99.09(7) . . ?
C1 P1 C21 98.12(11) . . ?
C31 P1 C21 105.02(8) . . ?
C61 B1 C41 108.22(15) . . ?
C61 B1 C22 104.46(14) . . ?
C41 B1 C22 116.89(16) . . ?
C61 B1 C45 105.43(16) . . ?
C41 B1 C45 104.50(15) . . ?
C22 B1 C45 116.61(15) . . ?
C66 B2 C32 109.44(16) . . ?
C66 B2 C51 106.69(16) . . ?
C32 B2 C51 115.81(16) . . ?
C66 B2 C55 105.19(17) . . ?
C32 B2 C55 115.53(16) . . ?
C51 B2 C55 103.31(16) . . ?
C61 N1 C62 173.40(17) . . ?
C66 N2 C67 173.35(18) . . ?
C6 C1 C2 117.70(17) . . ?
C6 C1 P1 125.18(14) . . ?
C2 C1 P1 117.12(13) . . ?
C3 C2 C1 121.39(17) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 120.13(18) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.36(19) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.64(18) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 120.77(18) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C26 C21 C22 119.99(15) . . ?
C26 C21 P1 118.80(13) . . ?
C22 C21 P1 121.01(14) . . ?
C23 C22 C21 115.69(17) . . ?
C23 C22 B1 118.66(15) . . ?
C21 C22 B1 125.57(15) . . ?
C24 C23 C22 123.91(17) . . ?
C24 C23 H23 118.0 . . ?
C22 C23 H23 118.0 . . ?
C25 C24 C23 119.44(17) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 118.93(18) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C25 C26 C21 122.00(17) . . ?
C25 C26 H26 119.0 . . ?
C21 C26 H26 119.0 . . ?
C36 C31 C32 120.03(17) . . ?
C36 C31 P1 119.43(13) . . ?
C32 C31 P1 119.99(13) . . ?
C33 C32 C31 115.26(16) . . ?
C33 C32 B2 118.23(15) . . ?
C31 C32 B2 126.45(16) . . ?
C34 C33 C32 124.01(17) . . ?
C34 C33 H33 118.0 . . ?
C32 C33 H33 118.0 . . ?
C35 C34 C33 119.39(18) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 118.99(17) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C35 C36 C31 121.82(17) . . ?
C35 C36 H36 119.1 . . ?
C31 C36 H36 119.1 . . ?
C42 C41 C48 113.46(15) . . ?
C42 C41 B1 108.04(15) . . ?
C48 C41 B1 110.73(17) . . ?
C42 C41 H41 108.2 . . ?
C48 C41 H41 108.2 . . ?
B1 C41 H41 108.2 . . ?
C43 C42 C41 114.52(18) . . ?
C43 C42 H42A 108.6 . . ?
C41 C42 H42A 108.6 . . ?
C43 C42 H42B 108.6 . . ?
C41 C42 H42B 108.6 . . ?
H42A C42 H42B 107.6 . . ?
C42 C43 C44 114.48(17) . . ?
C42 C43 H43A 108.6 . . ?
C44 C43 H43A 108.6 . . ?
C42 C43 H43B 108.6 . . ?
C44 C43 H43B 108.6 . . ?
H43A C43 H43B 107.6 . . ?
C43 C44 C45 116.38(17) . . ?
C43 C44 H44A 108.2 . . ?
C45 C44 H44A 108.2 . . ?
C43 C44 H44B 108.2 . . ?
C45 C44 H44B 108.2 . . ?
H44A C44 H44B 107.3 . . ?
C44 C45 C46 111.19(16) . . ?
C44 C45 B1 110.53(17) . . ?
C46 C45 B1 109.62(15) . . ?
C44 C45 H45 108.5 . . ?
C46 C45 H45 108.5 . . ?
B1 C45 H45 108.5 . . ?
C47 C46 C45 114.57(18) . . ?
C47 C46 H46A 108.6 . . ?
C45 C46 H46A 108.6 . . ?
C47 C46 H46B 108.6 . . ?
C45 C46 H46B 108.6 . . ?
H46A C46 H46B 107.6 . . ?
C46 C47 C48 115.57(17) . . ?
C46 C47 H47A 108.4 . . ?
C48 C47 H47A 108.4 . . ?
C46 C47 H47B 108.4 . . ?
C48 C47 H47B 108.4 . . ?
H47A C47 H47B 107.4 . . ?
C41 C48 C47 116.20(16) . . ?
C41 C48 H48A 108.2 . . ?
C47 C48 H48A 108.2 . . ?
C41 C48 H48B 108.2 . . ?
C47 C48 H48B 108.2 . . ?
H48A C48 H48B 107.4 . . ?
C52 C51 C58 114.03(17) . . ?
C52 C51 B2 108.17(17) . . ?
C58 C51 B2 110.79(16) . . ?
C52 C51 H51 107.9 . . ?
C58 C51 H51 107.9 . . ?
B2 C51 H51 107.9 . . ?
C53 C52 C51 114.80(18) . . ?
C53 C52 H52A 108.6 . . ?
C51 C52 H52A 108.6 . . ?
C53 C52 H52B 108.6 . . ?
C51 C52 H52B 108.6 . . ?
H52A C52 H52B 107.5 . . ?
C52 C53 C54 113.17(17) . . ?
C52 C53 H53A 108.9 . . ?
C54 C53 H53A 108.9 . . ?
C52 C53 H53B 108.9 . . ?
C54 C53 H53B 108.9 . . ?
H53A C53 H53B 107.8 . . ?
C53 C54 C55 116.09(18) . . ?
C53 C54 H54A 108.3 . . ?
C55 C54 H54A 108.3 . . ?
C53 C54 H54B 108.3 . . ?
C55 C54 H54B 108.3 . . ?
H54A C54 H54B 107.4 . . ?
C56 C55 C54 111.83(18) . . ?
C56 C55 B2 110.67(17) . . ?
C54 C55 B2 109.80(17) . . ?
C56 C55 H55 108.1 . . ?
C54 C55 H55 108.1 . . ?
B2 C55 H55 108.1 . . ?
C57 C56 C55 115.18(18) . . ?
C57 C56 H56A 108.5 . . ?
C55 C56 H56A 108.5 . . ?
C57 C56 H56B 108.5 . . ?
C55 C56 H56B 108.5 . . ?
H56A C56 H56B 107.5 . . ?
C56 C57 C58 115.07(17) . . ?
C56 C57 H57A 108.5 . . ?
C58 C57 H57A 108.5 . . ?
C56 C57 H57B 108.5 . . ?
C58 C57 H57B 108.5 . . ?
H57A C57 H57B 107.5 . . ?
C57 C58 C51 116.34(17) . . ?
C57 C58 H58A 108.2 . . ?
C51 C58 H58A 108.2 . . ?
C57 C58 H58B 108.2 . . ?
C51 C58 H58B 108.2 . . ?
H58A C58 H58B 107.4 . . ?
N1 C61 B1 175.91(18) . . ?
N1 C62 C65 107.10(17) . . ?
N1 C62 C64 108.09(16) . . ?
C65 C62 C64 111.13(19) . . ?
N1 C62 C63 106.27(17) . . ?
C65 C62 C63 111.8(2) . . ?
C64 C62 C63 112.2(2) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C62 C65 H65A 109.5 . . ?
C62 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C62 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N2 C66 B2 172.48(18) . . ?
N2 C67 C70 107.83(17) . . ?
N2 C67 C69 107.34(18) . . ?
C70 C67 C69 111.2(2) . . ?
N2 C67 C68 107.04(17) . . ?
C70 C67 C68 111.8(2) . . ?
C69 C67 C68 111.4(2) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C67 C70 H70A 109.5 . . ?
C67 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C67 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?

_refine_diff_density_max         0.260
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.040

_shelxl_version_number           2014/5


####################################################################### 
# 
# 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_1Int
_database_code_depnum_ccdc_archive 'CCDC 2096463'
loop_
_audit_author_name
_audit_author_address
'Rong Shang '
;Graduate School of Advanced Engineering and Science, Hiroshima University
Japan
;
_audit_update_record             
;
2021-07-14 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT413_1Int                
;
PROBLEM: Short Inter XH3 .. XHn     H42A     ..H42B     .       1.77 Ang.
RESPONSE: The short interactions belong to atoms of different parts of a disorder treatment. 
;
_vrf_PLAT220_1Int                
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        7.5 Ratio
RESPONSE: Due to the highly reactive nature of this compound, the crystal quality was not ideal. However, no discussions on bonding parameters were made in the publication. 
;
_vrf_PLAT230_1Int                
;
PROBLEM: Hirshfeld Test Diff for    C41      --C42      .        8.5 s.u.
RESPONSE: These belong to coordinated ether molecules which showed large ellipsoids due to thermal vibration. 
;
_vrf_PLAT934_1Int                
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          3 Check
RESPONSE: Due to the highly reactive nature of this compound, the crystal quality was not ideal. However, no discussions on bonding parameters were made in the publication. 
;
# Added during the CSD deposition process: Wednesday 14 July 2021 11:30 AM
# end Validation Reply Form

#data_20181119_exp250_oishi_0ma_a

_audit_creation_method           SHELXL-2014/5
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H29 B2 Cl0.25 Li2.25 O P'
_chemical_formula_weight         386.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   28.597(6)
_cell_length_b                   14.635(3)
_cell_length_c                   23.112(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.257(4)
_cell_angle_gamma                90
_cell_volume                     9286(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9974
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      26.19

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_F_000             3280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.204
_exptl_absorpt_coefficient_mu    0.155
_shelx_estimated_absorpt_T_min   0.949
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54701
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.717
_diffrn_reflns_theta_max         28.010
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11216
_reflns_number_gt                8071
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1527P)²+13.8358P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11216
_refine_ls_number_parameters     575
_refine_ls_number_restraints     193
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0761
_refine_ls_wR_factor_ref         0.2533
_refine_ls_wR_factor_gt          0.2264
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.5000 0.47595(7) 0.2500 0.0414(2) Uani 1 2 d S T P . .
