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

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

data_1_alpha_298K
_database_code_depnum_ccdc_archive 'CCDC 986256'
_audit_update_record             
;
2014-02-11 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H56 B P'
_chemical_formula_weight         578.63

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.311(3)
_cell_length_b                   18.895(5)
_cell_length_c                   20.770(6)
_cell_angle_alpha                69.618(7)
_cell_angle_beta                 85.946(7)
_cell_angle_gamma                76.898(6)
_cell_volume                     3694.1(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    2828
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      19.28

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9296
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_process_details   
;
SADABS; Sheldrick 1996
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21495
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.05
_diffrn_reflns_theta_max         25.03
_reflns_number_total             12972
_reflns_number_gt                4884
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12972
_refine_ls_number_parameters     765
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.2319
_refine_ls_R_factor_gt           0.1120
_refine_ls_wR_factor_ref         0.4207
_refine_ls_wR_factor_gt          0.3496
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.135
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.7494(7) 0.2695(4) 0.2436(3) 0.0690(18) Uani 1 1 d . . .
B2 B 0.3202(6) 0.2389(3) 0.7350(3) 0.0623(16) Uani 1 1 d . . .
C1 C 0.8155(6) 0.3362(3) 0.2538(3) 0.0698(15) Uani 1 1 d . . .
C2 C 0.7396(7) 0.3985(4) 0.2684(3) 0.0870(18) Uani 1 1 d . . .
H2 H 0.6475 0.4048 0.2690 0.104 Uiso 1 1 calc R . .
C3 C 0.7952(11) 0.4529(4) 0.2825(4) 0.105(2) Uani 1 1 d . . .
H3 H 0.7404 0.4942 0.2923 0.126 Uiso 1 1 calc R . .
C4 C 0.9281(11) 0.4448(5) 0.2816(4) 0.110(3) Uani 1 1 d . . .
H4 H 0.9664 0.4806 0.2905 0.132 Uiso 1 1 calc R . .
C5 C 1.0063(8) 0.3834(5) 0.2675(4) 0.105(2) Uani 1 1 d . . .
H5 H 1.0983 0.3778 0.2662 0.126 Uiso 1 1 calc R . .
C6 C 0.9510(7) 0.3298(4) 0.2553(3) 0.0822(17) Uani 1 1 d . . .
H6 H 1.0072 0.2875 0.2476 0.099 Uiso 1 1 calc R . .
C7 C 0.8343(6) 0.2260(3) 0.1934(3) 0.0721(16) Uani 1 1 d . . .
C8 C 0.9184(6) 0.2579(4) 0.1421(3) 0.0870(18) Uani 1 1 d . . .
H8 H 0.9315 0.3070 0.1358 0.104 Uiso 1 1 calc R . .
C9 C 0.9840(7) 0.2186(5) 0.0997(4) 0.108(2) Uani 1 1 d . . .
H9 H 1.0401 0.2418 0.0657 0.129 Uiso 1 1 calc R . .
C10 C 0.9678(9) 0.1476(6) 0.1068(4) 0.113(3) Uani 1 1 d . . .
H10 H 1.0148 0.1212 0.0791 0.136 Uiso 1 1 calc R . .
C11 C 0.8837(8) 0.1155(4) 0.1537(4) 0.104(2) Uani 1 1 d . . .
H11 H 0.8690 0.0674 0.1577 0.125 Uiso 1 1 calc R . .
C12 C 0.8179(7) 0.1542(4) 0.1970(4) 0.0901(19) Uani 1 1 d . . .
H12 H 0.7603 0.1305 0.2296 0.108 Uiso 1 1 calc R . .
C13 C 0.6022(6) 0.3078(4) 0.2068(3) 0.0774(17) Uani 1 1 d . . .
C14 C 0.5798(7) 0.3758(4) 0.1518(4) 0.096(2) Uani 1 1 d . . .
H14 H 0.6498 0.4009 0.1364 0.116 Uiso 1 1 calc R . .
C15 C 0.4559(10) 0.4093(5) 0.1175(4) 0.122(3) Uani 1 1 d . . .
H15 H 0.4448 0.4558 0.0809 0.146 Uiso 1 1 calc R . .
C16 C 0.3527(10) 0.3727(7) 0.1384(7) 0.138(4) Uani 1 1 d . . .
H16 H 0.2702 0.3943 0.1165 0.166 Uiso 1 1 calc R . .
C17 C 0.3713(8) 0.3054(6) 0.1907(6) 0.127(3) Uani 1 1 d . . .
H17 H 0.3010 0.2803 0.2046 0.152 Uiso 1 1 calc R . .
C18 C 0.4923(7) 0.2723(4) 0.2244(4) 0.103(2) Uani 1 1 d . . .
H18 H 0.5016 0.2250 0.2599 0.123 Uiso 1 1 calc R . .
C19 C 0.7401(6) 0.2094(3) 0.3216(3) 0.0722(16) Uani 1 1 d . . .
C20 C 0.6409(7) 0.2273(4) 0.3663(4) 0.098(2) Uani 1 1 d . . .
H20 H 0.5774 0.2731 0.3493 0.118 Uiso 1 1 calc R . .
C21 C 0.6307(10) 0.1828(6) 0.4327(4) 0.122(3) Uani 1 1 d . . .
H21 H 0.5627 0.1985 0.4598 0.147 Uiso 1 1 calc R . .
C22 C 0.7191(11) 0.1158(6) 0.4591(4) 0.120(3) Uani 1 1 d . . .
H22 H 0.7120 0.0846 0.5045 0.144 Uiso 1 1 calc R . .
C23 C 0.8200(9) 0.0932(4) 0.4189(5) 0.117(3) Uani 1 1 d . . .
H23 H 0.8809 0.0465 0.4368 0.140 Uiso 1 1 calc R . .
C24 C 0.8310(7) 0.1416(4) 0.3499(4) 0.0912(19) Uani 1 1 d . . .
H24 H 0.9014 0.1270 0.3234 0.109 Uiso 1 1 calc R . .
C25 C 0.4523(6) 0.2700(3) 0.7392(3) 0.0701(15) Uani 1 1 d . . .
C26 C 0.4408(6) 0.3392(4) 0.7519(3) 0.0797(17) Uani 1 1 d . . .
H26 H 0.3561 0.3668 0.7571 0.096 Uiso 1 1 calc R . .
C27 C 0.5504(10) 0.3687(5) 0.7570(3) 0.105(2) Uani 1 1 d . . .
H27 H 0.5379 0.4158 0.7640 0.125 Uiso 1 1 calc R . .
C28 C 0.6751(9) 0.3286(6) 0.7519(4) 0.113(3) Uani 1 1 d . . .
H28 H 0.7477 0.3485 0.7558 0.135 Uiso 1 1 calc R . .
C29 C 0.6965(7) 0.2596(5) 0.7412(4) 0.110(2) Uani 1 1 d . . .
H29 H 0.7823 0.2323 0.7375 0.132 Uiso 1 1 calc R . .
C30 C 0.5834(7) 0.2308(4) 0.7358(3) 0.0903(19) Uani 1 1 d . . .
H30 H 0.5974 0.1832 0.7297 0.108 Uiso 1 1 calc R . .
C31 C 0.3482(5) 0.1699(3) 0.7007(3) 0.0686(15) Uani 1 1 d . . .
C32 C 0.4222(6) 0.1762(4) 0.6409(3) 0.091(2) Uani 1 1 d . . .
H32 H 0.4597 0.2191 0.6206 0.110 Uiso 1 1 calc R . .
C33 C 0.4408(8) 0.1179(6) 0.6106(4) 0.119(3) Uani 1 1 d . . .
H33 H 0.4926 0.1221 0.5715 0.142 Uiso 1 1 calc R . .
C34 C 0.3842(10) 0.0569(5) 0.6379(5) 0.121(3) Uani 1 1 d . . .
H34 H 0.3969 0.0192 0.6175 0.145 Uiso 1 1 calc R . .
C35 C 0.3095(9) 0.0495(4) 0.6944(5) 0.109(2) Uani 1 1 d . . .
H35 H 0.2703 0.0070 0.7131 0.131 Uiso 1 1 calc R . .
C36 C 0.2915(6) 0.1057(4) 0.7246(3) 0.0850(18) Uani 1 1 d . . .
H36 H 0.2380 0.1001 0.7633 0.102 Uiso 1 1 calc R . .
C37 C 0.2054(5) 0.3088(3) 0.6859(3) 0.0618(14) Uani 1 1 d . . .
C38 C 0.2355(6) 0.3730(3) 0.6355(3) 0.0736(16) Uani 1 1 d . . .
H38 H 0.3237 0.3779 0.6304 0.088 Uiso 1 1 calc R . .
C39 C 0.1395(8) 0.4307(4) 0.5922(3) 0.0879(19) Uani 1 1 d . . .
H39 H 0.1642 0.4730 0.5588 0.105 Uiso 1 1 calc R . .
C40 C 0.0096(8) 0.4254(4) 0.5987(4) 0.091(2) Uani 1 1 d . . .
H40 H -0.0554 0.4646 0.5707 0.109 Uiso 1 1 calc R . .
C41 C -0.0242(6) 0.3626(4) 0.6461(4) 0.0873(19) Uani 1 1 d . . .
H41 H -0.1126 0.3581 0.6502 0.105 Uiso 1 1 calc R . .
C42 C 0.0716(6) 0.3054(4) 0.6884(3) 0.0763(16) Uani 1 1 d . . .
H42 H 0.0457 0.2625 0.7202 0.092 Uiso 1 1 calc R . .
C43 C 0.2763(5) 0.2058(3) 0.8150(3) 0.0632(14) Uani 1 1 d . . .
C44 C 0.1725(6) 0.2438(4) 0.8456(3) 0.0802(17) Uani 1 1 d . . .
H44 H 0.1203 0.2906 0.8189 0.096 Uiso 1 1 calc R . .
C45 C 0.1450(7) 0.2136(5) 0.9152(4) 0.098(2) Uani 1 1 d . . .
H45 H 0.0759 0.2409 0.9342 0.118 Uiso 1 1 calc R . .
C46 C 0.2169(8) 0.1454(5) 0.9555(4) 0.104(2) Uani 1 1 d . . .
H46 H 0.1967 0.1251 1.0018 0.125 Uiso 1 1 calc R . .
C47 C 0.3184(8) 0.1069(4) 0.9280(4) 0.099(2) Uani 1 1 d . . .
H47 H 0.3690 0.0600 0.9555 0.119 Uiso 1 1 calc R . .
C48 C 0.3477(6) 0.1365(4) 0.8593(3) 0.0788(17) Uani 1 1 d . . .
H48 H 0.4188 0.1087 0.8419 0.095 Uiso 1 1 calc R . .
C49 C 0.1626(7) 0.2968(4) 0.4938(4) 0.103(2) Uani 1 1 d . . .
H49A H 0.1275 0.3273 0.5228 0.124 Uiso 1 1 calc R . .
H49B H 0.2448 0.2620 0.5149 0.124 Uiso 1 1 calc R . .
C50 C 0.1950(8) 0.3504(4) 0.4253(4) 0.119(3) Uani 1 1 d . . .
H50A H 0.2134 0.3220 0.3936 0.143 Uiso 1 1 calc R . .
H50B H 0.1169 0.3914 0.4082 0.143 Uiso 1 1 calc R . .
C51 C 0.3102(9) 0.3863(5) 0.4249(5) 0.138(3) Uani 1 1 d . . .
H51A H 0.3885 0.3455 0.4424 0.166 Uiso 1 1 calc R . .
H51B H 0.2916 0.4158 0.4557 0.166 Uiso 1 1 calc R . .
C52 C 0.3399(10) 0.4383(6) 0.3551(6) 0.167(4) Uani 1 1 d . . .
H52A H 0.3641 0.4088 0.3250 0.251 Uiso 1 1 calc R . .
H52B H 0.4122 0.4612 0.3585 0.251 Uiso 1 1 calc R . .
H52C H 0.2624 0.4783 0.3371 0.251 Uiso 1 1 calc R . .
C53 C 0.1079(10) 0.1829(6) 0.4393(5) 0.138(3) Uani 1 1 d D . .
H53A H 0.0462 0.1495 0.4440 0.165 Uiso 1 1 calc R . .
H53B H 0.1011 0.2179 0.3921 0.165 Uiso 1 1 calc R . .
C54 C 0.2354(12) 0.1365(6) 0.4486(7) 0.190(5) Uani 1 1 d D . .
H54A H 0.2431 0.1030 0.4963 0.228 Uiso 1 1 calc R . .
H54B H 0.2970 0.1703 0.4422 0.228 Uiso 1 1 calc R . .
C55 C 0.2824(18) 0.0889(8) 0.4086(7) 0.247(8) Uani 1 1 d D . .
H55A H 0.3642 0.0540 0.4299 0.296 Uiso 1 1 calc R . .
H55B H 0.2180 0.0574 0.4124 0.296 Uiso 1 1 calc R . .
C56 C 0.307(2) 0.1213(10) 0.3401(9) 0.319(11) Uani 1 1 d D . .
H56A H 0.2789 0.1766 0.3263 0.478 Uiso 1 1 calc R . .
H56B H 0.2592 0.1024 0.3140 0.478 Uiso 1 1 calc R . .
H56C H 0.4009 0.1078 0.3321 0.478 Uiso 1 1 calc R . .
C57 C -0.1106(8) 0.2934(5) 0.4569(5) 0.138(3) Uani 1 1 d U . .
H57A H -0.0990 0.3283 0.4109 0.166 Uiso 1 1 calc R . .
H57B H -0.1614 0.2577 0.4530 0.166 Uiso 1 1 calc R . .
C58 C -0.1881(10) 0.3395(6) 0.4987(6) 0.165(3) Uani 1 1 d U . .
H58A H -0.1717 0.3083 0.5468 0.198 Uiso 1 1 calc R . .
H58B H -0.1505 0.3846 0.4902 0.198 Uiso 1 1 calc R . .
C59 C -0.3258(12) 0.3654(8) 0.4894(8) 0.199(4) Uani 1 1 d U . .
H59A H -0.3640 0.3221 0.4916 0.239 Uiso 1 1 calc R . .
H59B H -0.3438 0.4036 0.4438 0.239 Uiso 1 1 calc R . .
C60 C -0.3942(11) 0.4002(8) 0.5409(8) 0.213(5) Uani 1 1 d U . .
H60A H -0.4013 0.3598 0.5836 0.320 Uiso 1 1 calc R . .
H60B H -0.4816 0.4293 0.5242 0.320 Uiso 1 1 calc R . .
H60C H -0.3435 0.4338 0.5477 0.320 Uiso 1 1 calc R . .
C61 C 0.0342(8) 0.1804(5) 0.5805(4) 0.121(3) Uani 1 1 d D . .
H61A H 0.1227 0.1510 0.5970 0.145 Uiso 1 1 calc R . .
H61B H 0.0039 0.2138 0.6074 0.145 Uiso 1 1 calc R . .
C62 C -0.0528(10) 0.1264(5) 0.5948(5) 0.148(4) Uani 1 1 d D . .
H62A H -0.0206 0.0896 0.5713 0.177 Uiso 1 1 calc R . .
