# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_CaLe172
_database_code_depnum_ccdc_archive 'CCDC 2169207'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        1-Phen
_chemical_name_common            B2(Phen)2(NMe2)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H33 B2 N2'
_chemical_formula_sum            'C35 H33 B2 N2'
_chemical_formula_weight         503.25

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

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

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

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

_cell_length_a                   9.694(4)
_cell_length_b                   12.008(5)
_cell_length_c                   12.976(5)
_cell_angle_alpha                74.380(18)
_cell_angle_beta                 80.89(2)
_cell_angle_gamma                71.04(2)
_cell_volume                     1371.6(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    5019
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      26.76


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Oxford Cryostream 700).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_F_000             534
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.814
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.312
_exptl_absorpt_coefficient_mu    0.069
_shelx_estimated_absorpt_T_min   0.946
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4242
_exptl_absorpt_correction_T_max  0.7454
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4.00 3.00 2.00 0.1710
-4.00 -3.00 -2.00 0.3380
0.00 4.00 -1.00 0.0730
0.00 -4.00 1.00 0.1830
4.00 -1.00 3.00 0.2360
0.00 0.00 -1.00 0.0240
0.00 0.00 1.00 0.1560
0.00 2.00 1.00 0.1220
0.00 -2.00 -1.00 0.1640

_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            23775
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.635
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5402
_reflns_number_gt                3649
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_refine_special_details          
;

 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0396P)²+0.4065P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5402
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1293
_refine_ls_wR_factor_gt          0.1147
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1_1 B 1.1790(2) 0.60271(19) 0.75508(18) 0.0171(5) Uani 1 1 d . . . . .
N1_1 N 1.26025(18) 0.58866(15) 0.83964(13) 0.0206(4) Uani 1 1 d . . . . .
C1_1 C 1.3838(2) 0.63656(19) 0.83021(17) 0.0273(5) Uani 1 1 d . . . . .
H1A_1 H 1.468972 0.571029 0.859403 0.041 Uiso 1 1 calc R U . . .
H1B_1 H 1.357763 0.699798 0.870462 0.041 Uiso 1 1 calc R U . . .
H1C_1 H 1.407452 0.670897 0.754463 0.041 Uiso 1 1 calc R U . . .
B2_1 B 1.0307(2) 0.5518(2) 0.76580(17) 0.0162(5) Uani 1 1 d . . . . .
N2_1 N 1.03831(17) 0.42932(14) 0.78437(12) 0.0174(4) Uani 1 1 d . . . . .
C3_1 C 1.1712(2) 0.32976(18) 0.81065(16) 0.0230(5) Uani 1 1 d . . . . .
H3A_1 H 1.189780 0.275716 0.762014 0.035 Uiso 1 1 calc R U . . .
H3B_1 H 1.159115 0.284491 0.884876 0.035 Uiso 1 1 calc R U . . .
H3C_1 H 1.253938 0.362112 0.802745 0.035 Uiso 1 1 calc R U . . .
C4_1 C 0.9153(2) 0.38520(18) 0.78076(17) 0.0239(5) Uani 1 1 d . . . . .
H4A_1 H 0.903615 0.326602 0.848082 0.036 Uiso 1 1 calc R U . . .
H4B_1 H 0.934363 0.346023 0.720594 0.036 Uiso 1 1 calc R U . . .
H4C_1 H 0.825507 0.453470 0.771178 0.036 Uiso 1 1 calc R U . . .
C2_1 C 1.2325(2) 0.52304(19) 0.94920(16) 0.0273(5) Uani 1 1 d . . . . .
H2A_1 H 1.216056 0.576238 0.998300 0.041 Uiso 1 1 calc R U . . .
H2B_1 H 1.317119 0.452106 0.969214 0.041 Uiso 1 1 calc R U . . .
H2C_1 H 1.145617 0.496684 0.953676 0.041 Uiso 1 1 calc R U . . .
C1_2 C 1.2183(2) 0.67527(17) 0.63754(15) 0.0166(4) Uani 1 1 d . . . . .
C2_2 C 1.1841(2) 0.80641(17) 0.60923(15) 0.0159(4) Uani 1 1 d . . . . .
C3_2 C 1.1146(2) 0.87490(17) 0.68602(16) 0.0185(4) Uani 1 1 d . . . . .
H3_2 H 1.090008 0.834088 0.756687 0.022 Uiso 1 1 calc R U . . .
C4_2 C 1.0815(2) 0.99882(18) 0.66153(16) 0.0197(4) Uani 1 1 d . . . . .
H4_2 H 1.034599 1.042858 0.714664 0.024 Uiso 1 1 calc R U . . .
C5_2 C 1.1174(2) 1.05965(18) 0.55778(16) 0.0200(5) Uani 1 1 d . . . . .
H5_2 H 1.095309 1.145333 0.540374 0.024 Uiso 1 1 calc R U . . .
C6_2 C 1.1845(2) 0.99582(17) 0.48092(16) 0.0184(4) Uani 1 1 d . . . . .
H6_2 H 1.208535 1.038470 0.410865 0.022 Uiso 1 1 calc R U . . .
C7_2 C 1.2187(2) 0.86874(17) 0.50327(15) 0.0164(4) Uani 1 1 d . . . . .
C8_2 C 1.2876(2) 0.79988(17) 0.42221(15) 0.0175(4) Uani 1 1 d . . . . .
C9_2 C 1.3290(2) 0.85448(19) 0.31553(16) 0.0217(5) Uani 1 1 d . . . . .
H9_2 H 1.309946 0.939877 0.294453 0.026 Uiso 1 1 calc R U . . .
C10_2 C 1.3962(2) 0.7855(2) 0.24210(16) 0.0249(5) Uani 1 1 d . . . . .
H10_2 H 1.425012 0.823567 0.171491 0.030 Uiso 1 1 calc R U . . .
C11_2 C 1.4225(2) 0.65972(19) 0.27071(16) 0.0244(5) Uani 1 1 d . . . . .
H11_2 H 1.467210 0.612934 0.219203 0.029 Uiso 1 1 calc R U . . .
C12_2 C 1.3835(2) 0.60410(19) 0.37317(16) 0.0219(5) Uani 1 1 d . . . . .
H12_2 H 1.401942 0.518726 0.392285 0.026 Uiso 1 1 calc R U . . .
C13_2 C 1.3160(2) 0.67266(17) 0.45070(15) 0.0176(4) Uani 1 1 d . . . . .
C14_2 C 1.2794(2) 0.61410(17) 0.55875(15) 0.0184(4) Uani 1 1 d . . . . .
H14_2 H 1.298487 0.528668 0.576307 0.022 Uiso 1 1 calc R U . . .
C21_3 C 0.8765(2) 0.65186(17) 0.74689(15) 0.0160(4) Uani 1 1 d . . . . .
C22_3 C 0.8027(2) 0.68270(16) 0.64946(15) 0.0149(4) Uani 1 1 d . . . . .
C23_3 C 0.8694(2) 0.62552(17) 0.56453(15) 0.0184(4) Uani 1 1 d . . . . .
H23_3 H 0.963449 0.567698 0.571585 0.022 Uiso 1 1 calc R U . . .
C24_3 C 0.8014(2) 0.65161(17) 0.47200(15) 0.0191(4) Uani 1 1 d . . . . .
H24_3 H 0.848342 0.612142 0.415889 0.023 Uiso 1 1 calc R U . . .
C25_3 C 0.6632(2) 0.73630(18) 0.46077(16) 0.0210(5) Uani 1 1 d . . . . .
H25_3 H 0.615259 0.753460 0.397373 0.025 Uiso 1 1 calc R U . . .
C26_3 C 0.5963(2) 0.79488(18) 0.54100(15) 0.0200(4) Uani 1 1 d . . . . .
H26_3 H 0.502810 0.853222 0.531828 0.024 Uiso 1 1 calc R U . . .
C27_3 C 0.6634(2) 0.77024(17) 0.63677(15) 0.0167(4) Uani 1 1 d . . . . .
C28_3 C 0.5936(2) 0.83205(17) 0.72275(15) 0.0171(4) Uani 1 1 d . . . . .
C29_3 C 0.4546(2) 0.91930(18) 0.71750(16) 0.0200(4) Uani 1 1 d . . . . .
H29_3 H 0.404417 0.941934 0.654332 0.024 Uiso 1 1 calc R U . . .
C30_3 C 0.3902(2) 0.97218(18) 0.80162(16) 0.0232(5) Uani 1 1 d . . . . .
H30_3 H 0.296319 1.030410 0.796261 0.028 Uiso 1 1 calc R U . . .
C31_3 C 0.4624(2) 0.94063(18) 0.89517(16) 0.0238(5) Uani 1 1 d . . . . .
H31_3 H 0.417120 0.976632 0.953620 0.029 Uiso 1 1 calc R U . . .
C32_3 C 0.5984(2) 0.85768(18) 0.90232(16) 0.0217(5) Uani 1 1 d . . . . .
H32_3 H 0.647446 0.837607 0.965680 0.026 Uiso 1 1 calc R U . . .
C33_3 C 0.6675(2) 0.80119(17) 0.81690(15) 0.0174(4) Uani 1 1 d . . . . .
C34_3 C 0.8085(2) 0.71340(17) 0.82426(15) 0.0177(4) Uani 1 1 d . . . . .
H34_3 H 0.857939 0.696839 0.886818 0.021 Uiso 1 1 calc R U . . .
C1_4 C 0.1233(2) 0.9078(2) 1.03601(17) 0.0311(5) Uani 1 1 d . . . . .
H1_4 H 0.207945 0.844355 1.060852 0.037 Uiso 1 1 calc R U . . .
C2_4 C 0.0890(3) 1.0177(2) 1.06361(17) 0.0316(6) Uani 1 1 d . . . . .
H2_4 H 0.150307 1.029794 1.107225 0.038 Uiso 1 1 calc R U . . .
C3_4 C -0.0339(3) 1.1095(2) 1.02810(17) 0.0323(6) Uani 1 1 d . . . . .
H3_4 H -0.057500 1.184785 1.047481 0.039 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1_1 N1_1 1.393(3) . ?
B1_1 C1_2 1.596(3) . ?
B1_1 B2_1 1.709(3) . ?
N1_1 C2_1 1.459(3) . ?
N1_1 C1_1 1.464(3) . ?
C1_1 H1A_1 0.9800 . ?
C1_1 H1B_1 0.9800 . ?
C1_1 H1C_1 0.9800 . ?
B2_1 N2_1 1.404(3) . ?
B2_1 C21_3 1.590(3) . ?
N2_1 C3_1 1.457(2) . ?
N2_1 C4_1 1.465(3) . ?
C3_1 H3A_1 0.9800 . ?
C3_1 H3B_1 0.9800 . ?
C3_1 H3C_1 0.9800 . ?
C4_1 H4A_1 0.9800 . ?
C4_1 H4B_1 0.9800 . ?
C4_1 H4C_1 0.9800 . ?
C2_1 H2A_1 0.9800 . ?
C2_1 H2B_1 0.9800 . ?
C2_1 H2C_1 0.9800 . ?
C1_2 C14_2 1.366(3) . ?
C1_2 C2_2 1.453(3) . ?
C2_2 C3_2 1.411(3) . ?
C2_2 C7_2 1.423(3) . ?
C3_2 C4_2 1.373(3) . ?
C3_2 H3_2 0.9500 . ?
C4_2 C5_2 1.398(3) . ?
C4_2 H4_2 0.9500 . ?
C5_2 C6_2 1.374(3) . ?
C5_2 H5_2 0.9500 . ?
C6_2 C7_2 1.409(3) . ?
C6_2 H6_2 0.9500 . ?
C7_2 C8_2 1.457(3) . ?
C8_2 C13_2 1.415(3) . ?
C8_2 C9_2 1.419(3) . ?
C9_2 C10_2 1.377(3) . ?
C9_2 H9_2 0.9500 . ?
C10_2 C11_2 1.401(3) . ?
C10_2 H10_2 0.9500 . ?
C11_2 C12_2 1.372(3) . ?
C11_2 H11_2 0.9500 . ?
C12_2 C13_2 1.416(3) . ?
C12_2 H12_2 0.9500 . ?
C13_2 C14_2 1.435(3) . ?
C14_2 H14_2 0.9500 . ?
C21_3 C34_3 1.365(3) . ?
C21_3 C22_3 1.452(3) . ?
C22_3 C23_3 1.413(3) . ?
C22_3 C27_3 1.418(3) . ?
C23_3 C24_3 1.374(3) . ?
C23_3 H23_3 0.9500 . ?
C24_3 C25_3 1.396(3) . ?
C24_3 H24_3 0.9500 . ?
C25_3 C26_3 1.372(3) . ?
C25_3 H25_3 0.9500 . ?
C26_3 C27_3 1.410(3) . ?
C26_3 H26_3 0.9500 . ?
C27_3 C28_3 1.461(3) . ?
C28_3 C29_3 1.411(3) . ?
C28_3 C33_3 1.415(3) . ?
C29_3 C30_3 1.373(3) . ?
C29_3 H29_3 0.9500 . ?
C30_3 C31_3 1.398(3) . ?
C30_3 H30_3 0.9500 . ?
C31_3 C32_3 1.370(3) . ?
C31_3 H31_3 0.9500 . ?
C32_3 C33_3 1.418(3) . ?
C32_3 H32_3 0.9500 . ?
C33_3 C34_3 1.428(3) . ?
C34_3 H34_3 0.9500 . ?
C1_4 C2_4 1.382(3) . ?
C1_4 C3_4 1.388(3) 2_577 ?
C1_4 H1_4 0.9500 . ?
C2_4 C3_4 1.376(3) . ?
C2_4 H2_4 0.9500 . ?
C3_4 H3_4 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1_1 B1_1 C1_2 120.11(18) . . ?
N1_1 B1_1 B2_1 125.24(18) . . ?
C1_2 B1_1 B2_1 114.61(16) . . ?
B1_1 N1_1 C2_1 123.67(18) . . ?
B1_1 N1_1 C1_1 124.75(17) . . ?
C2_1 N1_1 C1_1 111.58(16) . . ?
N1_1 C1_1 H1A_1 109.5 . . ?
N1_1 C1_1 H1B_1 109.5 . . ?
H1A_1 C1_1 H1B_1 109.5 . . ?
N1_1 C1_1 H1C_1 109.5 . . ?
H1A_1 C1_1 H1C_1 109.5 . . ?
H1B_1 C1_1 H1C_1 109.5 . . ?
N2_1 B2_1 C21_3 118.90(18) . . ?
N2_1 B2_1 B1_1 124.26(18) . . ?
C21_3 B2_1 B1_1 116.75(17) . . ?
B2_1 N2_1 C3_1 123.60(17) . . ?
B2_1 N2_1 C4_1 124.84(17) . . ?
C3_1 N2_1 C4_1 111.56(16) . . ?
N2_1 C3_1 H3A_1 109.5 . . ?
N2_1 C3_1 H3B_1 109.5 . . ?
H3A_1 C3_1 H3B_1 109.5 . . ?
N2_1 C3_1 H3C_1 109.5 . . ?
H3A_1 C3_1 H3C_1 109.5 . . ?
H3B_1 C3_1 H3C_1 109.5 . . ?
N2_1 C4_1 H4A_1 109.5 . . ?
N2_1 C4_1 H4B_1 109.5 . . ?
H4A_1 C4_1 H4B_1 109.5 . . ?
N2_1 C4_1 H4C_1 109.5 . . ?
H4A_1 C4_1 H4C_1 109.5 . . ?
H4B_1 C4_1 H4C_1 109.5 . . ?
N1_1 C2_1 H2A_1 109.5 . . ?
N1_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
N1_1 C2_1 H2C_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
C14_2 C1_2 C2_2 118.16(17) . . ?
C14_2 C1_2 B1_1 119.67(17) . . ?
C2_2 C1_2 B1_1 122.09(17) . . ?
C3_2 C2_2 C7_2 118.51(18) . . ?
C3_2 C2_2 C1_2 120.69(17) . . ?
C7_2 C2_2 C1_2 120.80(17) . . ?
C4_2 C3_2 C2_2 121.90(18) . . ?
C4_2 C3_2 H3_2 119.1 . . ?
C2_2 C3_2 H3_2 119.1 . . ?
C3_2 C4_2 C5_2 119.46(19) . . ?
C3_2 C4_2 H4_2 120.3 . . ?
C5_2 C4_2 H4_2 120.3 . . ?
C6_2 C5_2 C4_2 120.16(19) . . ?
C6_2 C5_2 H5_2 119.9 . . ?
C4_2 C5_2 H5_2 119.9 . . ?
C5_2 C6_2 C7_2 121.73(18) . . ?
C5_2 C6_2 H6_2 119.1 . . ?
C7_2 C6_2 H6_2 119.1 . . ?
C6_2 C7_2 C2_2 118.23(18) . . ?
C6_2 C7_2 C8_2 122.41(17) . . ?
C2_2 C7_2 C8_2 119.35(17) . . ?
C13_2 C8_2 C9_2 118.10(18) . . ?
C13_2 C8_2 C7_2 118.90(17) . . ?
C9_2 C8_2 C7_2 122.99(18) . . ?
C10_2 C9_2 C8_2 120.98(19) . . ?
C10_2 C9_2 H9_2 119.5 . . ?
C8_2 C9_2 H9_2 119.5 . . ?
C9_2 C10_2 C11_2 120.50(19) . . ?
C9_2 C10_2 H10_2 119.7 . . ?
C11_2 C10_2 H10_2 119.7 . . ?
C12_2 C11_2 C10_2 119.97(19) . . ?
C12_2 C11_2 H11_2 120.0 . . ?
C10_2 C11_2 H11_2 120.0 . . ?
C11_2 C12_2 C13_2 120.68(19) . . ?
C11_2 C12_2 H12_2 119.7 . . ?
C13_2 C12_2 H12_2 119.7 . . ?
C8_2 C13_2 C12_2 119.75(18) . . ?
C8_2 C13_2 C14_2 119.57(18) . . ?
C12_2 C13_2 C14_2 120.67(18) . . ?
C1_2 C14_2 C13_2 123.17(18) . . ?
C1_2 C14_2 H14_2 118.4 . . ?
C13_2 C14_2 H14_2 118.4 . . ?
C34_3 C21_3 C22_3 117.26(17) . . ?
C34_3 C21_3 B2_1 119.70(17) . . ?
C22_3 C21_3 B2_1 123.04(17) . . ?
C23_3 C22_3 C27_3 118.43(17) . . ?
C23_3 C22_3 C21_3 120.21(17) . . ?
C27_3 C22_3 C21_3 121.36(17) . . ?
C24_3 C23_3 C22_3 121.54(18) . . ?
C24_3 C23_3 H23_3 119.2 . . ?
C22_3 C23_3 H23_3 119.2 . . ?
C23_3 C24_3 C25_3 119.75(18) . . ?
C23_3 C24_3 H24_3 120.1 . . ?
C25_3 C24_3 H24_3 120.1 . . ?
C26_3 C25_3 C24_3 120.21(18) . . ?
C26_3 C25_3 H25_3 119.9 . . ?
C24_3 C25_3 H25_3 119.9 . . ?
C25_3 C26_3 C27_3 121.35(19) . . ?
C25_3 C26_3 H26_3 119.3 . . ?
C27_3 C26_3 H26_3 119.3 . . ?
C26_3 C27_3 C22_3 118.70(18) . . ?
C26_3 C27_3 C28_3 121.96(18) . . ?
C22_3 C27_3 C28_3 119.34(17) . . ?
C29_3 C28_3 C33_3 118.33(18) . . ?
C29_3 C28_3 C27_3 123.17(17) . . ?
C33_3 C28_3 C27_3 118.49(17) . . ?
C30_3 C29_3 C28_3 121.47(19) . . ?
C30_3 C29_3 H29_3 119.3 . . ?
C28_3 C29_3 H29_3 119.3 . . ?
C29_3 C30_3 C31_3 120.23(19) . . ?
C29_3 C30_3 H30_3 119.9 . . ?
C31_3 C30_3 H30_3 119.9 . . ?
C32_3 C31_3 C30_3 119.83(19) . . ?
C32_3 C31_3 H31_3 120.1 . . ?
C30_3 C31_3 H31_3 120.1 . . ?
C31_3 C32_3 C33_3 121.24(19) . . ?
C31_3 C32_3 H32_3 119.4 . . ?
C33_3 C32_3 H32_3 119.4 . . ?
C28_3 C33_3 C32_3 118.89(18) . . ?
C28_3 C33_3 C34_3 119.50(17) . . ?
C32_3 C33_3 C34_3 121.60(18) . . ?
C21_3 C34_3 C33_3 123.98(18) . . ?
C21_3 C34_3 H34_3 118.0 . . ?
C33_3 C34_3 H34_3 118.0 . . ?
C2_4 C1_4 C3_4 119.8(2) . 2_577 ?
C2_4 C1_4 H1_4 120.1 . . ?
C3_4 C1_4 H1_4 120.1 2_577 . ?
C3_4 C2_4 C1_4 120.2(2) . . ?
C3_4 C2_4 H2_4 119.9 . . ?
C1_4 C2_4 H2_4 119.9 . . ?
C2_4 C3_4 C1_4 120.0(2) . 2_577 ?
C2_4 C3_4 H3_4 120.0 . . ?
C1_4 C3_4 H3_4 120.0 2_577 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1_2 B1_1 N1_1 C2_1 -179.53(18) . . . . ?
B2_1 B1_1 N1_1 C2_1 2.8(3) . . . . ?
C1_2 B1_1 N1_1 C1_1 0.1(3) . . . . ?
B2_1 B1_1 N1_1 C1_1 -177.65(18) . . . . ?
N1_1 B1_1 B2_1 N2_1 -71.3(3) . . . . ?
C1_2 B1_1 B2_1 N2_1 110.9(2) . . . . ?
N1_1 B1_1 B2_1 C21_3 112.1(2) . . . . ?
C1_2 B1_1 B2_1 C21_3 -65.7(2) . . . . ?
C21_3 B2_1 N2_1 C3_1 -175.20(17) . . . . ?
B1_1 B2_1 N2_1 C3_1 8.3(3) . . . . ?
C21_3 B2_1 N2_1 C4_1 4.3(3) . . . . ?
B1_1 B2_1 N2_1 C4_1 -172.16(17) . . . . ?
N1_1 B1_1 C1_2 C14_2 109.4(2) . . . . ?
B2_1 B1_1 C1_2 C14_2 -72.7(2) . . . . ?
N1_1 B1_1 C1_2 C2_2 -74.0(2) . . . . ?
B2_1 B1_1 C1_2 C2_2 104.0(2) . . . . ?
C14_2 C1_2 C2_2 C3_2 176.99(17) . . . . ?
B1_1 C1_2 C2_2 C3_2 0.3(3) . . . . ?
C14_2 C1_2 C2_2 C7_2 -2.4(3) . . . . ?
B1_1 C1_2 C2_2 C7_2 -179.08(17) . . . . ?
C7_2 C2_2 C3_2 C4_2 -0.8(3) . . . . ?
C1_2 C2_2 C3_2 C4_2 179.81(18) . . . . ?
C2_2 C3_2 C4_2 C5_2 0.0(3) . . . . ?
C3_2 C4_2 C5_2 C6_2 0.4(3) . . . . ?
C4_2 C5_2 C6_2 C7_2 0.2(3) . . . . ?
C5_2 C6_2 C7_2 C2_2 -1.1(3) . . . . ?
C5_2 C6_2 C7_2 C8_2 178.97(18) . . . . ?
C3_2 C2_2 C7_2 C6_2 1.4(3) . . . . ?
C1_2 C2_2 C7_2 C6_2 -179.26(17) . . . . ?
C3_2 C2_2 C7_2 C8_2 -178.71(17) . . . . ?
C1_2 C2_2 C7_2 C8_2 0.6(3) . . . . ?
C6_2 C7_2 C8_2 C13_2 -178.93(17) . . . . ?
C2_2 C7_2 C8_2 C13_2 1.2(3) . . . . ?
C6_2 C7_2 C8_2 C9_2 1.5(3) . . . . ?
C2_2 C7_2 C8_2 C9_2 -178.38(18) . . . . ?
C13_2 C8_2 C9_2 C10_2 -0.7(3) . . . . ?
C7_2 C8_2 C9_2 C10_2 178.87(18) . . . . ?
C8_2 C9_2 C10_2 C11_2 1.4(3) . . . . ?
C9_2 C10_2 C11_2 C12_2 -1.2(3) . . . . ?
C10_2 C11_2 C12_2 C13_2 0.3(3) . . . . ?
C9_2 C8_2 C13_2 C12_2 -0.2(3) . . . . ?
C7_2 C8_2 C13_2 C12_2 -179.78(17) . . . . ?
C9_2 C8_2 C13_2 C14_2 178.28(17) . . . . ?
C7_2 C8_2 C13_2 C14_2 -1.3(3) . . . . ?
C11_2 C12_2 C13_2 C8_2 0.4(3) . . . . ?
C11_2 C12_2 C13_2 C14_2 -178.09(18) . . . . ?
C2_2 C1_2 C14_2 C13_2 2.3(3) . . . . ?
B1_1 C1_2 C14_2 C13_2 179.10(18) . . . . ?
C8_2 C13_2 C14_2 C1_2 -0.5(3) . . . . ?
C12_2 C13_2 C14_2 C1_2 177.99(18) . . . . ?
N2_1 B2_1 C21_3 C34_3 108.6(2) . . . . ?
B1_1 B2_1 C21_3 C34_3 -74.6(2) . . . . ?
N2_1 B2_1 C21_3 C22_3 -71.8(2) . . . . ?
B1_1 B2_1 C21_3 C22_3 105.0(2) . . . . ?
C34_3 C21_3 C22_3 C23_3 177.77(17) . . . . ?
B2_1 C21_3 C22_3 C23_3 -1.9(3) . . . . ?
C34_3 C21_3 C22_3 C27_3 -2.1(3) . . . . ?
B2_1 C21_3 C22_3 C27_3 178.28(17) . . . . ?
C27_3 C22_3 C23_3 C24_3 -1.0(3) . . . . ?
C21_3 C22_3 C23_3 C24_3 179.11(18) . . . . ?
C22_3 C23_3 C24_3 C25_3 -0.1(3) . . . . ?
C23_3 C24_3 C25_3 C26_3 1.1(3) . . . . ?
C24_3 C25_3 C26_3 C27_3 -1.0(3) . . . . ?
C25_3 C26_3 C27_3 C22_3 -0.2(3) . . . . ?
C25_3 C26_3 C27_3 C28_3 179.86(18) . . . . ?
C23_3 C22_3 C27_3 C26_3 1.1(3) . . . . ?
C21_3 C22_3 C27_3 C26_3 -179.02(17) . . . . ?
C23_3 C22_3 C27_3 C28_3 -178.89(17) . . . . ?
C21_3 C22_3 C27_3 C28_3 1.0(3) . . . . ?
C26_3 C27_3 C28_3 C29_3 0.7(3) . . . . ?
C22_3 C27_3 C28_3 C29_3 -179.27(18) . . . . ?
C26_3 C27_3 C28_3 C33_3 179.31(18) . . . . ?
C22_3 C27_3 C28_3 C33_3 -0.7(3) . . . . ?
C33_3 C28_3 C29_3 C30_3 -1.1(3) . . . . ?
C27_3 C28_3 C29_3 C30_3 177.53(19) . . . . ?
C28_3 C29_3 C30_3 C31_3 0.3(3) . . . . ?
C29_3 C30_3 C31_3 C32_3 0.7(3) . . . . ?
C30_3 C31_3 C32_3 C33_3 -1.0(3) . . . . ?
C29_3 C28_3 C33_3 C32_3 0.8(3) . . . . ?
C27_3 C28_3 C33_3 C32_3 -177.84(17) . . . . ?
C29_3 C28_3 C33_3 C34_3 -179.85(17) . . . . ?
C27_3 C28_3 C33_3 C34_3 1.5(3) . . . . ?
C31_3 C32_3 C33_3 C28_3 0.2(3) . . . . ?
C31_3 C32_3 C33_3 C34_3 -179.14(19) . . . . ?
C22_3 C21_3 C34_3 C33_3 3.0(3) . . . . ?
B2_1 C21_3 C34_3 C33_3 -177.32(18) . . . . ?
C28_3 C33_3 C34_3 C21_3 -2.8(3) . . . . ?
C32_3 C33_3 C34_3 C21_3 176.49(18) . . . . ?
C3_4 C1_4 C2_4 C3_4 0.3(4) 2_577 . . . ?
C1_4 C2_4 C3_4 C1_4 -0.3(4) . . . 2_577 ?