P1 P 0.59560(2) 0.20030(5) 0.12430(3) 0.02909(18) Uani 1 1 d . . . . .
P2 P 0.63343(3) 0.39586(5) 0.36152(3) 0.0358(2) Uani 1 1 d . . . . .
B11 B 0.51338(11) 0.3439(2) 0.11878(13) 0.0308(6) Uani 1 1 d . . . . .
B12 B 0.52857(12) 0.0514(2) 0.16751(14) 0.0331(6) Uani 1 1 d . . . . .
H65 H 0.5215(12) 0.018(2) 0.2040(16) 0.050(10) Uiso 1 1 d . . . . .
H66 H 0.5003(12) 0.031(2) 0.1283(15) 0.043(9) Uiso 1 1 d . . . . .
H67 H 0.5928(12) 0.420(2) 0.2391(15) 0.043(9) Uiso 1 1 d . . . . .
H68 H 0.6446(14) 0.385(3) 0.2129(18) 0.063(11) Uiso 1 1 d . . . . .
H69 H 0.6160(12) 0.494(2) 0.1856(16) 0.048(9) Uiso 1 1 d . . . . .
H70 H 0.5643(12) 0.141(2) 0.3086(15) 0.044(9) Uiso 1 1 d . . . . .
H71 H 0.5706(12) 0.239(2) 0.3618(15) 0.044(9) Uiso 1 1 d . . . . .
H72 H 0.5491(12) 0.256(2) 0.2758(15) 0.043(9) Uiso 1 1 d . . . . .
B21 B 0.62856(16) 0.4524(3) 0.22723(17) 0.0540(10) Uani 1 1 d . . . . .
B22 B 0.57783(11) 0.2115(2) 0.31385(13) 0.0310(6) Uani 1 1 d . . . . .
Li1 Li 0.5946(2) 0.3000(4) 0.2127(2) 0.0500(13) Uani 1 1 d . . . . .
Li2 Li 0.54275(17) 0.3679(3) 0.3212(2) 0.0376(10) Uani 1 1 d . . . . .
Li3 Li 0.5454(2) 0.4926(4) 0.1724(3) 0.0585(15) Uani 1 1 d . . . . .
Li4 Li 0.5466(3) 0.1257(5) 0.3919(3) 0.0638(17) Uani 1 1 d . . . . .
Li5 Li 0.5000 0.1134(5) 0.2500 0.0378(14) Uani 1 2 d S T P . .
C1 C 0.53733(10) 0.19780(17) 0.06538(11) 0.0297(5) Uani 1 1 d . . . . .
C2 C 0.50226(9) 0.26436(17) 0.06795(11) 0.0286(5) Uani 1 1 d . . . . .
C3 C 0.45676(10) 0.2577(2) 0.02505(12) 0.0366(6) Uani 1 1 d . . . . .
H3 H 0.4322 0.3010 0.0257 0.044 Uiso 1 1 calc R U . . .
C4 C 0.44664(12) 0.1891(2) -0.01863(13) 0.0447(7) Uani 1 1 d . . . . .
H4 H 0.4154 0.1862 -0.0470 0.054 Uiso 1 1 calc R U . . .
C5 C 0.48175(13) 0.1253(2) -0.02088(13) 0.0453(7) Uani 1 1 d . . . . .
H5 H 0.4750 0.0792 -0.0510 0.054 Uiso 1 1 calc R U . . .
C6 C 0.52690(11) 0.12947(19) 0.02140(12) 0.0379(6) Uani 1 1 d . . . . .
H6 H 0.5511 0.0854 0.0205 0.045 Uiso 1 1 calc R U . . .
C7 C 0.61207(10) 0.07997(19) 0.13848(12) 0.0339(6) Uani 1 1 d . . . . .
C8 C 0.58136(10) 0.02328(18) 0.16143(11) 0.0324(5) Uani 1 1 d . . . . .
C9 C 0.59872(12) -0.0644(2) 0.17936(15) 0.0460(7) Uani 1 1 d . . . . .
H9 H 0.5789 -0.1046 0.1946 0.055 Uiso 1 1 calc R U . . .
C10 C 0.64369(15) -0.0952(3) 0.1759(2) 0.0680(11) Uani 1 1 d . . . . .
H10 H 0.6541 -0.1555 0.1884 0.082 Uiso 1 1 calc R U . . .
C11 C 0.67290(14) -0.0384(3) 0.1543(2) 0.0747(13) Uani 1 1 d . . . . .
H11 H 0.7041 -0.0588 0.1527 0.090 Uiso 1 1 calc R U . . .
C12 C 0.65709(12) 0.0489(2) 0.13476(17) 0.0516(8) Uani 1 1 d . . . . .
H12 H 0.6771 0.0876 0.1188 0.062 Uiso 1 1 calc R U . . .
C13 C 0.63889(10) 0.2465(2) 0.08618(13) 0.0376(6) Uani 1 1 d . . . . .
C14 C 0.63254(15) 0.2430(3) 0.02437(16) 0.0620(10) Uani 1 1 d . . . . .
H14 H 0.6044 0.2143 -0.0010 0.074 Uiso 1 1 calc R U . . .
C15 C 0.66730(17) 0.2815(3) -0.00086(19) 0.0732(12) Uani 1 1 d . . . . .
H15 H 0.6628 0.2774 -0.0431 0.088 Uiso 1 1 calc R U . . .
C16 C 0.70684(14) 0.3240(3) 0.03406(19) 0.0608(10) Uani 1 1 d . . . . .
H16 H 0.7303 0.3493 0.0166 0.073 Uiso 1 1 calc R U . . .
C17 C 0.71325(13) 0.3309(3) 0.0947(2) 0.0590(9) Uani 1 1 d . . . . .
H17 H 0.7409 0.3619 0.1192 0.071 Uiso 1 1 calc R U . . .
C18 C 0.67945(12) 0.2928(2) 0.12085(16) 0.0473(7) Uani 1 1 d . . . . .
H18 H 0.6842 0.2985 0.1631 0.057 Uiso 1 1 calc R U . . .
C21 C 0.66728(11) 0.4935(2) 0.34334(13) 0.0418(7) Uani 1 1 d . . . . .
C22 C 0.66110(12) 0.5131(3) 0.28217(14) 0.0497(8) Uani 1 1 d . . . . .
C23 C 0.68586(15) 0.5900(3) 0.27006(16) 0.0628(11) Uani 1 1 d . . . . .
H23 H 0.6827 0.6052 0.2292 0.075 Uiso 1 1 calc R U . . .
C24 C 0.71460(14) 0.6447(3) 0.31441(17) 0.0616(10) Uani 1 1 d . . . . .
H24 H 0.7304 0.6968 0.3040 0.074 Uiso 1 1 calc R U . . .
C25 C 0.72022(13) 0.6234(3) 0.37407(16) 0.0545(9) Uani 1 1 d . . . . .
H25 H 0.7400 0.6605 0.4052 0.065 Uiso 1 1 calc R U . . .
C26 C 0.69690(11) 0.5477(2) 0.38818(14) 0.0439(7) Uani 1 1 d . . . . .
H26 H 0.7012 0.5323 0.4293 0.053 Uiso 1 1 calc R U . . .
C27 C 0.66235(10) 0.2980(2) 0.33609(12) 0.0357(6) Uani 1 1 d . . . . .
C28 C 0.63379(9) 0.22053(19) 0.31340(11) 0.0308(5) Uani 1 1 d . . . . .
C29 C 0.65661(11) 0.1509(2) 0.28988(12) 0.0375(6) Uani 1 1 d . . . . .
H29 H 0.6386 0.0974 0.2745 0.045 Uiso 1 1 calc R U . . .
C30 C 0.70469(12) 0.1573(2) 0.28824(14) 0.0467(7) Uani 1 1 d . . . . .
H30 H 0.7187 0.1091 0.2712 0.056 Uiso 1 1 calc R U . . .
C31 C 0.73169(12) 0.2323(3) 0.31093(16) 0.0524(8) Uani 1 1 d . . . . .
H31 H 0.7647 0.2361 0.3104 0.063 Uiso 1 1 calc R U . . .
C32 C 0.71094(11) 0.3025(3) 0.33459(15) 0.0495(8) Uani 1 1 d . . . . .
H32 H 0.7298 0.3550 0.3502 0.059 Uiso 1 1 calc R U . . .
C33 C 0.65331(11) 0.3903(2) 0.44380(13) 0.0416(7) Uani 1 1 d . . . . .
C34 C 0.68417(17) 0.3255(4) 0.47603(17) 0.0774(13) Uani 1 1 d . . . . .
H34 H 0.6977 0.2806 0.4557 0.093 Uiso 1 1 calc R U . . .
C35 C 0.6958(2) 0.3252(5) 0.5385(2) 0.120(3) Uani 1 1 d . . . . .
H35 H 0.7179 0.2808 0.5606 0.144 Uiso 1 1 calc R U . . .
C36 C 0.6760(2) 0.3875(4) 0.56843(19) 0.0901(16) Uani 1 1 d . . . . .
H36 H 0.6842 0.3859 0.6112 0.108 Uiso 1 1 calc R U . . .
C37 C 0.64462(15) 0.4522(3) 0.53753(16) 0.0599(10) Uani 1 1 d . . . . .