H62B H -0.1418 0.1542 0.5777 0.177 Uiso 1 1 calc R . .
C63 C -0.0575(16) 0.0852(9) 0.6684(7) 0.248(8) Uani 1 1 d D . .
H63A H 0.0316 0.0566 0.6845 0.298 Uiso 1 1 calc R . .
H63B H -0.0851 0.1228 0.6915 0.298 Uiso 1 1 calc R . .
C64 C -0.1431(16) 0.0339(10) 0.6872(9) 0.301(10) Uani 1 1 d D . .
H64A H -0.2014 0.0438 0.7226 0.452 Uiso 1 1 calc R . .
H64B H -0.0918 -0.0182 0.7039 0.452 Uiso 1 1 calc R . .
H64C H -0.1948 0.0408 0.6480 0.452 Uiso 1 1 calc R . .
C65 C 0.6795(7) 0.3094(5) 0.9858(4) 0.113(2) Uani 1 1 d . . .
H65A H 0.6368 0.3450 1.0091 0.136 Uiso 1 1 calc R . .
H65B H 0.7583 0.2769 1.0122 0.136 Uiso 1 1 calc R . .
C66 C 0.7214(8) 0.3547(5) 0.9170(5) 0.127(3) Uani 1 1 d . . .
H66A H 0.6433 0.3898 0.8916 0.152 Uiso 1 1 calc R . .
H66B H 0.7588 0.3196 0.8925 0.152 Uiso 1 1 calc R . .
C67 C 0.8206(8) 0.4004(5) 0.9179(5) 0.125(3) Uani 1 1 d . . .
H67A H 0.8978 0.3659 0.9446 0.151 Uiso 1 1 calc R . .
H67B H 0.7821 0.4375 0.9403 0.151 Uiso 1 1 calc R . .
C68 C 0.8640(10) 0.4424(6) 0.8477(6) 0.154(4) Uani 1 1 d . . .
H68A H 0.9132 0.4057 0.8277 0.232 Uiso 1 1 calc R . .
H68B H 0.9195 0.4757 0.8505 0.232 Uiso 1 1 calc R . .
H68C H 0.7872 0.4728 0.8197 0.232 Uiso 1 1 calc R . .
C69 C 0.6368(11) 0.1822(6) 0.9404(5) 0.158(3) Uani 1 1 d DU . .
H69A H 0.5753 0.1487 0.9451 0.190 Uiso 1 1 calc R . .
H69B H 0.6394 0.2123 0.8920 0.190 Uiso 1 1 calc R . .
C70 C 0.7678(12) 0.1333(7) 0.9602(7) 0.194(4) Uani 1 1 d DU . .
H70A H 0.8319 0.1661 0.9502 0.233 Uiso 1 1 calc R . .
H70B H 0.7691 0.1069 1.0095 0.233 Uiso 1 1 calc R . .
C71 C 0.8113(15) 0.0758(9) 0.9274(8) 0.225(5) Uani 1 1 d DU . .
H71A H 0.8289 0.0253 0.9630 0.270 Uiso 1 1 calc R . .
H71B H 0.7382 0.0778 0.8995 0.270 Uiso 1 1 calc R . .
C72 C 0.9243(17) 0.0823(10) 0.8859(9) 0.290(7) Uani 1 1 d DU . .
H72A H 0.9257 0.1360 0.8633 0.435 Uiso 1 1 calc R . .
H72B H 0.9216 0.0587 0.8520 0.435 Uiso 1 1 calc R . .
H72C H 1.0030 0.0568 0.9138 0.435 Uiso 1 1 calc R . .
C73 C 0.4209(9) 0.3033(6) 0.9383(4) 0.135(3) Uani 1 1 d . . .
H73A H 0.4453 0.3266 0.8908 0.162 Uiso 1 1 calc R . .
H73B H 0.3643 0.2684 0.9392 0.162 Uiso 1 1 calc R . .
C74 C 0.3401(9) 0.3669(7) 0.9626(5) 0.159(4) Uani 1 1 d . . .
H74A H 0.3999 0.3978 0.9673 0.191 Uiso 1 1 calc R . .
H74B H 0.3070 0.3428 1.0080 0.191 Uiso 1 1 calc R . .
C75 C 0.2207(11) 0.4223(7) 0.9176(5) 0.163(4) Uani 1 1 d . . .
H75A H 0.2529 0.4458 0.8718 0.196 Uiso 1 1 calc R . .
H75B H 0.1591 0.3919 0.9140 0.196 Uiso 1 1 calc R . .
C76 C 0.1506(12) 0.4814(6) 0.9410(7) 0.189(5) Uani 1 1 d . . .
H76A H 0.1122 0.4590 0.9849 0.283 Uiso 1 1 calc R . .
H76B H 0.0811 0.5138 0.9087 0.283 Uiso 1 1 calc R . .
H76C H 0.2104 0.5117 0.9454 0.283 Uiso 1 1 calc R . .
C77 C 0.5409(9) 0.1980(5) 1.0734(4) 0.124(3) Uani 1 1 d . . .
H77A H 0.6268 0.1689 1.0942 0.149 Uiso 1 1 calc R . .
H77B H 0.5063 0.2356 1.0957 0.149 Uiso 1 1 calc R . .
C78 C 0.4501(10) 0.1441(6) 1.0878(4) 0.151(4) Uani 1 1 d . . .
H78A H 0.4741 0.1126 1.0587 0.181 Uiso 1 1 calc R . .
H78B H 0.3601 0.1740 1.0755 0.181 Uiso 1 1 calc R . .
C79 C 0.4516(13) 0.0922(7) 1.1603(6) 0.175(4) Uani 1 1 d . . .
H79A H 0.5422 0.0636 1.1729 0.210 Uiso 1 1 calc R . .
H79B H 0.4253 0.1238 1.1892 0.210 Uiso 1 1 calc R . .
C80 C 0.3676(12) 0.0387(6) 1.1747(6) 0.183(5) Uani 1 1 d . . .
H80A H 0.2762 0.0658 1.1717 0.274 Uiso 1 1 calc R . .
H80B H 0.3863 0.0018 1.2202 0.274 Uiso 1 1 calc R . .
H80C H 0.3835 0.0122 1.1421 0.274 Uiso 1 1 calc R . .
P1 P 0.04798(19) 0.24066(11) 0.49302(10) 0.0953(7) Uani 1 1 d . . .
P2 P 0.5664(2) 0.24870(13) 0.98532(11) 0.1098(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C19 1.632(9) . ?
B1 C7 1.634(9) . ?
B1 C13 1.641(9) . ?
B1 C1 1.642(9) . ?
B2 C25 1.620(8) . ?
B2 C43 1.630(8) . ?
B2 C37 1.646(8) . ?
B2 C31 1.654(8) . ?
C1 C2 1.373(8) . ?
C1 C6 1.376(8) . ?
C2 C3 1.404(9) . ?
C3 C4 1.344(10) . ?
C4 C5 1.364(11) . ?
C5 C6 1.368(9) . ?
C7 C12 1.382(8) . ?
C7 C8 1.383(8) . ?
C8 C9 1.389(9) . ?
C9 C10 1.345(11) . ?
C10 C11 1.334(10) . ?
C11 C12 1.395(9) . ?
C13 C14 1.375(9) . ?
C13 C18 1.408(9) . ?
C14 C15 1.410(10) . ?
C15 C16 1.363(12) . ?
C16 C17 1.339(12) . ?
C17 C18 1.379(10) . ?
C19 C24 1.369(8) . ?
C19 C20 1.397(8) . ?
C20 C21 1.354(10) . ?
C21 C22 1.341(11) . ?
C22 C23 1.372(11) . ?
C23 C24 1.420(10) . ?
C25 C30 1.396(8) . ?
C25 C26 1.400(8) . ?
C26 C27 1.394(9) . ?
C27 C28 1.355(10) . ?
C28 C29 1.365(10) . ?
C29 C30 1.420(10) . ?
C31 C36 1.386(8) . ?
C31 C32 1.395(8) . ?
C32 C33 1.421(10) . ?
C33 C34 1.339(11) . ?
C34 C35 1.340(11) . ?
C35 C36 1.385(9) . ?
C37 C38 1.380(7) . ?
C37 C42 1.392(7) . ?
C38 C39 1.389(8) . ?
C39 C40 1.360(9) . ?
C40 C41 1.350(9) . ?
C41 C42 1.376(8) . ?
C43 C48 1.387(7) . ?
C43 C44 1.393(7) . ?
C44 C45 1.391(9) . ?
C45 C46 1.347(9) . ?
C46 C47 1.345(10) . ?
C47 C48 1.378(8) . ?
C49 C50 1.498(10) . ?
C49 P1 1.762(7) . ?
C50 C51 1.493(11) . ?
C51 C52 1.498(12) . ?
C53 C54 1.389(9) . ?
C53 P1 1.806(9) . ?
C54 C55 1.414(9) . ?
C55 C56 1.369(10) . ?
C57 C58 1.505(12) . ?
C57 P1 1.773(8) . ?
C58 C59 1.397(13) . ?
C59 C60 1.498(15) . ?
C61 C62 1.449(9) . ?
C61 P1 1.793(8) . ?
C62 C63 1.457(11) . ?
C63 C64 1.394(11) . ?
C65 C66 1.480(10) . ?
C65 P2 1.814(7) . ?
C66 C67 1.484(10) . ?
C67 C68 1.489(12) . ?
C69 C70 1.448(10) . ?
C69 P2 1.812(10) . ?
C70 C71 1.448(10) . ?
C71 C72 1.403(11) . ?
C73 C74 1.518(12) . ?
C73 P2 1.753(9) . ?
C74 C75 1.542(12) . ?
C75 C76 1.403(13) . ?
C77 C78 1.478(11) . ?
C77 P2 1.777(8) . ?
C78 C79 1.483(12) . ?
C79 C80 1.418(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 B1 C7 111.8(5) . . ?
C19 B1 C13 111.8(5) . . ?
C7 B1 C13 104.6(5) . . ?
C19 B1 C1 104.1(5) . . ?
C7 B1 C1 114.0(5) . . ?
C13 B1 C1 110.6(5) . . ?
C25 B2 C43 103.5(4) . . ?
C25 B2 C37 110.8(4) . . ?
C43 B2 C37 113.6(4) . . ?
C25 B2 C31 113.1(4) . . ?
C43 B2 C31 110.6(4) . . ?
C37 B2 C31 105.5(4) . . ?
C2 C1 C6 115.2(6) . . ?
C2 C1 B1 122.0(6) . . ?
C6 C1 B1 122.5(5) . . ?
C1 C2 C3 122.8(7) . . ?
C4 C3 C2 119.5(7) . . ?
C3 C4 C5 119.1(7) . . ?
C4 C5 C6 120.8(8) . . ?
C5 C6 C1 122.5(7) . . ?
C12 C7 C8 114.7(6) . . ?
C12 C7 B1 120.4(6) . . ?
C8 C7 B1 124.8(6) . . ?
C7 C8 C9 121.7(7) . . ?
C10 C9 C8 121.2(7) . . ?
C11 C10 C9 119.5(8) . . ?
C10 C11 C12 119.9(8) . . ?
C7 C12 C11 123.0(7) . . ?
C14 C13 C18 114.3(6) . . ?
C14 C13 B1 121.5(6) . . ?
C18 C13 B1 124.0(6) . . ?
C13 C14 C15 123.2(8) . . ?
C16 C15 C14 119.3(9) . . ?
C17 C16 C15 119.3(9) . . ?
C16 C17 C18 121.6(9) . . ?
C17 C18 C13 122.2(8) . . ?
C24 C19 C20 114.8(6) . . ?
C24 C19 B1 124.1(6) . . ?
C20 C19 B1 121.0(6) . . ?
C21 C20 C19 124.6(7) . . ?
C22 C21 C20 119.7(8) . . ?
C21 C22 C23 119.9(8) . . ?
C22 C23 C24 119.7(7) . . ?
C19 C24 C23 121.3(7) . . ?
C30 C25 C26 114.2(6) . . ?
C30 C25 B2 125.6(6) . . ?
C26 C25 B2 120.1(5) . . ?
C27 C26 C25 123.0(7) . . ?
C28 C27 C26 119.8(8) . . ?
C27 C28 C29 121.4(8) . . ?
C28 C29 C30 117.8(7) . . ?
C25 C30 C29 123.7(7) . . ?
C36 C31 C32 114.8(6) . . ?
C36 C31 B2 123.5(5) . . ?
C32 C31 B2 121.4(6) . . ?
C31 C32 C33 120.7(7) . . ?
C34 C33 C32 120.5(8) . . ?
C33 C34 C35 120.8(8) . . ?
C34 C35 C36 119.2(8) . . ?
C35 C36 C31 123.9(7) . . ?
C38 C37 C42 114.5(5) . . ?
C38 C37 B2 122.6(5) . . ?
C42 C37 B2 122.8(5) . . ?
C37 C38 C39 122.8(6) . . ?
C40 C39 C38 120.0(6) . . ?
C41 C40 C39 119.3(6) . . ?
C40 C41 C42 120.3(6) . . ?
C41 C42 C37 123.1(6) . . ?
C48 C43 C44 114.6(5) . . ?
C48 C43 B2 120.4(5) . . ?
C44 C43 B2 124.9(5) . . ?
C45 C44 C43 121.6(6) . . ?
C46 C45 C44 121.1(7) . . ?
C47 C46 C45 119.1(7) . . ?
C46 C47 C48 120.5(7) . . ?
C47 C48 C43 123.1(6) . . ?
C50 C49 P1 116.1(6) . . ?
C51 C50 C49 115.4(7) . . ?
C50 C51 C52 113.4(9) . . ?
C54 C53 P1 120.6(8) . . ?
C53 C54 C55 121.4(13) . . ?
C56 C55 C54 120.2(15) . . ?
C58 C57 P1 112.8(7) . . ?
C59 C58 C57 119.5(11) . . ?
C58 C59 C60 114.4(12) . . ?
C62 C61 P1 117.8(6) . . ?
C61 C62 C63 110.5(10) . . ?
C64 C63 C62 114.5(15) . . ?
C66 C65 P2 114.8(6) . . ?
C65 C66 C67 114.5(7) . . ?
C66 C67 C68 112.6(8) . . ?
C70 C69 P2 119.0(8) . . ?
C71 C70 C69 115.8(12) . . ?
C72 C71 C70 116.8(15) . . ?
C74 C73 P2 116.1(6) . . ?
C73 C74 C75 117.5(8) . . ?
C76 C75 C74 115.7(9) . . ?
C78 C77 P2 116.2(6) . . ?
C77 C78 C79 114.4(9) . . ?
C80 C79 C78 115.2(10) . . ?
C49 P1 C57 115.6(4) . . ?
C49 P1 C61 106.0(4) . . ?
C57 P1 C61 111.2(4) . . ?
C49 P1 C53 110.2(4) . . ?
C57 P1 C53 103.0(5) . . ?
C61 P1 C53 110.9(4) . . ?
C73 P2 C77 114.9(4) . . ?
C73 P2 C69 103.4(5) . . ?
C77 P2 C69 111.0(5) . . ?
C73 P2 C65 111.4(4) . . ?