_refine_diff_density_max         0.234
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.047


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

data_AnLa062_AlOk_twin1_hklf5
_database_code_depnum_ccdc_archive 'CCDC 2169210'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT084_AnLa062_AlOk_twin1_hklf5 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.26 Report
RESPONSE: Due to twinning and poor diffraction
;

_audit_creation_method           'CIF-fill 1.2x (K.Radacki, 2005-21)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 B2 P2, 3(C6 H6)'
_chemical_formula_sum            'C52 H54 B2 P2'
_chemical_formula_weight         762.5660

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.1596(3)
_cell_length_b                   9.7622(4)
_cell_length_c                   13.7547(5)
_cell_angle_alpha                106.196(3)
_cell_angle_beta                 97.907(3)
_cell_angle_gamma                109.115(3)
_cell_volume                     1079.89(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7526
_cell_measurement_theta_min      3.4360
_cell_measurement_theta_max      72.7430


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800).
;
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_F_000             406
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.083
_exptl_absorpt_coefficient_mu    1.162
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.40282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 
ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0570
1 -1 1 0.0589
0 -1 1 0.0428
-1 -1 1 0.0861
-1 0 0 0.0861
-1 1 -1 0.0512
0 1 -1 0.0454
1 1 -1 0.0463
1 -1 0 0.0160
-1 1 0 0.0665
0 -1 0 0.0109
0 1 0 0.0838
0 1 0 0.0744
0 1 0 0.0635
1 1 0 0.0453
-1 -1 0 0.0311
1 0 1 0.0824
-1 0 -1 0.0452
-1 1 1 0.0523
1 -1 -1 0.0273
1 0 -1 0.0438
-1 0 1 0.0422
1 1 1 0.0818
-1 -1 -1 0.0469
0 0 1 0.0868
0 0 -1 0.0133

_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_details      
;
 List of Runs (angles in degrees, time in seconds):
 
   # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
 --------------------------------------------------------------------------
   1  ω     15.00  68.00   0.50    1.22    --   58.41 -97.00-138.00  106
   2  ω    -68.00 -16.00   0.50    1.22    --  -60.06  97.00 -30.00  104
   3  ω    -70.00 -44.00   0.50    1.22    --  -69.47  97.00 -30.00   52
   4  ω     43.00  69.00   0.50    1.22    --   71.12 -97.00-138.00   52
   5  ω    -83.00 -58.00   0.50    1.22    --  -76.33  97.00 -30.00   50
   6  ω     41.00  66.00   0.50    1.22    --   82.37 -97.00-138.00   50
   7  ω    -16.00   9.00   0.50    1.22    --  -14.00  89.00 166.73   50
   8  ω    -99.00 -65.00   0.50    1.22    --  -50.00 -48.00  17.09   68
   9  ω   -105.00 -65.00   0.50    1.22    --  -54.00 -35.00  52.70   80
  10  ω     34.00  59.00   0.50    1.22    --   58.41 -95.00  30.00   50
  11  ω   -115.00 -80.00   0.50    1.22    --  -66.00 -48.00 113.52   70
  12  ω   -118.00 -90.00   0.50    1.22    --  -74.00 -54.00 -49.67   56
  13  ω   -127.00 -99.00   0.50    1.22    --  -78.00 -47.00-118.04   56
  14  ω   -126.00 -96.00   0.50    1.22    --  -79.50 -52.00 -26.36   60
  15  ω    -91.00 -36.00   0.50    1.22    --  -79.50 101.00 124.47  110
  16  ω   -124.00 -91.00   0.50    1.22    --  -79.50 -62.00 176.74   66
  17  ω    -96.00 -47.00   0.50    1.22    --  -79.50 120.00  29.68   98
  18  ω   -130.00-105.00   0.50    1.22    --  -79.50 -40.00  43.28   50
  19  ω   -124.00 -98.00   0.50    1.22    --  -79.50 -65.00-137.79   52
  20  ω   -115.00 -89.00   0.50    1.22    --  -79.50-129.00-105.67   52
  21  ω    -99.00 -42.00   0.50    1.22    --  -79.50 118.00-132.92  114
  22  ω   -128.00 -93.00   0.50    1.22    --  -79.50 -52.00 -81.67   70
  23  ω     95.00 129.00   0.50    1.22    --   82.00  55.00 -65.67   68
  24  ω     36.00  62.00   0.50    1.22    --   82.37-112.00 -90.00   52
  25  ω     74.00 100.00   0.50    1.22    --   82.37-112.00-120.00   52
  26  ω     46.00  78.00   0.50    1.22    --   82.37 -95.00 -30.00   64
  27  ω     45.00 100.00   0.50    1.22    --   82.37-112.00  30.00  110
  28  ω     41.00  81.00   0.50    1.22    --   82.37 -95.00   0.00   80
  29  ω     56.00 100.00   0.50    1.22    --   82.37-112.00 -60.00   88
  30  ω     48.00  77.00   0.50    1.22    --   82.37 -95.00-150.00   58
  31  ω     74.00 100.00   0.50    1.22    --   82.37-112.00 120.00   52
  32  ω     46.00  72.00   0.50    1.22    --   82.37-112.00 -30.00   52
  33  ω     47.00  73.00   0.50    1.22    --   82.37 -95.00-120.00   52
  34  ω    107.00 132.00   0.50    1.22    --   82.37  15.00-150.00   50
  35  ω     79.00 105.00   0.50    1.22    --   82.37  15.00-120.00   52
  36  ω     43.00  69.00   0.50    1.22    --   82.37 -95.00-180.00   52
  37  ω     71.00 100.00   0.50    1.22    --   82.37-112.00 -90.00   58
  38  ω     74.00 100.00   0.50    1.22    --   82.37-112.00  60.00   52
  39  ω     73.00  99.00   0.50    1.22    --   82.37-112.00  90.00   52
  40  ω     71.00  97.00   0.50    1.22    --   82.37  15.00 -60.00   52
  41  ω     74.00 100.00   0.50    1.22    --   82.37-112.00 -30.00   52
  42  ω     42.00  68.00   0.50    1.22    --   82.37-112.00   0.00   52
  43  ω     75.00 100.00   0.50    1.22    --   82.37-112.00   0.00   50
  44  ω     73.00  99.00   0.50    1.22    --   82.37  15.00-150.00   52
  45  ω     41.00  67.00   0.50    1.22    --   82.37-112.00-120.00   52
  46  ω     45.00  70.00   0.50    1.22    --   85.25 -76.00 112.84   50
  47  ω    104.00 130.00   0.50    1.22    --   85.25 114.00  55.10   52
  48  ω    106.00 132.00   0.50    1.22    --   85.25  47.00 -44.86   52
  49  ω     97.00 122.00   0.50    1.22    --   85.25  38.00 100.75   50
  50  ω    100.00 132.00   0.50    1.22    --   85.25 130.00 -62.27   64
  51  ω     45.00  71.00   0.50    1.22    --   85.25 -95.00 -81.15   52
  52  ω    102.00 127.00   0.50    1.22    --   85.25  54.00 148.22   50
  53  ω    101.00 127.00   0.50    1.22    --   85.25  36.00 110.62   52
  54  ω     96.00 132.00   0.50    1.22    --   85.25 136.00  18.41   72
  55  ω     60.00 102.00   0.50    1.22    --   85.25-125.00  95.11   84
  56  ω    106.00 133.00   0.50    1.22    --   85.25 110.00   0.60   54
  57  ω     46.00  71.00   0.50    1.22    --   85.25 -77.00  12.02   50
  58  ω     40.00  90.00   0.50    1.22    --   85.25-130.00 -17.81  100
  59  ω    103.00 128.00   0.50    1.22    --   85.25 114.00-136.46   50
  60  ω    112.00 137.00   0.50    1.22    --   85.25  32.00  76.33   50
  61  ω     83.00 122.00   0.50    1.22    --   85.25  14.00  48.52   78
  62  ω     73.00  99.00   0.50    1.22    --   85.25-115.00-151.18   52
  63  ω     45.00  70.00   0.50    1.22    --   85.25 -75.00  24.93   50
  64  ω     49.00  84.00   0.50    1.22    --   85.25-128.00 -95.50   70
  65  ω     72.00  98.00   0.50    1.22    --   85.25-103.00 125.20   52
  66  ω     47.00  79.00   0.50    1.22    --   85.25 -76.00  56.20   64
  67  ω     40.00  67.00   0.50    1.22    --   85.25-103.00 125.20   54
  68  ω     99.00 125.00   0.50    1.22    --   85.25  50.00  49.73   52
  69  ω     98.00 132.00   0.50    1.22    --   85.25 130.00  91.92   68
  70  ω     90.00 120.00   0.50    1.22    --   85.25 140.00 146.40   60
  71  ω     47.00  89.00   0.50    1.22    --   85.25 -91.00 -95.96   84
  72  ω     46.00  71.00   0.50    1.22    --   85.25 -79.00 106.67   50
  73  ω     72.00  98.00   0.50    1.22    --   85.25-124.00 143.33   52
  74  ω     72.00 100.00   0.50    1.22    --   85.25-109.00 159.77   56
  75  ω     46.00  71.00   0.50    1.22    --   85.25 -87.00 144.85   50
  76  ω     44.00  69.00   0.50    1.22    --   85.25 -73.00 164.44   50
  77  ω     41.00  67.00   0.50    1.22    --   85.25-109.00 159.77   52
  78  ω     80.00 105.00   0.50    1.22    --   85.25-132.00  71.63   50
  79  ω     38.00  64.00   0.50    1.22    --   85.25-132.00  71.63   52
  80  ω     97.00 122.00   0.50    1.22    --   85.25  56.00  12.08   50
  81  ω     69.00 132.00   0.50    1.22    --   85.25  14.00-174.58  126

;
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 HPA
_diffrn_detector_type            'HyPix Arc150'
_diffrn_detector_area_resol_mean 10.0
_diffrn_reflns_number            7990
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.458
_diffrn_reflns_theta_max         68.233
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7990
_reflns_number_gt                6794
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'BIS 2011.8 / APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'

_twin_special_details            
;
 Component 2 rotated by 2.6239° around [-0.47 0.62 0.63] (reciprocal) or [-0.20 0.84 0.50] (direct)
;
loop_

_refine_special_details
;
Refined as a 2-component twin. Component 2 rotated by 2.6239Â° around [â\/E?0.47 0.62 0.63] (reciprocal) or [â\/E?0.20 0.84 0.50] (direct). 
The BASF parameter was refined to 53.7%. 

The asymmetric unit contains 1.5 benzene molecules, the half one being twofold disordered over an inversion centre 
and modelled using PART -1 10.5 and AFIX 66 and ISOR 0.01 restraints. 

The entire diborene is centrosymmetric and twofold disordered in a 1:1 ratio (PART 2 and 3, respectively, for the phenanthryl ligands, 
PART 1 and 4 for the BPMe3 fragments) via a mirror perpendicular to the boron planes and bisecting the B-B bond in its centre. 
The external aromatic rings of the phenanthryl ligands (C2 > C7 and C8 > C13) were modelled with AFIX 66.

The PMe3 ligand of PART 1 was modelled as threefold disordered by rotation about the B-P axis in a 1:1:3 ratio (PARTS 11, 12 and 13, respectively). 
All B-P bond lengths were restrained to similarity using SADI 0.002. All 1,2- and 1,3-distances 
in all four PMe3 fragments were restrained to similarity with SAME. 

The ADPs of the phenanthryl ligands (RESI 2 and 3 Phen) were restrained with SIMU 0.01, 
those of the BPMe3 fragments with SIMU 0.005 and those of the boron and phosphorus atoms with SIMU 0.002. 