H37 H 0.6307 0.4958 0.5583 0.072 Uiso 1 1 calc R U . . .
C38 C 0.63334(13) 0.4530(2) 0.47537(15) 0.0488(8) Uani 1 1 d . . . . .
H38 H 0.6113 0.4976 0.4535 0.059 Uiso 1 1 calc R U . . .
O2 O 0.60493(12) 0.0446(3) 0.42296(16) 0.0843(9) Uani 1 1 d D U . . .
C51 C 0.6132(8) -0.0463(8) 0.4051(11) 0.1116(15) Uani 0.357(9) 1 d D U P A 1
H51A H 0.6210 -0.0857 0.4414 0.134 Uiso 0.357(9) 1 calc R U P A 1
H51B H 0.5824 -0.0693 0.3775 0.134 Uiso 0.357(9) 1 calc R U P A 1
C52 C 0.6465(6) -0.0553(14) 0.3795(9) 0.1116(15) Uani 0.357(9) 1 d D U P A 1
H52A H 0.6348 -0.0335 0.3378 0.167 Uiso 0.357(9) 1 calc R U P A 1
H52B H 0.6555 -0.1199 0.3796 0.167 Uiso 0.357(9) 1 calc R U P A 1
H52C H 0.6750 -0.0195 0.4012 0.167 Uiso 0.357(9) 1 calc R U P A 1
C51A C 0.6021(5) -0.0517(6) 0.4134(6) 0.1116(15) Uani 0.643(9) 1 d D U P A 2
H51C H 0.5699 -0.0737 0.4156 0.134 Uiso 0.643(9) 1 calc R U P A 2
H51D H 0.6274 -0.0821 0.4458 0.134 Uiso 0.643(9) 1 calc R U P A 2
C52A C 0.6089(4) -0.0784(7) 0.3530(5) 0.1116(15) Uani 0.643(9) 1 d D U P A 2
H52D H 0.6009 -0.1432 0.3453 0.167 Uiso 0.643(9) 1 calc R U P A 2
H52E H 0.6429 -0.0680 0.3535 0.167 Uiso 0.643(9) 1 calc R U P A 2
H52F H 0.5874 -0.0414 0.3212 0.167 Uiso 0.643(9) 1 calc R U P A 2
C53 C 0.6447(5) 0.0569(11) 0.4735(7) 0.1116(15) Uani 0.484(8) 1 d . U P A 1
H53A H 0.6372 0.1220 0.4785 0.134 Uiso 0.484(8) 1 calc R U P A 1
H53B H 0.6290 0.0252 0.5011 0.134 Uiso 0.484(8) 1 calc R U P A 1
C54 C 0.6800(5) 0.0598(10) 0.5062(7) 0.1116(15) Uani 0.484(8) 1 d . U P A 1
H54A H 0.6951 -0.0009 0.5104 0.167 Uiso 0.484(8) 1 calc R U P A 1
H54B H 0.6763 0.0793 0.5453 0.167 Uiso 0.484(8) 1 calc R U P A 1
H54C H 0.7007 0.1035 0.4928 0.167 Uiso 0.484(8) 1 calc R U P A 1
C53A C 0.6514(4) 0.0932(10) 0.4463(7) 0.1116(15) Uani 0.516(8) 1 d . U P A 2
H53C H 0.6526 0.1404 0.4161 0.134 Uiso 0.516(8) 1 calc R U P A 2
H53D H 0.6494 0.1262 0.4829 0.134 Uiso 0.516(8) 1 calc R U P A 2
C54A C 0.6929(4) 0.0519(10) 0.4600(7) 0.1116(15) Uani 0.516(8) 1 d . U P A 2
H54D H 0.6943 0.0080 0.4925 0.167 Uiso 0.516(8) 1 calc R U P A 2
H54E H 0.7191 0.0968 0.4734 0.167 Uiso 0.516(8) 1 calc R U P A 2
H54F H 0.6968 0.0195 0.4245 0.167 Uiso 0.516(8) 1 calc R U P A 2
O1 O 0.52635(18) 0.6079(2) 0.13417(18) 0.1036(12) Uani 1 1 d D U . . .
C41 C 0.4847(3) 0.6236(5) 0.0785(4) 0.137(2) Uani 1 1 d . U . . .
H41A H 0.4533 0.6139 0.0878 0.165 Uiso 1 1 calc R U . . .
H41B H 0.4855 0.6871 0.0642 0.165 Uiso 1 1 calc R U . . .
C42 C 0.4892(5) 0.5579(8) 0.0306(5) 0.215(5) Uani 1 1 d . U . . .
H42A H 0.4746 0.4992 0.0363 0.322 Uiso 1 1 calc R U . . .
H42B H 0.5237 0.5488 0.0333 0.322 Uiso 1 1 calc R U . . .
H42C H 0.4723 0.5826 -0.0092 0.322 Uiso 1 1 calc R U . . .
C43 C 0.5647(5) 0.6799(7) 0.1592(5) 0.097(3) Uani 0.468(11) 1 d D U P B 1
H43A H 0.5963 0.6603 0.1538 0.116 Uiso 0.468(11) 1 calc R U P B 1
H43B H 0.5552 0.7383 0.1374 0.116 Uiso 0.468(11) 1 calc R U P B 1
C43A C 0.5211(5) 0.6927(7) 0.1676(5) 0.115(3) Uani 0.532(11) 1 d D U P B 2
H43C H 0.4913 0.6905 0.1812 0.138 Uiso 0.532(11) 1 calc R U P B 2
H43D H 0.5199 0.7476 0.1422 0.138 Uiso 0.532(11) 1 calc R U P B 2
C44 C 0.5693(3) 0.6927(4) 0.2241(4) 0.129(3) Uani 1 1 d D . . . .
H44A H 0.5374 0.7083 0.2293 0.193 Uiso 1 1 calc R U . B 1
H44B H 0.5924 0.7422 0.2400 0.193 Uiso 1 1 calc R U . B 1
H44C H 0.5811 0.6360 0.2458 0.193 Uiso 1 1 calc R U . B 1
H61_2 H 0.4798(11) 0.394(2) 0.1106(13) 0.032(7) Uiso 1 1 d . . . . .
H62_2 H 0.5156(12) 0.312(2) 0.1673(15) 0.040(8) Uiso 1 1 d . . . . .
H63_2 H 0.5505(10) 0.3862(19) 0.1202(12) 0.026(7) Uiso 1 1 d . . . . .
H644_2 H 0.5258(10) 0.1289(19) 0.1774(12) 0.027(7) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Li2 2.362(5) 2_655 ?
Cl1 Li2 2.362(5) . ?
Cl1 Li3 2.503(6) . ?
Cl1 Li3 2.503(6) 2_655 ?
P1 C7 1.829(3) . ?
P1 C1 1.834(3) . ?
P1 C13 1.838(3) . ?
P1 Li1 2.517(5) . ?
P2 C33 1.828(3) . ?
P2 C27 1.831(3) . ?
P2 C21 1.839(3) . ?
P2 Li2 2.531(5) . ?
B11 C2 1.621(4) . ?
B11 Li2 2.423(5) 2_655 ?
B11 Li3 2.544(7) . ?
B11 Li1 2.774(7) . ?
B11 H61_2 1.18(3) . ?
B11 H62_2 1.20(3) . ?
B11 H63_2 1.22(3) . ?
B12 C8 1.608(4) . ?
B12 Li5 2.449(4) . ?
B12 Li4 2.456(7) 2_655 ?
B12 H65 1.04(4) . ?
B12 H66 1.07(3) . ?
B12 H644_2 1.16(3) . ?
B21 C22 1.614(5) . ?
B21 Li1 2.418(7) . ?
B21 Li3 2.434(9) . ?
B21 H67 1.23(3) . ?
B21 H68 1.17(4) . ?
B21 H69 1.11(4) . ?
B22 C28 1.609(4) . ?
B22 Li2 2.524(6) . ?
B22 Li4 2.555(7) . ?
B22 Li5 2.712(5) . ?
B22 Li1 2.829(6) . ?
B22 H70 1.09(3) . ?
B22 H71 1.25(3) . ?
B22 H72 1.21(3) . ?
Li1 C28 2.562(7) . ?
Li1 Li3 3.172(9) . ?
Li1 Li2 3.399(7) . ?
Li1 H67 1.87(3) . ?
Li1 H68 1.89(4) . ?
Li1 H72 2.30(3) . ?
Li1 H62_2 2.21(3) . ?
Li2 B11 2.423(5) 2_655 ?
Li2 Li3 3.149(8) 2_655 ?
Li2 Li2 3.507(10) 2_655 ?
Li2 H71 2.16(3) . ?
Li2 H72 1.98(3) . ?
Li3 O1 1.912(8) . ?
Li3 Li2 3.148(8) 2_655 ?
Li3 H67 2.04(3) . ?
Li3 H69 1.96(3) . ?
Li3 H63_2 2.00(3) . ?
Li4 O2 2.010(9) . ?
Li4 B12 2.456(7) 2_655 ?
Li4 C3 2.744(8) 2_655 ?
Li4 C2 2.767(8) 2_655 ?
Li4 Li5 3.180(6) . ?
Li4 H70 2.14(3) . ?
Li4 H71 1.99(3) . ?
Li5 B12 2.449(4) 2_655 ?
Li5 B22 2.712(5) 2_655 ?
Li5 Li4 3.180(6) 2_655 ?
Li5 H65 1.96(4) . ?
Li5 H70 2.00(3) . ?
Li5 H644_2 2.03(3) . ?
C1 C6 1.397(4) . ?
C1 C2 1.411(3) . ?
C2 C3 1.401(4) . ?
C2 Li4 2.767(8) 2_655 ?