C77 P2 C65 105.0(4) . . ?
C69 P2 C65 111.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.100
####################################################################### 
# 
# 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_1_alpha_394K
_database_code_depnum_ccdc_archive 'CCDC 986257'
_audit_update_record             
;
2014-02-11 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H56 B P'
_chemical_formula_weight         578.63

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5582(11)
_cell_length_b                   19.131(2)
_cell_length_c                   20.915(2)
_cell_angle_alpha                68.892(2)
_cell_angle_beta                 85.501(3)
_cell_angle_gamma                77.175(2)
_cell_volume                     3842.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    394
_cell_measurement_reflns_used    1992
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      17.15

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9577
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_process_details   
;
SADABS; sheldrick, 1996
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      394
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22471
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.04
_diffrn_reflns_theta_max         25.02
_reflns_number_total             13522
_reflns_number_gt                3496
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1994P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13522
_refine_ls_number_parameters     765
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.2774
_refine_ls_R_factor_gt           0.0960
_refine_ls_wR_factor_ref         0.3982
_refine_ls_wR_factor_gt          0.2660
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_restrained_S_all      0.907
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.7595(6) 0.2663(4) 0.2427(3) 0.1061(19) Uani 1 1 d . . .
B2 B 0.3173(6) 0.2406(3) 0.7344(3) 0.0942(17) Uani 1 1 d . . .
C1 C 0.8238(8) 0.3316(4) 0.2506(3) 0.1115(17) Uani 1 1 d . . .
C2 C 0.7521(7) 0.3940(4) 0.2644(3) 0.145(2) Uani 1 1 d . . .
H2 H 0.6620 0.4010 0.2650 0.174 Uiso 1 1 calc R . .
C3 C 0.8070(12) 0.4468(5) 0.2774(4) 0.172(3) Uani 1 1 d . . .
H3 H 0.7541 0.4871 0.2878 0.206 Uiso 1 1 calc R . .
C4 C 0.9362(14) 0.4401(6) 0.2751(4) 0.176(4) Uani 1 1 d . . .
H4 H 0.9731 0.4762 0.2829 0.212 Uiso 1 1 calc R . .
C5 C 1.0127(9) 0.3801(7) 0.2612(4) 0.162(3) Uani 1 1 d . . .
H5 H 1.1024 0.3751 0.2585 0.194 Uiso 1 1 calc R . .
C6 C 0.9548(9) 0.3264(4) 0.2512(3) 0.134(2) Uani 1 1 d . . .
H6 H 1.0088 0.2840 0.2445 0.161 Uiso 1 1 calc R . .
C7 C 0.8382(6) 0.2246(4) 0.1913(3) 0.1080(16) Uani 1 1 d . . .
C8 C 0.9200(7) 0.2553(4) 0.1398(4) 0.138(2) Uani 1 1 d . . .
H8 H 0.9335 0.3037 0.1340 0.166 Uiso 1 1 calc R . .
C9 C 0.9840(8) 0.2199(6) 0.0957(4) 0.171(3) Uani 1 1 d . . .
H9 H 1.0395 0.2437 0.0623 0.206 Uiso 1 1 calc R . .
C10 C 0.9649(9) 0.1503(7) 0.1019(5) 0.174(3) Uani 1 1 d . . .
H10 H 1.0076 0.1257 0.0728 0.208 Uiso 1 1 calc R . .
C11 C 0.8831(9) 0.1163(4) 0.1506(5) 0.161(3) Uani 1 1 d . . .
H11 H 0.8687 0.0686 0.1549 0.194 Uiso 1 1 calc R . .
C12 C 0.8198(6) 0.1545(4) 0.1949(3) 0.132(2) Uani 1 1 d . . .
H12 H 0.7633 0.1309 0.2279 0.159 Uiso 1 1 calc R . .
C13 C 0.6142(7) 0.3029(4) 0.2085(4) 0.1209(19) Uani 1 1 d . . .
C14 C 0.5926(9) 0.3711(6) 0.1531(5) 0.162(3) Uani 1 1 d . . .
H14 H 0.6598 0.3972 0.1365 0.194 Uiso 1 1 calc R . .
C15 C 0.4635(14) 0.4026(6) 0.1205(5) 0.201(4) Uani 1 1 d . . .
H15 H 0.4512 0.4487 0.0836 0.241 Uiso 1 1 calc R . .
C16 C 0.3621(14) 0.3672(10) 0.1420(8) 0.231(7) Uani 1 1 d . . .
H16 H 0.2811 0.3877 0.1208 0.277 Uiso 1 1 calc R . .
C17 C 0.3845(11) 0.3015(8) 0.1950(7) 0.199(5) Uani 1 1 d . . .
H17 H 0.3165 0.2762 0.2114 0.239 Uiso 1 1 calc R . .
C18 C 0.5053(10) 0.2687(4) 0.2272(4) 0.155(2) Uani 1 1 d . . .
H18 H 0.5142 0.2217 0.2629 0.186 Uiso 1 1 calc R . .
C19 C 0.7519(7) 0.2065(4) 0.3199(3) 0.1158(17) Uani 1 1 d . . .
C20 C 0.6555(7) 0.2235(4) 0.3664(4) 0.152(2) Uani 1 1 d . . .
H20 H 0.5921 0.2682 0.3510 0.182 Uiso 1 1 calc R . .
C21 C 0.6535(13) 0.1745(8) 0.4350(6) 0.214(5) Uani 1 1 d . . .
H21 H 0.5900 0.1880 0.4643 0.257 Uiso 1 1 calc R . .
C22 C 0.7407(15) 0.1093(7) 0.4587(6) 0.213(6) Uani 1 1 d . . .
H22 H 0.7373 0.0769 0.5040 0.255 Uiso 1 1 calc R . .
C23 C 0.8347(11) 0.0904(5) 0.4162(6) 0.185(3) Uani 1 1 d . . .
H23 H 0.8958 0.0447 0.4324 0.222 Uiso 1 1 calc R . .
C24 C 0.8404(8) 0.1395(5) 0.3477(4) 0.143(2) Uani 1 1 d . . .
H24 H 0.9073 0.1257 0.3200 0.171 Uiso 1 1 calc R . .
C25 C 0.4425(6) 0.2734(4) 0.7375(3) 0.1152(17) Uani 1 1 d . . .
C26 C 0.4281(7) 0.3427(5) 0.7484(3) 0.1338(19) Uani 1 1 d U . .
H26 H 0.3441 0.3688 0.7524 0.161 Uiso 1 1 calc R . .
C27 C 0.5296(11) 0.3753(5) 0.7535(4) 0.161(3) Uani 1 1 d U . .
H27 H 0.5137 0.4220 0.7600 0.194 Uiso 1 1 calc R . .
C28 C 0.6533(11) 0.3376(7) 0.7487(4) 0.174(3) Uani 1 1 d . . .
H28 H 0.7224 0.3591 0.7516 0.208 Uiso 1 1 calc R . .
C29 C 0.6773(8) 0.2688(7) 0.7398(4) 0.178(3) Uani 1 1 d . . .
H29 H 0.7622 0.2430 0.7372 0.213 Uiso 1 1 calc R . .
C30 C 0.5724(8) 0.2374(4) 0.7345(3) 0.144(2) Uani 1 1 d . . .
H30 H 0.5900 0.1902 0.7288 0.173 Uiso 1 1 calc R . .
C31 C 0.3465(5) 0.1742(4) 0.6987(3) 0.1106(17) Uani 1 1 d . . .
C32 C 0.4188(7) 0.1833(4) 0.6397(4) 0.161(3) Uani 1 1 d . . .
H32 H 0.4550 0.2265 0.6213 0.193 Uiso 1 1 calc R . .
C33 C 0.4409(11) 0.1280(7) 0.6050(5) 0.196(4) Uani 1 1 d . . .
H33 H 0.4903 0.1345 0.5652 0.235 Uiso 1 1 calc R . .
C34 C 0.3861(13) 0.0676(8) 0.6337(6) 0.222(6) Uani 1 1 d . . .
H34 H 0.4026 0.0310 0.6128 0.267 Uiso 1 1 calc R . .
C35 C 0.3099(10) 0.0536(4) 0.6892(5) 0.181(3) Uani 1 1 d . . .
H35 H 0.2717 0.0111 0.7055 0.217 Uiso 1 1 calc R . .
C36 C 0.2923(7) 0.1088(5) 0.7209(3) 0.145(2) Uani 1 1 d . . .
H36 H 0.2403 0.1013 0.7598 0.174 Uiso 1 1 calc R . .
C37 C 0.2032(6) 0.3082(3) 0.6871(3) 0.1000(15) Uani 1 1 d . . .
C38 C 0.2291(6) 0.3728(4) 0.6359(3) 0.1210(18) Uani 1 1 d . . .
H38 H 0.3148 0.3788 0.6291 0.145 Uiso 1 1 calc R . .
C39 C 0.1357(11) 0.4285(4) 0.5947(4) 0.148(2) Uani 1 1 d . . .
H39 H 0.1587 0.4713 0.5614 0.178 Uiso 1 1 calc R . .
C40 C 0.0061(11) 0.4220(5) 0.6018(4) 0.156(3) Uani 1 1 d . . .
H40 H -0.0578 0.4604 0.5742 0.188 Uiso 1 1 calc R . .
C41 C -0.0252(7) 0.3580(6) 0.6503(5) 0.143(2) Uani 1 1 d . . .
H41 H -0.1106 0.3516 0.6553 0.172 Uiso 1 1 calc R . .
C42 C 0.0732(8) 0.3022(4) 0.6926(3) 0.1235(18) Uani 1 1 d . . .
H42 H 0.0506 0.2593 0.7258 0.148 Uiso 1 1 calc R . .
C43 C 0.2757(6) 0.2051(4) 0.8147(3) 0.1035(15) Uani 1 1 d . . .
C44 C 0.1772(6) 0.2410(3) 0.8472(3) 0.1219(18) Uani 1 1 d . . .
H44 H 0.1280 0.2883 0.8213 0.146 Uiso 1 1 calc R . .
C45 C 0.1483(8) 0.2106(6) 0.9157(4) 0.155(3) Uani 1 1 d . . .
H45 H 0.0802 0.2364 0.9349 0.186 Uiso 1 1 calc R . .
C46 C 0.2217(10) 0.1413(7) 0.9552(4) 0.169(3) Uani 1 1 d . . .
H46 H 0.2024 0.1202 1.0015 0.202 Uiso 1 1 calc R . .
C47 C 0.3214(8) 0.1037(4) 0.9275(4) 0.154(2) Uani 1 1 d . . .
H47 H 0.3720 0.0574 0.9544 0.185 Uiso 1 1 calc R . .
C48 C 0.3466(6) 0.1361(4) 0.8578(3) 0.1251(19) Uani 1 1 d . . .
H48 H 0.4151 0.1098 0.8390 0.150 Uiso 1 1 calc R . .
C49 C 0.1601(8) 0.2977(5) 0.4917(5) 0.175(3) Uani 1 1 d . . .
H49A H 0.1277 0.3270 0.5212 0.210 Uiso 1 1 calc R . .
H49B H 0.2393 0.2623 0.5125 0.210 Uiso 1 1 calc R . .
C50 C 0.1940(11) 0.3504(5) 0.4262(5) 0.212(4) Uani 1 1 d . . .
H50A H 0.1194 0.3922 0.4102 0.255 Uiso 1 1 calc R . .
H50B H 0.2080 0.3237 0.3938 0.255 Uiso 1 1 calc R . .
C51 C 0.3111(10) 0.3848(7) 0.4234(7) 0.252(5) Uani 1 1 d . . .
H51A H 0.2959 0.4142 0.4536 0.302 Uiso 1 1 calc R . .
H51B H 0.3857 0.3435 0.4410 0.302 Uiso 1 1 calc R . .
C52 C 0.3432(12) 0.4346(7) 0.3552(7) 0.291(7) Uani 1 1 d . . .
H52A H 0.3457 0.4090 0.3230 0.437 Uiso 1 1 calc R . .
H52B H 0.4266 0.4463 0.3566 0.437 Uiso 1 1 calc R . .
H52C H 0.2785 0.4813 0.3411 0.437 Uiso 1 1 calc R . .
C53 C 0.1027(12) 0.1884(6) 0.4379(5) 0.242(5) Uani 1 1 d . . .
H53A H 0.0399 0.1572 0.4412 0.290 Uiso 1 1 calc R . .
H53B H 0.0985 0.2245 0.3911 0.290 Uiso 1 1 calc R . .
C54 C 0.2235(17) 0.1406(7) 0.4460(7) 0.349(7) Uani 1 1 d DU . .
H54A H 0.2209 0.1046 0.4924 0.419 Uiso 1 1 calc R . .
H54B H 0.2811 0.1729 0.4480 0.419 Uiso 1 1 calc R . .
C55 C 0.3074(16) 0.0893(7) 0.4060(7) 0.366(7) Uani 1 1 d DU . .
H55A H 0.3987 0.0908 0.4055 0.440 Uiso 1 1 calc R . .
H55B H 0.2977 0.0365 0.4263 0.440 Uiso 1 1 calc R . .
C56 C 0.251(2) 0.1258(10) 0.3370(7) 0.474(10) Uani 1 1 d DU . .
H56A H 0.2412 0.1804 0.3231 0.711 Uiso 1 1 calc R . .
H56B H 0.1682 0.1133 0.3371 0.711 Uiso 1 1 calc R . .
H56C H 0.3081 0.1077 0.3055 0.711 Uiso 1 1 calc R . .
C57 C -0.1128(9) 0.2952(5) 0.4559(5) 0.206(3) Uani 1 1 d . . .
H57A H -0.1017 0.3285 0.4091 0.247 Uiso 1 1 calc R . .
H57B H -0.1622 0.2587 0.4541 0.247 Uiso 1 1 calc R . .
C58 C -0.1862(13) 0.3405(6) 0.4930(7) 0.258(5) Uani 1 1 d D . .
H58A H -0.1769 0.3098 0.5414 0.310 Uiso 1 1 calc R . .
H58B H -0.1455 0.3836 0.4854 0.310 Uiso 1 1 calc R . .
C59 C -0.3212(14) 0.3702(10) 0.4792(10) 0.346(9) Uani 1 1 d . . .
H59A H -0.3314 0.4081 0.4333 0.416 Uiso 1 1 calc R . .
H59B H -0.3612 0.3289 0.4800 0.416 Uiso 1 1 calc R . .
C60 C -0.3887(11) 0.4039(8) 0.5247(9) 0.326(8) Uani 1 1 d D . .
H60A H -0.4254 0.3665 0.5608 0.489 Uiso 1 1 calc R . .
H60B H -0.4569 0.4456 0.5005 0.489 Uiso 1 1 calc R . .
H60C H -0.3299 0.4229 0.5439 0.489 Uiso 1 1 calc R . .
C61 C 0.0341(9) 0.1840(5) 0.5799(4) 0.189(3) Uani 1 1 d U . .
H61A H 0.1202 0.1543 0.5955 0.227 Uiso 1 1 calc R . .
H61B H 0.0067 0.2169 0.6067 0.227 Uiso 1 1 calc R . .
C62 C -0.0545(11) 0.1312(5) 0.5943(5) 0.219(4) Uani 1 1 d U . .