Due to the disorders and the large number of restraints the data can only be used as proof of connectivity.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1471P)²+0.5284P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         7990
_refine_ls_number_parameters     465
_refine_ls_number_restraints     817
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0875
_refine_ls_wR_factor_ref         0.2577
_refine_ls_wR_factor_gt          0.2462
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1_1 B 0.5423(9) 0.5687(10) 0.0518(7) 0.0535(14) Uani 0.464(7) 1 d D U P A 1
P1_11 P 0.7754(8) 0.6423(9) 0.0632(6) 0.0430(11) Uani 0.464(7) 1 d D U P A 1
C16_11 C 0.8496(18) 0.5755(12) 0.1606(9) 0.062(3) Uani 0.464(7) 1 d D U P A 1
H16A_11 H 0.955660 0.651384 0.202406 0.094 Uiso 0.464(7) 1 calc R U P A 1
H16B_11 H 0.857134 0.476361 0.126379 0.094 Uiso 0.464(7) 1 calc R U P A 1
H16C_11 H 0.776750 0.562104 0.206182 0.094 Uiso 0.464(7) 1 calc R U P A 1
C17_11 C 0.9311(12) 0.6755(14) -0.0074(8) 0.063(3) Uani 0.464(7) 1 d D U P A 1
H17A_11 H 1.034700 0.741101 0.042537 0.095 Uiso 0.464(7) 1 calc R U P A 1
H17B_11 H 0.907920 0.726961 -0.055966 0.095 Uiso 0.464(7) 1 calc R U P A 1
H17C_11 H 0.934089 0.576351 -0.046795 0.095 Uiso 0.464(7) 1 calc R U P A 1
C18_11 C 0.7858(12) 0.8315(11) 0.1327(9) 0.061(3) Uani 0.464(7) 1 d D U P A 1
H18A_11 H 0.895298 0.896331 0.174677 0.092 Uiso 0.464(7) 1 calc R U P A 1
H18B_11 H 0.713233 0.823990 0.178878 0.092 Uiso 0.464(7) 1 calc R U P A 1
H18C_11 H 0.754648 0.877529 0.082700 0.092 Uiso 0.464(7) 1 calc R U P A 1
B1_4 B 0.4284(8) 0.4932(10) 0.0264(6) 0.0591(15) Uani 0.536(7) 1 d D U P A 2
P1_41 P 0.215(4) 0.359(4) -0.078(3) 0.048(2) Uani 0.1072(13) 1 d D U P A 3
C16_41 C 0.099(4) 0.471(4) -0.104(3) 0.049(5) Uani 0.1072(13) 1 d D U P A 3
H16A_41 H -0.006866 0.400057 -0.149993 0.074 Uiso 0.1072(13) 1 calc R U P A 3
H16B_41 H 0.153750 0.540068 -0.138924 0.074 Uiso 0.1072(13) 1 calc R U P A 3
H16C_41 H 0.086999 0.531517 -0.038280 0.074 Uiso 0.1072(13) 1 calc R U P A 3
C17_41 C 0.176(4) 0.221(4) -0.211(2) 0.052(5) Uani 0.1072(13) 1 d D U P A 3
H17A_41 H 0.067497 0.142173 -0.229792 0.078 Uiso 0.1072(13) 1 calc R U P A 3
H17B_41 H 0.253326 0.172181 -0.211638 0.078 Uiso 0.1072(13) 1 calc R U P A 3
H17C_41 H 0.184838 0.276151 -0.260671 0.078 Uiso 0.1072(13) 1 calc R U P A 3
C18_41 C 0.098(4) 0.250(4) -0.011(2) 0.049(4) Uani 0.1072(13) 1 d D U P A 3
H18A_41 H -0.014596 0.231812 -0.035794 0.074 Uiso 0.1072(13) 1 calc R U P A 3
H18B_41 H 0.134587 0.307977 0.064286 0.074 Uiso 0.1072(13) 1 calc R U P A 3
H18C_41 H 0.110083 0.150827 -0.025060 0.074 Uiso 0.1072(13) 1 calc R U P A 3
P1_42 P 0.232(4) 0.348(3) -0.0975(19) 0.048(2) Uani 0.1072(13) 1 d D U P A 4
C16_42 C 0.134(4) 0.484(3) -0.078(3) 0.052(4) Uani 0.1072(13) 1 d D U P A 4
H16A_42 H 0.139704 0.526149 -0.003124 0.078 Uiso 0.1072(13) 1 calc R U P A 4
H16B_42 H 0.021602 0.430568 -0.117295 0.078 Uiso 0.1072(13) 1 calc R U P A 4
H16C_42 H 0.187081 0.567710 -0.102086 0.078 Uiso 0.1072(13) 1 calc R U P A 4
C17_42 C 0.124(4) 0.216(4) -0.2320(19) 0.046(5) Uani 0.1072(13) 1 d D U P A 4
H17A_42 H 0.148018 0.123267 -0.246521 0.069 Uiso 0.1072(13) 1 calc R U P A 4
H17B_42 H 0.157003 0.268525 -0.281374 0.069 Uiso 0.1072(13) 1 calc R U P A 4
H17C_42 H 0.008559 0.187647 -0.239828 0.069 Uiso 0.1072(13) 1 calc R U P A 4
C18_42 C 0.168(4) 0.239(3) -0.016(2) 0.044(4) Uani 0.1072(13) 1 d D U P A 4
H18A_42 H 0.198206 0.149408 -0.032676 0.066 Uiso 0.1072(13) 1 calc R U P A 4
H18B_42 H 0.051332 0.203407 -0.028064 0.066 Uiso 0.1072(13) 1 calc R U P A 4
H18C_42 H 0.218150 0.303990 0.057454 0.066 Uiso 0.1072(13) 1 calc R U P A 4
P1_43 P 0.2295(13) 0.3453(16) -0.0814(10) 0.0492(16) Uani 0.322(4) 1 d D U P A
2
C16_43 C 0.125(2) 0.384(2) -0.1863(13) 0.050(3) Uani 0.322(4) 1 d D U P A 2
H16A_43 H 0.135436 0.325085 -0.253509 0.075 Uiso 0.322(4) 1 calc R U P A 2
H16B_43 H 0.170749 0.494585 -0.175270 0.075 Uiso 0.322(4) 1 calc R U P A 2
H16C_43 H 0.011430 0.352957 -0.186616 0.075 Uiso 0.322(4) 1 calc R U P A 2
C17_43 C 0.1329(15) 0.3913(16) 0.0229(9) 0.049(3) Uani 0.322(4) 1 d D U P A 2
H17A_43 H 0.165574 0.353918 0.077993 0.074 Uiso 0.322(4) 1 calc R U P A 2
H17B_43 H 0.016776 0.341437 -0.004997 0.074 Uiso 0.322(4) 1 calc R U P A 2
H17C_43 H 0.164270 0.503552 0.052111 0.074 Uiso 0.322(4) 1 calc R U P A 2
C18_43 C 0.1479(16) 0.1362(14) -0.1316(12) 0.049(3) Uani 0.322(4) 1 d D U P A 2
H18A_43 H 0.188447 0.097955 -0.079416 0.073 Uiso 0.322(4) 1 calc R U P A 2
H18B_43 H 0.179910 0.099798 -0.196015 0.073 Uiso 0.322(4) 1 calc R U P A 2
H18C_43 H 0.031117 0.097579 -0.146708 0.073 Uiso 0.322(4) 1 calc R U P A 2
C1_2 C 0.4777(11) 0.6805(11) 0.1264(7) 0.049(2) Uani 0.464(7) 1 d . U P A 1
C2_2 C 0.4537(13) 0.6790(16) 0.2336(10) 0.053(2) Uani 0.464(7) 1 d G U P A 1
C3_2 C 0.4939(14) 0.5796(14) 0.2771(10) 0.064(3) Uani 0.464(7) 1 d G U P A 1
H3_2 H 0.529231 0.505653 0.237745 0.076 Uiso 0.464(7) 1 calc R U P A 1
C4_2 C 0.482(2) 0.5884(16) 0.3782(11) 0.066(3) Uani 0.464(7) 1 d G U P A 1
H4_2 H 0.509752 0.520440 0.407931 0.080 Uiso 0.464(7) 1 calc R U P A 1
C5_2 C 0.431(2) 0.6965(19) 0.4358(11) 0.068(4) Uani 0.464(7) 1 d G U P A 1
H5_2 H 0.422621 0.702549 0.504891 0.082 Uiso 0.464(7) 1 calc R U P A 1
C6_2 C 0.390(2) 0.7959(18) 0.3923(14) 0.066(4) Uani 0.464(7) 1 d G U P A 1
H6_2 H 0.354969 0.869873 0.431666 0.079 Uiso 0.464(7) 1 calc R U P A 1
C7_2 C 0.4019(16) 0.7872(16) 0.2912(14) 0.044(3) Uani 0.464(7) 1 d G U P A 1
C8_2 C 0.335(2) 0.8816(18) 0.2415(14) 0.056(3) Uani 0.464(7) 1 d G U P A 1
C9_2 C 0.291(2) 0.997(2) 0.2974(11) 0.051(3) Uani 0.464(7) 1 d G U P A 1
H9_2 H 0.279444 1.005743 0.366141 0.062 Uiso 0.464(7) 1 calc R U P A 1
C10_2 C 0.2635(19) 1.1007(18) 0.2526(10) 0.056(3) Uani 0.464(7) 1 d G U P A 1
H10_2 H 0.233239 1.179814 0.290745 0.067 Uiso 0.464(7) 1 calc R U P A 1
C11_2 C 0.280(2) 1.0884(17) 0.1520(10) 0.063(3) Uani 0.464(7) 1 d G U P A 1
H11_2 H 0.261587 1.159106 0.121344 0.075 Uiso 0.464(7) 1 calc R U P A 1
C12_2 C 0.325(2) 0.9727(18) 0.0961(11) 0.069(3) Uani 0.464(7) 1 d G U P A 1
H12_2 H 0.336139 0.964329 0.027338 0.083 Uiso 0.464(7) 1 calc R U P A 1
C13_2 C 0.352(2) 0.8693(18) 0.1409(14) 0.061(3) Uani 0.464(7) 1 d G U P A 1
C14_2 C 0.4348(12) 0.7841(14) 0.0930(10) 0.054(2) Uani 0.464(7) 1 d . U P A 1
H14_2 H 0.463669 0.799534 0.032016 0.065 Uiso 0.464(7) 1 calc R U P A 1
C1_3 C 0.4068(10) 0.6329(10) 0.1116(7) 0.056(2) Uani 0.536(7) 1 d . U P A 2
C2_3 C 0.4117(11) 0.6518(13) 0.2212(8) 0.057(2) Uani 0.536(7) 1 d G U P A 2
C3_3 C 0.4552(12) 0.5458(12) 0.2550(9) 0.066(3) Uani 0.536(7) 1 d G U P A 2
H3_3 H 0.479623 0.469680 0.207844 0.080 Uiso 0.536(7) 1 calc R U P A 2
C4_3 C 0.4629(16) 0.5512(12) 0.3577(9) 0.062(3) Uani 0.536(7) 1 d G U P A 2
H4_3 H 0.492592 0.478738 0.380741 0.074 Uiso 0.536(7) 1 calc R U P A 2
C5_3 C 0.4271(19) 0.6626(14) 0.4266(9) 0.059(2) Uani 0.536(7) 1 d G U P A 2
H5_3 H 0.432404 0.666246 0.496788 0.071 Uiso 0.536(7) 1 calc R U P A 2
C6_3 C 0.3837(17) 0.7686(14) 0.3928(11) 0.047(2) Uani 0.536(7) 1 d G U P A 2
H6_3 H 0.359247 0.844697 0.439940 0.057 Uiso 0.536(7) 1 calc R U P A 2
C7_3 C 0.3760(13) 0.7632(13) 0.2901(11) 0.042(2) Uani 0.536(7) 1 d G U P A 2
C8_3 C 0.3542(18) 0.8853(15) 0.2541(12) 0.044(2) Uani 0.536(7) 1 d G U P A 2
C9_3 C 0.3059(18) 0.9901(18) 0.3189(9) 0.056(3) Uani 0.536(7) 1 d G U P A 2
H9_3 H 0.298509 0.987600 0.386624 0.067 Uiso 0.536(7) 1 calc R U P A 2
C10_3 C 0.2684(17) 1.0984(16) 0.2845(8) 0.063(3) Uani 0.536(7) 1 d G U P A 2
H10_3 H 0.235332 1.169969 0.328784 0.075 Uiso 0.536(7) 1 calc R U P A 2
C11_3 C 0.2792(17) 1.1020(13) 0.1854(8) 0.057(3) Uani 0.536(7) 1 d G U P A 2
H11_3 H 0.253541 1.176039 0.161893 0.069 Uiso 0.536(7) 1 calc R U P A 2
C12_3 C 0.3275(18) 0.9973(15) 0.1206(8) 0.056(2) Uani 0.536(7) 1 d G U P A 2
H12_3 H 0.334929 0.999741 0.052841 0.067 Uiso 0.536(7) 1 calc R U P A 2
C13_3 C 0.3651(18) 0.8889(15) 0.1550(11) 0.061(3) Uani 0.536(7) 1 d G U P A 2
C14_3 C 0.3750(11) 0.7471(13) 0.0795(10) 0.064(3) Uani 0.536(7) 1 d . U P A 2
H14_3 H 0.359074 0.735175 0.007401 0.077 Uiso 0.536(7) 1 calc R U P A 2
C1_5 C 0.8274(3) 0.4210(3) 0.36952(18) 0.0693(11) Uani 1 1 d G . . . .
H1_5 H 0.797048 0.483620 0.422580 0.083 Uiso 1 1 calc R U . . .
C2_5 C 0.7146(2) 0.2810(3) 0.2993(2) 0.0647(10) Uani 1 1 d G . . . .
H2_5 H 0.607038 0.248023 0.304399 0.078 Uiso 1 1 calc R U . . .
C3_5 C 0.7590(3) 0.1894(2) 0.22168(19) 0.0679(11) Uani 1 1 d G . . . .
H3_5 H 0.681897 0.093728 0.173701 0.081 Uiso 1 1 calc R U . . .
C4_5 C 0.9164(3) 0.2377(3) 0.21425(19) 0.0701(11) Uani 1 1 d G . . . .
H4_5 H 0.946765 0.175037 0.161185 0.084 Uiso 1 1 calc R U . . .
C5_5 C 1.0292(2) 0.3776(3) 0.2844(2) 0.0609(10) Uani 1 1 d G . . . .
H5_5 H 1.136770 0.410630 0.279367 0.073 Uiso 1 1 calc R U . . .
C6_5 C 0.9848(2) 0.4693(3) 0.36208(18) 0.0637(10) Uani 1 1 d G . . . .
H6_5 H 1.061927 0.564922 0.410063 0.076 Uiso 1 1 calc R U . . .
C1_6 C 0.1175(16) 0.1560(17) 0.5343(8) 0.078(4) Uani 0.5 1 d G U P B -1
H1_6 H 0.193434 0.256745 0.547133 0.093 Uiso 0.5 1 calc R U P B -1
C2_6 C 0.1597(16) 0.0574(18) 0.5776(8) 0.071(4) Uani 0.5 1 d G U P B -1
H2_6 H 0.264350 0.090695 0.620133 0.085 Uiso 0.5 1 calc R U P B -1
C3_6 C 0.0486(17) -0.0900(18) 0.5588(8) 0.066(4) Uani 0.5 1 d G U P B -1
H3_6 H 0.077445 -0.157376 0.588383 0.079 Uiso 0.5 1 calc R U P B -1
C4_6 C -0.1045(16) -0.1387(16) 0.4966(8) 0.069(3) Uani 0.5 1 d G U P B -1
H4_6 H -0.180396 -0.239394 0.483678 0.083 Uiso 0.5 1 calc R U P B -1
C5_6 C -0.1466(16) -0.0400(15) 0.4532(8) 0.061(3) Uani 0.5 1 d G U P B -1
H5_6 H -0.251313 -0.073350 0.410672 0.074 Uiso 0.5 1 calc R U P B -1
C6_6 C -0.0356(17) 0.1073(15) 0.4720(8) 0.061(3) Uani 0.5 1 d G U P B -1
H6_6 H -0.064406 0.174721 0.442409 0.073 Uiso 0.5 1 calc R U P B -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1_1 B1_1 1.542(16) 2_665 ?
B1_1 C1_2 1.600(11) . ?
B1_1 P1_11 1.985(8) . ?
P1_11 C16_11 1.791(11) . ?
P1_11 C18_11 1.791(11) . ?
P1_11 C17_11 1.826(11) . ?
B1_4 B1_4 1.571(15) 2_665 ?
B1_4 C1_3 1.618(11) . ?
B1_4 P1_43 1.986(9) . ?
P1_41 C18_41 1.80(2) . ?
P1_41 C16_41 1.82(2) . ?
P1_41 C17_41 1.84(3) . ?
P1_42 C18_42 1.78(2) . ?
P1_42 C16_42 1.81(2) . ?
P1_42 C17_42 1.84(2) . ?
P1_43 C18_43 1.810(15) . ?
P1_43 C17_43 1.815(17) . ?
P1_43 C16_43 1.818(16) . ?
C1_2 C14_2 1.363(15) . ?
C1_2 C2_2 1.524(16) . ?
C2_2 C3_2 1.3900 . ?
C2_2 C7_2 1.3900 . ?
C3_2 C4_2 1.3900 . ?
C4_2 C5_2 1.3900 . ?
C5_2 C6_2 1.3900 . ?
C6_2 C7_2 1.3900 . ?
C7_2 C8_2 1.52(2) . ?
C8_2 C9_2 1.3900 . ?
C8_2 C13_2 1.3900 . ?
C9_2 C10_2 1.3900 . ?
C10_2 C11_2 1.3900 . ?
C11_2 C12_2 1.3900 . ?
C12_2 C13_2 1.3900 . ?
C13_2 C14_2 1.394(19) . ?
C1_3 C14_3 1.406(15) . ?
C1_3 C2_3 1.459(14) . ?
C2_3 C3_3 1.3900 . ?
C2_3 C7_3 1.3900 . ?
C3_3 C4_3 1.3900 . ?
C4_3 C5_3 1.3900 . ?
C5_3 C6_3 1.3900 . ?
C6_3 C7_3 1.3900 . ?
C7_3 C8_3 1.471(17) . ?
C8_3 C9_3 1.3900 . ?
C8_3 C13_3 1.3900 . ?
C9_3 C10_3 1.3900 . ?
C10_3 C11_3 1.3900 . ?
C11_3 C12_3 1.3900 . ?
C12_3 C13_3 1.3900 . ?
C13_3 C14_3 1.520(16) . ?
C1_5 C2_5 1.3900 . ?
C1_5 C6_5 1.3900 . ?
C2_5 C3_5 1.3900 . ?
C3_5 C4_5 1.3900 . ?
C4_5 C5_5 1.3900 . ?
C5_5 C6_5 1.3899 . ?
C1_6 C6_6 1.3900 . ?
C1_6 C2_6 1.3901 . ?
C2_6 C3_6 1.3900 . ?
C3_6 C4_6 1.3900 . ?
C4_6 C5_6 1.3901 . ?
C5_6 C6_6 1.3900 . ?

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
B1_1 B1_1 C1_2 131.6(9) 2_665 . ?
B1_1 B1_1 P1_11 107.9(7) 2_665 . ?
C1_2 B1_1 P1_11 117.9(6) . . ?
C16_11 P1_11 C18_11 105.8(7) . . ?
C16_11 P1_11 C17_11 103.8(7) . . ?
C18_11 P1_11 C17_11 104.6(7) . . ?
C16_11 P1_11 B1_1 103.7(7) . . ?
C18_11 P1_11 B1_1 87.0(5) . . ?
C17_11 P1_11 B1_1 145.8(6) . . ?
B1_4 B1_4 C1_3 126.3(8) 2_665 . ?
B1_4 B1_4 P1_43 107.8(8) 2_665 . ?
C1_3 B1_4 P1_43 114.6(6) . . ?
C18_41 P1_41 C16_41 101(2) . . ?
C18_41 P1_41 C17_41 105(2) . . ?
C16_41 P1_41 C17_41 101.0(19) . . ?
C18_42 P1_42 C16_42 105(2) . . ?
C18_42 P1_42 C17_42 105.4(18) . . ?
C16_42 P1_42 C17_42 101.6(18) . . ?
C18_43 P1_43 C17_43 103.4(9) . . ?
C18_43 P1_43 C16_43 100.4(9) . . ?
C17_43 P1_43 C16_43 103.3(10) . . ?
C18_43 P1_43 B1_4 130.1(9) . . ?
C17_43 P1_43 B1_4 84.1(7) . . ?
C16_43 P1_43 B1_4 126.2(10) . . ?
C14_2 C1_2 C2_2 115.3(9) . . ?
C14_2 C1_2 B1_1 119.4(9) . . ?
C2_2 C1_2 B1_1 125.3(9) . . ?
C3_2 C2_2 C7_2 120.0 . . ?
C3_2 C2_2 C1_2 121.1(9) . . ?
C7_2 C2_2 C1_2 118.8(9) . . ?
C4_2 C3_2 C2_2 120.0 . . ?
C5_2 C4_2 C3_2 120.0 . . ?
C4_2 C5_2 C6_2 120.0 . . ?
C7_2 C6_2 C5_2 120.0 . . ?
C6_2 C7_2 C2_2 120.0 . . ?
C6_2 C7_2 C8_2 118.1(13) . . ?
C2_2 C7_2 C8_2 121.4(13) . . ?
C9_2 C8_2 C13_2 120.0 . . ?
C9_2 C8_2 C7_2 123.3(12) . . ?
C13_2 C8_2 C7_2 115.3(13) . . ?
C10_2 C9_2 C8_2 120.0 . . ?
C9_2 C10_2 C11_2 120.0 . . ?
C12_2 C11_2 C10_2 120.0 . . ?
C13_2 C12_2 C11_2 120.0 . . ?
C12_2 C13_2 C8_2 120.0 . . ?
C12_2 C13_2 C14_2 116.3(14) . . ?
C8_2 C13_2 C14_2 121.6(14) . . ?
C1_2 C14_2 C13_2 125.5(14) . . ?
C14_3 C1_3 C2_3 114.6(8) . . ?
C14_3 C1_3 B1_4 119.0(8) . . ?
C2_3 C1_3 B1_4 126.4(9) . . ?
C3_3 C2_3 C7_3 120.0 . . ?
C3_3 C2_3 C1_3 114.6(8) . . ?
C7_3 C2_3 C1_3 125.4(8) . . ?
C2_3 C3_3 C4_3 120.0 . . ?
C5_3 C4_3 C3_3 120.0 . . ?
C4_3 C5_3 C6_3 120.0 . . ?
C5_3 C6_3 C7_3 120.0 . . ?
C6_3 C7_3 C2_3 120.0 . . ?
C6_3 C7_3 C8_3 122.4(10) . . ?
C2_3 C7_3 C8_3 117.0(11) . . ?
C9_3 C8_3 C13_3 120.0 . . ?
C9_3 C8_3 C7_3 117.5(11) . . ?
C13_3 C8_3 C7_3 122.2(11) . . ?
C8_3 C9_3 C10_3 120.0 . . ?
C9_3 C10_3 C11_3 120.0 . . ?
C12_3 C11_3 C10_3 120.0 . . ?
C11_3 C12_3 C13_3 120.0 . . ?
C12_3 C13_3 C8_3 120.0 . . ?
C12_3 C13_3 C14_3 121.8(11) . . ?
C8_3 C13_3 C14_3 116.3(11) . . ?
C1_3 C14_3 C13_3 122.9(12) . . ?
C2_5 C1_5 C6_5 120.0 . . ?
C1_5 C2_5 C3_5 120.0 . . ?
C4_5 C3_5 C2_5 120.0 . . ?
C3_5 C4_5 C5_5 120.0 . . ?
C6_5 C5_5 C4_5 120.0 . . ?
C5_5 C6_5 C1_5 120.0 . . ?
C6_6 C1_6 C2_6 120.0 . . ?
C3_6 C2_6 C1_6 120.0 . . ?
C4_6 C3_6 C2_6 120.0 . . ?
C3_6 C4_6 C5_6 120.0 . . ?
C6_6 C5_6 C4_6 120.0 . . ?
C5_6 C6_6 C1_6 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
B1_1 B1_1 C1_2 C14_2 -69.6(17) 2_665 . . . ?
P1_11 B1_1 C1_2 C14_2 89.6(10) . . . . ?
B1_1 B1_1 C1_2 C2_2 108.3(15) 2_665 . . . ?
P1_11 B1_1 C1_2 C2_2 -92.4(10) . . . . ?
C14_2 C1_2 C2_2 C3_2 -179.5(7) . . . . ?
B1_1 C1_2 C2_2 C3_2 2.5(11) . . . . ?
C14_2 C1_2 C2_2 C7_2 -4.3(11) . . . . ?
B1_1 C1_2 C2_2 C7_2 177.7(8) . . . . ?
C7_2 C2_2 C3_2 C4_2 0.0 . . . . ?
C1_2 C2_2 C3_2 C4_2 175.1(9) . . . . ?
C2_2 C3_2 C4_2 C5_2 0.0 . . . . ?
C3_2 C4_2 C5_2 C6_2 0.0 . . . . ?
C4_2 C5_2 C6_2 C7_2 0.0 . . . . ?
C5_2 C6_2 C7_2 C2_2 0.0 . . . . ?
C5_2 C6_2 C7_2 C8_2 171.6(13) . . . . ?
C3_2 C2_2 C7_2 C6_2 0.0 . . . . ?
C1_2 C2_2 C7_2 C6_2 -175.2(8) . . . . ?
C3_2 C2_2 C7_2 C8_2 -171.3(14) . . . . ?
C1_2 C2_2 C7_2 C8_2 13.5(14) . . . . ?
C6_2 C7_2 C8_2 C9_2 12.5(15) . . . . ?
C2_2 C7_2 C8_2 C9_2 -176.1(8) . . . . ?
C6_2 C7_2 C8_2 C13_2 179.3(7) . . . . ?
C2_2 C7_2 C8_2 C13_2 -9.3(16) . . . . ?
C13_2 C8_2 C9_2 C10_2 0.0 . . . . ?
C7_2 C8_2 C9_2 C10_2 166.2(16) . . . . ?
C8_2 C9_2 C10_2 C11_2 0.0 . . . . ?
C9_2 C10_2 C11_2 C12_2 0.0 . . . . ?
C10_2 C11_2 C12_2 C13_2 0.0 . . . . ?
C11_2 C12_2 C13_2 C8_2 0.0 . . . . ?
C11_2 C12_2 C13_2 C14_2 -163.8(14) . . . . ?
C9_2 C8_2 C13_2 C12_2 0.0 . . . . ?
C7_2 C8_2 C13_2 C12_2 -167.3(15) . . . . ?
C9_2 C8_2 C13_2 C14_2 163.0(15) . . . . ?
C7_2 C8_2 C13_2 C14_2 -4.3(14) . . . . ?
C2_2 C1_2 C14_2 C13_2 -9.7(17) . . . . ?
B1_1 C1_2 C14_2 C13_2 168.4(12) . . . . ?
C12_2 C13_2 C14_2 C1_2 178.0(9) . . . . ?
C8_2 C13_2 C14_2 C1_2 14.4(18) . . . . ?
B1_4 B1_4 C1_3 C14_3 69.5(13) 2_665 . . . ?
P1_43 B1_4 C1_3 C14_3 -69.5(10) . . . . ?
B1_4 B1_4 C1_3 C2_3 -112.7(13) 2_665 . . . ?
P1_43 B1_4 C1_3 C2_3 108.3(10) . . . . ?
C14_3 C1_3 C2_3 C3_3 -175.3(7) . . . . ?
B1_4 C1_3 C2_3 C3_3 6.8(10) . . . . ?
C14_3 C1_3 C2_3 C7_3 5.3(10) . . . . ?
B1_4 C1_3 C2_3 C7_3 -172.7(6) . . . . ?
C7_3 C2_3 C3_3 C4_3 0.0 . . . . ?
C1_3 C2_3 C3_3 C4_3 -179.5(7) . . . . ?
C2_3 C3_3 C4_3 C5_3 0.0 . . . . ?
C3_3 C4_3 C5_3 C6_3 0.0 . . . . ?
C4_3 C5_3 C6_3 C7_3 0.0 . . . . ?
C5_3 C6_3 C7_3 C2_3 0.0 . . . . ?
C5_3 C6_3 C7_3 C8_3 -170.7(12) . . . . ?
C3_3 C2_3 C7_3 C6_3 0.0 . . . . ?
C1_3 C2_3 C7_3 C6_3 179.4(8) . . . . ?
C3_3 C2_3 C7_3 C8_3 171.2(11) . . . . ?
C1_3 C2_3 C7_3 C8_3 -9.4(12) . . . . ?
C6_3 C7_3 C8_3 C9_3 -14.1(12) . . . . ?
C2_3 C7_3 C8_3 C9_3 174.9(6) . . . . ?
C6_3 C7_3 C8_3 C13_3 172.4(7) . . . . ?
C2_3 C7_3 C8_3 C13_3 1.4(13) . . . . ?
C13_3 C8_3 C9_3 C10_3 0.0 . . . . ?
C7_3 C8_3 C9_3 C10_3 -173.7(12) . . . . ?
C8_3 C9_3 C10_3 C11_3 0.0 . . . . ?
C9_3 C10_3 C11_3 C12_3 0.0 . . . . ?
C10_3 C11_3 C12_3 C13_3 0.0 . . . . ?
C11_3 C12_3 C13_3 C8_3 0.0 . . . . ?
C11_3 C12_3 C13_3 C14_3 163.4(12) . . . . ?
C9_3 C8_3 C13_3 C12_3 0.0 . . . . ?
C7_3 C8_3 C13_3 C12_3 173.4(13) . . . . ?
C9_3 C8_3 C13_3 C14_3 -164.3(11) . . . . ?
C7_3 C8_3 C13_3 C14_3 9.1(12) . . . . ?
C2_3 C1_3 C14_3 C13_3 6.6(14) . . . . ?
B1_4 C1_3 C14_3 C13_3 -175.3(10) . . . . ?
C12_3 C13_3 C14_3 C1_3 -177.5(8) . . . . ?
C8_3 C13_3 C14_3 C1_3 -13.6(13) . . . . ?
C6_5 C1_5 C2_5 C3_5 0.0 . . . . ?
C1_5 C2_5 C3_5 C4_5 0.0 . . . . ?
C2_5 C3_5 C4_5 C5_5 0.0 . . . . ?
C3_5 C4_5 C5_5 C6_5 0.0 . . . . ?
C4_5 C5_5 C6_5 C1_5 0.0 . . . . ?
C2_5 C1_5 C6_5 C5_5 0.0 . . . . ?
C6_6 C1_6 C2_6 C3_6 0.0 . . . . ?
C1_6 C2_6 C3_6 C4_6 0.0 . . . . ?
C2_6 C3_6 C4_6 C5_6 0.0 . . . . ?
C3_6 C4_6 C5_6 C6_6 0.0 . . . . ?
C4_6 C5_6 C6_6 C1_6 0.0 . . . . ?
C2_6 C1_6 C6_6 C5_6 0.0 . . . . ?