C3 C4 1.395(4) . ?
C3 Li4 2.744(8) 2_655 ?
C3 H3 0.9500 . ?
C4 C5 1.382(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.390(4) . ?
C7 C8 1.415(4) . ?
C8 C9 1.396(4) . ?
C9 C10 1.386(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.367(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.387(5) . ?
C13 C14 1.390(4) . ?
C14 C15 1.403(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.344(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.366(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C21 C26 1.389(4) . ?
C21 C22 1.404(4) . ?
C22 C23 1.399(5) . ?
C23 C24 1.377(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.379(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.379(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.401(4) . ?
C27 C28 1.409(4) . ?
C28 C29 1.399(4) . ?
C29 C30 1.389(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.360(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.366(5) . ?
C33 C38 1.390(4) . ?
C34 C35 1.387(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.359(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.362(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.382(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
O2 C53 1.395(14) . ?
O2 C51A 1.426(9) . ?
O2 C51 1.432(11) . ?
O2 C53A 1.470(14) . ?
C51 C52 1.26(2) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C51A C52A 1.512(17) . ?
C51A H51C 0.9900 . ?
C51A H51D 0.9900 . ?
C52A H52D 0.9800 . ?
C52A H52E 0.9800 . ?
C52A H52F 0.9800 . ?
C53 C54 1.080(16) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C53A C54A 1.290(15) . ?
C53A H53C 0.9900 . ?
C53A H53D 0.9900 . ?
C54A H54D 0.9800 . ?
C54A H54E 0.9800 . ?
C54A H54F 0.9800 . ?
O1 C43A 1.490(11) . ?
O1 C41 1.507(9) . ?
O1 C43 1.514(11) . ?
C41 C42 1.500(13) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.479(11) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43A C44 1.612(13) . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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
Li2 Cl1 Li2 95.9(2) 2_655 . ?
Li2 Cl1 Li3 80.62(18) 2_655 . ?
Li2 Cl1 Li3 107.1(2) . . ?
Li2 Cl1 Li3 107.1(2) 2_655 2_655 ?
Li2 Cl1 Li3 80.61(18) . 2_655 ?
Li3 Cl1 Li3 168.8(3) . 2_655 ?
C7 P1 C1 104.41(12) . . ?
C7 P1 C13 105.43(12) . . ?
C1 P1 C13 104.20(13) . . ?
C7 P1 Li1 118.28(17) . . ?
C1 P1 Li1 113.57(16) . . ?
C13 P1 Li1 109.74(16) . . ?
C33 P2 C27 105.20(14) . . ?
C33 P2 C21 104.01(13) . . ?
C27 P2 C21 102.73(14) . . ?
C33 P2 Li2 111.36(14) . . ?
C27 P2 Li2 105.26(14) . . ?
C21 P2 Li2 126.30(16) . . ?
C2 B11 Li2 119.5(2) . 2_655 ?
C2 B11 Li3 159.7(2) . . ?
Li2 B11 Li3 78.6(2) 2_655 . ?
C2 B11 Li1 110.6(2) . . ?
Li2 B11 Li1 97.42(19) 2_655 . ?
Li3 B11 Li1 73.1(2) . . ?
C2 B11 H61_2 110.3(14) . . ?
Li2 B11 H61_2 50.5(14) 2_655 . ?
Li3 B11 H61_2 73.0(14) . . ?
Li1 B11 H61_2 137.1(14) . . ?
C2 B11 H62_2 110.3(15) . . ?
Li2 B11 H62_2 52.5(15) 2_655 . ?
Li3 B11 H62_2 87.7(15) . . ?
Li1 B11 H62_2 50.5(15) . . ?
H61_2 B11 H62_2 103(2) . . ?
C2 B11 H63_2 112.1(13) . . ?
Li2 B11 H63_2 128.4(13) 2_655 . ?
Li3 B11 H63_2 50.3(13) . . ?
Li1 B11 H63_2 64.2(13) . . ?
H61_2 B11 H63_2 110.3(19) . . ?
H62_2 B11 H63_2 111(2) . . ?
C8 B12 Li5 133.5(2) . . ?
C8 B12 Li4 139.5(3) . 2_655 ?
Li5 B12 Li4 80.82(18) . 2_655 ?
C8 B12 H65 110.5(19) . . ?
Li5 B12 H65 50(2) . . ?
Li4 B12 H65 108.8(19) 2_655 . ?
C8 B12 H66 111.1(17) . . ?
Li5 B12 H66 115.0(17) . . ?
Li4 B12 H66 46.8(18) 2_655 . ?
H65 B12 H66 106(3) . . ?
C8 B12 H644_2 112.6(14) . . ?
Li5 B12 H644_2 55.2(14) . . ?
Li4 B12 H644_2 65.2(14) 2_655 . ?
H65 B12 H644_2 105(2) . . ?
H66 B12 H644_2 111(2) . . ?
C22 B21 Li1 137.5(3) . . ?
C22 B21 Li3 122.7(3) . . ?
Li1 B21 Li3 81.6(2) . . ?
C22 B21 H67 111.6(15) . . ?
Li1 B21 H67 49.5(15) . . ?
Li3 B21 H67 56.9(15) . . ?
C22 B21 H68 120(2) . . ?
Li1 B21 H68 50.2(19) . . ?
Li3 B21 H68 117.2(19) . . ?
H67 B21 H68 99(2) . . ?
C22 B21 H69 111.0(18) . . ?
Li1 B21 H69 111.3(18) . . ?
Li3 B21 H69 52.0(18) . . ?
H67 B21 H69 108(2) . . ?
H68 B21 H69 106(3) . . ?
C28 B22 Li2 109.9(2) . . ?
C28 B22 Li4 126.2(2) . . ?
Li2 B22 Li4 100.0(2) . . ?
C28 B22 Li5 134.94(19) . . ?
Li2 B22 Li5 103.63(19) . . ?
Li4 B22 Li5 74.21(17) . . ?
C28 B22 Li1 63.76(18) . . ?
Li2 B22 Li1 78.62(18) . . ?
Li4 B22 Li1 169.1(2) . . ?
Li5 B22 Li1 95.50(16) . . ?
C28 B22 H70 113.4(18) . . ?
Li2 B22 H70 136.6(18) . . ?
Li4 B22 H70 55.5(18) . . ?
Li5 B22 H70 39.8(17) . . ?
Li1 B22 H70 118.4(18) . . ?
C28 B22 H71 113.1(15) . . ?
Li2 B22 H71 59.0(15) . . ?
Li4 B22 H71 49.6(16) . . ?
Li5 B22 H71 109.7(15) . . ?
Li1 B22 H71 134.2(16) . . ?
H70 B22 H71 105(2) . . ?
C28 B22 H72 115.1(16) . . ?
Li2 B22 H72 50.2(15) . . ?
Li4 B22 H72 118.5(16) . . ?
Li5 B22 H72 66.7(15) . . ?
Li1 B22 H72 52.4(16) . . ?
H70 B22 H72 106(2) . . ?
H71 B22 H72 103(2) . . ?
B21 Li1 P1 123.5(2) . . ?
B21 Li1 C28 103.6(2) . . ?
P1 Li1 C28 111.9(2) . . ?
B21 Li1 B11 96.4(2) . . ?
P1 Li1 B11 72.33(15) . . ?
C28 Li1 B11 150.9(2) . . ?
B21 Li1 B22 117.5(2) . . ?
P1 Li1 B22 116.6(2) . . ?
C28 Li1 B22 34.27(11) . . ?
B11 Li1 B22 117.0(2) . . ?
B21 Li1 Li3 49.4(2) . . ?
P1 Li1 Li3 112.4(2) . . ?
C28 Li1 Li3 135.7(2) . . ?
B11 Li1 Li3 50.12(17) . . ?
B22 Li1 Li3 119.1(2) . . ?
B21 Li1 Li2 82.49(19) . . ?
P1 Li1 Li2 151.0(2) . . ?
C28 Li1 Li2 68.46(16) . . ?
B11 Li1 Li2 93.84(19) . . ?
B22 Li1 Li2 46.70(13) . . ?
Li3 Li1 Li2 73.00(19) . . ?
B21 Li1 H67 29.9(10) . . ?
P1 Li1 H67 145.0(10) . . ?
C28 Li1 H67 100.1(10) . . ?
B11 Li1 H67 86.8(10) . . ?
B22 Li1 H67 97.7(10) . . ?
Li3 Li1 H67 37.7(10) . . ?
Li2 Li1 H67 54.9(10) . . ?
B21 Li1 H68 28.4(12) . . ?
P1 Li1 H68 101.7(13) . . ?
C28 Li1 H68 99.1(12) . . ?
B11 Li1 H68 108.4(12) . . ?
B22 Li1 H68 127.0(12) . . ?
Li3 Li1 H68 71.9(12) . . ?
Li2 Li1 H68 106.9(13) . . ?
H67 Li1 H68 58.0(16) . . ?
B21 Li1 H72 116.5(8) . . ?
P1 Li1 H72 119.3(8) . . ?
C28 Li1 H72 58.6(8) . . ?
B11 Li1 H72 93.6(8) . . ?
B22 Li1 H72 24.7(8) . . ?
Li3 Li1 H72 98.7(8) . . ?
Li2 Li1 H72 34.3(8) . . ?
H67 Li1 H72 89.1(13) . . ?
H68 Li1 H72 137.9(15) . . ?
B21 Li1 H62_2 108.0(9) . . ?
P1 Li1 H62_2 84.5(8) . . ?
C28 Li1 H62_2 126.5(9) . . ?
B11 Li1 H62_2 24.7(8) . . ?
B22 Li1 H62_2 92.4(9) . . ?
Li3 Li1 H62_2 58.7(8) . . ?