H62A H -0.0236 0.0943 0.5717 0.263 Uiso 1 1 calc R . .
H62B H -0.1402 0.1595 0.5763 0.263 Uiso 1 1 calc R . .
C63 C -0.0632(14) 0.0878(8) 0.6741(8) 0.301(6) Uani 1 1 d D . .
H63A H 0.0225 0.0604 0.6926 0.361 Uiso 1 1 calc R . .
H63B H -0.0975 0.1242 0.6968 0.361 Uiso 1 1 calc R . .
C64 C -0.1477(15) 0.0349(10) 0.6855(8) 0.378(10) Uani 1 1 d D . .
H64A H -0.2065 0.0382 0.7222 0.567 Uiso 1 1 calc R . .
H64B H -0.0967 -0.0163 0.6974 0.567 Uiso 1 1 calc R . .
H64C H -0.1963 0.0475 0.6445 0.567 Uiso 1 1 calc R . .
C65 C 0.6710(8) 0.3039(5) 0.9901(5) 0.194(3) Uani 1 1 d . . .
H65A H 0.6285 0.3385 1.0133 0.233 Uiso 1 1 calc R . .
H65B H 0.7461 0.2707 1.0172 0.233 Uiso 1 1 calc R . .
C66 C 0.7170(10) 0.3506(6) 0.9203(6) 0.228(4) Uani 1 1 d . . .
H66A H 0.7560 0.3164 0.8961 0.274 Uiso 1 1 calc R . .
H66B H 0.6426 0.3858 0.8939 0.274 Uiso 1 1 calc R . .
C67 C 0.8148(11) 0.3957(7) 0.9249(7) 0.259(5) Uani 1 1 d U . .
H67A H 0.7762 0.4308 0.9483 0.311 Uiso 1 1 calc R . .
H67B H 0.8898 0.3610 0.9511 0.311 Uiso 1 1 calc R . .
C68 C 0.8554(11) 0.4385(7) 0.8567(7) 0.277(5) Uani 1 1 d U . .
H68A H 0.9023 0.4035 0.8355 0.415 Uiso 1 1 calc R . .
H68B H 0.9104 0.4709 0.8598 0.415 Uiso 1 1 calc R . .
H68C H 0.7802 0.4695 0.8295 0.415 Uiso 1 1 calc R . .
C69 C 0.6242(11) 0.1879(7) 0.9368(5) 0.220(4) Uani 1 1 d . . .
H69A H 0.5642 0.1553 0.9392 0.264 Uiso 1 1 calc R . .
H69B H 0.6291 0.2206 0.8893 0.264 Uiso 1 1 calc R . .
C70 C 0.7555(16) 0.1386(8) 0.9593(7) 0.295(7) Uani 1 1 d . . .
H70A H 0.7572 0.1082 1.0078 0.354 Uiso 1 1 calc R . .
H70B H 0.8221 0.1688 0.9493 0.354 Uiso 1 1 calc R . .
C71 C 0.7716(17) 0.0852(11) 0.9119(12) 0.391(12) Uani 1 1 d D . .
H71A H 0.7475 0.0363 0.9359 0.469 Uiso 1 1 calc R . .
H71B H 0.7250 0.1112 0.8688 0.469 Uiso 1 1 calc R . .
C72 C 0.9110(16) 0.0787(12) 0.9038(12) 0.404(13) Uani 1 1 d D . .
H72A H 0.9322 0.1271 0.8971 0.606 Uiso 1 1 calc R . .
H72B H 0.9390 0.0641 0.8648 0.606 Uiso 1 1 calc R . .
H72C H 0.9540 0.0406 0.9442 0.606 Uiso 1 1 calc R . .
C73 C 0.4139(9) 0.3038(6) 0.9405(4) 0.201(4) Uani 1 1 d . . .
H73A H 0.4378 0.3283 0.8932 0.242 Uiso 1 1 calc R . .
H73B H 0.3596 0.2690 0.9406 0.242 Uiso 1 1 calc R . .
C74 C 0.3328(11) 0.3635(7) 0.9628(7) 0.255(6) Uani 1 1 d D . .
H74A H 0.3894 0.3949 0.9676 0.305 Uiso 1 1 calc R . .
H74B H 0.3015 0.3381 1.0083 0.305 Uiso 1 1 calc R . .
C75 C 0.2189(13) 0.4164(9) 0.9222(7) 0.272(6) Uani 1 1 d . . .
H75A H 0.2477 0.4412 0.8759 0.327 Uiso 1 1 calc R . .
H75B H 0.1580 0.3863 0.9194 0.327 Uiso 1 1 calc R . .
C76 C 0.1555(13) 0.4710(8) 0.9464(8) 0.311(8) Uani 1 1 d D . .
H76A H 0.1148 0.4476 0.9892 0.466 Uiso 1 1 calc R . .
H76B H 0.0904 0.5059 0.9140 0.466 Uiso 1 1 calc R . .
H76C H 0.2160 0.4983 0.9534 0.466 Uiso 1 1 calc R . .
C77 C 0.5361(9) 0.1945(6) 1.0737(4) 0.207(3) Uani 1 1 d . . .
H77A H 0.6195 0.1649 1.0940 0.248 Uiso 1 1 calc R . .
H77B H 0.5040 0.2310 1.0967 0.248 Uiso 1 1 calc R . .
C78 C 0.4470(12) 0.1430(7) 1.0878(5) 0.248(5) Uani 1 1 d . . .
H78A H 0.4742 0.1093 1.0618 0.297 Uiso 1 1 calc R . .
H78B H 0.3612 0.1730 1.0717 0.297 Uiso 1 1 calc R . .
C79 C 0.4382(18) 0.0963(8) 1.1600(8) 0.327(9) Uani 1 1 d . . .
H79A H 0.5255 0.0719 1.1776 0.393 Uiso 1 1 calc R . .
H79B H 0.4001 0.1299 1.1850 0.393 Uiso 1 1 calc R . .
C80 C 0.3681(15) 0.0414(8) 1.1734(7) 0.312(7) Uani 1 1 d . . .
H80A H 0.2775 0.0648 1.1666 0.467 Uiso 1 1 calc R . .
H80B H 0.3824 0.0072 1.2200 0.467 Uiso 1 1 calc R . .
H80C H 0.3947 0.0132 1.1431 0.467 Uiso 1 1 calc R . .
P1 P 0.0449(2) 0.24350(11) 0.49178(10) 0.1476(8) Uani 1 1 d . . .
P2 P 0.5611(2) 0.24636(13) 0.98642(11) 0.1636(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C1 1.611(8) . ?
B1 C19 1.617(8) . ?
B1 C7 1.632(8) . ?
B1 C13 1.640(9) . ?
B2 C25 1.599(8) . ?
B2 C37 1.635(8) . ?
B2 C43 1.635(7) . ?
B2 C31 1.655(8) . ?
C1 C6 1.365(8) . ?
C1 C2 1.375(7) . ?
C2 C3 1.383(9) . ?
C3 C4 1.341(10) . ?
C4 C5 1.358(10) . ?
C5 C6 1.389(9) . ?
C7 C8 1.369(7) . ?
C7 C12 1.374(7) . ?
C8 C9 1.384(8) . ?
C9 C10 1.350(10) . ?
C10 C11 1.357(10) . ?
C11 C12 1.418(8) . ?
C13 C14 1.385(9) . ?
C13 C18 1.409(9) . ?
C14 C15 1.474(11) . ?
C15 C16 1.355(14) . ?
C16 C17 1.331(15) . ?
C17 C18 1.395(11) . ?
C19 C24 1.368(8) . ?
C19 C20 1.418(8) . ?
C20 C21 1.404(11) . ?
C21 C22 1.329(13) . ?
C22 C23 1.357(12) . ?
C23 C24 1.408(10) . ?
C25 C26 1.398(7) . ?
C25 C30 1.399(8) . ?
C26 C27 1.383(9) . ?
C27 C28 1.359(10) . ?
C28 C29 1.361(10) . ?
C29 C30 1.401(9) . ?
C31 C32 1.376(8) . ?
C31 C36 1.402(8) . ?
C32 C33 1.455(11) . ?
C33 C34 1.333(14) . ?
C34 C35 1.339(12) . ?
C35 C36 1.410(8) . ?
C37 C38 1.379(7) . ?
C37 C42 1.395(7) . ?
C38 C39 1.362(8) . ?
C39 C40 1.393(9) . ?
C40 C41 1.367(9) . ?
C41 C42 1.404(8) . ?
C43 C44 1.387(7) . ?
C43 C48 1.388(7) . ?
C44 C45 1.375(8) . ?
C45 C46 1.376(9) . ?
C46 C47 1.353(9) . ?
C47 C48 1.394(8) . ?
C49 C50 1.452(10) . ?
C49 P1 1.765(7) . ?
C50 C51 1.513(11) . ?
C51 C52 1.465(13) . ?
C53 C54 1.377(16) . ?
C53 P1 1.793(9) . ?
C54 C55 1.593(9) . ?
C55 C56 1.465(9) . ?
C57 C58 1.431(11) . ?
C57 P1 1.801(9) . ?
C58 C59 1.423(14) . ?
C59 C60 1.399(15) . ?
C61 C62 1.464(10) . ?
C61 P1 1.794(8) . ?
C62 C63 1.580(15) . ?
C63 C64 1.439(9) . ?
C65 C66 1.519(11) . ?
C65 P2 1.790(8) . ?
C66 C67 1.514(12) . ?
C67 C68 1.452(13) . ?
C69 C70 1.495(13) . ?
C69 P2 1.780(10) . ?
C70 C71 1.64(2) . ?
C71 C72 1.451(9) . ?
C73 C74 1.464(11) . ?
C73 P2 1.807(9) . ?
C74 C75 1.480(13) . ?
C75 C76 1.348(13) . ?
C77 C78 1.450(11) . ?
C77 P2 1.768(8) . ?
C78 C79 1.461(14) . ?
C79 C80 1.353(15) . ?

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 B1 C19 104.9(4) . . ?
C1 B1 C7 114.2(5) . . ?
C19 B1 C7 112.2(5) . . ?
C1 B1 C13 110.9(5) . . ?
C19 B1 C13 110.9(5) . . ?
C7 B1 C13 103.9(4) . . ?
C25 B2 C37 111.0(5) . . ?
C25 B2 C43 103.8(4) . . ?
C37 B2 C43 113.2(4) . . ?
C25 B2 C31 113.2(5) . . ?
C37 B2 C31 104.9(4) . . ?
C43 B2 C31 111.0(4) . . ?
C6 C1 C2 113.7(6) . . ?
C6 C1 B1 123.1(6) . . ?
C2 C1 B1 122.8(7) . . ?
C1 C2 C3 123.4(7) . . ?
C4 C3 C2 120.3(9) . . ?
C3 C4 C5 119.3(10) . . ?
C4 C5 C6 119.0(9) . . ?
C1 C6 C5 124.2(7) . . ?
C8 C7 C12 113.9(5) . . ?
C8 C7 B1 125.7(6) . . ?
C12 C7 B1 120.3(6) . . ?
C7 C8 C9 124.9(7) . . ?
C10 C9 C8 119.1(8) . . ?
C9 C10 C11 119.9(9) . . ?
C10 C11 C12 119.2(8) . . ?
C7 C12 C11 122.9(7) . . ?
C14 C13 C18 113.9(7) . . ?
C14 C13 B1 120.1(7) . . ?
C18 C13 B1 125.9(7) . . ?
C13 C14 C15 120.2(8) . . ?
C16 C15 C14 122.8(13) . . ?
C17 C16 C15 116.3(16) . . ?
C16 C17 C18 123.2(15) . . ?
C17 C18 C13 123.6(9) . . ?
C24 C19 C20 114.5(6) . . ?
C24 C19 B1 124.2(6) . . ?
C20 C19 B1 121.1(6) . . ?
C21 C20 C19 121.6(8) . . ?
C22 C21 C20 121.2(11) . . ?
C21 C22 C23 119.4(12) . . ?
C22 C23 C24 120.4(10) . . ?
C19 C24 C23 122.9(8) . . ?
C26 C25 C30 113.2(6) . . ?
C26 C25 B2 120.0(6) . . ?
C30 C25 B2 126.7(7) . . ?
C27 C26 C25 124.7(7) . . ?
C28 C27 C26 118.7(8) . . ?
C27 C28 C29 120.9(9) . . ?
C28 C29 C30 119.1(8) . . ?
C29 C30 C25 123.3(7) . . ?
C32 C31 C36 114.3(6) . . ?
C32 C31 B2 121.1(6) . . ?
C36 C31 B2 124.4(5) . . ?
C31 C32 C33 122.6(8) . . ?
C34 C33 C32 115.8(10) . . ?
C33 C34 C35 127.3(13) . . ?
C34 C35 C36 114.3(10) . . ?
C31 C36 C35 125.5(7) . . ?
C38 C37 C42 114.9(5) . . ?
C38 C37 B2 122.7(6) . . ?
C42 C37 B2 122.3(6) . . ?
C39 C38 C37 123.4(6) . . ?
C38 C39 C40 120.7(7) . . ?
C41 C40 C39 118.7(7) . . ?
C40 C41 C42 119.2(7) . . ?
C37 C42 C41 123.1(6) . . ?
C44 C43 C48 114.1(5) . . ?
C44 C43 B2 125.3(6) . . ?
C48 C43 B2 120.4(5) . . ?
C45 C44 C43 123.7(6) . . ?
C44 C45 C46 119.0(7) . . ?
C47 C46 C45 120.8(8) . . ?
C46 C47 C48 118.4(8) . . ?
C43 C48 C47 123.9(6) . . ?
C50 C49 P1 117.7(7) . . ?
C49 C50 C51 118.1(10) . . ?
C52 C51 C50 115.2(11) . . ?
C54 C53 P1 122.6(9) . . ?
C53 C54 C55 135.8(13) . . ?
C56 C55 C54 102.4(8) . . ?
C58 C57 P1 114.3(8) . . ?
C59 C58 C57 119.5(12) . . ?
C60 C59 C58 115.3(14) . . ?
C62 C61 P1 115.8(7) . . ?
C61 C62 C63 110.2(10) . . ?
C64 C63 C62 108.1(14) . . ?
C66 C65 P2 113.9(6) . . ?
C67 C66 C65 112.9(9) . . ?
C68 C67 C66 110.1(11) . . ?
C70 C69 P2 113.9(8) . . ?
C69 C70 C71 100.4(13) . . ?
C72 C71 C70 94.7(18) . . ?
C74 C73 P2 120.3(8) . . ?
C73 C74 C75 121.2(11) . . ?
C76 C75 C74 115.6(12) . . ?
C78 C77 P2 116.2(7) . . ?
C77 C78 C79 114.4(11) . . ?
C80 C79 C78 115.4(15) . . ?
C49 P1 C61 104.5(4) . . ?
C49 P1 C53 108.8(4) . . ?
C61 P1 C53 112.2(4) . . ?
C49 P1 C57 117.5(4) . . ?
C61 P1 C57 111.7(4) . . ?
C53 P1 C57 102.4(5) . . ?
C77 P2 C69 114.2(5) . . ?