_refine_diff_density_max         0.530
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.060

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

data_test_a
_database_code_depnum_ccdc_archive 'CCDC 2169208'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_test_a              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         23 Report
RESPONSE: Reflections affected by beamstop
;


_audit_creation_method           'CIF-fill 1.2r (K.Radacki 2005-21)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        6-Pyr
_chemical_name_common            B2(Pyr)2Cl2(PMe3)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 B2 Cl2 P2, C4 H8 O'
_chemical_formula_sum            'C42 H44 B2 Cl2 O P2'
_chemical_formula_weight         719.23

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.987(4)
_cell_length_b                   12.467(4)
_cell_length_c                   12.683(4)
_cell_angle_alpha                83.308(9)
_cell_angle_beta                 88.82(2)
_cell_angle_gamma                76.780(13)
_cell_volume                     1832.5(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7006
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.89


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_F_000             756
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.121
_exptl_absorpt_coefficient_mu    0.298
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5986
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2.00 1.00 3.00 0.1020
-2.00 -1.00 3.00 0.0540
2.00 1.00 -2.00 0.0820
0.00 0.00 -1.00 0.0460
0.00 0.00 1.00 0.0730
2.00 1.00 0.00 0.1150
1.00 1.00 -3.00 0.0610
-1.00 -1.00 3.00 0.0590
-3.00 -1.00 -3.00 0.0990
3.00 3.00 -2.00 0.1090
-3.00 -3.00 2.00 0.0620
1.00 2.00 -3.00 0.0730
-1.00 -3.00 3.00 0.0550
-1.00 2.00 -3.00 0.0750
-1.00 -3.00 1.00 0.0580
1.00 3.00 -1.00 0.1080
1.00 3.00 0.00 0.1240
-1.00 -3.00 0.00 0.0660
1.00 -3.00 1.00 0.0430
-2.00 1.00 -1.00 0.1010
-1.00 3.00 0.00 0.1000
1.00 -3.00 0.00 0.0410