Li2 Li1 H62_2 74.2(9) . . ?
H67 Li1 H62_2 87.8(13) . . ?
H68 Li1 H62_2 128.1(15) . . ?
H72 Li1 H62_2 68.9(12) . . ?
Cl1 Li2 B11 101.49(19) . 2_655 ?
Cl1 Li2 B22 134.3(2) . . ?
B11 Li2 B22 104.3(2) 2_655 . ?
Cl1 Li2 P2 115.17(19) . . ?
B11 Li2 P2 125.9(2) 2_655 . ?
B22 Li2 P2 77.64(15) . . ?
Cl1 Li2 Li3 51.65(15) . 2_655 ?
B11 Li2 Li3 52.39(16) 2_655 2_655 ?
B22 Li2 Li3 150.2(2) . 2_655 ?
P2 Li2 Li3 129.8(2) . 2_655 ?
Cl1 Li2 Li1 85.95(17) . . ?
B11 Li2 Li1 151.1(2) 2_655 . ?
B22 Li2 Li1 54.67(15) . . ?
P2 Li2 Li1 72.88(15) . . ?
Li3 Li2 Li1 136.4(2) 2_655 . ?
Cl1 Li2 Li2 42.05(12) . 2_655 ?
B11 Li2 Li2 97.9(2) 2_655 2_655 ?
B22 Li2 Li2 97.05(14) . 2_655 ?
P2 Li2 Li2 135.9(2) . 2_655 ?
Li3 Li2 Li2 71.78(17) 2_655 2_655 ?
Li1 Li2 Li2 68.98(17) . 2_655 ?
Cl1 Li2 H71 160.8(9) . . ?
B11 Li2 H71 81.2(9) 2_655 . ?
B22 Li2 H71 29.6(9) . . ?
P2 Li2 H71 76.5(9) . . ?
Li3 Li2 H71 133.6(9) 2_655 . ?
Li1 Li2 H71 83.1(9) . . ?
Li2 Li2 H71 118.8(9) 2_655 . ?
Cl1 Li2 H72 106.9(10) . . ?
B11 Li2 H72 111.0(10) 2_655 . ?
B22 Li2 H72 28.0(9) . . ?
P2 Li2 H72 95.3(10) . . ?
Li3 Li2 H72 134.3(10) 2_655 . ?
Li1 Li2 H72 40.8(10) . . ?
Li2 Li2 H72 69.3(9) 2_655 . ?
H71 Li2 H72 55.2(12) . . ?
O1 Li3 B21 124.3(3) . . ?
O1 Li3 Cl1 106.2(3) . . ?
B21 Li3 Cl1 103.3(3) . . ?
O1 Li3 B11 120.9(3) . . ?
B21 Li3 B11 102.3(3) . . ?
Cl1 Li3 B11 94.5(2) . . ?
O1 Li3 Li2 113.9(3) . 2_655 ?
B21 Li3 Li2 120.9(3) . 2_655 ?
Cl1 Li3 Li2 47.74(14) . 2_655 ?
B11 Li3 Li2 48.98(15) . 2_655 ?
O1 Li3 Li1 164.9(3) . . ?
B21 Li3 Li1 48.96(19) . . ?
Cl1 Li3 Li1 88.8(2) . . ?
B11 Li3 Li1 56.80(18) . . ?
Li2 Li3 Li1 76.48(19) 2_655 . ?
O1 Li3 H67 148.1(10) . . ?
B21 Li3 H67 30.2(9) . . ?
Cl1 Li3 H67 77.0(9) . . ?
B11 Li3 H67 89.8(9) . . ?
Li2 Li3 H67 92.0(9) 2_655 . ?
Li1 Li3 H67 34.0(9) . . ?
O1 Li3 H69 102.3(11) . . ?
B21 Li3 H69 26.5(11) . . ?
Cl1 Li3 H69 127.5(11) . . ?
B11 Li3 H69 107.3(10) . . ?
Li2 Li3 H69 143.4(11) 2_655 . ?
Li1 Li3 H69 66.9(11) . . ?
H67 Li3 H69 56.5(14) . . ?
O1 Li3 H63_2 117.9(9) . . ?
B21 Li3 H63_2 84.3(8) . . ?
Cl1 Li3 H63_2 119.7(8) . . ?
B11 Li3 H63_2 28.0(8) . . ?
Li2 Li3 H63_2 76.8(8) 2_655 . ?
Li1 Li3 H63_2 51.9(8) . . ?
H67 Li3 H63_2 84.7(12) . . ?
H69 Li3 H63_2 81.6(13) . . ?
O2 Li4 B12 116.6(3) . 2_655 ?
O2 Li4 B22 97.1(3) . . ?
B12 Li4 B22 104.3(2) 2_655 . ?
O2 Li4 C3 110.7(3) . 2_655 ?
B12 Li4 C3 120.4(3) 2_655 2_655 ?
B22 Li4 C3 103.6(2) . 2_655 ?
O2 Li4 C2 139.4(3) . 2_655 ?
B12 Li4 C2 93.9(3) 2_655 2_655 ?
B22 Li4 C2 100.7(3) . 2_655 ?
C3 Li4 C2 29.46(11) 2_655 2_655 ?
O2 Li4 Li5 113.7(3) . . ?
B12 Li4 Li5 49.49(15) 2_655 . ?
B22 Li4 Li5 55.14(16) . . ?
C3 Li4 Li5 132.5(3) 2_655 . ?
C2 Li4 Li5 106.4(3) 2_655 . ?
O2 Li4 H70 90.1(9) . . ?
B12 Li4 H70 86.3(9) 2_655 . ?
B22 Li4 H70 25.0(9) . . ?
C3 Li4 H70 128.3(10) 2_655 . ?
C2 Li4 H70 119.7(9) 2_655 . ?
Li5 Li4 H70 38.1(9) . . ?
O2 Li4 H71 106.4(10) . . ?
B12 Li4 H71 120.5(10) 2_655 . ?
B22 Li4 H71 28.5(10) . . ?
C3 Li4 H71 75.1(10) 2_655 . ?
C2 Li4 H71 76.4(10) 2_655 . ?
Li5 Li4 H71 76.9(10) . . ?
H70 Li4 H71 53.4(13) . . ?
B12 Li5 B12 136.5(3) 2_655 . ?
B12 Li5 B22 102.59(11) 2_655 2_655 ?
B12 Li5 B22 100.05(10) . 2_655 ?
B12 Li5 B22 100.04(10) 2_655 . ?
B12 Li5 B22 102.59(11) . . ?
B22 Li5 B22 116.1(3) 2_655 . ?
B12 Li5 Li4 133.55(19) 2_655 2_655 ?
B12 Li5 Li4 49.69(14) . 2_655 ?
B22 Li5 Li4 50.65(13) 2_655 2_655 ?
B22 Li5 Li4 125.0(2) . 2_655 ?
B12 Li5 Li4 49.68(14) 2_655 . ?
B12 Li5 Li4 133.55(19) . . ?
B22 Li5 Li4 125.0(2) 2_655 . ?
B22 Li5 Li4 50.65(13) . . ?
Li4 Li5 Li4 173.5(4) 2_655 . ?
B12 Li5 H65 112.5(11) 2_655 . ?
B12 Li5 H65 24.3(11) . . ?
B22 Li5 H65 114.7(10) 2_655 . ?
B22 Li5 H65 109.8(10) . . ?
Li4 Li5 H65 65.5(10) 2_655 . ?
Li4 Li5 H65 119.7(10) . . ?
B12 Li5 H70 89.6(10) 2_655 . ?
B12 Li5 H70 99.1(10) . . ?
B22 Li5 H70 136.2(10) 2_655 . ?
B22 Li5 H70 20.5(10) . . ?
Li4 Li5 H70 136.7(10) 2_655 . ?
Li4 Li5 H70 41.3(10) . . ?
H65 Li5 H70 98.3(14) . . ?
B12 Li5 H644_2 164.7(9) 2_655 . ?
B12 Li5 H644_2 28.2(8) . . ?
B22 Li5 H644_2 85.6(8) 2_655 . ?
B22 Li5 H644_2 87.6(8) . . ?
Li4 Li5 H644_2 44.3(8) 2_655 . ?
Li4 Li5 H644_2 134.7(8) . . ?
H65 Li5 H644_2 52.2(13) . . ?
H70 Li5 H644_2 93.4(13) . . ?
C6 C1 C2 121.0(2) . . ?
C6 C1 P1 121.3(2) . . ?
C2 C1 P1 117.63(18) . . ?
C3 C2 C1 116.9(2) . . ?
C3 C2 B11 121.2(2) . . ?
C1 C2 B11 121.9(2) . . ?
C3 C2 Li4 74.4(2) . 2_655 ?
C1 C2 Li4 86.5(2) . 2_655 ?
B11 C2 Li4 107.4(2) . 2_655 ?
C4 C3 C2 121.7(3) . . ?
C4 C3 Li4 87.7(2) . 2_655 ?
C2 C3 Li4 76.2(2) . 2_655 ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
Li4 C3 H3 106.7 2_655 . ?
C5 C4 C3 120.5(3) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 119.2(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C1 120.8(3) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C12 C7 C8 120.9(3) . . ?
C12 C7 P1 120.0(2) . . ?
C8 C7 P1 118.42(19) . . ?
C9 C8 C7 116.3(3) . . ?
C9 C8 B12 118.3(3) . . ?
C7 C8 B12 125.4(2) . . ?
C10 C9 C8 122.7(3) . . ?
C10 C9 H9 118.6 . . ?
C8 C9 H9 118.6 . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
C18 C13 C14 117.3(3) . . ?
C18 C13 P1 118.0(2) . . ?