C77 P2 C65 103.1(5) . . ?
C69 P2 C65 112.1(4) . . ?
C77 P2 C73 113.9(4) . . ?
C69 P2 C73 102.0(5) . . ?
C65 P2 C73 112.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.092
####################################################################### 
# 
# 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_1_beta_403K
_database_code_depnum_ccdc_archive 'CCDC 986258'
_audit_update_record             
;
2014-02-11 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H56 B P'
_chemical_formula_weight         578.63

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   12.1401(14)
_cell_length_b                   36.975(4)
_cell_length_c                   17.688(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.611(2)
_cell_angle_gamma                90.00
_cell_volume                     7748.1(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    403
_cell_measurement_reflns_used    3563
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      17.22

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9118
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_process_details   
;
SADABS; Sheldrick 1996
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      403
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57189
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_sigmaI/netI    0.1359
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.10
_diffrn_reflns_theta_max         28.28
_reflns_number_total             19194
_reflns_number_gt                3231
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         19194
_refine_ls_number_parameters     635
_refine_ls_number_restraints     469
_refine_ls_R_factor_all          0.4430
_refine_ls_R_factor_gt           0.1668
_refine_ls_wR_factor_ref         0.5654
_refine_ls_wR_factor_gt          0.4463
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.401
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.2558(9) 0.4864(3) 0.2486(6) 0.128(3) Uani 1 1 d . . .
B2 B 0.8134(7) 0.2352(2) 0.2510(5) 0.097(3) Uani 1 1 d . . .
C1 C 0.15218(17) 0.46212(7) 0.19289(14) 0.208(4) Uani 1 1 d GU . .
C2 C 0.13107(15) 0.42814(7) 0.22023(16) 0.253(5) Uani 1 1 d GU . .
H2 H 0.1762 0.4193 0.2659 0.304 Uiso 1 1 calc R . .
C3 C 0.04252(15) 0.40731(8) 0.1793(2) 0.277(5) Uani 1 1 d GU . .
H3 H 0.0284 0.3846 0.1976 0.333 Uiso 1 1 calc R . .
C4 C -0.02491(18) 0.42047(9) 0.1111(2) 0.257(5) Uani 1 1 d GU . .
H4 H -0.0842 0.4065 0.0837 0.309 Uiso 1 1 calc R . .
C5 C -0.0038(2) 0.45444(9) 0.08375(18) 0.255(5) Uani 1 1 d GU . .
H5 H -0.0489 0.4632 0.0381 0.306 Uiso 1 1 calc R . .
C6 C 0.0847(2) 0.47527(8) 0.12465(15) 0.243(4) Uani 1 1 d GU . .
H6 H 0.0989 0.4980 0.1063 0.292 Uiso 1 1 calc R . .
C7 C 0.19016(19) 0.51090(6) 0.30328(15) 0.119(3) Uani 1 1 d G . .
C8 C 0.1659(2) 0.49677(7) 0.36960(15) 0.147(3) Uani 1 1 d G . .
H8 H 0.1916 0.4737 0.3854 0.176 Uiso 1 1 calc R . .
C9 C 0.0982(2) 0.51767(7) 0.41784(17) 0.171(4) Uani 1 1 d G . .
H9 H 0.0815 0.5090 0.4634 0.205 Uiso 1 1 calc R . .
C10 C 0.0642(2) 0.55128(7) 0.38583(18) 0.195(6) Uani 1 1 d G . .
H10 H 0.0238 0.5656 0.4135 0.234 Uiso 1 1 calc R . .
C11 C 0.0816(2) 0.56494(7) 0.32274(18) 0.191(6) Uani 1 1 d G . .
H11 H 0.0518 0.5875 0.3065 0.229 Uiso 1 1 calc R . .
C12 C 0.1476(2) 0.54545(7) 0.27654(16) 0.146(3) Uani 1 1 d G . .
H12 H 0.1614 0.5553 0.2311 0.175 Uiso 1 1 calc R . .
C13 C 0.3282(2) 0.51161(6) 0.19778(15) 0.137(3) Uani 1 1 d GDU . .
C14 C 0.3424(2) 0.49772(7) 0.12686(15) 0.200(3) Uani 1 1 d GDU . .
H14 H 0.3131 0.4751 0.1106 0.240 Uiso 1 1 calc R . .
C15 C 0.4002(3) 0.51744(8) 0.08006(18) 0.200(3) Uani 1 1 d GDU . .
H15 H 0.4039 0.5106 0.0301 0.240 Uiso 1 1 calc R . .
C16 C 0.4517(3) 0.54859(7) 0.1167(2) 0.200(3) Uani 1 1 d GDU . .
H16 H 0.5018 0.5602 0.0917 0.240 Uiso 1 1 calc R . .
C17 C 0.4380(3) 0.56465(6) 0.1857(2) 0.196(4) Uani 1 1 d GDU . .
H17 H 0.4687 0.5871 0.2021 0.235 Uiso 1 1 calc R . .
C18 C 0.3748(2) 0.54455(6) 0.22827(18) 0.169(4) Uani 1 1 d GDU . .
H18 H 0.3640 0.5529 0.2757 0.203 Uiso 1 1 calc R . .
C19 C 0.35105(16) 0.46175(6) 0.30226(12) 0.174(3) Uani 1 1 d GDU . .
C20 C 0.37577(15) 0.42833(6) 0.27261(11) 0.214(4) Uani 1 1 d GDU . .
H20 H 0.3365 0.4209 0.2239 0.257 Uiso 1 1 calc R . .
C21 C 0.45940(15) 0.40606(6) 0.31597(11) 0.230(4) Uani 1 1 d GDU . .
H21 H 0.4714 0.3825 0.3010 0.276 Uiso 1 1 calc R . .
C22 C 0.52316(18) 0.42151(6) 0.38280(12) 0.218(4) Uani 1 1 d GDU . .
H22 H 0.5865 0.4085 0.4073 0.262 Uiso 1 1 calc R . .
C23 C 0.5049(2) 0.45385(6) 0.41800(13) 0.239(4) Uani 1 1 d GDU . .
H23 H 0.5453 0.4611 0.4665 0.287 Uiso 1 1 calc R . .
C24 C 0.41833(19) 0.47426(6) 0.37190(13) 0.199(4) Uani 1 1 d GDU . .
H24 H 0.4049 0.4974 0.3885 0.238 Uiso 1 1 calc R . .
C25 C 0.73792(19) 0.26317(6) 0.28973(16) 0.107(2) Uani 1 1 d GDU . .
C26 C 0.7137(2) 0.25354(6) 0.35979(16) 0.136(3) Uani 1 1 d GDU . .
H26 H 0.7426 0.2321 0.3836 0.163 Uiso 1 1 calc R . .
C27 C 0.6428(2) 0.27677(6) 0.39721(15) 0.158(3) Uani 1 1 d GDU . .
H27 H 0.6276 0.2700 0.4445 0.190 Uiso 1 1 calc R . .
C28 C 0.5996(2) 0.30794(6) 0.36296(13) 0.166(4) Uani 1 1 d GU . .
H28 H 0.5538 0.3225 0.3860 0.200 Uiso 1 1 calc R . .
C29 C 0.62394(17) 0.31733(6) 0.29562(13) 0.162(3) Uani 1 1 d GU . .
H29 H 0.5959 0.3390 0.2726 0.194 Uiso 1 1 calc R . .
C30 C 0.69004(17) 0.29566(6) 0.25863(15) 0.133(3) Uani 1 1 d GU . .
H30 H 0.7028 0.3032 0.2111 0.160 Uiso 1 1 calc R . .
C31 C 0.7218(2) 0.20528(7) 0.20996(19) 0.103(2) Uani 1 1 d G . .
C32 C 0.7065(3) 0.17143(6) 0.2435(2) 0.137(3) Uani 1 1 d G . .
H32 H 0.7509 0.1647 0.2912 0.165 Uiso 1 1 calc R . .
C33 C 0.6228(3) 0.14833(7) 0.2030(2) 0.157(4) Uani 1 1 d G . .
H33 H 0.6146 0.1260 0.2253 0.189 Uiso 1 1 calc R . .
C34 C 0.5540(3) 0.15572(7) 0.1355(2) 0.193(6) Uani 1 1 d G . .
H34 H 0.4992 0.1392 0.1120 0.232 Uiso 1 1 calc R . .
C35 C 0.5662(3) 0.18865(8) 0.1011(2) 0.157(4) Uani 1 1 d G . .
H35 H 0.5211 0.1948 0.0533 0.189 Uiso 1 1 calc R . .
C36 C 0.6475(2) 0.21196(7) 0.14028(18) 0.129(3) Uani 1 1 d G . .
H36 H 0.6529 0.2344 0.1176 0.155 Uiso 1 1 calc R . .
C37 C 0.8737(6) 0.2549(2) 0.1872(5) 0.106(2) Uani 1 1 d DU . .
C38 C 0.8856(8) 0.2380(3) 0.1201(6) 0.144(3) Uani 1 1 d DU . .
H38 H 0.8545 0.2151 0.1091 0.173 Uiso 1 1 calc R . .
C39 C 0.9423(9) 0.2538(3) 0.0679(6) 0.178(4) Uani 1 1 d DU . .
H39 H 0.9505 0.2421 0.0229 0.214 Uiso 1 1 calc R . .
C40 C 0.9848(10) 0.2875(3) 0.0870(7) 0.184(5) Uani 1 1 d DU . .
H40 H 1.0222 0.2987 0.0527 0.221 Uiso 1 1 calc R . .
C41 C 0.9771(10) 0.3064(3) 0.1526(7) 0.193(5) Uani 1 1 d DU . .
H41 H 1.0080 0.3294 0.1628 0.231 Uiso 1 1 calc R . .
C42 C 0.9202(8) 0.2890(3) 0.2030(6) 0.154(3) Uani 1 1 d DU . .
H42 H 0.9134 0.3007 0.2484 0.184 Uiso 1 1 calc R . .
C43 C 0.9197(4) 0.2182(2) 0.3157(4) 0.110(2) Uani 1 1 d G . .
C44 C 0.9643(7) 0.1849(2) 0.3010(4) 0.148(4) Uani 1 1 d G . .
H44 H 0.9313 0.1720 0.2567 0.178 Uiso 1 1 calc R . .
C45 C 1.0580(7) 0.17105(16) 0.3523(6) 0.199(6) Uani 1 1 d G . .
H45 H 1.0878 0.1488 0.3424 0.238 Uiso 1 1 calc R . .
C46 C 1.1072(5) 0.1904(3) 0.4184(5) 0.209(7) Uani 1 1 d G . .
H46 H 1.1699 0.1811 0.4528 0.251 Uiso 1 1 calc R . .
C47 C 1.0627(7) 0.2236(3) 0.4332(3) 0.172(4) Uani 1 1 d G . .
H47 H 1.0956 0.2366 0.4775 0.207 Uiso 1 1 calc R . .
C48 C 0.9689(7) 0.23751(15) 0.3819(5) 0.137(3) Uani 1 1 d G . .
H48 H 0.9392 0.2597 0.3918 0.165 Uiso 1 1 calc R . .
C49 C 0.1952(11) 0.2079(4) 0.1844(8) 0.259(7) Uani 1 1 d DU . .
H49A H 0.1532 0.1974 0.2198 0.311 Uiso 1 1 calc R . .
H49B H 0.1446 0.2241 0.1503 0.311 Uiso 1 1 calc R . .
C50 C 0.2273(13) 0.1786(3) 0.1373(9) 0.283(7) Uani 1 1 d DU . .
H50A H 0.2764 0.1618 0.1710 0.340 Uiso 1 1 calc R . .
H50B H 0.2697 0.1888 0.1018 0.340 Uiso 1 1 calc R . .
C51 C 0.1289(12) 0.1585(4) 0.0921(9) 0.309(7) Uani 1 1 d DU . .
H51A H 0.1205 0.1647 0.0378 0.371 Uiso 1 1 calc R . .
H51B H 0.0617 0.1668 0.1080 0.371 Uiso 1 1 calc R . .
C52 C 0.1341(16) 0.1181(3) 0.0993(11) 0.369(9) Uani 1 1 d DU . .
H52A H 0.0709 0.1077 0.0638 0.553 Uiso 1 1 calc R . .
H52B H 0.1317 0.1113 0.1513 0.553 Uiso 1 1 calc R . .
H52C H 0.2030 0.1095 0.0874 0.553 Uiso 1 1 calc R . .
C53 C 0.3822(11) 0.2585(3) 0.1832(7) 0.199(4) Uani 1 1 d DU . .
H53A H 0.4388 0.2721 0.2192 0.239 Uiso 1 1 calc R . .
H53B H 0.4218 0.2419 0.1560 0.239 Uiso 1 1 calc R . .
C54 C 0.3185(14) 0.2835(4) 0.1272(8) 0.242(5) Uani 1 1 d DU . .
H54A H 0.2632 0.2693 0.0914 0.291 Uiso 1 1 calc R . .
H54B H 0.2768 0.2991 0.1551 0.291 Uiso 1 1 calc R . .
C55 C 0.3733(15) 0.3066(4) 0.0812(9) 0.275(6) Uani 1 1 d DU . .
H55A H 0.4321 0.3198 0.1164 0.330 Uiso 1 1 calc R . .
H55B H 0.4103 0.2912 0.0499 0.330 Uiso 1 1 calc R . .
C56 C 0.3064(16) 0.3326(5) 0.0304(10) 0.326(8) Uani 1 1 d DU . .
H56A H 0.3534 0.3452 0.0019 0.488 Uiso 1 1 calc R . .
H56B H 0.2741 0.3495 0.0604 0.488 Uiso 1 1 calc R . .
H56C H 0.2472 0.3202 -0.0052 0.488 Uiso 1 1 calc R . .
C57 C 0.4129(10) 0.2065(3) 0.2930(7) 0.214(5) Uani 1 1 d DU . .
H57A H 0.4487 0.1931 0.2578 0.256 Uiso 1 1 calc R . .
H57B H 0.4690 0.2228 0.3222 0.256 Uiso 1 1 calc R . .
C58 C 0.3812(12) 0.1807(4) 0.3475(8) 0.242(5) Uani 1 1 d DU . .
H58A H 0.3610 0.1948 0.3888 0.290 Uiso 1 1 calc R . .
H58B H 0.3129 0.1687 0.3205 0.290 Uiso 1 1 calc R . .
C59 C 0.4594(14) 0.1525(4) 0.3843(9) 0.262(6) Uani 1 1 d DU . .
H59A H 0.5189 0.1633 0.4233 0.314 Uiso 1 1 calc R . .
H59B H 0.4939 0.1413 0.3456 0.314 Uiso 1 1 calc R . .
C60 C 0.4006(16) 0.1245(4) 0.4209(9) 0.299(7) Uani 1 1 d DU . .
H60A H 0.3650 0.1357 0.4584 0.449 Uiso 1 1 calc R . .
H60B H 0.4543 0.1069 0.4461 0.449 Uiso 1 1 calc R . .
H60C H 0.3444 0.1129 0.3819 0.449 Uiso 1 1 calc R . .
C61 C 0.2232(11) 0.2590(3) 0.2885(8) 0.205(4) Uani 1 1 d DU . .