_exptl_absorpt_special_details   ?
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 CPA
_diffrn_detector_type            'Photon II'
_diffrn_detector_area_resol_mean 7.5
_diffrn_reflns_number            25797
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.745
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             7665
_reflns_number_gt                5019
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BIS 6.2.14 / APEX3 ver. 2019.1 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          
;
The asymmetric unit contains one molecule of THF, which was modelled as 
twofold disordered and refined to a 58:42 ratio. The displacement parameters 
of all atoms in the residues RESI 6 and 16 THF were restrained to the same 
value with similarity restraint SIMU 0.01.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0196P)²+6.0996P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7665
_refine_ls_number_parameters     494
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0852
_refine_ls_wR_factor_ref         0.1604
_refine_ls_wR_factor_gt          0.1426
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1_1 B 0.2344(4) 0.1851(4) 0.3025(4) 0.0207(11) Uani 1 1 d . . . . .
Cl1_1 Cl 0.24825(10) 0.10686(9) 0.17456(8) 0.0229(2) Uani 1 1 d . . . . .
B2_1 B 0.1038(4) 0.2881(4) 0.2934(4) 0.0193(10) Uani 1 1 d . . . . .
Cl2_1 Cl 0.00518(9) 0.25411(9) 0.41280(8) 0.0200(2) Uani 1 1 d . . . . .
P1_2 P 0.23946(11) 0.05202(10) 0.40812(10) 0.0238(3) Uani 1 1 d . . . . .
C2_2 C 0.3703(4) -0.0493(4) 0.3891(4) 0.0388(13) Uani 1 1 d . . . . .
H2A_2 H 0.373946 -0.115171 0.440446 0.058 Uiso 1 1 calc R U . . .
H2B_2 H 0.436240 -0.017472 0.399758 0.058 Uiso 1 1 calc R U . . .
H2C_2 H 0.371700 -0.070155 0.316894 0.058 Uiso 1 1 calc R U . . .
C3_2 C 0.1273(4) -0.0211(4) 0.3981(4) 0.0294(11) Uani 1 1 d . . . . .
H3A_2 H 0.142744 -0.088926 0.448229 0.044 Uiso 1 1 calc R U . . .
H3B_2 H 0.124550 -0.040571 0.325710 0.044 Uiso 1 1 calc R U . . .
H3C_2 H 0.053521 0.026361 0.415053 0.044 Uiso 1 1 calc R U . . .
C1_2 C 0.2435(5) 0.0697(4) 0.5483(4) 0.0332(12) Uani 1 1 d . . . . .
H1A_2 H 0.255191 -0.002911 0.590772 0.050 Uiso 1 1 calc R U . . .
H1B_2 H 0.170833 0.117025 0.568097 0.050 Uiso 1 1 calc R U . . .
H1C_2 H 0.306600 0.104449 0.561496 0.050 Uiso 1 1 calc R U . . .
P1_3 P -0.00495(10) 0.28292(10) 0.17695(9) 0.0232(3) Uani 1 1 d . . . . .
C2_3 C -0.1336(4) 0.3899(4) 0.1893(4) 0.0292(11) Uani 1 1 d . . . . .
H2A_3 H -0.192679 0.380976 0.140949 0.044 Uiso 1 1 calc R U . . .
H2B_3 H -0.116385 0.462935 0.171223 0.044 Uiso 1 1 calc R U . . .
H2C_3 H -0.161262 0.383528 0.262522 0.044 Uiso 1 1 calc R U . . .
C3_3 C 0.0382(4) 0.3116(4) 0.0409(4) 0.0343(12) Uani 1 1 d . . . . .
H3A_3 H -0.024180 0.309835 -0.007160 0.051 Uiso 1 1 calc R U . . .
H3B_3 H 0.106473 0.255451 0.025652 0.051 Uiso 1 1 calc R U . . .
H3C_3 H 0.055691 0.385182 0.030452 0.051 Uiso 1 1 calc R U . . .
C1_3 C -0.0537(4) 0.1552(4) 0.1792(4) 0.0304(11) Uani 1 1 d . . . . .
H1A_3 H -0.119228 0.167093 0.130857 0.046 Uiso 1 1 calc R U . . .
H1B_3 H -0.076803 0.132615 0.251441 0.046 Uiso 1 1 calc R U . . .
H1C_3 H 0.008611 0.096889 0.156546 0.046 Uiso 1 1 calc R U . . .
C1_4 C 0.3559(4) 0.2170(3) 0.3262(3) 0.0196(9) Uani 1 1 d . . . . .
C3_4 C 0.2771(4) 0.3199(3) 0.4801(3) 0.0210(9) Uani 1 1 d . . . . .
H3_4 H 0.202465 0.311437 0.465072 0.025 Uiso 1 1 calc R U . . .
C2_4 C 0.3698(4) 0.2759(3) 0.4137(3) 0.0187(9) Uani 1 1 d . . . . .
C4_4 C 0.2923(4) 0.3740(4) 0.5647(3) 0.0210(9) Uani 1 1 d . . . . .
H4_4 H 0.227973 0.402819 0.606184 0.025 Uiso 1 1 calc R U . . .
C5_4 C 0.4022(4) 0.3880(3) 0.5920(3) 0.0211(9) Uani 1 1 d . . . . .
C6_4 C 0.4195(4) 0.4435(4) 0.6783(3) 0.0249(10) Uani 1 1 d . . . . .
H6_4 H 0.356686 0.471566 0.721830 0.030 Uiso 1 1 calc R U . . .
C7_4 C 0.5278(4) 0.4575(4) 0.7005(4) 0.0267(10) Uani 1 1 d . . . . .
H7_4 H 0.538687 0.494338 0.759690 0.032 Uiso 1 1 calc R U . . .
C8_4 C 0.6197(4) 0.4184(4) 0.6374(4) 0.0282(11) Uani 1 1 d . . . . .
H8_4 H 0.692987 0.430028 0.652754 0.034 Uiso 1 1 calc R U . . .
C16_4 C 0.4973(4) 0.3468(3) 0.5266(3) 0.0186(9) Uani 1 1 d . . . . .
C15_4 C 0.4811(4) 0.2911(3) 0.4380(3) 0.0195(9) Uani 1 1 d . . . . .
C14_4 C 0.4536(4) 0.1778(4) 0.2675(4) 0.0236(10) Uani 1 1 d . . . . .
H14_4 H 0.446129 0.138699 0.209001 0.028 Uiso 1 1 calc R U . . .
C13_4 C 0.5611(4) 0.1933(4) 0.2906(4) 0.0243(10) Uani 1 1 d . . . . .
H13_4 H 0.624657 0.165144 0.247784 0.029 Uiso 1 1 calc R U . . .
C12_4 C 0.5771(4) 0.2494(3) 0.3755(3) 0.0209(10) Uani 1 1 d . . . . .
C11_4 C 0.6880(4) 0.2663(4) 0.4033(4) 0.0232(10) Uani 1 1 d . . . . .
H11_4 H 0.752522 0.238716 0.361419 0.028 Uiso 1 1 calc R U . . .
C10_4 C 0.7026(4) 0.3194(4) 0.4855(4) 0.0250(10) Uani 1 1 d . . . . .
H10_4 H 0.776657 0.329164 0.500845 0.030 Uiso 1 1 calc R U . . .
C9_4 C 0.6068(4) 0.3622(4) 0.5518(4) 0.0238(10) Uani 1 1 d . . . . .
C21_5 C 0.1033(4) 0.4200(3) 0.2826(3) 0.0193(9) Uani 1 1 d . . . . .
C24_5 C 0.3117(4) 0.4512(4) 0.0602(3) 0.0238(10) Uani 1 1 d . . . . .
H24_5 H 0.359953 0.405828 0.014537 0.029 Uiso 1 1 calc R U . . .
C25_5 C 0.3082(4) 0.5673(4) 0.0510(3) 0.0239(10) Uani 1 1 d . . . . .
C26_5 C 0.3786(4) 0.6168(4) -0.0194(4) 0.0310(12) Uani 1 1 d . . . . .
H26_5 H 0.429267 0.573194 -0.064704 0.037 Uiso 1 1 calc R U . . .
C27_5 C 0.3744(4) 0.7295(5) -0.0230(4) 0.0362(13) Uani 1 1 d . . . . .
H27_5 H 0.425103 0.761361 -0.068578 0.043 Uiso 1 1 calc R U . . .
C28_5 C 0.2979(5) 0.7962(4) 0.0385(4) 0.0357(13) Uani 1 1 d . . . . .
H28_5 H 0.294924 0.873396 0.033293 0.043 Uiso 1 1 calc R U . . .
C29_5 C 0.2256(4) 0.7508(4) 0.1074(4) 0.0295(11) Uani 1 1 d . . . . .
C30_5 C 0.1433(5) 0.8177(4) 0.1708(4) 0.0352(12) Uani 1 1 d . . . . .
H30_5 H 0.135315 0.895788 0.162598 0.042 Uiso 1 1 calc R U . . .
C31_5 C 0.0782(4) 0.7729(4) 0.2408(4) 0.0309(11) Uani 1 1 d . . . . .
H31_5 H 0.026053 0.819588 0.282526 0.037 Uiso 1 1 calc R U . . .
C32_5 C 0.0847(4) 0.6540(4) 0.2551(4) 0.0238(10) Uani 1 1 d . . . . .
C33_5 C 0.0227(4) 0.6058(4) 0.3328(4) 0.0248(10) Uani 1 1 d . . . . .
H33_5 H -0.026906 0.651023 0.377634 0.030 Uiso 1 1 calc R U . . .
C34_5 C 0.0328(4) 0.4914(4) 0.3457(3) 0.0220(10) Uani 1 1 d . . . . .
H34_5 H -0.010434 0.460652 0.399883 0.026 Uiso 1 1 calc R U . . .
C35_5 C 0.1610(4) 0.5857(4) 0.1913(3) 0.0208(9) Uani 1 1 d . . . . .
C36_5 C 0.2308(4) 0.6346(4) 0.1161(3) 0.0196(9) Uani 1 1 d . . . . .
C23_5 C 0.2467(4) 0.4044(4) 0.1340(3) 0.0211(9) Uani 1 1 d . . . . .
H23_5 H 0.253090 0.326590 0.139488 0.025 Uiso 1 1 calc R U . . .
C22_5 C 0.1699(4) 0.4679(3) 0.2028(3) 0.0192(9) Uani 1 1 d . . . . .
O1_6 O 0.3545(17) 0.0194(18) 0.8742(11) 0.053(2) Uani 0.581(11) 1 d . U P A 1
C1_6 C 0.247(2) 0.0712(13) 0.861(2) 0.049(3) Uani 0.581(11) 1 d . U P A 1
H1A_6 H 0.205246 0.068468 0.928831 0.058 Uiso 0.581(11) 1 calc R U P A 1
H1B_6 H 0.209327 0.037103 0.809028 0.058 Uiso 0.581(11) 1 calc R U P A 1
C2_6 C 0.2488(15) 0.1903(12) 0.8190(14) 0.048(3) Uani 0.581(11) 1 d . U P A 1
H2A_6 H 0.177480 0.242659 0.836985 0.058 Uiso 0.581(11) 1 calc R U P A 1
H2AB_6 H 0.259991 0.198921 0.741210 0.058 Uiso 0.581(11) 1 calc R U P A 1
C3_6 C 0.3527(11) 0.2065(8) 0.8787(10) 0.050(2) Uani 0.581(11) 1 d . U P A 1
H3A_6 H 0.384405 0.267776 0.842970 0.060 Uiso 0.581(11) 1 calc R U P A 1
H3AB_6 H 0.334610 0.219023 0.953446 0.060 Uiso 0.581(11) 1 calc R U P A 1
C4_6 C 0.4321(17) 0.0931(16) 0.8699(12) 0.058(3) Uani 0.581(11) 1 d . U P A 1
H4A_6 H 0.474537 0.092819 0.802090 0.069 Uiso 0.581(11) 1 calc R U P A 1
H4AB_6 H 0.487722 0.071801 0.929550 0.069 Uiso 0.581(11) 1 calc R U P A 1
O1_16 O 0.368(2) 0.016(2) 0.9021(14) 0.046(3) Uani 0.419(11) 1 d . U P A 2
C1_16 C 0.249(3) 0.0947(18) 0.859(3) 0.048(3) Uani 0.419(11) 1 d . U P A 2
H1A_16 H 0.223386 0.068575 0.794408 0.057 Uiso 0.419(11) 1 calc R U P A 2
H1AB_16 H 0.188806 0.095881 0.913238 0.057 Uiso 0.419(11) 1 calc R U P A 2
C2_16 C 0.273(2) 0.2095(18) 0.832(2) 0.051(3) Uani 0.419(11) 1 d . U P A 2
H2A_16 H 0.232064 0.248235 0.766300 0.061 Uiso 0.419(11) 1 calc R U P A 2
H2AB_16 H 0.249605 0.255459 0.890894 0.061 Uiso 0.419(11) 1 calc R U P A 2
C3_16 C 0.4012(14) 0.1835(12) 0.8171(13) 0.053(3) Uani 0.419(11) 1 d . U P A 2
H3A_16 H 0.433360 0.248394 0.825989 0.063 Uiso 0.419(11) 1 calc R U P A 2
H3AB_16 H 0.422604 0.158957 0.746547 0.063 Uiso 0.419(11) 1 calc R U P A 2
C4_16 C 0.441(2) 0.090(2) 0.9059(15) 0.049(3) Uani 0.419(11) 1 d . U P A 2
H4A_16 H 0.521289 0.051666 0.895109 0.059 Uiso 0.419(11) 1 calc R U P A 2
H4AB_16 H 0.434571 0.119191 0.975540 0.059 Uiso 0.419(11) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1_1 C1_4 1.637(7) . ?
B1_1 B2_1 1.779(7) . ?
B1_1 Cl1_1 1.974(5) . ?
B1_1 P1_2 1.997(5) . ?
B2_1 C21_5 1.634(6) . ?
B2_1 Cl2_1 1.969(5) . ?
B2_1 P1_3 2.005(5) . ?
P1_2 C3_2 1.803(5) . ?
P1_2 C2_2 1.806(5) . ?
P1_2 C1_2 1.820(5) . ?
C2_2 H2A_2 0.9800 . ?
C2_2 H2B_2 0.9800 . ?
C2_2 H2C_2 0.9800 . ?
C3_2 H3A_2 0.9800 . ?
C3_2 H3B_2 0.9800 . ?
C3_2 H3C_2 0.9800 . ?
C1_2 H1A_2 0.9800 . ?
C1_2 H1B_2 0.9800 . ?
C1_2 H1C_2 0.9800 . ?
P1_3 C2_3 1.810(5) . ?
P1_3 C3_3 1.811(5) . ?
P1_3 C1_3 1.814(5) . ?
C2_3 H2A_3 0.9800 . ?
C2_3 H2B_3 0.9800 . ?
C2_3 H2C_3 0.9800 . ?
C3_3 H3A_3 0.9800 . ?
C3_3 H3B_3 0.9800 . ?
C3_3 H3C_3 0.9800 . ?
C1_3 H1A_3 0.9800 . ?
C1_3 H1B_3 0.9800 . ?
C1_3 H1C_3 0.9800 . ?
C1_4 C14_4 1.398(6) . ?
C1_4 C2_4 1.432(6) . ?
C3_4 C4_4 1.368(6) . ?
C3_4 C2_4 1.426(6) . ?
C3_4 H3_4 0.9500 . ?
C2_4 C15_4 1.435(6) . ?
C4_4 C5_4 1.422(6) . ?
C4_4 H4_4 0.9500 . ?
C5_4 C6_4 1.405(6) . ?
C5_4 C16_4 1.429(6) . ?
C6_4 C7_4 1.387(7) . ?
C6_4 H6_4 0.9500 . ?
C7_4 C8_4 1.379(7) . ?
C7_4 H7_4 0.9500 . ?
C8_4 C9_4 1.389(7) . ?
C8_4 H8_4 0.9500 . ?
C16_4 C9_4 1.417(6) . ?
C16_4 C15_4 1.426(6) . ?
C15_4 C12_4 1.417(6) . ?
C14_4 C13_4 1.388(6) . ?
C14_4 H14_4 0.9500 . ?
C13_4 C12_4 1.389(6) . ?
C13_4 H13_4 0.9500 . ?
C12_4 C11_4 1.450(6) . ?
C11_4 C10_4 1.333(7) . ?
C11_4 H11_4 0.9500 . ?
C10_4 C9_4 1.448(6) . ?
C10_4 H10_4 0.9500 . ?
C21_5 C34_5 1.393(6) . ?
C21_5 C22_5 1.435(6) . ?
C24_5 C23_5 1.368(6) . ?
C24_5 C25_5 1.429(6) . ?
C24_5 H24_5 0.9500 . ?
C25_5 C26_5 1.404(6) . ?
C25_5 C36_5 1.422(6) . ?
C26_5 C27_5 1.389(7) . ?
C26_5 H26_5 0.9500 . ?
C27_5 C28_5 1.384(8) . ?
C27_5 H27_5 0.9500 . ?
C28_5 C29_5 1.383(7) . ?
C28_5 H28_5 0.9500 . ?
C29_5 C36_5 1.427(6) . ?
C29_5 C30_5 1.436(7) . ?
C30_5 C31_5 1.328(7) . ?
C30_5 H30_5 0.9500 . ?
C31_5 C32_5 1.456(6) . ?
C31_5 H31_5 0.9500 . ?
C32_5 C33_5 1.385(6) . ?
C32_5 C35_5 1.411(6) . ?
C33_5 C34_5 1.395(6) . ?
C33_5 H33_5 0.9500 . ?
C34_5 H34_5 0.9500 . ?
C35_5 C36_5 1.431(6) . ?
C35_5 C22_5 1.438(6) . ?
C23_5 C22_5 1.426(6) . ?
C23_5 H23_5 0.9500 . ?
O1_6 C1_6 1.31(3) . ?
O1_6 C4_6 1.45(2) . ?
C1_6 C2_6 1.521(18) . ?
C1_6 H1A_6 0.9900 . ?
C1_6 H1B_6 0.9900 . ?
C2_6 C3_6 1.535(19) . ?
C2_6 H2A_6 0.9900 . ?
C2_6 H2AB_6 0.9900 . ?
C3_6 C4_6 1.53(2) . ?
C3_6 H3A_6 0.9900 . ?
C3_6 H3AB_6 0.9900 . ?
C4_6 H4A_6 0.9900 . ?
C4_6 H4AB_6 0.9900 . ?
O1_16 C4_16 1.42(3) . ?
O1_16 C1_16 1.60(5) . ?
C1_16 C2_16 1.52(3) . ?
C1_16 H1A_16 0.9900 . ?
C1_16 H1AB_16 0.9900 . ?
C2_16 C3_16 1.51(3) . ?
C2_16 H2A_16 0.9900 . ?
C2_16 H2AB_16 0.9900 . ?
C3_16 C4_16 1.52(3) . ?
C3_16 H3A_16 0.9900 . ?
C3_16 H3AB_16 0.9900 . ?
C4_16 H4A_16 0.9900 . ?
C4_16 H4AB_16 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1_4 B1_1 B2_1 120.8(4) . . ?
C1_4 B1_1 Cl1_1 109.9(3) . . ?
B2_1 B1_1 Cl1_1 108.3(3) . . ?
C1_4 B1_1 P1_2 101.9(3) . . ?
B2_1 B1_1 P1_2 116.6(3) . . ?
Cl1_1 B1_1 P1_2 96.7(2) . . ?
C21_5 B2_1 B1_1 121.2(4) . . ?
C21_5 B2_1 Cl2_1 108.9(3) . . ?
B1_1 B2_1 Cl2_1 108.7(3) . . ?
C21_5 B2_1 P1_3 101.7(3) . . ?
B1_1 B2_1 P1_3 116.7(3) . . ?
Cl2_1 B2_1 P1_3 96.8(2) . . ?
C3_2 P1_2 C2_2 104.6(2) . . ?
C3_2 P1_2 C1_2 104.3(2) . . ?
C2_2 P1_2 C1_2 103.7(3) . . ?
C3_2 P1_2 B1_1 116.5(2) . . ?
C2_2 P1_2 B1_1 108.6(2) . . ?
C1_2 P1_2 B1_1 117.8(2) . . ?
P1_2 C2_2 H2A_2 109.5 . . ?
P1_2 C2_2 H2B_2 109.5 . . ?
H2A_2 C2_2 H2B_2 109.5 . . ?
P1_2 C2_2 H2C_2 109.5 . . ?
H2A_2 C2_2 H2C_2 109.5 . . ?
H2B_2 C2_2 H2C_2 109.5 . . ?
P1_2 C3_2 H3A_2 109.5 . . ?
P1_2 C3_2 H3B_2 109.5 . . ?
H3A_2 C3_2 H3B_2 109.5 . . ?
P1_2 C3_2 H3C_2 109.5 . . ?
H3A_2 C3_2 H3C_2 109.5 . . ?
H3B_2 C3_2 H3C_2 109.5 . . ?
P1_2 C1_2 H1A_2 109.5 . . ?
P1_2 C1_2 H1B_2 109.5 . . ?
H1A_2 C1_2 H1B_2 109.5 . . ?
P1_2 C1_2 H1C_2 109.5 . . ?
H1A_2 C1_2 H1C_2 109.5 . . ?
H1B_2 C1_2 H1C_2 109.5 . . ?
C2_3 P1_3 C3_3 103.5(2) . . ?
C2_3 P1_3 C1_3 105.2(2) . . ?
C3_3 P1_3 C1_3 104.4(2) . . ?
C2_3 P1_3 B2_1 108.1(2) . . ?
C3_3 P1_3 B2_1 118.2(2) . . ?
C1_3 P1_3 B2_1 116.0(2) . . ?
P1_3 C2_3 H2A_3 109.5 . . ?
P1_3 C2_3 H2B_3 109.5 . . ?
H2A_3 C2_3 H2B_3 109.5 . . ?
P1_3 C2_3 H2C_3 109.5 . . ?
H2A_3 C2_3 H2C_3 109.5 . . ?
H2B_3 C2_3 H2C_3 109.5 . . ?
P1_3 C3_3 H3A_3 109.5 . . ?
P1_3 C3_3 H3B_3 109.5 . . ?
H3A_3 C3_3 H3B_3 109.5 . . ?
P1_3 C3_3 H3C_3 109.5 . . ?
H3A_3 C3_3 H3C_3 109.5 . . ?
H3B_3 C3_3 H3C_3 109.5 . . ?
P1_3 C1_3 H1A_3 109.5 . . ?
P1_3 C1_3 H1B_3 109.5 . . ?
H1A_3 C1_3 H1B_3 109.5 . . ?
P1_3 C1_3 H1C_3 109.5 . . ?
H1A_3 C1_3 H1C_3 109.5 . . ?
H1B_3 C1_3 H1C_3 109.5 . . ?
C14_4 C1_4 C2_4 117.2(4) . . ?
C14_4 C1_4 B1_1 120.6(4) . . ?
C2_4 C1_4 B1_1 121.9(4) . . ?
C4_4 C3_4 C2_4 122.1(4) . . ?
C4_4 C3_4 H3_4 119.0 . . ?
C2_4 C3_4 H3_4 119.0 . . ?
C3_4 C2_4 C1_4 122.8(4) . . ?
C3_4 C2_4 C15_4 117.5(4) . . ?
C1_4 C2_4 C15_4 119.7(4) . . ?
C3_4 C4_4 C5_4 121.6(4) . . ?
C3_4 C4_4 H4_4 119.2 . . ?
C5_4 C4_4 H4_4 119.2 . . ?
C6_4 C5_4 C4_4 122.5(4) . . ?
C6_4 C5_4 C16_4 119.2(4) . . ?
C4_4 C5_4 C16_4 118.3(4) . . ?
C7_4 C6_4 C5_4 120.5(4) . . ?
C7_4 C6_4 H6_4 119.7 . . ?
C5_4 C6_4 H6_4 119.7 . . ?
C8_4 C7_4 C6_4 120.5(4) . . ?
C8_4 C7_4 H7_4 119.8 . . ?
C6_4 C7_4 H7_4 119.8 . . ?
C7_4 C8_4 C9_4 121.0(4) . . ?
C7_4 C8_4 H8_4 119.5 . . ?
C9_4 C8_4 H8_4 119.5 . . ?
C9_4 C16_4 C15_4 121.2(4) . . ?
C9_4 C16_4 C5_4 118.8(4) . . ?
C15_4 C16_4 C5_4 120.0(4) . . ?
C12_4 C15_4 C16_4 119.0(4) . . ?
C12_4 C15_4 C2_4 120.5(4) . . ?
C16_4 C15_4 C2_4 120.5(4) . . ?
C13_4 C14_4 C1_4 123.1(4) . . ?
C13_4 C14_4 H14_4 118.5 . . ?
C1_4 C14_4 H14_4 118.5 . . ?
C14_4 C13_4 C12_4 120.9(4) . . ?
C14_4 C13_4 H13_4 119.6 . . ?
C12_4 C13_4 H13_4 119.6 . . ?
C13_4 C12_4 C15_4 118.7(4) . . ?
C13_4 C12_4 C11_4 122.7(4) . . ?
C15_4 C12_4 C11_4 118.6(4) . . ?
C10_4 C11_4 C12_4 122.3(4) . . ?
C10_4 C11_4 H11_4 118.9 . . ?
C12_4 C11_4 H11_4 118.9 . . ?
C11_4 C10_4 C9_4 120.7(4) . . ?
C11_4 C10_4 H10_4 119.7 . . ?
C9_4 C10_4 H10_4 119.7 . . ?
C8_4 C9_4 C16_4 120.0(4) . . ?
C8_4 C9_4 C10_4 121.7(4) . . ?
C16_4 C9_4 C10_4 118.3(4) . . ?
C34_5 C21_5 C22_5 117.6(4) . . ?
C34_5 C21_5 B2_1 121.2(4) . . ?
C22_5 C21_5 B2_1 121.1(4) . . ?
C23_5 C24_5 C25_5 120.9(4) . . ?
C23_5 C24_5 H24_5 119.5 . . ?
C25_5 C24_5 H24_5 119.5 . . ?
C26_5 C25_5 C36_5 119.0(4) . . ?
C26_5 C25_5 C24_5 122.4(5) . . ?
C36_5 C25_5 C24_5 118.6(4) . . ?
C27_5 C26_5 C25_5 120.2(5) . . ?
C27_5 C26_5 H26_5 119.9 . . ?
C25_5 C26_5 H26_5 119.9 . . ?
C28_5 C27_5 C26_5 121.2(4) . . ?
C28_5 C27_5 H27_5 119.4 . . ?
C26_5 C27_5 H27_5 119.4 . . ?
C29_5 C28_5 C27_5 120.3(5) . . ?
C29_5 C28_5 H28_5 119.9 . . ?
C27_5 C28_5 H28_5 119.9 . . ?
C28_5 C29_5 C36_5 119.9(5) . . ?
C28_5 C29_5 C30_5 121.9(5) . . ?
C36_5 C29_5 C30_5 118.2(4) . . ?
C31_5 C30_5 C29_5 121.6(4) . . ?
C31_5 C30_5 H30_5 119.2 . . ?
C29_5 C30_5 H30_5 119.2 . . ?
C30_5 C31_5 C32_5 121.7(5) . . ?
C30_5 C31_5 H31_5 119.1 . . ?
C32_5 C31_5 H31_5 119.1 . . ?
C33_5 C32_5 C35_5 119.3(4) . . ?
C33_5 C32_5 C31_5 122.0(4) . . ?
C35_5 C32_5 C31_5 118.6(4) . . ?
C32_5 C33_5 C34_5 120.5(4) . . ?
C32_5 C33_5 H33_5 119.8 . . ?
C34_5 C33_5 H33_5 119.8 . . ?
C21_5 C34_5 C33_5 122.9(4) . . ?
C21_5 C34_5 H34_5 118.5 . . ?
C33_5 C34_5 H34_5 118.5 . . ?
C32_5 C35_5 C36_5 119.3(4) . . ?
C32_5 C35_5 C22_5 120.4(4) . . ?
C36_5 C35_5 C22_5 120.3(4) . . ?
C25_5 C36_5 C29_5 119.3(4) . . ?
C25_5 C36_5 C35_5 120.2(4) . . ?
C29_5 C36_5 C35_5 120.5(4) . . ?
C24_5 C23_5 C22_5 122.6(4) . . ?
C24_5 C23_5 H23_5 118.7 . . ?
C22_5 C23_5 H23_5 118.7 . . ?
C23_5 C22_5 C21_5 123.4(4) . . ?
C23_5 C22_5 C35_5 117.3(4) . . ?
C21_5 C22_5 C35_5 119.3(4) . . ?
C1_6 O1_6 C4_6 113.5(16) . . ?
O1_6 C1_6 C2_6 105.5(18) . . ?
O1_6 C1_6 H1A_6 110.6 . . ?
C2_6 C1_6 H1A_6 110.6 . . ?
O1_6 C1_6 H1B_6 110.6 . . ?
C2_6 C1_6 H1B_6 110.6 . . ?
H1A_6 C1_6 H1B_6 108.8 . . ?
C1_6 C2_6 C3_6 101.2(16) . . ?
C1_6 C2_6 H2A_6 111.5 . . ?
C3_6 C2_6 H2A_6 111.5 . . ?
C1_6 C2_6 H2AB_6 111.5 . . ?
C3_6 C2_6 H2AB_6 111.5 . . ?
H2A_6 C2_6 H2AB_6 109.3 . . ?
C4_6 C3_6 C2_6 98.4(12) . . ?
C4_6 C3_6 H3A_6 112.1 . . ?
C2_6 C3_6 H3A_6 112.1 . . ?
C4_6 C3_6 H3AB_6 112.1 . . ?
C2_6 C3_6 H3AB_6 112.1 . . ?
H3A_6 C3_6 H3AB_6 109.7 . . ?
O1_6 C4_6 C3_6 103.4(14) . . ?
O1_6 C4_6 H4A_6 111.1 . . ?
C3_6 C4_6 H4A_6 111.1 . . ?
O1_6 C4_6 H4AB_6 111.1 . . ?
C3_6 C4_6 H4AB_6 111.1 . . ?
H4A_6 C4_6 H4AB_6 109.0 . . ?
C4_16 O1_16 C1_16 103.4(19) . . ?
C2_16 C1_16 O1_16 106(2) . . ?
C2_16 C1_16 H1A_16 110.5 . . ?
O1_16 C1_16 H1A_16 110.5 . . ?
C2_16 C1_16 H1AB_16 110.5 . . ?
O1_16 C1_16 H1AB_16 110.5 . . ?
H1A_16 C1_16 H1AB_16 108.7 . . ?
C3_16 C2_16 C1_16 102(2) . . ?
C3_16 C2_16 H2A_16 111.3 . . ?
C1_16 C2_16 H2A_16 111.3 . . ?
C3_16 C2_16 H2AB_16 111.3 . . ?
C1_16 C2_16 H2AB_16 111.3 . . ?
H2A_16 C2_16 H2AB_16 109.2 . . ?
C2_16 C3_16 C4_16 101.6(15) . . ?
C2_16 C3_16 H3A_16 111.5 . . ?
C4_16 C3_16 H3A_16 111.5 . . ?
C2_16 C3_16 H3AB_16 111.5 . . ?
C4_16 C3_16 H3AB_16 111.5 . . ?
H3A_16 C3_16 H3AB_16 109.3 . . ?
O1_16 C4_16 C3_16 106.5(16) . . ?
O1_16 C4_16 H4A_16 110.4 . . ?
C3_16 C4_16 H4A_16 110.4 . . ?
O1_16 C4_16 H4AB_16 110.4 . . ?
C3_16 C4_16 H4AB_16 110.4 . . ?
H4A_16 C4_16 H4AB_16 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1_4 B1_1 B2_1 C21_5 13.3(6) . . . . ?
Cl1_1 B1_1 B2_1 C21_5 -114.6(4) . . . . ?
P1_2 B1_1 B2_1 C21_5 137.8(3) . . . . ?
C1_4 B1_1 B2_1 Cl2_1 -113.9(4) . . . . ?
Cl1_1 B1_1 B2_1 Cl2_1 118.2(3) . . . . ?
P1_2 B1_1 B2_1 Cl2_1 10.6(4) . . . . ?
C1_4 B1_1 B2_1 P1_3 138.1(3) . . . . ?
Cl1_1 B1_1 B2_1 P1_3 10.1(4) . . . . ?
P1_2 B1_1 B2_1 P1_3 -97.4(3) . . . . ?
B2_1 B1_1 C1_4 C14_4 -134.6(4) . . . . ?
Cl1_1 B1_1 C1_4 C14_4 -7.4(5) . . . . ?
P1_2 B1_1 C1_4 C14_4 94.3(4) . . . . ?
B2_1 B1_1 C1_4 C2_4 51.8(6) . . . . ?
Cl1_1 B1_1 C1_4 C2_4 179.0(3) . . . . ?
P1_2 B1_1 C1_4 C2_4 -79.3(4) . . . . ?
C4_4 C3_4 C2_4 C1_4 178.6(4) . . . . ?
C4_4 C3_4 C2_4 C15_4 -0.5(6) . . . . ?
C14_4 C1_4 C2_4 C3_4 -179.8(4) . . . . ?
B1_1 C1_4 C2_4 C3_4 -6.0(6) . . . . ?
C14_4 C1_4 C2_4 C15_4 -0.7(6) . . . . ?
B1_1 C1_4 C2_4 C15_4 173.1(4) . . . . ?
C2_4 C3_4 C4_4 C5_4 -0.8(6) . . . . ?
C3_4 C4_4 C5_4 C6_4 179.8(4) . . . . ?
C3_4 C4_4 C5_4 C16_4 1.8(6) . . . . ?
C4_4 C5_4 C6_4 C7_4 -178.5(4) . . . . ?
C16_4 C5_4 C6_4 C7_4 -0.5(6) . . . . ?
C5_4 C6_4 C7_4 C8_4 0.8(7) . . . . ?
C6_4 C7_4 C8_4 C9_4 -1.4(7) . . . . ?
C6_4 C5_4 C16_4 C9_4 0.7(6) . . . . ?
C4_4 C5_4 C16_4 C9_4 178.8(4) . . . . ?
C6_4 C5_4 C16_4 C15_4 -179.5(4) . . . . ?
C4_4 C5_4 C16_4 C15_4 -1.4(6) . . . . ?
C9_4 C16_4 C15_4 C12_4 0.9(6) . . . . ?
C5_4 C16_4 C15_4 C12_4 -179.0(4) . . . . ?
C9_4 C16_4 C15_4 C2_4 179.9(4) . . . . ?
C5_4 C16_4 C15_4 C2_4 0.0(6) . . . . ?
C3_4 C2_4 C15_4 C12_4 179.9(4) . . . . ?
C1_4 C2_4 C15_4 C12_4 0.7(6) . . . . ?
C3_4 C2_4 C15_4 C16_4 0.9(6) . . . . ?
C1_4 C2_4 C15_4 C16_4 -178.2(4) . . . . ?
C2_4 C1_4 C14_4 C13_4 0.2(6) . . . . ?
B1_1 C1_4 C14_4 C13_4 -173.7(4) . . . . ?
C1_4 C14_4 C13_4 C12_4 0.3(7) . . . . ?
C14_4 C13_4 C12_4 C15_4 -0.3(6) . . . . ?
C14_4 C13_4 C12_4 C11_4 179.3(4) . . . . ?
C16_4 C15_4 C12_4 C13_4 178.7(4) . . . . ?
C2_4 C15_4 C12_4 C13_4 -0.2(6) . . . . ?
C16_4 C15_4 C12_4 C11_4 -0.8(6) . . . . ?
C2_4 C15_4 C12_4 C11_4 -179.8(4) . . . . ?
C13_4 C12_4 C11_4 C10_4 -179.3(4) . . . . ?
C15_4 C12_4 C11_4 C10_4 0.2(6) . . . . ?
C12_4 C11_4 C10_4 C9_4 0.4(6) . . . . ?
C7_4 C8_4 C9_4 C16_4 1.6(7) . . . . ?
C7_4 C8_4 C9_4 C10_4 -179.2(4) . . . . ?
C15_4 C16_4 C9_4 C8_4 178.9(4) . . . . ?
C5_4 C16_4 C9_4 C8_4 -1.2(6) . . . . ?
C15_4 C16_4 C9_4 C10_4 -0.3(6) . . . . ?
C5_4 C16_4 C9_4 C10_4 179.5(4) . . . . ?
C11_4 C10_4 C9_4 C8_4 -179.5(4) . . . . ?
C11_4 C10_4 C9_4 C16_4 -0.3(6) . . . . ?
B1_1 B2_1 C21_5 C34_5 -132.4(4) . . . . ?
Cl2_1 B2_1 C21_5 C34_5 -5.3(5) . . . . ?
P1_3 B2_1 C21_5 C34_5 96.1(4) . . . . ?
B1_1 B2_1 C21_5 C22_5 51.8(6) . . . . ?
Cl2_1 B2_1 C21_5 C22_5 178.9(3) . . . . ?
P1_3 B2_1 C21_5 C22_5 -79.6(4) . . . . ?
C23_5 C24_5 C25_5 C26_5 176.2(4) . . . . ?
C23_5 C24_5 C25_5 C36_5 -3.4(6) . . . . ?
C36_5 C25_5 C26_5 C27_5 1.6(7) . . . . ?
C24_5 C25_5 C26_5 C27_5 -178.0(4) . . . . ?
C25_5 C26_5 C27_5 C28_5 -3.0(7) . . . . ?
C26_5 C27_5 C28_5 C29_5 1.8(8) . . . . ?
C27_5 C28_5 C29_5 C36_5 0.7(7) . . . . ?
C27_5 C28_5 C29_5 C30_5 -178.7(5) . . . . ?
C28_5 C29_5 C30_5 C31_5 -176.6(5) . . . . ?
C36_5 C29_5 C30_5 C31_5 4.1(7) . . . . ?
C29_5 C30_5 C31_5 C32_5 -1.5(8) . . . . ?
C30_5 C31_5 C32_5 C33_5 175.5(5) . . . . ?
C30_5 C31_5 C32_5 C35_5 -1.1(7) . . . . ?
C35_5 C32_5 C33_5 C34_5 -2.1(7) . . . . ?
C31_5 C32_5 C33_5 C34_5 -178.7(4) . . . . ?
C22_5 C21_5 C34_5 C33_5 1.4(6) . . . . ?
B2_1 C21_5 C34_5 C33_5 -174.5(4) . . . . ?
C32_5 C33_5 C34_5 C21_5 -0.4(7) . . . . ?
C33_5 C32_5 C35_5 C36_5 -175.7(4) . . . . ?
C31_5 C32_5 C35_5 C36_5 1.0(6) . . . . ?
C33_5 C32_5 C35_5 C22_5 3.4(6) . . . . ?
C31_5 C32_5 C35_5 C22_5 -179.9(4) . . . . ?
C26_5 C25_5 C36_5 C29_5 0.8(6) . . . . ?
C24_5 C25_5 C36_5 C29_5 -179.6(4) . . . . ?
C26_5 C25_5 C36_5 C35_5 -177.7(4) . . . . ?
C24_5 C25_5 C36_5 C35_5 1.9(6) . . . . ?
C28_5 C29_5 C36_5 C25_5 -2.0(7) . . . . ?
C30_5 C29_5 C36_5 C25_5 177.4(4) . . . . ?
C28_5 C29_5 C36_5 C35_5 176.6(4) . . . . ?
C30_5 C29_5 C36_5 C35_5 -4.1(6) . . . . ?
C32_5 C35_5 C36_5 C25_5 -179.9(4) . . . . ?
C22_5 C35_5 C36_5 C25_5 1.0(6) . . . . ?
C32_5 C35_5 C36_5 C29_5 1.6(6) . . . . ?
C22_5 C35_5 C36_5 C29_5 -177.5(4) . . . . ?
C25_5 C24_5 C23_5 C22_5 2.0(7) . . . . ?
C24_5 C23_5 C22_5 C21_5 -178.2(4) . . . . ?
C24_5 C23_5 C22_5 C35_5 0.9(6) . . . . ?
C34_5 C21_5 C22_5 C23_5 179.0(4) . . . . ?
B2_1 C21_5 C22_5 C23_5 -5.1(6) . . . . ?
C34_5 C21_5 C22_5 C35_5 -0.1(6) . . . . ?
B2_1 C21_5 C22_5 C35_5 175.8(4) . . . . ?
C32_5 C35_5 C22_5 C23_5 178.5(4) . . . . ?
C36_5 C35_5 C22_5 C23_5 -2.4(6) . . . . ?
C32_5 C35_5 C22_5 C21_5 -2.3(6) . . . . ?
C36_5 C35_5 C22_5 C21_5 176.8(4) . . . . ?
C4_6 O1_6 C1_6 C2_6 13(2) . . . . ?
O1_6 C1_6 C2_6 C3_6 -35(2) . . . . ?
C1_6 C2_6 C3_6 C4_6 40.7(15) . . . . ?
C1_6 O1_6 C4_6 C3_6 13.9(19) . . . . ?
C2_6 C3_6 C4_6 O1_6 -33.7(12) . . . . ?
C4_16 O1_16 C1_16 C2_16 5(3) . . . . ?
O1_16 C1_16 C2_16 C3_16 22(3) . . . . ?
C1_16 C2_16 C3_16 C4_16 -40(2) . . . . ?
C1_16 O1_16 C4_16 C3_16 -31(2) . . . . ?
C2_16 C3_16 C4_16 O1_16 46(2) . . . . ?