C14 C13 P1 124.6(3) . . ?
C13 C14 C15 120.6(4) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C16 C15 C14 120.7(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 119.9(3) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 120.4(4) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 121.0(3) . . ?
C13 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C26 C21 C22 120.9(3) . . ?
C26 C21 P2 121.5(2) . . ?
C22 C21 P2 117.6(2) . . ?
C23 C22 C21 115.9(3) . . ?
C23 C22 B21 119.9(3) . . ?
C21 C22 B21 124.2(3) . . ?
C24 C23 C22 123.3(3) . . ?
C24 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
C23 C24 C25 119.4(3) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C24 C25 C26 119.3(3) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C25 C26 C21 121.1(3) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
C32 C27 C28 120.3(3) . . ?
C32 C27 P2 120.7(2) . . ?
C28 C27 P2 118.8(2) . . ?
C29 C28 C27 116.4(2) . . ?
C29 C28 B22 121.0(2) . . ?
C27 C28 B22 122.5(2) . . ?
C29 C28 Li1 96.3(2) . . ?
C27 C28 Li1 91.9(2) . . ?
B22 C28 Li1 82.0(2) . . ?
C30 C29 C28 122.3(3) . . ?
C30 C29 H29 118.8 . . ?
C28 C29 H29 118.8 . . ?
C31 C30 C29 120.2(3) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 119.7(3) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C31 C32 C27 121.0(3) . . ?
C31 C32 H32 119.5 . . ?
C27 C32 H32 119.5 . . ?
C34 C33 C38 118.0(3) . . ?
C34 C33 P2 124.3(3) . . ?
C38 C33 P2 117.6(3) . . ?
C33 C34 C35 120.0(4) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 121.0(5) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C37 120.4(4) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C36 C37 C38 118.6(4) . . ?
C36 C37 H37 120.7 . . ?
C38 C37 H37 120.7 . . ?
C37 C38 C33 122.0(4) . . ?
C37 C38 H38 119.0 . . ?
C33 C38 H38 119.0 . . ?
C53 O2 C51 101.6(12) . . ?
C51A O2 C53A 122.9(8) . . ?
C53 O2 Li4 128.5(7) . . ?
C51A O2 Li4 121.5(6) . . ?
C51 O2 Li4 129.3(10) . . ?
C53A O2 Li4 114.8(6) . . ?
C52 C51 O2 116.0(17) . . ?
C52 C51 H51A 108.3 . . ?
O2 C51 H51A 108.3 . . ?
C52 C51 H51B 108.3 . . ?
O2 C51 H51B 108.3 . . ?
H51A C51 H51B 107.4 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O2 C51A C52A 112.5(9) . . ?
O2 C51A H51C 109.1 . . ?
C52A C51A H51C 109.1 . . ?
O2 C51A H51D 109.1 . . ?
C52A C51A H51D 109.1 . . ?
H51C C51A H51D 107.8 . . ?
C51A C52A H52D 109.5 . . ?
C51A C52A H52E 109.5 . . ?
H52D C52A H52E 109.5 . . ?
C51A C52A H52F 109.5 . . ?
H52D C52A H52F 109.5 . . ?
H52E C52A H52F 109.5 . . ?
C54 C53 O2 167.0(18) . . ?
C54 C53 H53A 94.0 . . ?
O2 C53 H53A 94.0 . . ?
C54 C53 H53B 94.0 . . ?
O2 C53 H53B 94.0 . . ?
H53A C53 H53B 103.1 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C54A C53A O2 122.5(13) . . ?
C54A C53A H53C 106.7 . . ?
O2 C53A H53C 106.7 . . ?
C54A C53A H53D 106.7 . . ?
O2 C53A H53D 106.7 . . ?
H53C C53A H53D 106.6 . . ?
C53A C54A H54D 109.5 . . ?
C53A C54A H54E 109.5 . . ?
H54D C54A H54E 109.5 . . ?
C53A C54A H54F 109.5 . . ?
H54D C54A H54F 109.5 . . ?
H54E C54A H54F 109.5 . . ?
C43A O1 C41 98.4(7) . . ?
C41 O1 C43 122.4(6) . . ?
C43A O1 Li3 123.5(5) . . ?
C41 O1 Li3 125.7(4) . . ?
C43 O1 Li3 110.8(6) . . ?
C42 C41 O1 108.8(8) . . ?
C42 C41 H41A 109.9 . . ?
O1 C41 H41A 109.9 . . ?
C42 C41 H41B 109.9 . . ?
O1 C41 H41B 109.9 . . ?
H41A C41 H41B 108.3 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 O1 109.0(7) . . ?
C44 C43 H43A 109.9 . . ?
O1 C43 H43A 109.9 . . ?
C44 C43 H43B 109.9 . . ?
O1 C43 H43B 109.9 . . ?
H43A C43 H43B 108.3 . . ?
O1 C43A C44 103.4(8) . . ?
O1 C43A H43C 111.1 . . ?
C44 C43A H43C 111.1 . . ?
O1 C43A H43D 111.1 . . ?
C44 C43A H43D 111.1 . . ?
H43C C43A H43D 109.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

_refine_diff_density_max         1.208
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.091

_shelxl_version_number           2014/5


####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2096465'
loop_
_audit_author_name
_audit_author_address
'Rong Shang '
;Graduate School of Advanced Engineering and Science, Hiroshima University
Japan
;
_audit_update_record             
;
2021-07-14 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
#data_20201007oishiexp507_0m_a

_audit_creation_method           SHELXL-2014/5
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H49 B2 O2 P'
_chemical_formula_weight         590.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   10.020(8)
_cell_length_b                   15.571(12)
_cell_length_c                   21.243(17)
_cell_angle_alpha                90
_cell_angle_beta                 102.039(14)
_cell_angle_gamma                90
_cell_volume                     3242(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9920
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      28.88

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.106
_exptl_absorpt_coefficient_mu    0.118
_shelx_estimated_absorpt_T_min   0.967
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39296
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.960
_diffrn_reflns_theta_max         29.319
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8268
_reflns_number_gt                6906
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0564P)²+1.5660P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8268
_refine_ls_number_parameters     434
_refine_ls_number_restraints     242
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.1221
_refine_ls_wR_factor_gt          0.1150
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.28980(15) 0.24596(10) 0.60011(7) 0.0209(3) Uani 1 1 d . . . . .
B2 B 0.23473(16) 0.35363(10) 0.83407(7) 0.0222(3) Uani 1 1 d . . . . .
P1 P 0.38289(3) 0.25685(2) 0.72659(2) 0.01857(9) Uani 1 1 d . . . . .
O1 O 0.26409(9) 0.27628(7) 0.67022(4) 0.0228(2) Uani 1 1 d . . . . .
C1 C 0.33457(14) 0.17669(9) 0.77814(6) 0.0221(3) Uani 1 1 d . . . . .
C2 C 0.41738(17) 0.15837(10) 0.83792(7) 0.0322(3) Uani 1 1 d . . . . .
H2 H 0.4956 0.1926 0.8539 0.039 Uiso 1 1 calc R U . . .
C3 C 0.38549(19) 0.09012(11) 0.87409(8) 0.0411(4) Uani 1 1 d . . . . .
H3 H 0.4422 0.0775 0.9147 0.049 Uiso 1 1 calc R U . . .
C4 C 0.27134(19) 0.04048(10) 0.85105(9) 0.0376(4) Uani 1 1 d . . . . .
H4 H 0.2498 -0.0061 0.8760 0.045 Uiso 1 1 calc R U . . .
C5 C 0.18841(17) 0.05820(10) 0.79193(8) 0.0320(3) Uani 1 1 d . . . . .
H5 H 0.1098 0.0240 0.7765 0.038 Uiso 1 1 calc R U . . .
C6 C 0.21984(15) 0.12584(9) 0.75508(7) 0.0266(3) Uani 1 1 d . . . . .
H6 H 0.1634 0.1376 0.7142 0.032 Uiso 1 1 calc R U . . .
C21 C 0.50767(13) 0.21791(9) 0.68502(7) 0.0219(3) Uani 1 1 d . . . . .
C22 C 0.45035(14) 0.21984(9) 0.61883(6) 0.0214(3) Uani 1 1 d . . . . .
C23 C 0.53930(15) 0.19607(10) 0.57864(7) 0.0283(3) Uani 1 1 d . . . . .
H23 H 0.5067 0.1964 0.5333 0.034 Uiso 1 1 calc R U . . .
C24 C 0.67332(15) 0.17211(10) 0.60340(8) 0.0319(3) Uani 1 1 d . . . . .
H24 H 0.7310 0.1576 0.5747 0.038 Uiso 1 1 calc R U . . .
C25 C 0.72465(15) 0.16896(10) 0.66934(8) 0.0322(3) Uani 1 1 d . . . . .
H25 H 0.8160 0.1512 0.6857 0.039 Uiso 1 1 calc R U . . .
C26 C 0.64138(14) 0.19203(10) 0.71102(7) 0.0280(3) Uani 1 1 d . . . . .
H26 H 0.6744 0.1903 0.7563 0.034 Uiso 1 1 calc R U . . .
C31 C 0.44873(13) 0.34685(8) 0.77660(6) 0.0187(2) Uani 1 1 d . . . . .
C32 C 0.38200(13) 0.37820(8) 0.82466(6) 0.0198(2) Uani 1 1 d . . . . .
C33 C 0.44843(15) 0.44405(9) 0.86421(7) 0.0246(3) Uani 1 1 d . . . . .
H33 H 0.4086 0.4651 0.8980 0.030 Uiso 1 1 calc R U . . .