H61A H 0.1613 0.2696 0.2511 0.246 Uiso 1 1 calc R . .
H61B H 0.1904 0.2428 0.3207 0.246 Uiso 1 1 calc R . .
C62 C 0.2783(12) 0.2867(3) 0.3357(8) 0.229(4) Uani 1 1 d DU . .
H62A H 0.3141 0.3020 0.3034 0.275 Uiso 1 1 calc R . .
H62B H 0.3384 0.2756 0.3738 0.275 Uiso 1 1 calc R . .
C63 C 0.2185(14) 0.3098(4) 0.3764(9) 0.262(5) Uani 1 1 d DU . .
H63A H 0.1643 0.3232 0.3381 0.315 Uiso 1 1 calc R . .
H63B H 0.1755 0.2946 0.4040 0.315 Uiso 1 1 calc R . .
C64 C 0.2759(15) 0.3347(4) 0.4290(11) 0.309(7) Uani 1 1 d DU . .
H64A H 0.2230 0.3480 0.4514 0.463 Uiso 1 1 calc R . .
H64B H 0.3164 0.3511 0.4030 0.463 Uiso 1 1 calc R . .
H64C H 0.3281 0.3223 0.4692 0.463 Uiso 1 1 calc R . .
C65 C 0.6765(12) 0.5092(3) 0.3111(8) 0.226(5) Uani 1 1 d DU . .
H65A H 0.6148 0.5204 0.2744 0.271 Uiso 1 1 calc R . .
H65B H 0.6436 0.4930 0.3432 0.271 Uiso 1 1 calc R . .
C66 C 0.7361(13) 0.5366(4) 0.3588(8) 0.235(5) Uani 1 1 d DU . .
H66A H 0.7647 0.5536 0.3260 0.282 Uiso 1 1 calc R . .
H66B H 0.8008 0.5255 0.3929 0.282 Uiso 1 1 calc R . .
C67 C 0.6745(14) 0.5566(4) 0.4056(9) 0.274(6) Uani 1 1 d DU . .
H67A H 0.6453 0.5393 0.4378 0.329 Uiso 1 1 calc R . .
H67B H 0.6099 0.5675 0.3712 0.329 Uiso 1 1 calc R . .
C68 C 0.7319(16) 0.5846(4) 0.4555(10) 0.314(8) Uani 1 1 d DU . .
H68A H 0.6802 0.5958 0.4824 0.472 Uiso 1 1 calc R . .
H68B H 0.7601 0.6024 0.4250 0.472 Uiso 1 1 calc R . .
H68C H 0.7937 0.5742 0.4924 0.472 Uiso 1 1 calc R . .
C69 C 0.8388(10) 0.5088(3) 0.2035(7) 0.209(4) Uani 1 1 d DU . .
H69A H 0.8978 0.5216 0.2394 0.251 Uiso 1 1 calc R . .
H69B H 0.8750 0.4923 0.1738 0.251 Uiso 1 1 calc R . .
C70 C 0.7709(12) 0.5352(4) 0.1503(8) 0.233(5) Uani 1 1 d DU . .
H70A H 0.7065 0.5227 0.1190 0.279 Uiso 1 1 calc R . .
H70B H 0.7423 0.5532 0.1808 0.279 Uiso 1 1 calc R . .
C71 C 0.8321(12) 0.5537(4) 0.0981(9) 0.257(5) Uani 1 1 d DU . .
H71A H 0.8587 0.5357 0.0662 0.309 Uiso 1 1 calc R . .
H71B H 0.8978 0.5656 0.1291 0.309 Uiso 1 1 calc R . .
C72 C 0.7636(13) 0.5807(4) 0.0470(9) 0.296(7) Uani 1 1 d DU . .
H72A H 0.7210 0.5689 0.0016 0.445 Uiso 1 1 calc R . .
H72B H 0.8124 0.5985 0.0321 0.445 Uiso 1 1 calc R . .
H72C H 0.7128 0.5923 0.0742 0.445 Uiso 1 1 calc R . .
C73 C 0.8661(12) 0.4551(4) 0.3112(9) 0.253(6) Uani 1 1 d DU . .
H73A H 0.9065 0.4447 0.2749 0.303 Uiso 1 1 calc R . .
H73B H 0.9187 0.4706 0.3459 0.303 Uiso 1 1 calc R . .
C74 C 0.8342(14) 0.4264(4) 0.3559(9) 0.278(6) Uani 1 1 d DU . .
H74A H 0.7810 0.4106 0.3224 0.334 Uiso 1 1 calc R . .
H74B H 0.7973 0.4363 0.3947 0.334 Uiso 1 1 calc R . .
C75 C 0.9311(14) 0.4059(4) 0.3932(10) 0.304(6) Uani 1 1 d DU . .
H75A H 0.9642 0.4165 0.4432 0.365 Uiso 1 1 calc R . .
H75B H 0.9873 0.4061 0.3618 0.365 Uiso 1 1 calc R . .
C76 C 0.8964(17) 0.3692(4) 0.4034(11) 0.345(9) Uani 1 1 d DU . .
H76A H 0.8548 0.3685 0.4437 0.518 Uiso 1 1 calc R . .
H76B H 0.9619 0.3541 0.4174 0.518 Uiso 1 1 calc R . .
H76C H 0.8495 0.3607 0.3559 0.518 Uiso 1 1 calc R . .
C77 C 0.6444(10) 0.4584(3) 0.2013(7) 0.204(5) Uani 1 1 d DU . .
H77A H 0.6068 0.4449 0.2354 0.244 Uiso 1 1 calc R . .
H77B H 0.5902 0.4754 0.1724 0.244 Uiso 1 1 calc R . .
C78 C 0.6797(12) 0.4329(4) 0.1460(8) 0.243(5) Uani 1 1 d DU . .
H78A H 0.7413 0.4182 0.1743 0.292 Uiso 1 1 calc R . .
H78B H 0.7086 0.4469 0.1082 0.292 Uiso 1 1 calc R . .
C79 C 0.5889(13) 0.4082(4) 0.1036(9) 0.274(6) Uani 1 1 d DU . .
H79A H 0.5459 0.3987 0.1394 0.329 Uiso 1 1 calc R . .
H79B H 0.5377 0.4217 0.0637 0.329 Uiso 1 1 calc R . .
C80 C 0.6388(16) 0.3774(4) 0.0671(10) 0.324(8) Uani 1 1 d DU . .
H80A H 0.6978 0.3863 0.0439 0.487 Uiso 1 1 calc R . .
H80B H 0.5812 0.3663 0.0281 0.487 Uiso 1 1 calc R . .
H80C H 0.6692 0.3598 0.1061 0.487 Uiso 1 1 calc R . .
P1 P 0.3040(2) 0.23280(7) 0.23729(18) 0.1539(12) Uani 1 1 d . . .
P2 P 0.7571(3) 0.48284(8) 0.25817(18) 0.1603(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C19 1.609(9) . ?
B1 C7 1.651(10) . ?
B1 C13 1.672(11) . ?
B1 C1 1.679(11) . ?
B2 C31 1.624(9) . ?
B2 C25 1.628(8) . ?
B2 C37 1.642(11) . ?
B2 C43 1.652(10) . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C7 C8 1.3735 . ?
C7 C12 1.4200 . ?
C8 C9 1.5186 . ?
C9 C10 1.3902 . ?
C10 C11 1.2840 . ?
C11 C12 1.4538 . ?
C13 C18 1.4003 . ?
C13 C14 1.4006 . ?
C14 C15 1.4007 . ?
C15 C16 1.3998 . ?
C16 C17 1.4000 . ?
C17 C18 1.4002 . ?
C19 C24 1.3996 . ?
C19 C20 1.4002 . ?
C20 C21 1.3989 . ?
C21 C22 1.3869 . ?
C22 C23 1.3881 . ?
C23 C24 1.4014 . ?
C25 C26 1.3815 . ?
C25 C30 1.3943 . ?
C26 C27 1.4716 . ?
C27 C28 1.3531 . ?
C28 C29 1.3343 . ?
C29 C30 1.3940 . ?
C31 C36 1.3813 . ?
C31 C32 1.4146 . ?
C32 C33 1.3991 . ?
C33 C34 1.3277 . ?
C34 C35 1.3836 . ?
C35 C36 1.3782 . ?
C37 C38 1.375(7) . ?
C37 C42 1.386(7) . ?
C38 C39 1.395(8) . ?
C39 C40 1.362(7) . ?
C40 C41 1.374(8) . ?
C41 C42 1.399(8) . ?
C43 C44 1.3900 . ?
C43 C48 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?
C46 C47 1.3900 . ?
C47 C48 1.3900 . ?
C49 C50 1.469(10) . ?
C49 P1 1.712(12) . ?
C50 C51 1.484(10) . ?
C51 C52 1.4981(13) . ?
C53 C54 1.449(11) . ?
C53 P1 1.765(11) . ?
C54 C55 1.439(12) . ?
C55 C56 1.438(12) . ?
C57 C58 1.466(12) . ?
C57 P1 1.759(11) . ?
C58 C59 1.464(12) . ?
C59 C60 1.484(12) . ?
C61 C62 1.398(11) . ?
C61 P1 1.763(11) . ?
C62 C63 1.416(11) . ?
C63 C64 1.384(11) . ?
C65 C66 1.412(11) . ?
C65 P2 1.784(13) . ?
C66 C67 1.436(11) . ?
C67 C68 1.438(9) . ?
C69 C70 1.476(10) . ?
C69 P2 1.805(12) . ?
C70 C71 1.474(10) . ?
C71 C72 1.476(8) . ?
C73 C74 1.429(12) . ?
C73 P2 1.771(14) . ?
C74 C75 1.433(12) . ?
C75 C76 1.441(9) . ?
C77 C78 1.488(11) . ?
C77 P2 1.759(11) . ?
C78 C79 1.501(11) . ?
C79 C80 1.500(9) . ?

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
C19 B1 C7 110.0(6) . . ?
C19 B1 C13 103.8(6) . . ?
C7 B1 C13 112.8(6) . . ?
C19 B1 C1 113.1(6) . . ?
C7 B1 C1 104.0(6) . . ?
C13 B1 C1 113.4(6) . . ?
C31 B2 C25 103.2(5) . . ?
C31 B2 C37 111.0(6) . . ?
C25 B2 C37 112.6(6) . . ?
C31 B2 C43 113.9(6) . . ?
C25 B2 C43 112.2(6) . . ?
C37 B2 C43 104.3(6) . . ?
C2 C1 C6 120.0 . . ?
C2 C1 B1 116.8(3) . . ?
C6 C1 B1 123.1(3) . . ?
C1 C2 C3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C4 C5 C6 120.0 . . ?
C5 C6 C1 120.0 . . ?
C8 C7 C12 119.7 . . ?
C8 C7 B1 120.8(4) . . ?
C12 C7 B1 119.0(3) . . ?
C7 C8 C9 122.0 . . ?
C10 C9 C8 112.0 . . ?
C11 C10 C9 127.9 . . ?
C10 C11 C12 120.6 . . ?
C7 C12 C11 117.6 . . ?
C18 C13 C14 123.0 . . ?
C18 C13 B1 119.6(3) . . ?
C14 C13 B1 117.4(3) . . ?
C13 C14 C15 120.9 . . ?
C16 C15 C14 112.7 . . ?
C15 C16 C17 128.8 . . ?
C16 C17 C18 115.3 . . ?
C17 C18 C13 118.5 . . ?
C24 C19 C20 119.3 . . ?
C24 C19 B1 122.5(4) . . ?
C20 C19 B1 117.7(4) . . ?
C21 C20 C19 120.2 . . ?
C22 C21 C20 115.3 . . ?
C21 C22 C23 128.5 . . ?
C22 C23 C24 112.1 . . ?
C19 C24 C23 123.6 . . ?
C26 C25 C30 115.1 . . ?
C26 C25 B2 117.6(3) . . ?
C30 C25 B2 127.3(3) . . ?
C25 C26 C27 120.9 . . ?
C28 C27 C26 120.2 . . ?
C29 C28 C27 118.8 . . ?
C28 C29 C30 122.1 . . ?
C29 C30 C25 122.9 . . ?
C36 C31 C32 114.4 . . ?
C36 C31 B2 121.8(3) . . ?
C32 C31 B2 123.7(3) . . ?
C33 C32 C31 118.2 . . ?
C34 C33 C32 125.4 . . ?
C33 C34 C35 118.0 . . ?
C36 C35 C34 117.6 . . ?
C35 C36 C31 126.4 . . ?
C38 C37 C42 118.1(9) . . ?
C38 C37 B2 122.7(8) . . ?
C42 C37 B2 119.2(8) . . ?
C37 C38 C39 122.9(10) . . ?
C40 C39 C38 115.6(11) . . ?
C39 C40 C41 125.7(12) . . ?
C40 C41 C42 116.0(11) . . ?
C37 C42 C41 121.8(10) . . ?
C44 C43 C48 120.0 . . ?
C44 C43 B2 119.0(7) . . ?
C48 C43 B2 120.9(7) . . ?
C43 C44 C45 120.0 . . ?
C46 C45 C44 120.0 . . ?
C45 C46 C47 120.0 . . ?
C46 C47 C48 120.0 . . ?
C47 C48 C43 120.0 . . ?
C50 C49 P1 116.0(11) . . ?
C49 C50 C51 113.1(15) . . ?
C50 C51 C52 116.1(6) . . ?
C54 C53 P1 116.4(11) . . ?
C55 C54 C53 121.5(16) . . ?
C56 C55 C54 118.9(18) . . ?
C58 C57 P1 117.0(11) . . ?
C59 C58 C57 121.2(16) . . ?
C58 C59 C60 111.3(16) . . ?
C62 C61 P1 117.5(11) . . ?
C61 C62 C63 121.0(15) . . ?
C64 C63 C62 120.3(17) . . ?
C66 C65 P2 115.9(11) . . ?
C65 C66 C67 116.8(15) . . ?
C66 C67 C68 118.7(17) . . ?
C70 C69 P2 113.4(10) . . ?
C71 C70 C69 114.8(13) . . ?
C70 C71 C72 113.8(13) . . ?
C74 C73 P2 117.5(13) . . ?
C73 C74 C75 110.8(17) . . ?
C74 C75 C76 108.8(16) . . ?
C78 C77 P2 113.7(10) . . ?
C77 C78 C79 115.5(14) . . ?
C80 C79 C78 110.9(15) . . ?
C49 P1 C57 113.9(6) . . ?
C49 P1 C61 97.3(7) . . ?
C57 P1 C61 116.7(6) . . ?
C49 P1 C53 115.8(7) . . ?
C57 P1 C53 100.0(6) . . ?
C61 P1 C53 114.1(6) . . ?
C77 P2 C73 113.8(6) . . ?
C77 P2 C65 97.6(6) . . ?
C73 P2 C65 118.1(7) . . ?
C77 P2 C69 114.6(6) . . ?
C73 P2 C69 99.0(6) . . ?