_refine_diff_density_max         0.689
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.090


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

data_test_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2169212'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_test_a              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: Reflections affected by beamstop
;


_audit_creation_method           'CIF-fill 1.2r (K.Radacki 2005-21)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        1-Pyr
_chemical_name_common            B2(Pyr)2(NMe2)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 B2 N2'
_chemical_formula_sum            'C36 H30 B2 N2'
_chemical_formula_weight         512.24

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

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

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

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

_cell_length_a                   13.398(4)
_cell_length_b                   18.112(6)
_cell_length_c                   23.412(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.273(13)
_cell_angle_gamma                90
_cell_volume                     5506(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    101(2)
_cell_measurement_reflns_used    9620
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.08


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_F_000             2160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.244
_exptl_absorpt_coefficient_mu    0.070
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6925
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 1.00 0.1250
1.00 0.00 -1.00 0.1520
-1.00 -1.00 1.00 0.1220
0.00 -1.00 0.00 0.1530
0.00 1.00 0.00 0.1140
1.00 -2.00 -1.00 0.1670
2.00 2.00 -1.00 0.1270
-2.00 -1.00 1.00 0.1270
2.00 0.00 -1.00 0.1420
1.00 1.00 0.00 0.1190
0.00 2.00 1.00 0.1220
0.00 -2.00 -1.00 0.1570
-2.00 -1.00 0.00 0.1220
2.00 1.00 0.00 0.1150
2.00 -1.00 -1.00 0.1570
2.00 2.00 1.00 0.1190
1.00 0.00 0.00 0.1220
-1.00 -2.00 -2.00 0.1370
-1.00 2.00 2.00 0.1380
1.00 -2.00 -2.00 0.1600
2.00 0.00 1.00 0.1210
-2.00 0.00 -1.00 0.1150
1.00 1.00 2.00 0.1340
-1.00 -1.00 -2.00 0.1090
2.00 -1.00 1.00 0.1360
-2.00 1.00 -1.00 0.1270
1.00 -1.00 2.00 0.1330
-1.00 1.00 -2.00 0.1420
0.00 -1.00 1.00 0.1380
-1.00 0.00 2.00 0.1250
1.00 0.00 -2.00 0.1560
0.00 1.00 -1.00 0.1520
1.00 1.00 -2.00 0.1210
-1.00 -1.00 2.00 0.1220