C34 C 0.57065(15) 0.47963(9) 0.85560(7) 0.0268(3) Uani 1 1 d . . . . .
H34 H 0.6120 0.5247 0.8830 0.032 Uiso 1 1 calc R U . . .
C35 C 0.63195(14) 0.44980(9) 0.80758(7) 0.0264(3) Uani 1 1 d . . . . .
H35 H 0.7144 0.4750 0.8011 0.032 Uiso 1 1 calc R U . . .
C36 C 0.57225(14) 0.38240(9) 0.76860(7) 0.0234(3) Uani 1 1 d . . . . .
H36 H 0.6158 0.3604 0.7363 0.028 Uiso 1 1 calc R U . . .
C41 C 0.18841(14) 0.16627(9) 0.57566(6) 0.0231(3) Uani 1 1 d . . . . .
H41 H 0.2128 0.1179 0.6069 0.028 Uiso 1 1 calc R U . . .
C42 C 0.03904(15) 0.19180(10) 0.57362(7) 0.0288(3) Uani 1 1 d . . . . .
H42A H 0.0261 0.1970 0.6184 0.035 Uiso 1 1 calc R U . . .
H42B H -0.0207 0.1447 0.5529 0.035 Uiso 1 1 calc R U . . .
C43 C -0.00837(15) 0.27606(11) 0.53780(8) 0.0326(3) Uani 1 1 d . . . . .
H43A H -0.0266 0.2651 0.4909 0.039 Uiso 1 1 calc R U . . .
H43B H -0.0951 0.2944 0.5490 0.039 Uiso 1 1 calc R U . . .
C44 C 0.09549(15) 0.34929(10) 0.55356(7) 0.0286(3) Uani 1 1 d . . . . .
H44A H 0.0952 0.3708 0.5974 0.034 Uiso 1 1 calc R U . . .
H44B H 0.0663 0.3971 0.5231 0.034 Uiso 1 1 calc R U . . .
C45 C 0.24245(14) 0.32337(9) 0.55025(7) 0.0236(3) Uani 1 1 d . . . . .
H45 H 0.3038 0.3736 0.5639 0.028 Uiso 1 1 calc R U . . .
C46 C 0.25710(17) 0.29558(10) 0.48215(7) 0.0303(3) Uani 1 1 d . . . . .
H46A H 0.2139 0.3400 0.4512 0.036 Uiso 1 1 calc R U . . .
H46B H 0.3555 0.2945 0.4812 0.036 Uiso 1 1 calc R U . . .
C47 C 0.19513(19) 0.20776(11) 0.45846(7) 0.0350(4) Uani 1 1 d . . . . .
H47A H 0.0964 0.2157 0.4408 0.042 Uiso 1 1 calc R U . . .
H47B H 0.2374 0.1881 0.4228 0.042 Uiso 1 1 calc R U . . .
C48 C 0.21271(16) 0.13673(10) 0.50975(7) 0.0287(3) Uani 1 1 d . . . . .
H48A H 0.3064 0.1133 0.5157 0.034 Uiso 1 1 calc R U . . .
H48B H 0.1484 0.0895 0.4937 0.034 Uiso 1 1 calc R U . . .
C51 C 0.19998(16) 0.33370(10) 0.90122(7) 0.0304(3) Uani 1 1 d . . . . .
H51 H 0.2859 0.3203 0.9331 0.036 Uiso 1 1 calc R U . . .
C52 C 0.13422(18) 0.41673(11) 0.92229(8) 0.0350(3) Uani 1 1 d . . . . .
H52A H 0.0929 0.4026 0.9595 0.042 Uiso 1 1 calc R U . . .
H52B H 0.2075 0.4593 0.9371 0.042 Uiso 1 1 calc R U . . .
C53 C 0.02505(18) 0.45854(11) 0.87019(9) 0.0385(4) Uani 1 1 d . . . . .
H53A H -0.0622 0.4275 0.8676 0.046 Uiso 1 1 calc R U . . .
H53B H 0.0114 0.5185 0.8830 0.046 Uiso 1 1 calc R U . . .
C54 C 0.06031(17) 0.45887(11) 0.80364(8) 0.0361(4) Uani 1 1 d . . . . .
H54A H 0.1356 0.5001 0.8039 0.043 Uiso 1 1 calc R U . . .
H54B H -0.0200 0.4796 0.7719 0.043 Uiso 1 1 calc R U . . .
C55 C 0.10377(15) 0.36919(11) 0.78099(7) 0.0306(3) Uani 1 1 d . . . . .
H55 H 0.1288 0.3749 0.7380 0.037 Uiso 1 1 calc R U . . .
C56 C -0.00690(17) 0.30025(12) 0.77795(10) 0.0440(4) Uani 1 1 d . . . . .
H56A H -0.0948 0.3247 0.7550 0.053 Uiso 1 1 calc R U . . .
H56B H 0.0153 0.2517 0.7518 0.053 Uiso 1 1 calc R U . . .
C57 C -0.0267(2) 0.26476(13) 0.84218(12) 0.0534(5) Uani 1 1 d . . . . .
H57A H -0.0714 0.2079 0.8346 0.064 Uiso 1 1 calc R U . . .
H57B H -0.0893 0.3033 0.8592 0.064 Uiso 1 1 calc R U . . .
C58 C 0.1045(2) 0.25486(11) 0.89331(10) 0.0445(5) Uani 1 1 d . . . . .
H58A H 0.1553 0.2045 0.8822 0.053 Uiso 1 1 calc R U . . .
H58B H 0.0798 0.2428 0.9352 0.053 Uiso 1 1 calc R U . . .
O60 O 0.7608(2) 0.46701(16) 0.67664(9) 0.0686(6) Uani 0.861(4) 1 d D U P A 1
C61 C 0.7962(3) 0.4212(2) 0.62638(13) 0.0693(8) Uani 0.861(4) 1 d D U P A 1
H61A H 0.7898 0.3588 0.6344 0.083 Uiso 0.861(4) 1 calc R U P A 1
H61B H 0.8916 0.4345 0.6240 0.083 Uiso 0.861(4) 1 calc R U P A 1
C62 C 0.7040(5) 0.4440(3) 0.56488(18) 0.0934(12) Uani 0.861(4) 1 d D U P A 1
H62A H 0.6628 0.3922 0.5416 0.112 Uiso 0.861(4) 1 calc R U P A 1
H62B H 0.7522 0.4773 0.5368 0.112 Uiso 0.861(4) 1 calc R U P A 1
C63 C 0.5945(4) 0.4997(3) 0.5885(2) 0.0899(11) Uani 0.861(4) 1 d D U P A 1
H63A H 0.5623 0.5475 0.5584 0.108 Uiso 0.861(4) 1 calc R U P A 1
H63B H 0.5153 0.4647 0.5941 0.108 Uiso 0.861(4) 1 calc R U P A 1
C64 C 0.6727(4) 0.5315(3) 0.6507(2) 0.0719(8) Uani 0.861(4) 1 d D U P A 1
H64A H 0.7242 0.5839 0.6442 0.086 Uiso 0.861(4) 1 calc R U P A 1
H64B H 0.6104 0.5457 0.6797 0.086 Uiso 0.861(4) 1 calc R U P A 1
O70 O 0.7828(15) 0.5175(11) 0.6524(8) 0.086(2) Uani 0.139(4) 1 d D U P A 2
C71 C 0.6491(18) 0.536(2) 0.6540(17) 0.081(3) Uani 0.139(4) 1 d D U P A 2
H71A H 0.6230 0.5925 0.6347 0.098 Uiso 0.139(4) 1 calc R U P A 2
H71B H 0.6362 0.5358 0.6989 0.098 Uiso 0.139(4) 1 calc R U P A 2
C72 C 0.5654(15) 0.4677(15) 0.6167(11) 0.083(3) Uani 0.139(4) 1 d D U P A 2
H72A H 0.4722 0.4884 0.5978 0.100 Uiso 0.139(4) 1 calc R U P A 2
H72B H 0.5596 0.4162 0.6433 0.100 Uiso 0.139(4) 1 calc R U P A 2
C73 C 0.6474(19) 0.449(2) 0.5641(9) 0.085(3) Uani 0.139(4) 1 d D U P A 2
H73A H 0.6346 0.3897 0.5481 0.102 Uiso 0.139(4) 1 calc R U P A 2
H73B H 0.6229 0.4897 0.5274 0.102 Uiso 0.139(4) 1 calc R U P A 2
C74 C 0.7892(16) 0.4644(15) 0.6012(10) 0.085(2) Uani 0.139(4) 1 d D U P A 2
H74A H 0.8322 0.4091 0.6170 0.102 Uiso 0.139(4) 1 calc R U P A 2
H74B H 0.8448 0.4916 0.5732 0.102 Uiso 0.139(4) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C45 1.609(2) . ?
B1 C41 1.619(2) . ?
B1 C22 1.626(2) . ?
B1 O1 1.633(2) . ?
B2 C55 1.560(2) . ?
B2 C51 1.568(2) . ?
B2 C32 1.577(2) . ?
P1 O1 1.5322(13) . ?
P1 C21 1.7809(16) . ?
P1 C1 1.7925(17) . ?
P1 C31 1.7987(16) . ?
C1 C2 1.394(2) . ?
C1 C6 1.398(2) . ?
C2 C3 1.387(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C21 C26 1.398(2) . ?
C21 C22 1.404(2) . ?
C22 C23 1.406(2) . ?
C23 C24 1.387(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.398(2) . ?
C31 C32 1.4186(19) . ?
C32 C33 1.403(2) . ?
C33 C34 1.391(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(2) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.540(2) . ?
C41 C48 1.541(2) . ?
C41 H41 1.0000 . ?
C42 C43 1.541(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.533(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.543(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.546(2) . ?