C65 P2 C69 114.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_1_a_183K
_database_code_depnum_ccdc_archive 'CCDC 1422938'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-11-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H56 B P'
_chemical_formula_weight         578.63

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1868(7)
_cell_length_b                   18.7141(13)
_cell_length_c                   20.7566(15)
_cell_angle_alpha                70.748(2)
_cell_angle_beta                 86.972(2)
_cell_angle_gamma                76.006(2)
_cell_volume                     3623.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    183
_cell_measurement_reflns_used    1471
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9656
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_process_details   
;
SADABS; Sheldrick 1996
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21308
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_sigmaI/netI    0.1739
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.04
_diffrn_reflns_theta_max         25.03
_reflns_number_total             12760
_reflns_number_gt                5053
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0987P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12760
_refine_ls_number_parameters     765
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.2179
_refine_ls_R_factor_gt           0.0888
_refine_ls_wR_factor_ref         0.2639
_refine_ls_wR_factor_gt          0.1966
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.013
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
B2 B 0.3247(5) 0.7386(3) 0.7353(3) 0.0347(14) Uani 1 1 d . . .
B1 B 0.7472(5) 0.7686(3) 0.2466(3) 0.0377(14) Uani 1 1 d . . .
C25 C 0.4611(5) 0.7695(3) 0.7402(2) 0.0366(12) Uani 1 1 d . . .
C26 C 0.4482(5) 0.8401(3) 0.7526(2) 0.0452(14) Uani 1 1 d . . .
H26 H 0.3598 0.8685 0.7578 0.054 Uiso 1 1 calc R . .
C27 C 0.5557(6) 0.8708(4) 0.7576(3) 0.0582(16) Uani 1 1 d . . .
H27 H 0.5407 0.9192 0.7657 0.070 Uiso 1 1 calc R . .
C28 C 0.6839(7) 0.8310(5) 0.7508(3) 0.071(2) Uani 1 1 d . . .
H28 H 0.7588 0.8522 0.7530 0.085 Uiso 1 1 calc R . .
C29 C 0.7044(6) 0.7600(4) 0.7406(3) 0.0666(19) Uani 1 1 d . . .
H29 H 0.7939 0.7315 0.7373 0.080 Uiso 1 1 calc R . .
C30 C 0.5944(5) 0.7294(3) 0.7352(3) 0.0555(16) Uani 1 1 d . . .
H30 H 0.6105 0.6805 0.7280 0.067 Uiso 1 1 calc R . .
C31 C 0.3509(4) 0.6687(3) 0.7024(2) 0.0356(12) Uani 1 1 d . . .
C32 C 0.4270(5) 0.6719(3) 0.6428(3) 0.0482(14) Uani 1 1 d . . .
H32 H 0.4655 0.7153 0.6226 0.058 Uiso 1 1 calc R . .
C33 C 0.4473(6) 0.6139(4) 0.6128(3) 0.0630(17) Uani 1 1 d . . .
H33 H 0.4986 0.6183 0.5727 0.076 Uiso 1 1 calc R . .
C34 C 0.3933(6) 0.5499(4) 0.6409(3) 0.0649(18) Uani 1 1 d . . .
H34 H 0.4093 0.5095 0.6212 0.078 Uiso 1 1 calc R . .
C35 C 0.3165(6) 0.5456(3) 0.6974(3) 0.0545(15) Uani 1 1 d . . .
H35 H 0.2761 0.5027 0.7163 0.065 Uiso 1 1 calc R . .
C36 C 0.2972(5) 0.6029(3) 0.7270(2) 0.0411(13) Uani 1 1 d . . .
H36 H 0.2442 0.5975 0.7666 0.049 Uiso 1 1 calc R . .
C37 C 0.2099(4) 0.8102(3) 0.6851(2) 0.0329(12) Uani 1 1 d . . .
C38 C 0.2388(5) 0.8752(3) 0.6352(2) 0.0406(13) Uani 1 1 d . . .
H38 H 0.3302 0.8793 0.6309 0.049 Uiso 1 1 calc R . .
C39 C 0.1420(5) 0.9339(3) 0.5918(2) 0.0443(13) Uani 1 1 d . . .
H39 H 0.1685 0.9766 0.5589 0.053 Uiso 1 1 calc R . .
C40 C 0.0092(5) 0.9315(3) 0.5954(3) 0.0477(14) Uani 1 1 d . . .
H40 H -0.0575 0.9724 0.5662 0.057 Uiso 1 1 calc R . .
C41 C -0.0258(5) 0.8678(3) 0.6428(3) 0.0470(14) Uani 1 1 d . . .
H41 H -0.1177 0.8645 0.6459 0.056 Uiso 1 1 calc R . .
C42 C 0.0720(5) 0.8086(3) 0.6859(2) 0.0388(13) Uani 1 1 d . . .
H42 H 0.0449 0.7651 0.7173 0.047 Uiso 1 1 calc R . .
C43 C 0.2782(4) 0.7085(3) 0.8153(2) 0.0332(12) Uani 1 1 d . . .
C44 C 0.1741(5) 0.7494(3) 0.8446(3) 0.0452(14) Uani 1 1 d . . .
H44 H 0.1215 0.7982 0.8168 0.054 Uiso 1 1 calc R . .
C45 C 0.1439(5) 0.7217(4) 0.9131(3) 0.0550(16) Uani 1 1 d . . .
H45 H 0.0709 0.7514 0.9308 0.066 Uiso 1 1 calc R . .
C46 C 0.2181(6) 0.6519(4) 0.9557(3) 0.0596(17) Uani 1 1 d . . .
H46 H 0.1974 0.6327 1.0025 0.072 Uiso 1 1 calc R . .
C47 C 0.3224(5) 0.6111(3) 0.9286(3) 0.0526(15) Uani 1 1 d . . .
H47 H 0.3749 0.5627 0.9570 0.063 Uiso 1 1 calc R . .
C48 C 0.3531(5) 0.6385(3) 0.8610(2) 0.0438(13) Uani 1 1 d . . .
H48 H 0.4282 0.6088 0.8445 0.053 Uiso 1 1 calc R . .
C1 C 0.8133(5) 0.8353(3) 0.2576(2) 0.0398(13) Uani 1 1 d . . .
C2 C 0.7353(5) 0.8987(3) 0.2732(2) 0.0440(13) Uani 1 1 d . . .
H2 H 0.6398 0.9054 0.2738 0.053 Uiso 1 1 calc R . .
C3 C 0.7894(6) 0.9531(3) 0.2881(3) 0.0538(15) Uani 1 1 d . . .
H3 H 0.7314 0.9951 0.2993 0.065 Uiso 1 1 calc R . .
C4 C 0.9278(7) 0.9462(3) 0.2865(3) 0.0601(17) Uani 1 1 d . . .
H4 H 0.9656 0.9838 0.2955 0.072 Uiso 1 1 calc R . .
C5 C 1.0099(6) 0.8837(3) 0.2715(3) 0.0550(15) Uani 1 1 d . . .
H5 H 1.1051 0.8780 0.2698 0.066 Uiso 1 1 calc R . .
C6 C 0.9536(5) 0.8295(3) 0.2590(2) 0.0430(13) Uani 1 1 d . . .
H6 H 1.0127 0.7858 0.2508 0.052 Uiso 1 1 calc R . .
C7 C 0.8350(5) 0.7227(3) 0.1975(2) 0.0377(12) Uani 1 1 d . . .
C8 C 0.9209(5) 0.7531(3) 0.1473(2) 0.0484(14) Uani 1 1 d . . .
H8 H 0.9326 0.8037 0.1413 0.058 Uiso 1 1 calc R . .
C9 C 0.9902(5) 0.7131(4) 0.1056(3) 0.0551(15) Uani 1 1 d . . .
H9 H 1.0476 0.7364 0.0718 0.066 Uiso 1 1 calc R . .
C10 C 0.9759(5) 0.6397(4) 0.1132(3) 0.0567(16) Uani 1 1 d . . .
H10 H 1.0258 0.6111 0.0859 0.068 Uiso 1 1 calc R . .
C11 C 0.8889(5) 0.6079(3) 0.1607(3) 0.0526(15) Uani 1 1 d . . .
H11 H 0.8755 0.5580 0.1653 0.063 Uiso 1 1 calc R . .
C12 C 0.8208(5) 0.6490(3) 0.2017(3) 0.0480(14) Uani 1 1 d . . .
H12 H 0.7614 0.6259 0.2344 0.058 Uiso 1 1 calc R . .
C13 C 0.5990(5) 0.8081(3) 0.2071(2) 0.0388(13) Uani 1 1 d . . .
C14 C 0.5748(5) 0.8780(3) 0.1530(3) 0.0527(15) Uani 1 1 d . . .
H14 H 0.6461 0.9041 0.1399 0.063 Uiso 1 1 calc R . .
C15 C 0.4517(6) 0.9115(3) 0.1174(3) 0.0664(18) Uani 1 1 d . . .
H15 H 0.4399 0.9592 0.0806 0.080 Uiso 1 1 calc R . .
C16 C 0.3456(6) 0.8746(4) 0.1359(3) 0.0650(18) Uani 1 1 d . . .
H16 H 0.2597 0.8977 0.1131 0.078 Uiso 1 1 calc R . .
C17 C 0.3665(6) 0.8054(4) 0.1868(3) 0.0613(17) Uani 1 1 d . . .
H17 H 0.2958 0.7787 0.1987 0.074 Uiso 1 1 calc R . .
C18 C 0.4900(5) 0.7731(3) 0.2217(3) 0.0500(14) Uani 1 1 d . . .
H18 H 0.5011 0.7246 0.2575 0.060 Uiso 1 1 calc R . .
C19 C 0.7349(5) 0.7111(3) 0.3235(2) 0.0389(12) Uani 1 1 d . . .
C20 C 0.6308(5) 0.7314(3) 0.3666(3) 0.0489(14) Uani 1 1 d . . .
H20 H 0.5641 0.7787 0.3487 0.059 Uiso 1 1 calc R . .
C21 C 0.6213(6) 0.6864(3) 0.4327(3) 0.0594(16) Uani 1 1 d . . .
H21 H 0.5484 0.7028 0.4591 0.071 Uiso 1 1 calc R . .
C22 C 0.7159(6) 0.6177(3) 0.4617(3) 0.0611(17) Uani 1 1 d . . .
H22 H 0.7089 0.5865 0.5077 0.073 Uiso 1 1 calc R . .
C23 C 0.8205(6) 0.5953(3) 0.4227(3) 0.0601(16) Uani 1 1 d . . .
H23 H 0.8866 0.5479 0.4416 0.072 Uiso 1 1 calc R . .
C24 C 0.8301(5) 0.6421(3) 0.3546(3) 0.0494(14) Uani 1 1 d . . .
H24 H 0.9046 0.6260 0.3290 0.059 Uiso 1 1 calc R . .
C65 C 0.6933(5) 0.8118(3) 0.9836(3) 0.0586(16) Uani 1 1 d . . .
H65A H 0.6486 0.8497 1.0066 0.070 Uiso 1 1 calc R . .
H65B H 0.7755 0.7785 1.0112 0.070 Uiso 1 1 calc R . .
C66 C 0.7361(6) 0.8564(4) 0.9136(3) 0.0652(17) Uani 1 1 d . . .
H66A H 0.7794 0.8187 0.8903 0.078 Uiso 1 1 calc R . .
H66B H 0.6542 0.8907 0.8863 0.078 Uiso 1 1 calc R . .
C67 C 0.8326(5) 0.9055(3) 0.9152(3) 0.0594(16) Uani 1 1 d . . .
H67A H 0.9151 0.8716 0.9421 0.071 Uiso 1 1 calc R . .
H67B H 0.7897 0.9437 0.9382 0.071 Uiso 1 1 calc R . .
C68 C 0.8722(6) 0.9489(4) 0.8440(3) 0.0741(19) Uani 1 1 d . . .
H68A H 0.9188 0.9112 0.8219 0.111 Uiso 1 1 calc R . .
H68B H 0.9327 0.9812 0.8472 0.111 Uiso 1 1 calc R . .
H68C H 0.7907 0.9821 0.8170 0.111 Uiso 1 1 calc R . .
C69 C 0.6550(6) 0.6808(4) 0.9400(3) 0.0701(18) Uani 1 1 d . . .
H69A H 0.5872 0.6515 0.9378 0.084 Uiso 1 1 calc R . .
H69B H 0.6737 0.7097 0.8924 0.084 Uiso 1 1 calc R . .
C70 C 0.7838(8) 0.6229(5) 0.9726(4) 0.116(3) Uani 1 1 d . . .
H70A H 0.7688 0.5970 1.0214 0.139 Uiso 1 1 calc R . .
H70B H 0.8558 0.6510 0.9701 0.139 Uiso 1 1 calc R . .
C71 C 0.8330(10) 0.5585(5) 0.9362(5) 0.145(4) Uani 1 1 d D . .
H71A H 0.8891 0.5103 0.9685 0.174 Uiso 1 1 calc R . .
H71B H 0.7540 0.5456 0.9208 0.174 Uiso 1 1 calc R . .
C72 C 0.9112(11) 0.5901(6) 0.8787(5) 0.180(5) Uani 1 1 d D . .
H72A H 0.8781 0.6469 0.8610 0.270 Uiso 1 1 calc R . .
H72B H 0.9021 0.5681 0.8428 0.270 Uiso 1 1 calc R . .
H72C H 1.0066 0.5769 0.8930 0.270 Uiso 1 1 calc R . .
C73 C 0.4296(5) 0.8072(4) 0.9361(3) 0.0628(17) Uani 1 1 d . . .
H73A H 0.4524 0.8295 0.8878 0.075 Uiso 1 1 calc R . .
H73B H 0.3705 0.7718 0.9377 0.075 Uiso 1 1 calc R . .
C74 C 0.3498(6) 0.8729(4) 0.9593(3) 0.075(2) Uani 1 1 d . . .
H74A H 0.4125 0.9030 0.9660 0.090 Uiso 1 1 calc R . .
H74B H 0.3113 0.8504 1.0041 0.090 Uiso 1 1 calc R . .
C75 C 0.2344(6) 0.9290(4) 0.9100(3) 0.076(2) Uani 1 1 d . . .
H75A H 0.2732 0.9538 0.8659 0.092 Uiso 1 1 calc R . .
H75B H 0.1740 0.8986 0.9014 0.092 Uiso 1 1 calc R . .
C76 C 0.1515(6) 0.9918(4) 0.9358(3) 0.084(2) Uani 1 1 d . . .
H76A H 0.1057 0.9681 0.9772 0.125 Uiso 1 1 calc R . .
H76B H 0.0839 1.0275 0.9007 0.125 Uiso 1 1 calc R . .
H76C H 0.2110 1.0209 0.9462 0.125 Uiso 1 1 calc R . .
C77 C 0.5537(6) 0.7026(3) 1.0706(3) 0.0617(17) Uani 1 1 d . . .
H77A H 0.6423 0.6714 1.0928 0.074 Uiso 1 1 calc R . .
H77B H 0.5186 0.7424 1.0929 0.074 Uiso 1 1 calc R . .
C78 C 0.4583(6) 0.6497(4) 1.0835(3) 0.0681(18) Uani 1 1 d . . .
H78A H 0.3643 0.6819 1.0743 0.082 Uiso 1 1 calc R . .
H78B H 0.4769 0.6198 1.0513 0.082 Uiso 1 1 calc R . .