_exptl_absorpt_special_details   ?
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 CPA
_diffrn_detector_type            'Photon II'
_diffrn_detector_area_resol_mean 7.5
_diffrn_reflns_number            160710
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.930
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11259
_reflns_number_gt                9621
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BIS 6.2.14 / APEX3 ver. 2019.1 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0568P)²+3.3039P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         11259
_refine_ls_number_parameters     729
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1286
_refine_ls_wR_factor_gt          0.1217
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.15875(14) 0.50774(10) 0.74350(9) 0.0399(4) Uani 1 1 d . . . . .
H1A H 1.231204 0.506556 0.742042 0.060 Uiso 1 1 calc R U . . .
H1B H 1.153415 0.528414 0.781320 0.060 Uiso 1 1 calc R U . . .
H1C H 1.119527 0.538520 0.711285 0.060 Uiso 1 1 calc R U . . .
N1 N 1.11702(10) 0.43258(8) 0.73731(6) 0.0328(3) Uani 1 1 d . . . . .
B1 B 1.02499(14) 0.41142(11) 0.69798(8) 0.0305(4) Uani 1 1 d . . . . .
C2 C 1.18043(13) 0.38162(11) 0.77924(8) 0.0399(4) Uani 1 1 d . . . . .
H2A H 1.150032 0.332131 0.773514 0.060 Uiso 1 1 calc R U . . .
H2B H 1.183867 0.398323 0.819495 0.060 Uiso 1 1 calc R U . . .
H2C H 1.250027 0.380153 0.772895 0.060 Uiso 1 1 calc R U . . .
N2 N 0.98557(11) 0.26591(8) 0.66571(6) 0.0359(3) Uani 1 1 d . . . . .
B2 B 0.96636(14) 0.32695(11) 0.69788(8) 0.0325(4) Uani 1 1 d . . . . .
C4 C 0.92801(15) 0.19633(11) 0.65961(9) 0.0445(4) Uani 1 1 d . . . . .
H4A H 0.975358 0.155629 0.674709 0.067 Uiso 1 1 calc R U . . .
H4B H 0.894815 0.187674 0.617930 0.067 Uiso 1 1 calc R U . . .
H4C H 0.875366 0.199182 0.682095 0.067 Uiso 1 1 calc R U . . .
C3 C 1.06239(15) 0.26559(12) 0.63146(10) 0.0494(5) Uani 1 1 d . . . . .
H3A H 1.110793 0.224890 0.644633 0.074 Uiso 1 1 calc R U . . .
H3B H 1.099881 0.312546 0.637003 0.074 Uiso 1 1 calc R U . . .
H3C H 1.028331 0.259111 0.589639 0.074 Uiso 1 1 calc R U . . .
C1_1 C 0.95992(12) 0.46892(9) 0.65219(7) 0.0304(3) Uani 1 1 d . . . . .
C2_1 C 0.89551(12) 0.52231(9) 0.66892(7) 0.0280(3) Uani 1 1 d . . . . .
C3_1 C 0.89618(13) 0.53426(9) 0.72996(7) 0.0328(3) Uani 1 1 d . . . . .
H3_1 H 0.940914 0.505540 0.759449 0.039 Uiso 1 1 calc R U . . .
C4_1 C 0.83496(14) 0.58514(10) 0.74628(7) 0.0361(4) Uani 1 1 d . . . . .
H4_1 H 0.837974 0.591524 0.786949 0.043 Uiso 1 1 calc R U . . .
C5_1 C 0.76571(13) 0.62965(10) 0.70383(8) 0.0343(4) Uani 1 1 d . . . . .
C6_1 C 0.70257(15) 0.68345(11) 0.71957(9) 0.0436(4) Uani 1 1 d . . . . .
H6_1 H 0.705524 0.691546 0.760043 0.052 Uiso 1 1 calc R U . . .
C7_1 C 0.63592(15) 0.72505(12) 0.67724(10) 0.0490(5) Uani 1 1 d . . . . .
H7_1 H 0.593907 0.761443 0.688948 0.059 Uiso 1 1 calc R U . . .
C8_1 C 0.62984(15) 0.71422(11) 0.61812(9) 0.0449(4) Uani 1 1 d . . . . .
H8_1 H 0.583286 0.743029 0.589575 0.054 Uiso 1 1 calc R U . . .
C9_1 C 0.69129(13) 0.66142(9) 0.59972(8) 0.0346(4) Uani 1 1 d . . . . .
C10_1 C 0.68850(14) 0.64921(10) 0.53885(8) 0.0389(4) Uani 1 1 d . . . . .
H10_1 H 0.640927 0.676192 0.509450 0.047 Uiso 1 1 calc R U . . .
C11_1 C 0.75150(14) 0.60060(9) 0.52256(7) 0.0360(4) Uani 1 1 d . . . . .
H11_1 H 0.748876 0.595075 0.481859 0.043 Uiso 1 1 calc R U . . .
C12_1 C 0.82324(13) 0.55637(9) 0.56494(7) 0.0310(3) Uani 1 1 d . . . . .
C13_1 C 0.88986(14) 0.50528(10) 0.54946(7) 0.0355(4) Uani 1 1 d . . . . .
H13_1 H 0.890764 0.499904 0.509228 0.043 Uiso 1 1 calc R U . . .
C14_1 C 0.95480(14) 0.46219(10) 0.59175(7) 0.0355(4) Uani 1 1 d . . . . .
H14_1 H 0.997427 0.426785 0.579406 0.043 Uiso 1 1 calc R U . . .
C15_1 C 0.82638(12) 0.56541(9) 0.62581(7) 0.0277(3) Uani 1 1 d . . . . .
C16_1 C 0.76098(12) 0.61853(9) 0.64296(7) 0.0298(3) Uani 1 1 d . . . . .
C21_1 C 0.87472(12) 0.32364(9) 0.73072(7) 0.0318(3) Uani 1 1 d . . . . .
C22_1 C 0.87692(12) 0.28095(9) 0.78085(7) 0.0295(3) Uani 1 1 d . . . . .
C23_1 C 0.96259(12) 0.23235(9) 0.80666(8) 0.0336(4) Uani 1 1 d . . . . .
H23_1 H 1.019025 0.229373 0.788900 0.040 Uiso 1 1 calc R U . . .
C24_1 C 0.96443(13) 0.19139(9) 0.85498(8) 0.0345(4) Uani 1 1 d . . . . .
H24_1 H 1.021793 0.160070 0.869949 0.041 Uiso 1 1 calc R U . . .
C25_1 C 0.88199(12) 0.19360(9) 0.88474(7) 0.0315(3) Uani 1 1 d . . . . .
C26_1 C 0.88457(14) 0.15534(10) 0.93645(8) 0.0393(4) Uani 1 1 d . . . . .
H26_1 H 0.941953 0.124738 0.953102 0.047 Uiso 1 1 calc R U . . .
C27_1 C 0.80474(15) 0.16114(10) 0.96410(9) 0.0427(4) Uani 1 1 d . . . . .
H27_1 H 0.808361 0.135257 0.999849 0.051 Uiso 1 1 calc R U . . .
C28_1 C 0.71937(14) 0.20459(10) 0.93990(8) 0.0404(4) Uani 1 1 d . . . . .
H28_1 H 0.664444 0.207452 0.958867 0.048 Uiso 1 1 calc R U . . .
C29_1 C 0.71345(12) 0.24430(9) 0.88771(7) 0.0318(3) Uani 1 1 d . . . . .
C30_1 C 0.62597(13) 0.28997(11) 0.86149(9) 0.0418(4) Uani 1 1 d . . . . .
H30_1 H 0.569657 0.292148 0.879406 0.050 Uiso 1 1 calc R U . . .
C31_1 C 0.62216(12) 0.32736(9) 0.81511(9) 0.0383(4) Uani 1 1 d . . . . .
H31_1 H 0.562745 0.356527 0.799543 0.046 Uiso 1 1 calc R U . . .
C32_1 C 0.70508(12) 0.32750(8) 0.78463(7) 0.0307(3) Uani 1 1 d . . . . .
C33_1 C 0.70413(12) 0.36856(9) 0.73462(7) 0.0319(3) Uani 1 1 d . . . . .
H33_1 H 0.645864 0.398164 0.717573 0.038 Uiso 1 1 calc R U . . .
C34_1 C 0.78714(12) 0.36702(9) 0.70912(8) 0.0335(4) Uani 1 1 d . . . . .
H34_1 H 0.784438 0.396827 0.675385 0.040 Uiso 1 1 calc R U . . .
C35_1 C 0.79374(12) 0.28224(8) 0.80867(7) 0.0293(3) Uani 1 1 d . . . . .
C36_1 C 0.79611(12) 0.24009(9) 0.86005(7) 0.0299(3) Uani 1 1 d . . . . .
B1_3 B 0.51552(12) 0.10794(9) 0.65033(8) 0.0256(3) Uani 1 1 d . . . . .
C1_3 C 0.59338(15) 0.14071(9) 0.75731(8) 0.0386(4) Uani 1 1 d . . . . .
H1A_3 H 0.654374 0.115113 0.780598 0.058 Uiso 1 1 calc R U . . .
H1B_3 H 0.548421 0.154379 0.782881 0.058 Uiso 1 1 calc R U . . .
H1C_3 H 0.614725 0.185338 0.739827 0.058 Uiso 1 1 calc R U . . .
N1_3 N 0.53757(10) 0.09190(7) 0.71046(6) 0.0288(3) Uani 1 1 d . . . . .
B2_3 B 0.44337(12) 0.05089(9) 0.59758(7) 0.0239(3) Uani 1 1 d . . . . .
C3_3 C 0.57836(12) -0.04855(9) 0.60912(8) 0.0328(3) Uani 1 1 d . . . . .
H3A_3 H 0.617749 -0.056006 0.579437 0.049 Uiso 1 1 calc R U . . .
H3B_3 H 0.568483 -0.096099 0.626927 0.049 Uiso 1 1 calc R U . . .
H3C_3 H 0.616103 -0.014985 0.639740 0.049 Uiso 1 1 calc R U . . .
C4_3 C 0.41989(12) -0.06279(9) 0.53312(7) 0.0287(3) Uani 1 1 d . . . . .
H4A_3 H 0.462332 -0.073402 0.505484 0.043 Uiso 1 1 calc R U . . .
H4B_3 H 0.357306 -0.036716 0.512444 0.043 Uiso 1 1 calc R U . . .
H4C_3 H 0.401026 -0.109201 0.549271 0.043 Uiso 1 1 calc R U . . .
C2_3 C 0.50302(14) 0.02479(9) 0.73422(7) 0.0372(4) Uani 1 1 d . . . . .
H2A_3 H 0.562846 -0.002302 0.757219 0.056 Uiso 1 1 calc R U . . .
H2B_3 H 0.465409 -0.006281 0.701723 0.056 Uiso 1 1 calc R U . . .
H2C_3 H 0.457597 0.037875 0.759670 0.056 Uiso 1 1 calc R U . . .
N2_3 N 0.47816(9) -0.01658(7) 0.58118(5) 0.0250(3) Uani 1 1 d . . . . .
C1_4 C 0.54864(11) 0.18589(8) 0.62924(7) 0.0265(3) Uani 1 1 d . . . . .
C2_4 C 0.48879(11) 0.24987(8) 0.63147(6) 0.0261(3) Uani 1 1 d . . . . .
C3_4 C 0.40023(12) 0.24731(9) 0.65589(7) 0.0310(3) Uani 1 1 d . . . . .
H3_4 H 0.381944 0.201656 0.670515 0.037 Uiso 1 1 calc R U . . .
C4_4 C 0.34217(13) 0.30755(10) 0.65875(7) 0.0339(4) Uani 1 1 d . . . . .
H4_4 H 0.284733 0.303224 0.675556 0.041 Uiso 1 1 calc R U . . .
C5_4 C 0.36527(13) 0.37771(9) 0.63702(7) 0.0307(3) Uani 1 1 d . . . . .
C6_4 C 0.30342(14) 0.44043(10) 0.63771(7) 0.0363(4) Uani 1 1 d . . . . .
H6_4 H 0.243965 0.436767 0.652800 0.044 Uiso 1 1 calc R U . . .
C7_4 C 0.32881(15) 0.50734(10) 0.61653(8) 0.0397(4) Uani 1 1 d . . . . .
H7_4 H 0.286387 0.549244 0.617006 0.048 Uiso 1 1 calc R U . . .
C8_4 C 0.41513(15) 0.51382(9) 0.59471(7) 0.0377(4) Uani 1 1 d . . . . .
H8_4 H 0.432111 0.560490 0.581152 0.045 Uiso 1 1 calc R U . . .
C9_4 C 0.47842(13) 0.45257(9) 0.59217(7) 0.0339(4) Uani 1 1 d . . . . .
C10_4 C 0.56754(14) 0.45652(10) 0.56928(8) 0.0395(4) Uani 1 1 d . . . . .
H10_4 H 0.586308 0.502834 0.555976 0.047 Uiso 1 1 calc R U . . .
C11_4 C 0.62604(13) 0.39712(10) 0.56582(8) 0.0365(4) Uani 1 1 d . . . . .
H11_4 H 0.684452 0.402307 0.549963 0.044 Uiso 1 1 calc R U . . .
C12_4 C 0.60109(12) 0.32491(9) 0.58606(7) 0.0316(3) Uani 1 1 d . . . . .
C13_4 C 0.65963(12) 0.26172(10) 0.58425(7) 0.0347(4) Uani 1 1 d . . . . .
H13_4 H 0.718741 0.264894 0.568803 0.042 Uiso 1 1 calc R U . . .
C14_4 C 0.63309(12) 0.19375(9) 0.60470(7) 0.0316(3) Uani 1 1 d . . . . .
H14_4 H 0.673767 0.151602 0.601814 0.038 Uiso 1 1 calc R U . . .
C15_4 C 0.51393(12) 0.31911(9) 0.61006(6) 0.0273(3) Uani 1 1 d . . . . .
C16_4 C 0.45248(12) 0.38310(8) 0.61331(7) 0.0293(3) Uani 1 1 d . . . . .
C21_4 C 0.33349(11) 0.08160(8) 0.56398(6) 0.0236(3) Uani 1 1 d . . . . .
C22_4 C 0.24007(11) 0.05631(8) 0.57528(6) 0.0216(3) Uani 1 1 d . . . . .
C23_4 C 0.23688(11) -0.00400(8) 0.61496(6) 0.0248(3) Uani 1 1 d . . . . .
H23_4 H 0.299381 -0.027819 0.634057 0.030 Uiso 1 1 calc R U . . .
C24_4 C 0.14747(12) -0.02777(8) 0.62586(7) 0.0270(3) Uani 1 1 d . . . . .
H24_4 H 0.148820 -0.067577 0.652470 0.032 Uiso 1 1 calc R U . . .
C25_4 C 0.05062(11) 0.00601(8) 0.59799(6) 0.0254(3) Uani 1 1 d . . . . .
C26_4 C -0.04293(12) -0.01792(9) 0.60805(7) 0.0309(3) Uani 1 1 d . . . . .
H26_4 H -0.043460 -0.057158 0.634898 0.037 Uiso 1 1 calc R U . . .
C27_4 C -0.13491(12) 0.01523(10) 0.57911(8) 0.0339(4) Uani 1 1 d . . . . .
H27_4 H -0.197857 -0.001471 0.586383 0.041 Uiso 1 1 calc R U . . .
C28_4 C -0.13579(12) 0.07238(9) 0.53976(7) 0.0316(3) Uani 1 1 d . . . . .
H28_4 H -0.199454 0.094397 0.520292 0.038 Uiso 1 1 calc R U . . .
C29_4 C -0.04454(11) 0.09814(8) 0.52824(7) 0.0261(3) Uani 1 1 d . . . . .
C30_4 C -0.04270(12) 0.15716(9) 0.48745(7) 0.0319(3) Uani 1 1 d . . . . .
H30_4 H -0.105591 0.179944 0.467650 0.038 Uiso 1 1 calc R U . . .
C31_4 C 0.04513(13) 0.18061(9) 0.47681(7) 0.0317(3) Uani 1 1 d . . . . .
H31_4 H 0.043419 0.219665 0.449497 0.038 Uiso 1 1 calc R U . . .
C32_4 C 0.14278(11) 0.14817(8) 0.50572(6) 0.0260(3) Uani 1 1 d . . . . .
C33_4 C 0.23518(12) 0.17146(9) 0.49435(7) 0.0295(3) Uani 1 1 d . . . . .
H33_4 H 0.234666 0.209420 0.466282 0.035 Uiso 1 1 calc R U . . .
C34_4 C 0.32789(12) 0.13967(9) 0.52369(7) 0.0278(3) Uani 1 1 d . . . . .
H34_4 H 0.389908 0.157938 0.516206 0.033 Uiso 1 1 calc R U . . .
C35_4 C 0.14467(11) 0.09003(8) 0.54670(6) 0.0224(3) Uani 1 1 d . . . . .
C36_4 C 0.05043(11) 0.06496(8) 0.55792(6) 0.0234(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.465(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
N1 B1 1.398(2) . ?
N1 C2 1.458(2) . ?
B1 C1_1 1.592(3) . ?
B1 B2 1.720(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N2 B2 1.397(2) . ?
N2 C3 1.452(2) . ?
N2 C4 1.466(2) . ?
B2 C21_1 1.602(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C1_1 C14_1 1.405(2) . ?
C1_1 C2_1 1.414(2) . ?
C2_1 C15_1 1.423(2) . ?
C2_1 C3_1 1.443(2) . ?
C3_1 C4_1 1.350(2) . ?
C3_1 H3_1 0.9500 . ?
C4_1 C5_1 1.430(3) . ?
C4_1 H4_1 0.9500 . ?
C5_1 C6_1 1.398(3) . ?
C5_1 C16_1 1.425(2) . ?
C6_1 C7_1 1.382(3) . ?
C6_1 H6_1 0.9500 . ?
C7_1 C8_1 1.380(3) . ?
C7_1 H7_1 0.9500 . ?
C8_1 C9_1 1.397(3) . ?
C8_1 H8_1 0.9500 . ?
C9_1 C16_1 1.426(2) . ?
C9_1 C10_1 1.433(3) . ?
C10_1 C11_1 1.339(3) . ?
C10_1 H10_1 0.9500 . ?
C11_1 C12_1 1.442(2) . ?
C11_1 H11_1 0.9500 . ?
C12_1 C13_1 1.394(2) . ?
C12_1 C15_1 1.425(2) . ?
C13_1 C14_1 1.386(3) . ?
C13_1 H13_1 0.9500 . ?
C14_1 H14_1 0.9500 . ?
C15_1 C16_1 1.424(2) . ?
C21_1 C34_1 1.399(2) . ?
C21_1 C22_1 1.399(2) . ?
C22_1 C35_1 1.423(2) . ?
C22_1 C23_1 1.455(2) . ?
C23_1 C24_1 1.348(3) . ?
C23_1 H23_1 0.9500 . ?
C24_1 C25_1 1.444(2) . ?
C24_1 H24_1 0.9500 . ?
C25_1 C26_1 1.388(3) . ?
C25_1 C36_1 1.428(2) . ?
C26_1 C27_1 1.384(3) . ?
C26_1 H26_1 0.9500 . ?
C27_1 C28_1 1.389(3) . ?
C27_1 H27_1 0.9500 . ?
C28_1 C29_1 1.403(3) . ?
C28_1 H28_1 0.9500 . ?
C29_1 C36_1 1.416(2) . ?
C29_1 C30_1 1.442(3) . ?
C30_1 C31_1 1.270(3) . ?
C30_1 H30_1 0.9500 . ?
C31_1 C32_1 1.461(2) . ?
C31_1 H31_1 0.9500 . ?
C32_1 C33_1 1.385(2) . ?
C32_1 C35_1 1.439(2) . ?
C33_1 C34_1 1.386(2) . ?
C33_1 H33_1 0.9500 . ?
C34_1 H34_1 0.9500 . ?
C35_1 C36_1 1.419(2) . ?
B1_3 N1_3 1.396(2) . ?
B1_3 C1_4 1.594(2) . ?
B1_3 B2_3 1.714(2) . ?
C1_3 N1_3 1.462(2) . ?
C1_3 H1A_3 0.9800 . ?
C1_3 H1B_3 0.9800 . ?
C1_3 H1C_3 0.9800 . ?
N1_3 C2_3 1.459(2) . ?
B2_3 N2_3 1.395(2) . ?
B2_3 C21_4 1.589(2) . ?
C3_3 N2_3 1.4602(19) . ?
C3_3 H3A_3 0.9800 . ?
C3_3 H3B_3 0.9800 . ?
C3_3 H3C_3 0.9800 . ?
C4_3 N2_3 1.4638(19) . ?
C4_3 H4A_3 0.9800 . ?
C4_3 H4B_3 0.9800 . ?
C4_3 H4C_3 0.9800 . ?
C2_3 H2A_3 0.9800 . ?
C2_3 H2B_3 0.9800 . ?
C2_3 H2C_3 0.9800 . ?
C1_4 C14_4 1.397(2) . ?
C1_4 C2_4 1.418(2) . ?
C2_4 C15_4 1.422(2) . ?
C2_4 C3_4 1.439(2) . ?
C3_4 C4_4 1.351(2) . ?
C3_4 H3_4 0.9500 . ?
C4_4 C5_4 1.431(2) . ?
C4_4 H4_4 0.9500 . ?
C5_4 C6_4 1.409(2) . ?
C5_4 C16_4 1.415(2) . ?
C6_4 C7_4 1.383(3) . ?
C6_4 H6_4 0.9500 . ?
C7_4 C8_4 1.380(3) . ?
C7_4 H7_4 0.9500 . ?
C8_4 C9_4 1.407(2) . ?
C8_4 H8_4 0.9500 . ?
C9_4 C16_4 1.426(2) . ?
C9_4 C10_4 1.426(3) . ?
C10_4 C11_4 1.345(3) . ?
C10_4 H10_4 0.9500 . ?
C11_4 C12_4 1.458(2) . ?
C11_4 H11_4 0.9500 . ?
C12_4 C13_4 1.394(2) . ?
C12_4 C15_4 1.419(2) . ?
C13_4 C14_4 1.398(2) . ?
C13_4 H13_4 0.9500 . ?
C14_4 H14_4 0.9500 . ?
C15_4 C16_4 1.435(2) . ?
C21_4 C34_4 1.402(2) . ?
C21_4 C22_4 1.418(2) . ?
C22_4 C35_4 1.426(2) . ?
C22_4 C23_4 1.441(2) . ?
C23_4 C24_4 1.355(2) . ?
C23_4 H23_4 0.9500 . ?
C24_4 C25_4 1.437(2) . ?
C24_4 H24_4 0.9500 . ?
C25_4 C26_4 1.400(2) . ?
C25_4 C36_4 1.421(2) . ?
C26_4 C27_4 1.388(2) . ?
C26_4 H26_4 0.9500 . ?
C27_4 C28_4 1.384(3) . ?
C27_4 H27_4 0.9500 . ?
C28_4 C29_4 1.396(2) . ?
C28_4 H28_4 0.9500 . ?
C29_4 C36_4 1.424(2) . ?
C29_4 C30_4 1.438(2) . ?
C30_4 C31_4 1.331(2) . ?
C30_4 H30_4 0.9500 . ?
C31_4 C32_4 1.442(2) . ?
C31_4 H31_4 0.9500 . ?
C32_4 C33_4 1.394(2) . ?
C32_4 C35_4 1.421(2) . ?
C33_4 C34_4 1.388(2) . ?
C33_4 H33_4 0.9500 . ?
C34_4 H34_4 0.9500 . ?
C35_4 C36_4 1.426(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
B1 N1 C2 122.86(15) . . ?
B1 N1 C1 124.95(15) . . ?
C2 N1 C1 112.13(14) . . ?
N1 B1 C1_1 120.79(15) . . ?
N1 B1 B2 124.97(15) . . ?
C1_1 B1 B2 114.03(14) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
B2 N2 C3 123.41(16) . . ?
B2 N2 C4 124.79(15) . . ?
C3 N2 C4 111.72(14) . . ?
N2 B2 C21_1 119.59(15) . . ?
N2 B2 B1 124.07(15) . . ?
C21_1 B2 B1 115.88(14) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C14_1 C1_1 C2_1 117.17(15) . . ?
C14_1 C1_1 B1 120.29(15) . . ?
C2_1 C1_1 B1 122.08(14) . . ?
C1_1 C2_1 C15_1 120.90(14) . . ?
C1_1 C2_1 C3_1 121.44(15) . . ?
C15_1 C2_1 C3_1 117.65(15) . . ?
C4_1 C3_1 C2_1 121.79(16) . . ?
C4_1 C3_1 H3_1 119.1 . . ?
C2_1 C3_1 H3_1 119.1 . . ?
C3_1 C4_1 C5_1 121.57(15) . . ?
C3_1 C4_1 H4_1 119.2 . . ?
C5_1 C4_1 H4_1 119.2 . . ?
C6_1 C5_1 C16_1 118.79(16) . . ?
C6_1 C5_1 C4_1 122.74(16) . . ?
C16_1 C5_1 C4_1 118.47(15) . . ?
C7_1 C6_1 C5_1 121.12(18) . . ?
C7_1 C6_1 H6_1 119.4 . . ?
C5_1 C6_1 H6_1 119.4 . . ?
C8_1 C7_1 C6_1 120.62(18) . . ?
C8_1 C7_1 H7_1 119.7 . . ?
C6_1 C7_1 H7_1 119.7 . . ?
C7_1 C8_1 C9_1 120.85(18) . . ?
C7_1 C8_1 H8_1 119.6 . . ?
C9_1 C8_1 H8_1 119.6 . . ?
C8_1 C9_1 C16_1 119.09(17) . . ?
C8_1 C9_1 C10_1 122.62(17) . . ?
C16_1 C9_1 C10_1 118.28(16) . . ?
C11_1 C10_1 C9_1 121.40(16) . . ?
C11_1 C10_1 H10_1 119.3 . . ?
C9_1 C10_1 H10_1 119.3 . . ?
C10_1 C11_1 C12_1 121.96(16) . . ?
C10_1 C11_1 H11_1 119.0 . . ?
C12_1 C11_1 H11_1 119.0 . . ?
C13_1 C12_1 C15_1 118.25(15) . . ?
C13_1 C12_1 C11_1 123.41(15) . . ?
C15_1 C12_1 C11_1 118.34(15) . . ?
C14_1 C13_1 C12_1 121.15(15) . . ?
C14_1 C13_1 H13_1 119.4 . . ?
C12_1 C13_1 H13_1 119.4 . . ?
C13_1 C14_1 C1_1 122.46(16) . . ?
C13_1 C14_1 H14_1 118.8 . . ?
C1_1 C14_1 H14_1 118.8 . . ?
C2_1 C15_1 C16_1 120.58(14) . . ?
C2_1 C15_1 C12_1 120.00(15) . . ?
C16_1 C15_1 C12_1 119.42(15) . . ?
C15_1 C16_1 C5_1 119.92(15) . . ?
C15_1 C16_1 C9_1 120.56(15) . . ?
C5_1 C16_1 C9_1 119.52(15) . . ?
C34_1 C21_1 C22_1 117.12(15) . . ?
C34_1 C21_1 B2 118.62(16) . . ?
C22_1 C21_1 B2 124.25(15) . . ?
C21_1 C22_1 C35_1 121.19(15) . . ?
C21_1 C22_1 C23_1 122.28(15) . . ?
C35_1 C22_1 C23_1 116.53(15) . . ?
C24_1 C23_1 C22_1 122.07(15) . . ?
C24_1 C23_1 H23_1 119.0 . . ?
C22_1 C23_1 H23_1 119.0 . . ?
C23_1 C24_1 C25_1 122.12(15) . . ?
C23_1 C24_1 H24_1 118.9 . . ?
C25_1 C24_1 H24_1 118.9 . . ?
C26_1 C25_1 C36_1 119.45(16) . . ?
C26_1 C25_1 C24_1 123.33(16) . . ?
C36_1 C25_1 C24_1 117.18(15) . . ?
C27_1 C26_1 C25_1 120.95(17) . . ?
C27_1 C26_1 H26_1 119.5 . . ?
C25_1 C26_1 H26_1 119.5 . . ?
C26_1 C27_1 C28_1 120.38(18) . . ?
C26_1 C27_1 H27_1 119.8 . . ?
C28_1 C27_1 H27_1 119.8 . . ?
C27_1 C28_1 C29_1 120.65(17) . . ?
C27_1 C28_1 H28_1 119.7 . . ?
C29_1 C28_1 H28_1 119.7 . . ?
C28_1 C29_1 C36_1 119.21(16) . . ?
C28_1 C29_1 C30_1 122.02(16) . . ?
C36_1 C29_1 C30_1 118.77(16) . . ?
C31_1 C30_1 C29_1 121.79(17) . . ?
C31_1 C30_1 H30_1 119.1 . . ?
C29_1 C30_1 H30_1 119.1 . . ?
C30_1 C31_1 C32_1 122.92(16) . . ?
C30_1 C31_1 H31_1 118.5 . . ?
C32_1 C31_1 H31_1 118.5 . . ?
C33_1 C32_1 C35_1 118.13(15) . . ?
C33_1 C32_1 C31_1 124.36(15) . . ?
C35_1 C32_1 C31_1 117.51(16) . . ?
C32_1 C33_1 C34_1 120.82(15) . . ?
C32_1 C33_1 H33_1 119.6 . . ?
C34_1 C33_1 H33_1 119.6 . . ?
C33_1 C34_1 C21_1 123.09(16) . . ?
C33_1 C34_1 H34_1 118.5 . . ?
C21_1 C34_1 H34_1 118.5 . . ?
C36_1 C35_1 C22_1 121.54(15) . . ?
C36_1 C35_1 C32_1 118.82(15) . . ?
C22_1 C35_1 C32_1 119.64(15) . . ?
C29_1 C36_1 C35_1 120.15(15) . . ?
C29_1 C36_1 C25_1 119.31(16) . . ?
C35_1 C36_1 C25_1 120.53(15) . . ?
N1_3 B1_3 C1_4 119.40(14) . . ?
N1_3 B1_3 B2_3 122.86(14) . . ?
C1_4 B1_3 B2_3 117.46(13) . . ?
N1_3 C1_3 H1A_3 109.5 . . ?
N1_3 C1_3 H1B_3 109.5 . . ?
H1A_3 C1_3 H1B_3 109.5 . . ?
N1_3 C1_3 H1C_3 109.5 . . ?
H1A_3 C1_3 H1C_3 109.5 . . ?
H1B_3 C1_3 H1C_3 109.5 . . ?
B1_3 N1_3 C2_3 123.35(13) . . ?
B1_3 N1_3 C1_3 124.92(14) . . ?
C2_3 N1_3 C1_3 111.68(13) . . ?
N2_3 B2_3 C21_4 120.13(13) . . ?
N2_3 B2_3 B1_3 123.99(13) . . ?
C21_4 B2_3 B1_3 115.77(13) . . ?
N2_3 C3_3 H3A_3 109.5 . . ?
N2_3 C3_3 H3B_3 109.5 . . ?
H3A_3 C3_3 H3B_3 109.5 . . ?
N2_3 C3_3 H3C_3 109.5 . . ?
H3A_3 C3_3 H3C_3 109.5 . . ?
H3B_3 C3_3 H3C_3 109.5 . . ?
N2_3 C4_3 H4A_3 109.5 . . ?
N2_3 C4_3 H4B_3 109.5 . . ?
H4A_3 C4_3 H4B_3 109.5 . . ?
N2_3 C4_3 H4C_3 109.5 . . ?
H4A_3 C4_3 H4C_3 109.5 . . ?
H4B_3 C4_3 H4C_3 109.5 . . ?
N1_3 C2_3 H2A_3 109.5 . . ?
N1_3 C2_3 H2B_3 109.5 . . ?
H2A_3 C2_3 H2B_3 109.5 . . ?
N1_3 C2_3 H2C_3 109.5 . . ?
H2A_3 C2_3 H2C_3 109.5 . . ?
H2B_3 C2_3 H2C_3 109.5 . . ?
B2_3 N2_3 C3_3 123.82(13) . . ?
B2_3 N2_3 C4_3 124.15(12) . . ?
C3_3 N2_3 C4_3 112.01(12) . . ?
C14_4 C1_4 C2_4 117.05(14) . . ?
C14_4 C1_4 B1_3 122.23(14) . . ?
C2_4 C1_4 B1_3 120.62(13) . . ?
C1_4 C2_4 C15_4 121.53(14) . . ?
C1_4 C2_4 C3_4 121.17(14) . . ?
C15_4 C2_4 C3_4 117.30(14) . . ?
C4_4 C3_4 C2_4 122.33(15) . . ?
C4_4 C3_4 H3_4 118.8 . . ?
C2_4 C3_4 H3_4 118.8 . . ?
C3_4 C4_4 C5_4 121.47(15) . . ?
C3_4 C4_4 H4_4 119.3 . . ?
C5_4 C4_4 H4_4 119.3 . . ?
C6_4 C5_4 C16_4 119.59(15) . . ?
C6_4 C5_4 C4_4 122.20(16) . . ?
C16_4 C5_4 C4_4 118.21(14) . . ?
C7_4 C6_4 C5_4 120.33(17) . . ?
C7_4 C6_4 H6_4 119.8 . . ?
C5_4 C6_4 H6_4 119.8 . . ?
C8_4 C7_4 C6_4 120.67(16) . . ?
C8_4 C7_4 H7_4 119.7 . . ?
C6_4 C7_4 H7_4 119.7 . . ?
C7_4 C8_4 C9_4 121.17(16) . . ?
C7_4 C8_4 H8_4 119.4 . . ?
C9_4 C8_4 H8_4 119.4 . . ?
C8_4 C9_4 C16_4 118.70(16) . . ?
C8_4 C9_4 C10_4 123.07(16) . . ?
C16_4 C9_4 C10_4 118.23(16) . . ?
C11_4 C10_4 C9_4 122.46(16) . . ?
C11_4 C10_4 H10_4 118.8 . . ?
C9_4 C10_4 H10_4 118.8 . . ?
C10_4 C11_4 C12_4 120.96(16) . . ?
C10_4 C11_4 H11_4 119.5 . . ?
C12_4 C11_4 H11_4 119.5 . . ?
C13_4 C12_4 C15_4 118.38(15) . . ?
C13_4 C12_4 C11_4 123.43(15) . . ?
C15_4 C12_4 C11_4 118.17(15) . . ?
C12_4 C13_4 C14_4 121.33(15) . . ?
C12_4 C13_4 H13_4 119.3 . . ?
C14_4 C13_4 H13_4 119.3 . . ?
C1_4 C14_4 C13_4 122.06(15) . . ?
C1_4 C14_4 H14_4 119.0 . . ?
C13_4 C14_4 H14_4 119.0 . . ?
C12_4 C15_4 C2_4 119.64(15) . . ?
C12_4 C15_4 C16_4 120.01(14) . . ?
C2_4 C15_4 C16_4 120.34(14) . . ?
C5_4 C16_4 C9_4 119.50(15) . . ?
C5_4 C16_4 C15_4 120.34(14) . . ?
C9_4 C16_4 C15_4 120.15(15) . . ?
C34_4 C21_4 C22_4 117.68(13) . . ?
C34_4 C21_4 B2_3 119.01(13) . . ?
C22_4 C21_4 B2_3 123.19(13) . . ?
C21_4 C22_4 C35_4 120.31(13) . . ?
C21_4 C22_4 C23_4 122.20(13) . . ?
C35_4 C22_4 C23_4 117.49(13) . . ?
C24_4 C23_4 C22_4 122.02(13) . . ?
C24_4 C23_4 H23_4 119.0 . . ?
C22_4 C23_4 H23_4 119.0 . . ?
C23_4 C24_4 C25_4 121.34(14) . . ?
C23_4 C24_4 H24_4 119.3 . . ?
C25_4 C24_4 H24_4 119.3 . . ?
C26_4 C25_4 C36_4 119.19(14) . . ?
C26_4 C25_4 C24_4 122.50(14) . . ?
C36_4 C25_4 C24_4 118.30(13) . . ?
C27_4 C26_4 C25_4 120.53(15) . . ?
C27_4 C26_4 H26_4 119.7 . . ?
C25_4 C26_4 H26_4 119.7 . . ?
C28_4 C27_4 C26_4 120.62(15) . . ?
C28_4 C27_4 H27_4 119.7 . . ?
C26_4 C27_4 H27_4 119.7 . . ?
C27_4 C28_4 C29_4 120.97(15) . . ?
C27_4 C28_4 H28_4 119.5 . . ?
C29_4 C28_4 H28_4 119.5 . . ?
C28_4 C29_4 C36_4 118.98(15) . . ?
C28_4 C29_4 C30_4 122.43(14) . . ?
C36_4 C29_4 C30_4 118.59(14) . . ?
C31_4 C30_4 C29_4 121.49(14) . . ?
C31_4 C30_4 H30_4 119.3 . . ?
C29_4 C30_4 H30_4 119.3 . . ?
C30_4 C31_4 C32_4 121.59(15) . . ?
C30_4 C31_4 H31_4 119.2 . . ?
C32_4 C31_4 H31_4 119.2 . . ?
C33_4 C32_4 C35_4 118.97(13) . . ?
C33_4 C32_4 C31_4 122.20(14) . . ?
C35_4 C32_4 C31_4 118.83(14) . . ?
C34_4 C33_4 C32_4 120.57(14) . . ?
C34_4 C33_4 H33_4 119.7 . . ?
C32_4 C33_4 H33_4 119.7 . . ?
C33_4 C34_4 C21_4 122.49(14) . . ?
C33_4 C34_4 H34_4 118.8 . . ?
C21_4 C34_4 H34_4 118.8 . . ?
C32_4 C35_4 C22_4 119.95(13) . . ?
C32_4 C35_4 C36_4 119.43(13) . . ?
C22_4 C35_4 C36_4 120.61(13) . . ?
C25_4 C36_4 C29_4 119.70(14) . . ?
C25_4 C36_4 C35_4 120.23(13) . . ?
C29_4 C36_4 C35_4 120.06(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 B1 C1_1 -178.70(15) . . . . ?
C1 N1 B1 C1_1 4.2(2) . . . . ?
C2 N1 B1 B2 7.0(2) . . . . ?
C1 N1 B1 B2 -170.02(15) . . . . ?
C3 N2 B2 C21_1 175.87(16) . . . . ?
C4 N2 B2 C21_1 -0.7(3) . . . . ?
C3 N2 B2 B1 4.0(3) . . . . ?
C4 N2 B2 B1 -172.54(16) . . . . ?
N1 B1 B2 N2 -90.1(2) . . . . ?
C1_1 B1 B2 N2 95.3(2) . . . . ?
N1 B1 B2 C21_1 97.77(19) . . . . ?
C1_1 B1 B2 C21_1 -76.83(18) . . . . ?
N1 B1 C1_1 C14_1 109.30(19) . . . . ?
B2 B1 C1_1 C14_1 -75.85(19) . . . . ?
N1 B1 C1_1 C2_1 -78.7(2) . . . . ?
B2 B1 C1_1 C2_1 96.14(18) . . . . ?
C14_1 C1_1 C2_1 C15_1 1.9(2) . . . . ?
B1 C1_1 C2_1 C15_1 -170.28(14) . . . . ?
C14_1 C1_1 C2_1 C3_1 -179.07(15) . . . . ?
B1 C1_1 C2_1 C3_1 8.7(2) . . . . ?
C1_1 C2_1 C3_1 C4_1 179.96(16) . . . . ?
C15_1 C2_1 C3_1 C4_1 -1.0(2) . . . . ?
C2_1 C3_1 C4_1 C5_1 0.4(3) . . . . ?
C3_1 C4_1 C5_1 C6_1 -179.06(18) . . . . ?
C3_1 C4_1 C5_1 C16_1 1.0(3) . . . . ?
C16_1 C5_1 C6_1 C7_1 0.5(3) . . . . ?
C4_1 C5_1 C6_1 C7_1 -179.48(18) . . . . ?
C5_1 C6_1 C7_1 C8_1 0.2(3) . . . . ?
C6_1 C7_1 C8_1 C9_1 -0.4(3) . . . . ?
C7_1 C8_1 C9_1 C16_1 -0.1(3) . . . . ?
C7_1 C8_1 C9_1 C10_1 -179.03(18) . . . . ?
C8_1 C9_1 C10_1 C11_1 176.95(17) . . . . ?
C16_1 C9_1 C10_1 C11_1 -2.0(2) . . . . ?
C9_1 C10_1 C11_1 C12_1 1.9(3) . . . . ?
C10_1 C11_1 C12_1 C13_1 180.00(16) . . . . ?
C10_1 C11_1 C12_1 C15_1 -0.1(2) . . . . ?
C15_1 C12_1 C13_1 C14_1 2.5(2) . . . . ?
C11_1 C12_1 C13_1 C14_1 -177.65(16) . . . . ?
C12_1 C13_1 C14_1 C1_1 -2.1(3) . . . . ?
C2_1 C1_1 C14_1 C13_1 -0.1(2) . . . . ?
B1 C1_1 C14_1 C13_1 172.24(16) . . . . ?
C1_1 C2_1 C15_1 C16_1 179.34(14) . . . . ?
C3_1 C2_1 C15_1 C16_1 0.3(2) . . . . ?
C1_1 C2_1 C15_1 C12_1 -1.6(2) . . . . ?
C3_1 C2_1 C15_1 C12_1 179.40(14) . . . . ?
C13_1 C12_1 C15_1 C2_1 -0.7(2) . . . . ?
C11_1 C12_1 C15_1 C2_1 179.47(14) . . . . ?
C13_1 C12_1 C15_1 C16_1 178.45(14) . . . . ?
C11_1 C12_1 C15_1 C16_1 -1.4(2) . . . . ?
C2_1 C15_1 C16_1 C5_1 1.0(2) . . . . ?
C12_1 C15_1 C16_1 C5_1 -178.07(14) . . . . ?
C2_1 C15_1 C16_1 C9_1 -179.65(14) . . . . ?
C12_1 C15_1 C16_1 C9_1 1.3(2) . . . . ?
C6_1 C5_1 C16_1 C15_1 178.39(15) . . . . ?
C4_1 C5_1 C16_1 C15_1 -1.7(2) . . . . ?
C6_1 C5_1 C16_1 C9_1 -1.0(2) . . . . ?
C4_1 C5_1 C16_1 C9_1 178.99(15) . . . . ?
C8_1 C9_1 C16_1 C15_1 -178.58(15) . . . . ?
C10_1 C9_1 C16_1 C15_1 0.4(2) . . . . ?
C8_1 C9_1 C16_1 C5_1 0.8(2) . . . . ?
C10_1 C9_1 C16_1 C5_1 179.77(15) . . . . ?
N2 B2 C21_1 C34_1 -110.12(19) . . . . ?
B1 B2 C21_1 C34_1 62.4(2) . . . . ?
N2 B2 C21_1 C22_1 71.2(2) . . . . ?
B1 B2 C21_1 C22_1 -116.31(17) . . . . ?
C34_1 C21_1 C22_1 C35_1 -0.4(2) . . . . ?
B2 C21_1 C22_1 C35_1 178.29(14) . . . . ?
C34_1 C21_1 C22_1 C23_1 178.57(14) . . . . ?
B2 C21_1 C22_1 C23_1 -2.7(2) . . . . ?
C21_1 C22_1 C23_1 C24_1 179.93(15) . . . . ?
C35_1 C22_1 C23_1 C24_1 -1.1(2) . . . . ?
C22_1 C23_1 C24_1 C25_1 -0.7(3) . . . . ?
C23_1 C24_1 C25_1 C26_1 -176.15(16) . . . . ?
C23_1 C24_1 C25_1 C36_1 1.4(2) . . . . ?
C36_1 C25_1 C26_1 C27_1 0.6(3) . . . . ?
C24_1 C25_1 C26_1 C27_1 178.06(16) . . . . ?
C25_1 C26_1 C27_1 C28_1 1.1(3) . . . . ?
C26_1 C27_1 C28_1 C29_1 -1.2(3) . . . . ?
C27_1 C28_1 C29_1 C36_1 -0.5(2) . . . . ?
C27_1 C28_1 C29_1 C30_1 -179.92(16) . . . . ?
C28_1 C29_1 C30_1 C31_1 178.10(17) . . . . ?
C36_1 C29_1 C30_1 C31_1 -1.3(2) . . . . ?
C29_1 C30_1 C31_1 C32_1 -0.1(3) . . . . ?
C30_1 C31_1 C32_1 C33_1 -178.84(16) . . . . ?
C30_1 C31_1 C32_1 C35_1 0.7(2) . . . . ?
C35_1 C32_1 C33_1 C34_1 -1.1(2) . . . . ?
C31_1 C32_1 C33_1 C34_1 178.41(15) . . . . ?
C32_1 C33_1 C34_1 C21_1 1.5(2) . . . . ?
C22_1 C21_1 C34_1 C33_1 -0.7(2) . . . . ?
B2 C21_1 C34_1 C33_1 -179.46(15) . . . . ?
C21_1 C22_1 C35_1 C36_1 -178.93(14) . . . . ?
C23_1 C22_1 C35_1 C36_1 2.0(2) . . . . ?
C21_1 C22_1 C35_1 C32_1 0.7(2) . . . . ?
C23_1 C22_1 C35_1 C32_1 -178.32(13) . . . . ?
C33_1 C32_1 C35_1 C36_1 179.71(14) . . . . ?
C31_1 C32_1 C35_1 C36_1 0.2(2) . . . . ?
C33_1 C32_1 C35_1 C22_1 0.1(2) . . . . ?
C31_1 C32_1 C35_1 C22_1 -179.50(13) . . . . ?
C28_1 C29_1 C36_1 C35_1 -177.30(15) . . . . ?
C30_1 C29_1 C36_1 C35_1 2.2(2) . . . . ?
C28_1 C29_1 C36_1 C25_1 2.1(2) . . . . ?
C30_1 C29_1 C36_1 C25_1 -178.42(14) . . . . ?
C22_1 C35_1 C36_1 C29_1 178.09(14) . . . . ?
C32_1 C35_1 C36_1 C29_1 -1.6(2) . . . . ?
C22_1 C35_1 C36_1 C25_1 -1.3(2) . . . . ?
C32_1 C35_1 C36_1 C25_1 179.02(13) . . . . ?
C26_1 C25_1 C36_1 C29_1 -2.2(2) . . . . ?
C24_1 C25_1 C36_1 C29_1 -179.83(14) . . . . ?
C26_1 C25_1 C36_1 C35_1 177.25(15) . . . . ?
C24_1 C25_1 C36_1 C35_1 -0.4(2) . . . . ?
C1_4 B1_3 N1_3 C2_3 174.81(14) . . . . ?
B2_3 B1_3 N1_3 C2_3 1.0(2) . . . . ?
C1_4 B1_3 N1_3 C1_3 -2.4(2) . . . . ?
B2_3 B1_3 N1_3 C1_3 -176.14(15) . . . . ?
N1_3 B1_3 B2_3 N2_3 -72.4(2) . . . . ?
C1_4 B1_3 B2_3 N2_3 113.65(16) . . . . ?
N1_3 B1_3 B2_3 C21_4 111.42(16) . . . . ?
C1_4 B1_3 B2_3 C21_4 -62.48(18) . . . . ?
C21_4 B2_3 N2_3 C3_3 179.27(14) . . . . ?
B1_3 B2_3 N2_3 C3_3 3.3(2) . . . . ?
C21_4 B2_3 N2_3 C4_3 0.8(2) . . . . ?
B1_3 B2_3 N2_3 C4_3 -175.14(14) . . . . ?
N1_3 B1_3 C1_4 C14_4 104.36(18) . . . . ?
B2_3 B1_3 C1_4 C14_4 -81.52(18) . . . . ?
N1_3 B1_3 C1_4 C2_4 -79.56(19) . . . . ?
B2_3 B1_3 C1_4 C2_4 94.57(17) . . . . ?
C14_4 C1_4 C2_4 C15_4 -0.4(2) . . . . ?
B1_3 C1_4 C2_4 C15_4 -176.70(13) . . . . ?
C14_4 C1_4 C2_4 C3_4 179.94(14) . . . . ?
B1_3 C1_4 C2_4 C3_4 3.7(2) . . . . ?
C1_4 C2_4 C3_4 C4_4 179.72(15) . . . . ?
C15_4 C2_4 C3_4 C4_4 0.1(2) . . . . ?
C2_4 C3_4 C4_4 C5_4 0.5(3) . . . . ?
C3_4 C4_4 C5_4 C6_4 177.66(16) . . . . ?
C3_4 C4_4 C5_4 C16_4 -1.3(2) . . . . ?
C16_4 C5_4 C6_4 C7_4 -1.4(2) . . . . ?
C4_4 C5_4 C6_4 C7_4 179.68(16) . . . . ?
C5_4 C6_4 C7_4 C8_4 -0.3(3) . . . . ?
C6_4 C7_4 C8_4 C9_4 1.4(3) . . . . ?
C7_4 C8_4 C9_4 C16_4 -0.7(2) . . . . ?
C7_4 C8_4 C9_4 C10_4 179.16(16) . . . . ?
C8_4 C9_4 C10_4 C11_4 -178.38(17) . . . . ?
C16_4 C9_4 C10_4 C11_4 1.5(3) . . . . ?
C9_4 C10_4 C11_4 C12_4 -0.5(3) . . . . ?
C10_4 C11_4 C12_4 C13_4 -179.15(17) . . . . ?
C10_4 C11_4 C12_4 C15_4 -0.6(2) . . . . ?
C15_4 C12_4 C13_4 C14_4 0.9(2) . . . . ?
C11_4 C12_4 C13_4 C14_4 179.40(16) . . . . ?
C2_4 C1_4 C14_4 C13_4 1.4(2) . . . . ?
B1_3 C1_4 C14_4 C13_4 177.58(15) . . . . ?
C12_4 C13_4 C14_4 C1_4 -1.6(3) . . . . ?
C13_4 C12_4 C15_4 C2_4 0.1(2) . . . . ?
C11_4 C12_4 C15_4 C2_4 -178.55(14) . . . . ?
C13_4 C12_4 C15_4 C16_4 179.28(14) . . . . ?
C11_4 C12_4 C15_4 C16_4 0.7(2) . . . . ?
C1_4 C2_4 C15_4 C12_4 -0.3(2) . . . . ?
C3_4 C2_4 C15_4 C12_4 179.38(14) . . . . ?
C1_4 C2_4 C15_4 C16_4 -179.49(13) . . . . ?
C3_4 C2_4 C15_4 C16_4 0.2(2) . . . . ?
C6_4 C5_4 C16_4 C9_4 2.0(2) . . . . ?
C4_4 C5_4 C16_4 C9_4 -179.00(14) . . . . ?
C6_4 C5_4 C16_4 C15_4 -177.47(14) . . . . ?
C4_4 C5_4 C16_4 C15_4 1.5(2) . . . . ?
C8_4 C9_4 C16_4 C5_4 -1.0(2) . . . . ?
C10_4 C9_4 C16_4 C5_4 179.14(15) . . . . ?
C8_4 C9_4 C16_4 C15_4 178.49(14) . . . . ?
C10_4 C9_4 C16_4 C15_4 -1.4(2) . . . . ?
C12_4 C15_4 C16_4 C5_4 179.81(14) . . . . ?
C2_4 C15_4 C16_4 C5_4 -1.0(2) . . . . ?
C12_4 C15_4 C16_4 C9_4 0.3(2) . . . . ?
C2_4 C15_4 C16_4 C9_4 179.54(14) . . . . ?
N2_3 B2_3 C21_4 C34_4 -104.90(17) . . . . ?
B1_3 B2_3 C21_4 C34_4 71.40(18) . . . . ?
N2_3 B2_3 C21_4 C22_4 79.15(19) . . . . ?
B1_3 B2_3 C21_4 C22_4 -104.56(16) . . . . ?
C34_4 C21_4 C22_4 C35_4 -0.7(2) . . . . ?
B2_3 C21_4 C22_4 C35_4 175.34(13) . . . . ?
C34_4 C21_4 C22_4 C23_4 178.71(13) . . . . ?
B2_3 C21_4 C22_4 C23_4 -5.3(2) . . . . ?
C21_4 C22_4 C23_4 C24_4 179.66(14) . . . . ?
C35_4 C22_4 C23_4 C24_4 -0.9(2) . . . . ?
C22_4 C23_4 C24_4 C25_4 0.3(2) . . . . ?
C23_4 C24_4 C25_4 C26_4 179.38(15) . . . . ?
C23_4 C24_4 C25_4 C36_4 0.6(2) . . . . ?
C36_4 C25_4 C26_4 C27_4 0.3(2) . . . . ?
C24_4 C25_4 C26_4 C27_4 -178.48(15) . . . . ?
C25_4 C26_4 C27_4 C28_4 0.1(2) . . . . ?
C26_4 C27_4 C28_4 C29_4 -0.1(2) . . . . ?
C27_4 C28_4 C29_4 C36_4 -0.3(2) . . . . ?
C27_4 C28_4 C29_4 C30_4 179.73(15) . . . . ?
C28_4 C29_4 C30_4 C31_4 -179.56(15) . . . . ?
C36_4 C29_4 C30_4 C31_4 0.5(2) . . . . ?
C29_4 C30_4 C31_4 C32_4 -0.2(2) . . . . ?
C30_4 C31_4 C32_4 C33_4 179.05(16) . . . . ?
C30_4 C31_4 C32_4 C35_4 -0.3(2) . . . . ?
C35_4 C32_4 C33_4 C34_4 -1.6(2) . . . . ?
C31_4 C32_4 C33_4 C34_4 179.04(15) . . . . ?
C32_4 C33_4 C34_4 C21_4 2.4(2) . . . . ?
C22_4 C21_4 C34_4 C33_4 -1.2(2) . . . . ?
B2_3 C21_4 C34_4 C33_4 -177.40(14) . . . . ?
C33_4 C32_4 C35_4 C22_4 -0.2(2) . . . . ?
C31_4 C32_4 C35_4 C22_4 179.13(13) . . . . ?
C33_4 C32_4 C35_4 C36_4 -178.97(14) . . . . ?
C31_4 C32_4 C35_4 C36_4 0.4(2) . . . . ?
C21_4 C22_4 C35_4 C32_4 1.4(2) . . . . ?
C23_4 C22_4 C35_4 C32_4 -178.03(13) . . . . ?
C21_4 C22_4 C35_4 C36_4 -179.89(13) . . . . ?
C23_4 C22_4 C35_4 C36_4 0.7(2) . . . . ?
C26_4 C25_4 C36_4 C29_4 -0.7(2) . . . . ?
C24_4 C25_4 C36_4 C29_4 178.13(13) . . . . ?
C26_4 C25_4 C36_4 C35_4 -179.64(13) . . . . ?
C24_4 C25_4 C36_4 C35_4 -0.8(2) . . . . ?
C28_4 C29_4 C36_4 C25_4 0.7(2) . . . . ?
C30_4 C29_4 C36_4 C25_4 -179.35(13) . . . . ?
C28_4 C29_4 C36_4 C35_4 179.68(13) . . . . ?
C30_4 C29_4 C36_4 C35_4 -0.4(2) . . . . ?
C32_4 C35_4 C36_4 C25_4 178.91(13) . . . . ?
C22_4 C35_4 C36_4 C25_4 0.2(2) . . . . ?
C32_4 C35_4 C36_4 C29_4 -0.1(2) . . . . ?
C22_4 C35_4 C36_4 C29_4 -178.79(13) . . . . ?