C45 H45 1.0000 . ?
C46 C47 1.542(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.537(2) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C51 C58 1.544(3) . ?
C51 C52 1.559(2) . ?
C51 H51 1.0000 . ?
C52 C53 1.530(3) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.527(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.568(3) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.535(2) . ?
C55 H55 1.0000 . ?
C56 C57 1.523(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.529(3) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
O60 C64 1.375(5) . ?
O60 C61 1.390(3) . ?
C61 C62 1.477(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.562(5) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.474(5) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
O70 C71 1.377(8) . ?
O70 C74 1.378(8) . ?
C71 C72 1.473(9) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.545(11) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 C74 1.492(9) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 H74A 0.9900 . ?
C74 H74B 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
C45 B1 C41 106.49(12) . . ?
C45 B1 C22 119.28(11) . . ?
C41 B1 C22 114.15(12) . . ?
C45 B1 O1 107.62(12) . . ?
C41 B1 O1 107.84(11) . . ?
C22 B1 O1 100.69(10) . . ?
C55 B2 C51 112.04(13) . . ?
C55 B2 C32 122.61(13) . . ?
C51 B2 C32 123.67(13) . . ?
O1 P1 C21 101.01(8) . . ?
O1 P1 C1 110.49(8) . . ?
C21 P1 C1 111.89(8) . . ?
O1 P1 C31 115.92(7) . . ?
C21 P1 C31 110.44(8) . . ?
C1 P1 C31 107.12(8) . . ?
P1 O1 B1 114.27(9) . . ?
C2 C1 C6 119.55(14) . . ?
C2 C1 P1 120.92(12) . . ?
C6 C1 P1 119.19(11) . . ?
C3 C2 C1 119.95(15) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 120.09(16) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.43(15) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.02(15) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 119.96(14) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C26 C21 C22 124.06(13) . . ?
C26 C21 P1 128.05(12) . . ?
C22 C21 P1 107.85(11) . . ?
C21 C22 C23 115.07(14) . . ?
C21 C22 B1 115.30(11) . . ?
C23 C22 B1 129.59(13) . . ?
C24 C23 C22 121.78(15) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C25 121.16(14) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C26 C25 C24 119.34(15) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C21 118.55(15) . . ?
C25 C26 H26 120.7 . . ?
C21 C26 H26 120.7 . . ?
C36 C31 C32 120.89(12) . . ?
C36 C31 P1 117.49(10) . . ?
C32 C31 P1 121.55(10) . . ?
C33 C32 C31 116.53(13) . . ?
C33 C32 B2 116.17(12) . . ?
C31 C32 B2 126.99(12) . . ?
C34 C33 C32 122.23(13) . . ?
C34 C33 H33 118.9 . . ?
C32 C33 H33 118.9 . . ?
C35 C34 C33 120.30(13) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 119.49(14) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C31 120.50(13) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C42 C41 C48 112.85(12) . . ?
C42 C41 B1 110.62(12) . . ?
C48 C41 B1 108.23(11) . . ?
C42 C41 H41 108.3 . . ?
C48 C41 H41 108.3 . . ?
B1 C41 H41 108.3 . . ?
C41 C42 C43 115.54(12) . . ?
C41 C42 H42A 108.4 . . ?
C43 C42 H42A 108.4 . . ?
C41 C42 H42B 108.4 . . ?
C43 C42 H42B 108.4 . . ?
H42A C42 H42B 107.5 . . ?
C44 C43 C42 113.59(13) . . ?
C44 C43 H43A 108.8 . . ?
C42 C43 H43A 108.8 . . ?
C44 C43 H43B 108.8 . . ?
C42 C43 H43B 108.8 . . ?
H43A C43 H43B 107.7 . . ?
C43 C44 C45 113.98(13) . . ?
C43 C44 H44A 108.8 . . ?
C45 C44 H44A 108.8 . . ?
C43 C44 H44B 108.8 . . ?
C45 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
C44 C45 C46 113.19(12) . . ?
C44 C45 B1 108.61(11) . . ?
C46 C45 B1 109.49(12) . . ?
C44 C45 H45 108.5 . . ?
C46 C45 H45 108.5 . . ?
B1 C45 H45 108.5 . . ?
C47 C46 C45 116.31(12) . . ?
C47 C46 H46A 108.2 . . ?
C45 C46 H46A 108.2 . . ?
C47 C46 H46B 108.2 . . ?
C45 C46 H46B 108.2 . . ?
H46A C46 H46B 107.4 . . ?
C48 C47 C46 115.35(13) . . ?
C48 C47 H47A 108.4 . . ?
C46 C47 H47A 108.4 . . ?
C48 C47 H47B 108.4 . . ?
C46 C47 H47B 108.4 . . ?
H47A C47 H47B 107.5 . . ?
C47 C48 C41 114.39(13) . . ?
C47 C48 H48A 108.7 . . ?
C41 C48 H48A 108.7 . . ?
C47 C48 H48B 108.7 . . ?
C41 C48 H48B 108.7 . . ?
H48A C48 H48B 107.6 . . ?
C58 C51 C52 113.68(14) . . ?
C58 C51 B2 107.96(13) . . ?
C52 C51 B2 106.53(12) . . ?
C58 C51 H51 109.5 . . ?
C52 C51 H51 109.5 . . ?
B2 C51 H51 109.5 . . ?
C53 C52 C51 115.25(14) . . ?
C53 C52 H52A 108.5 . . ?
C51 C52 H52A 108.5 . . ?
C53 C52 H52B 108.5 . . ?
C51 C52 H52B 108.5 . . ?
H52A C52 H52B 107.5 . . ?
C54 C53 C52 113.74(14) . . ?
C54 C53 H53A 108.8 . . ?
C52 C53 H53A 108.8 . . ?
C54 C53 H53B 108.8 . . ?
C52 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
C53 C54 C55 114.45(13) . . ?
C53 C54 H54A 108.6 . . ?
C55 C54 H54A 108.6 . . ?
C53 C54 H54B 108.6 . . ?
C55 C54 H54B 108.6 . . ?
H54A C54 H54B 107.6 . . ?
C56 C55 B2 114.40(15) . . ?
C56 C55 C54 113.03(14) . . ?
B2 C55 C54 99.33(12) . . ?
C56 C55 H55 109.9 . . ?
B2 C55 H55 109.9 . . ?
C54 C55 H55 109.9 . . ?
C57 C56 C55 116.36(15) . . ?
C57 C56 H56A 108.2 . . ?
C55 C56 H56A 108.2 . . ?
C57 C56 H56B 108.2 . . ?
C55 C56 H56B 108.2 . . ?
H56A C56 H56B 107.4 . . ?
C56 C57 C58 114.82(15) . . ?
C56 C57 H57A 108.6 . . ?
C58 C57 H57A 108.6 . . ?
C56 C57 H57B 108.6 . . ?
C58 C57 H57B 108.6 . . ?
H57A C57 H57B 107.5 . . ?
C57 C58 C51 114.76(15) . . ?
C57 C58 H58A 108.6 . . ?
C51 C58 H58A 108.6 . . ?
C57 C58 H58B 108.6 . . ?
C51 C58 H58B 108.6 . . ?
H58A C58 H58B 107.6 . . ?
C64 O60 C61 108.2(2) . . ?
O60 C61 C62 110.1(3) . . ?
O60 C61 H61A 109.6 . . ?
C62 C61 H61A 109.6 . . ?
O60 C61 H61B 109.6 . . ?
C62 C61 H61B 109.6 . . ?
H61A C61 H61B 108.2 . . ?
C61 C62 C63 101.6(3) . . ?
C61 C62 H62A 111.5 . . ?
C63 C62 H62A 111.5 . . ?
C61 C62 H62B 111.5 . . ?
C63 C62 H62B 111.5 . . ?
H62A C62 H62B 109.3 . . ?
C64 C63 C62 101.3(3) . . ?
C64 C63 H63A 111.5 . . ?
C62 C63 H63A 111.5 . . ?
C64 C63 H63B 111.5 . . ?
C62 C63 H63B 111.5 . . ?
H63A C63 H63B 109.3 . . ?
O60 C64 C63 106.9(3) . . ?
O60 C64 H64A 110.3 . . ?
C63 C64 H64A 110.3 . . ?
O60 C64 H64B 110.3 . . ?
C63 C64 H64B 110.3 . . ?
H64A C64 H64B 108.6 . . ?
C71 O70 C74 110.3(9) . . ?
O70 C71 C72 106.8(10) . . ?
O70 C71 H71A 110.4 . . ?
C72 C71 H71A 110.4 . . ?
O70 C71 H71B 110.4 . . ?
C72 C71 H71B 110.4 . . ?
H71A C71 H71B 108.6 . . ?
C71 C72 C73 101.1(10) . . ?
C71 C72 H72A 111.6 . . ?
C73 C72 H72A 111.6 . . ?
C71 C72 H72B 111.6 . . ?
C73 C72 H72B 111.6 . . ?
H72A C72 H72B 109.4 . . ?
C74 C73 C72 100.4(8) . . ?
C74 C73 H73A 111.7 . . ?
C72 C73 H73A 111.7 . . ?
C74 C73 H73B 111.7 . . ?
C72 C73 H73B 111.7 . . ?
H73A C73 H73B 109.5 . . ?
O70 C74 C73 108.4(8) . . ?
O70 C74 H74A 110.0 . . ?
C73 C74 H74A 110.0 . . ?
O70 C74 H74B 110.0 . . ?
C73 C74 H74B 110.0 . . ?
H74A C74 H74B 108.4 . . ?

_refine_diff_density_max         0.398
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.047

_shelxl_version_number           2014/5



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