C79 C 0.4696(6) 0.5938(4) 1.1552(3) 0.0740(19) Uani 1 1 d . . .
H79A H 0.5627 0.5604 1.1637 0.089 Uiso 1 1 calc R . .
H79B H 0.4548 0.6238 1.1873 0.089 Uiso 1 1 calc R . .
C80 C 0.3720(6) 0.5427(4) 1.1701(3) 0.085(2) Uani 1 1 d . . .
H80A H 0.2793 0.5750 1.1633 0.128 Uiso 1 1 calc R . .
H80B H 0.3858 0.5078 1.2174 0.128 Uiso 1 1 calc R . .
H80C H 0.3870 0.5117 1.1392 0.128 Uiso 1 1 calc R . .
C49 C 0.1693(5) 0.7963(3) 0.4942(3) 0.0519(15) Uani 1 1 d . . .
H49A H 0.1318 0.8295 0.5225 0.062 Uiso 1 1 calc R . .
H49B H 0.2557 0.7613 0.5164 0.062 Uiso 1 1 calc R . .
C50 C 0.1999(5) 0.8485(3) 0.4245(3) 0.0579(16) Uani 1 1 d . . .
H50A H 0.2246 0.8171 0.3936 0.069 Uiso 1 1 calc R . .
H50B H 0.1171 0.8894 0.4051 0.069 Uiso 1 1 calc R . .
C51 C 0.3137(5) 0.8870(3) 0.4271(3) 0.0611(16) Uani 1 1 d . . .
H51A H 0.2898 0.9176 0.4586 0.073 Uiso 1 1 calc R . .
H51B H 0.3970 0.8461 0.4456 0.073 Uiso 1 1 calc R . .
C52 C 0.3417(6) 0.9401(3) 0.3578(3) 0.079(2) Uani 1 1 d . . .
H52A H 0.3658 0.9100 0.3264 0.118 Uiso 1 1 calc R . .
H52B H 0.4168 0.9626 0.3622 0.118 Uiso 1 1 calc R . .
H52C H 0.2606 0.9819 0.3401 0.118 Uiso 1 1 calc R . .
C53 C 0.1149(6) 0.6791(4) 0.4407(3) 0.0729(19) Uani 1 1 d . . .
H53A H 0.0527 0.6448 0.4439 0.087 Uiso 1 1 calc R . .
H53B H 0.1103 0.7141 0.3928 0.087 Uiso 1 1 calc R . .
C54 C 0.2509(7) 0.6310(4) 0.4558(4) 0.093(2) Uani 1 1 d . . .
H54A H 0.2574 0.5954 0.5036 0.111 Uiso 1 1 calc R . .
H54B H 0.3150 0.6644 0.4513 0.111 Uiso 1 1 calc R . .
C55 C 0.2905(8) 0.5820(4) 0.4063(4) 0.114(3) Uani 1 1 d . . .
H55A H 0.3782 0.5443 0.4229 0.137 Uiso 1 1 calc R . .
H55B H 0.2221 0.5514 0.4098 0.137 Uiso 1 1 calc R . .
C56 C 0.3030(8) 0.6252(5) 0.3330(4) 0.143(4) Uani 1 1 d . . .
H56A H 0.2172 0.6629 0.3153 0.214 Uiso 1 1 calc R . .
H56B H 0.3246 0.5884 0.3073 0.214 Uiso 1 1 calc R . .
H56C H 0.3753 0.6528 0.3279 0.214 Uiso 1 1 calc R . .
C57 C -0.1102(5) 0.7936(3) 0.4585(3) 0.0607(17) Uani 1 1 d . . .
H57A H -0.0992 0.8302 0.4128 0.073 Uiso 1 1 calc R . .
H57B H -0.1624 0.7579 0.4524 0.073 Uiso 1 1 calc R . .
C58 C -0.1910(7) 0.8397(4) 0.5013(5) 0.113(3) Uani 1 1 d . . .
H58A H -0.1672 0.8077 0.5496 0.136 Uiso 1 1 calc R . .
H58B H -0.1547 0.8864 0.4925 0.136 Uiso 1 1 calc R . .
C59 C -0.3267(9) 0.8649(6) 0.4974(6) 0.160(4) Uani 1 1 d U . .
H59A H -0.3638 0.8199 0.4994 0.192 Uiso 1 1 calc R . .
H59B H -0.3505 0.9036 0.4513 0.192 Uiso 1 1 calc R . .
C60 C -0.4016(7) 0.9002(5) 0.5469(4) 0.112(3) Uani 1 1 d . . .
H60A H -0.4007 0.8596 0.5912 0.168 Uiso 1 1 calc R . .
H60B H -0.4953 0.9248 0.5303 0.168 Uiso 1 1 calc R . .
H60C H -0.3583 0.9396 0.5519 0.168 Uiso 1 1 calc R . .
C61 C 0.0429(5) 0.6797(3) 0.5815(3) 0.0594(16) Uani 1 1 d . . .
H61A H 0.1351 0.6489 0.5988 0.071 Uiso 1 1 calc R . .
H61B H 0.0118 0.7153 0.6083 0.071 Uiso 1 1 calc R . .
C62 C -0.0486(6) 0.6246(3) 0.5952(3) 0.0698(19) Uani 1 1 d . . .
H62A H -0.0154 0.5864 0.5710 0.084 Uiso 1 1 calc R . .
H62B H -0.1407 0.6543 0.5769 0.084 Uiso 1 1 calc R . .
C63 C -0.0557(8) 0.5808(5) 0.6718(4) 0.130(4) Uani 1 1 d . . .
H63A H 0.0367 0.5507 0.6893 0.156 Uiso 1 1 calc R . .
H63B H -0.0853 0.6197 0.6956 0.156 Uiso 1 1 calc R . .
C64 C -0.1410(8) 0.5305(5) 0.6887(4) 0.140(4) Uani 1 1 d . . .
H64A H -0.2319 0.5589 0.6694 0.209 Uiso 1 1 calc R . .
H64B H -0.1448 0.5091 0.7385 0.209 Uiso 1 1 calc R . .
H64C H -0.1066 0.4879 0.6701 0.209 Uiso 1 1 calc R . .
P2 P 0.58040(15) 0.75140(10) 0.98280(7) 0.0570(5) Uani 1 1 d . . .
P1 P 0.05412(14) 0.73759(8) 0.49422(7) 0.0476(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B2 C31 1.628(7) . ?
B2 C37 1.642(7) . ?
B2 C25 1.649(7) . ?
B2 C43 1.653(7) . ?
B1 C19 1.623(7) . ?
B1 C1 1.635(8) . ?
B1 C7 1.639(7) . ?
B1 C13 1.640(7) . ?
C25 C30 1.401(6) . ?
C25 C26 1.401(7) . ?
C26 C27 1.377(7) . ?
C27 C28 1.364(8) . ?
C28 C29 1.380(8) . ?
C29 C30 1.401(7) . ?
C31 C36 1.399(6) . ?
C31 C32 1.416(6) . ?
C32 C33 1.392(7) . ?
C33 C34 1.377(8) . ?
C34 C35 1.367(7) . ?
C35 C36 1.374(7) . ?
C37 C38 1.396(6) . ?
C37 C42 1.411(6) . ?
C38 C39 1.382(6) . ?
C39 C40 1.362(6) . ?
C40 C41 1.382(7) . ?
C41 C42 1.388(6) . ?
C43 C44 1.389(6) . ?
C43 C48 1.404(6) . ?
C44 C45 1.388(6) . ?
C45 C46 1.375(7) . ?
C46 C47 1.362(7) . ?
C47 C48 1.372(6) . ?
C1 C2 1.384(6) . ?
C1 C6 1.408(6) . ?
C2 C3 1.392(7) . ?
C3 C4 1.384(7) . ?
C4 C5 1.380(7) . ?
C5 C6 1.378(7) . ?
C7 C8 1.389(6) . ?
C7 C12 1.396(7) . ?
C8 C9 1.384(7) . ?
C9 C10 1.374(8) . ?
C10 C11 1.374(7) . ?
C11 C12 1.381(7) . ?
C13 C14 1.392(6) . ?
C13 C18 1.392(6) . ?
C14 C15 1.388(7) . ?
C15 C16 1.391(7) . ?
C16 C17 1.351(8) . ?
C17 C18 1.384(7) . ?
C19 C24 1.390(6) . ?
C19 C20 1.414(6) . ?
C20 C21 1.366(7) . ?
C21 C22 1.377(7) . ?
C22 C23 1.373(7) . ?
C23 C24 1.409(7) . ?
C65 C66 1.519(7) . ?
C65 P2 1.801(5) . ?
C66 C67 1.507(7) . ?
C67 C68 1.520(7) . ?
C69 C70 1.509(8) . ?
C69 P2 1.825(6) . ?
C70 C71 1.595(11) . ?
C71 C72 1.440(7) . ?
C73 C74 1.506(8) . ?
C73 P2 1.762(5) . ?
C74 C75 1.534(8) . ?
C75 C76 1.507(8) . ?
C77 C78 1.503(8) . ?
C77 P2 1.789(5) . ?
C78 C79 1.501(7) . ?
C79 C80 1.493(8) . ?
C49 C50 1.520(7) . ?
C49 P1 1.791(5) . ?
C50 C51 1.516(7) . ?
C51 C52 1.512(7) . ?
C53 C54 1.444(8) . ?
C53 P1 1.795(6) . ?
C54 C55 1.568(9) . ?
C55 C56 1.484(9) . ?
C57 C58 1.515(8) . ?
C57 P1 1.795(5) . ?
C58 C59 1.346(9) . ?
C59 C60 1.482(10) . ?
C61 C62 1.502(7) . ?
C61 P1 1.792(5) . ?
C62 C63 1.536(8) . ?
C63 C64 1.382(10) . ?

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
C31 B2 C37 105.7(4) . . ?
C31 B2 C25 113.7(4) . . ?
C37 B2 C25 109.5(4) . . ?
C31 B2 C43 110.9(4) . . ?
C37 B2 C43 113.3(4) . . ?
C25 B2 C43 103.9(4) . . ?
C19 B1 C1 104.1(4) . . ?
C19 B1 C7 112.8(4) . . ?
C1 B1 C7 113.8(4) . . ?
C19 B1 C13 111.8(4) . . ?
C1 B1 C13 110.6(4) . . ?
C7 B1 C13 104.0(4) . . ?
C30 C25 C26 115.0(5) . . ?
C30 C25 B2 125.3(5) . . ?
C26 C25 B2 119.7(4) . . ?
C27 C26 C25 124.1(5) . . ?
C28 C27 C26 119.3(6) . . ?
C27 C28 C29 119.7(6) . . ?
C28 C29 C30 120.6(6) . . ?
C25 C30 C29 121.3(6) . . ?
C36 C31 C32 113.8(5) . . ?
C36 C31 B2 124.6(4) . . ?
C32 C31 B2 121.5(4) . . ?
C33 C32 C31 122.4(5) . . ?
C34 C33 C32 120.4(5) . . ?
C35 C34 C33 119.0(6) . . ?
C34 C35 C36 120.4(6) . . ?
C35 C36 C31 124.0(5) . . ?
C38 C37 C42 113.6(4) . . ?
C38 C37 B2 124.1(4) . . ?
C42 C37 B2 122.2(4) . . ?
C39 C38 C37 123.8(5) . . ?
C40 C39 C38 120.9(5) . . ?
C39 C40 C41 118.2(5) . . ?
C40 C41 C42 120.6(5) . . ?
C41 C42 C37 122.9(5) . . ?
C44 C43 C48 114.6(4) . . ?
C44 C43 B2 125.6(4) . . ?
C48 C43 B2 119.7(4) . . ?
C45 C44 C43 122.5(5) . . ?
C46 C45 C44 121.0(5) . . ?
C47 C46 C45 117.8(5) . . ?
C46 C47 C48 121.4(5) . . ?
C47 C48 C43 122.7(5) . . ?
C2 C1 C6 114.3(5) . . ?
C2 C1 B1 121.9(4) . . ?
C6 C1 B1 123.5(5) . . ?
C1 C2 C3 123.4(5) . . ?
C4 C3 C2 120.0(5) . . ?
C5 C4 C3 118.7(5) . . ?
C6 C5 C4 119.9(5) . . ?
C5 C6 C1 123.6(5) . . ?
C8 C7 C12 114.8(5) . . ?
C8 C7 B1 125.0(5) . . ?
C12 C7 B1 120.1(4) . . ?
C9 C8 C7 123.0(5) . . ?
C10 C9 C8 119.9(5) . . ?
C11 C10 C9 119.3(5) . . ?
C10 C11 C12 119.7(5) . . ?
C11 C12 C7 123.2(5) . . ?
C14 C13 C18 114.5(5) . . ?
C14 C13 B1 122.0(5) . . ?
C18 C13 B1 123.4(4) . . ?
C15 C14 C13 123.2(5) . . ?
C14 C15 C16 119.5(5) . . ?
C17 C16 C15 119.0(5) . . ?
C16 C17 C18 120.5(6) . . ?
C17 C18 C13 123.3(5) . . ?
C24 C19 C20 114.3(5) . . ?
C24 C19 B1 123.8(4) . . ?
C20 C19 B1 121.6(4) . . ?
C21 C20 C19 123.3(5) . . ?
C20 C21 C22 120.9(5) . . ?
C23 C22 C21 118.5(5) . . ?
C22 C23 C24 120.2(5) . . ?
C19 C24 C23 122.6(5) . . ?
C66 C65 P2 114.8(4) . . ?
C67 C66 C65 114.2(5) . . ?
C66 C67 C68 112.1(5) . . ?
C70 C69 P2 115.7(5) . . ?
C69 C70 C71 112.1(7) . . ?
C72 C71 C70 107.5(9) . . ?
C74 C73 P2 116.4(4) . . ?
C73 C74 C75 114.6(5) . . ?
C76 C75 C74 113.7(5) . . ?
C78 C77 P2 115.7(4) . . ?
C79 C78 C77 113.2(5) . . ?
C80 C79 C78 114.2(5) . . ?
C50 C49 P1 115.9(4) . . ?
C51 C50 C49 113.0(5) . . ?
C52 C51 C50 112.7(5) . . ?
C54 C53 P1 116.0(5) . . ?
C53 C54 C55 110.9(6) . . ?
C56 C55 C54 117.4(6) . . ?
C58 C57 P1 114.2(4) . . ?
C59 C58 C57 124.1(8) . . ?
C58 C59 C60 121.6(9) . . ?
C62 C61 P1 116.6(4) . . ?
C61 C62 C63 112.1(6) . . ?
C64 C63 C62 115.6(7) . . ?
C73 P2 C77 113.3(3) . . ?
C73 P2 C65 111.2(3) . . ?
C77 P2 C65 105.5(3) . . ?
C73 P2 C69 105.4(3) . . ?
C77 P2 C69 110.4(3) . . ?
C65 P2 C69 111.2(3) . . ?
C49 P1 C61 106.2(3) . . ?
C49 P1 C57 113.4(3) . . ?
C61 P1 C57 110.8(3) . . ?
C49 P1 C53 109.9(3) . . ?
C61 P1 C53 112.3(3) . . ?
C57 P1 C53 104.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.052