_refine_diff_density_max         0.509
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.042


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

data_test_a_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2169211'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_test_a              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report
RESPONSE: Reflections affected by beamstop
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        10-Anth
_chemical_name_common            B(Anth)H2(PMe3)
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H20 B P'
_chemical_formula_sum            'C17 H20 B P'
_chemical_formula_weight         266.11

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'

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

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

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

_cell_length_a                   25.718(9)
_cell_length_b                   7.093(2)
_cell_length_c                   18.318(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.062(10)
_cell_angle_gamma                90
_cell_volume                     3001.7(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9952
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.07


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_F_000             1136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.238
_exptl_absorpt_coefficient_mu    0.166
_shelx_estimated_absorpt_T_min   0.941
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7064
_exptl_absorpt_correction_T_max  0.7453
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 -1.00 0.0740
0.00 1.00 1.00 0.1190
0.00 -1.00 -2.00 0.1010
0.00 1.00 2.00 0.1330
-1.00 2.00 -2.00 0.1590
-1.00 2.00 -1.00 0.1510
1.00 -2.00 0.00 0.0700
-1.00 2.00 0.00 0.1370
1.00 -2.00 -1.00 0.0780
-1.00 2.00 1.00 0.1350
1.00 -2.00 -2.00 0.0910
-1.00 2.00 2.00 0.1380
0.00 0.00 -1.00 0.1360
0.00 0.00 1.00 0.1670
-1.00 1.00 2.00 0.1640
1.00 -1.00 1.00 0.0830
2.00 -2.00 1.00 0.0870
1.00 -1.00 0.00 0.0890
1.00 -1.00 -1.00 0.1000
-2.00 2.00 -1.00 0.1570
2.00 -1.00 -2.00 0.1160
-2.00 1.00 0.00 0.1550
-1.00 0.00 2.00 0.1830
-1.00 0.00 1.00 0.1760
2.00 0.00 -1.00 0.1160
-2.00 -1.00 2.00 0.1980
-1.00 0.00 -1.00 0.1720
1.00 1.00 -2.00 0.1610
-1.00 -1.00 2.00 0.2110
-2.00 -1.00 1.00 0.1900
2.00 1.00 -1.00 0.1340
-2.00 -1.00 0.00 0.1810
2.00 1.00 0.00 0.1270
1.00 2.00 -2.00 0.1660
-1.00 -2.00 2.00 0.2180
-2.00 -2.00 -1.00 0.1860
2.00 2.00 1.00 0.1290
0.00 1.00 -2.00 0.1520
0.00 -1.00 2.00 0.1790
-1.00 -1.00 -1.00 0.1770
1.00 1.00 1.00 0.1350
0.00 1.00 0.00 0.1420
0.00 -1.00 0.00 0.1520

_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            42864
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.004
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3061
_reflns_number_gt                2817
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.37A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.37A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;

 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0578P)²+2.5611P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         3061
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.1112
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.56068(2) 0.73104(5) 0.64829(2) 0.03009(14) Uani 1 1 d . . . . .
B1 B 0.55229(7) 0.4611(2) 0.63957(10) 0.0288(3) Uani 1 1 d . . . . .
H1A H 0.5234 0.4206 0.6585 0.035 Uiso 1 1 calc R U . . .
H1B H 0.5380 0.4233 0.5820 0.035 Uiso 1 1 calc R U . . .
C1 C 0.61366(6) 0.3580(2) 0.69360(9) 0.0277(3) Uani 1 1 d . . . . .
C3 C 0.64085(7) 0.3522(2) 0.57791(9) 0.0335(3) Uani 1 1 d . . . . .
H3 H 0.6069 0.4213 0.5450 0.040 Uiso 1 1 calc R U . . .
C2 C 0.65243(6) 0.3093(2) 0.66018(9) 0.0287(3) Uani 1 1 d . . . . .
C5 C 0.72855(8) 0.1946(2) 0.59300(11) 0.0401(4) Uani 1 1 d . . . . .
H5 H 0.7533 0.1555 0.5697 0.048 Uiso 1 1 calc R U . . .
C4 C 0.67706(8) 0.2967(3) 0.54541(10) 0.0402(4) Uani 1 1 d . . . . .
H4 H 0.6678 0.3266 0.4905 0.048 Uiso 1 1 calc R U . . .
C6 C 0.74236(7) 0.1532(2) 0.67156(10) 0.0355(3) Uani 1 1 d . . . . .
H6 H 0.7770 0.0861 0.7030 0.043 Uiso 1 1 calc R U . . .
C7 C 0.70555(6) 0.2087(2) 0.70800(9) 0.0297(3) Uani 1 1 d . . . . .
C9 C 0.68288(6) 0.2085(2) 0.82345(9) 0.0304(3) Uani 1 1 d . . . . .
C8 C 0.71934(6) 0.1618(2) 0.78825(9) 0.0307(3) Uani 1 1 d . . . . .
H8 H 0.7544 0.0965 0.8196 0.037 Uiso 1 1 calc R U . . .
C10 C 0.69694(7) 0.1561(2) 0.90559(10) 0.0378(4) Uani 1 1 d . . . . .
H10 H 0.7322 0.0919 0.9368 0.045 Uiso 1 1 calc R U . . .
C11 C 0.66078(8) 0.1964(3) 0.93964(11) 0.0445(4) Uani 1 1 d . . . . .
H11 H 0.6708 0.1604 0.9941 0.053 Uiso 1 1 calc R U . . .
C12 C 0.60826(7) 0.2920(3) 0.89377(11) 0.0419(4) Uani 1 1 d . . . . .
H12 H 0.5830 0.3197 0.9177 0.050 Uiso 1 1 calc R U . . .
C13 C 0.59328(7) 0.3450(2) 0.81548(10) 0.0354(3) Uani 1 1 d . . . . .
H13 H 0.5577 0.4093 0.7862 0.042 Uiso 1 1 calc R U . . .
C14 C 0.62950(6) 0.3069(2) 0.77583(9) 0.0286(3) Uani 1 1 d . . . . .
C15 C 0.49323(8) 0.8533(3) 0.59155(11) 0.0474(4) Uani 1 1 d . . . . .
H15A H 0.4990 0.9889 0.6024 0.071 Uiso 1 1 calc R U . . .
H15B H 0.4641 0.8071 0.6081 0.071 Uiso 1 1 calc R U . . .
H15C H 0.4800 0.8302 0.5333 0.071 Uiso 1 1 calc R U . . .
C16 C 0.58679(8) 0.8152(3) 0.75127(11) 0.0480(4) Uani 1 1 d . . . . .
H16A H 0.5869 0.9534 0.7514 0.072 Uiso 1 1 calc R U . . .
H16B H 0.6262 0.7689 0.7837 0.072 Uiso 1 1 calc R U . . .
H16C H 0.5615 0.7691 0.7747 0.072 Uiso 1 1 calc R U . . .
C17 C 0.60906(8) 0.8263(2) 0.61028(12) 0.0439(4) Uani 1 1 d . . . . .
H17A H 0.6107 0.9638 0.6161 0.066 Uiso 1 1 calc R U . . .
H17B H 0.5950 0.7933 0.5528 0.066 Uiso 1 1 calc R U . . .
H17C H 0.6479 0.7736 0.6413 0.066 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C17 1.8029(18) . ?
P1 C16 1.8035(18) . ?
P1 C15 1.8047(17) . ?
P1 B1 1.9253(18) . ?
B1 C1 1.623(2) . ?
B1 H1A 0.9900 . ?
B1 H1B 0.9900 . ?
C1 C2 1.423(2) . ?
C1 C14 1.424(2) . ?
C3 C4 1.365(2) . ?
C3 C2 1.434(2) . ?
C3 H3 0.9500 . ?
C2 C7 1.446(2) . ?
C5 C6 1.354(2) . ?
C5 C4 1.422(3) . ?
C5 H5 0.9500 . ?
C4 H4 0.9500 . ?
C6 C7 1.432(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.393(2) . ?
C9 C8 1.391(2) . ?
C9 C10 1.434(2) . ?
C9 C14 1.442(2) . ?
C8 H8 0.9500 . ?
C10 C11 1.358(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.412(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.364(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.436(2) . ?
C13 H13 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 P1 C16 106.08(9) . . ?
C17 P1 C15 104.44(9) . . ?
C16 P1 C15 105.39(9) . . ?
C17 P1 B1 114.31(8) . . ?
C16 P1 B1 113.12(8) . . ?
C15 P1 B1 112.68(9) . . ?
C1 B1 P1 110.74(10) . . ?
C1 B1 H1A 109.5 . . ?
P1 B1 H1A 109.5 . . ?
C1 B1 H1B 109.5 . . ?
P1 B1 H1B 109.5 . . ?
H1A B1 H1B 108.1 . . ?
C2 C1 C14 117.68(13) . . ?
C2 C1 B1 121.65(13) . . ?
C14 C1 B1 120.63(13) . . ?
C4 C3 C2 122.03(15) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C1 C2 C3 122.62(13) . . ?
C1 C2 C7 120.88(13) . . ?
C3 C2 C7 116.49(13) . . ?
C6 C5 C4 120.05(15) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C3 C4 C5 120.60(15) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C5 C6 C7 121.12(15) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 120.81(14) . . ?
C8 C7 C2 119.47(13) . . ?
C6 C7 C2 119.68(14) . . ?
C8 C9 C10 120.93(14) . . ?
C8 C9 C14 119.41(14) . . ?
C10 C9 C14 119.64(14) . . ?
C9 C8 C7 121.42(13) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C11 C10 C9 121.29(15) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 119.80(15) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 120.83(15) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 122.23(14) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C1 C14 C13 122.65(13) . . ?
C1 C14 C9 121.12(13) . . ?
C13 C14 C9 116.21(13) . . ?
P1 C15 H15A 109.5 . . ?
P1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
P1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P1 C16 H16A 109.5 . . ?
P1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
P1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P1 C17 H17A 109.5 . . ?
P1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 B1 C1 C2 -91.25(14) . . . . ?
P1 B1 C1 C14 91.09(14) . . . . ?
C14 C1 C2 C3 179.51(13) . . . . ?
B1 C1 C2 C3 1.8(2) . . . . ?
C14 C1 C2 C7 0.9(2) . . . . ?
B1 C1 C2 C7 -176.78(12) . . . . ?
C4 C3 C2 C1 -176.82(14) . . . . ?
C4 C3 C2 C7 1.8(2) . . . . ?
C2 C3 C4 C5 -0.6(2) . . . . ?
C6 C5 C4 C3 -0.7(3) . . . . ?
C4 C5 C6 C7 0.7(2) . . . . ?
C5 C6 C7 C8 178.50(15) . . . . ?
C5 C6 C7 C2 0.6(2) . . . . ?
C1 C2 C7 C8 -1.1(2) . . . . ?
C3 C2 C7 C8 -179.71(13) . . . . ?
C1 C2 C7 C6 176.88(13) . . . . ?
C3 C2 C7 C6 -1.8(2) . . . . ?
C10 C9 C8 C7 178.71(14) . . . . ?
C14 C9 C8 C7 0.3(2) . . . . ?
C6 C7 C8 C9 -177.49(14) . . . . ?
C2 C7 C8 C9 0.4(2) . . . . ?
C8 C9 C10 C11 -178.10(16) . . . . ?
C14 C9 C10 C11 0.3(3) . . . . ?
C9 C10 C11 C12 -0.1(3) . . . . ?
C10 C11 C12 C13 -0.1(3) . . . . ?
C11 C12 C13 C14 0.1(3) . . . . ?
C2 C1 C14 C13 -178.61(14) . . . . ?
B1 C1 C14 C13 -0.9(2) . . . . ?
C2 C1 C14 C9 -0.2(2) . . . . ?
B1 C1 C14 C9 177.51(13) . . . . ?
C12 C13 C14 C1 178.59(16) . . . . ?
C12 C13 C14 C9 0.1(2) . . . . ?
C8 C9 C14 C1 -0.4(2) . . . . ?
C10 C9 C14 C1 -178.83(14) . . . . ?
C8 C9 C14 C13 178.10(14) . . . . ?
C10 C9 C14 C13 -0.4(2) . . . . ?

_refine_diff_density_max         0.369
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.045


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

data_CaLe197
_database_code_depnum_ccdc_archive 'CCDC 2169213'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT303_CaLe197             
;
PROBLEM: Full Occupancy Atom H1B_1     with # Connections       2.00 Check
RESPONSE: bridging H
;
_vrf_PLAT340_CaLe197             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00432 Ang.
RESPONSE: weakly diffracting crystal
;
_vrf_PLAT911_CaLe197             
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          4 Report
RESPONSE: reflections affected by beamstop
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        9-Anth
_chemical_name_common            (mu-H)B2H2(Anth)(1,9-Anth)(PMe3)
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H29 B2 P, C6 H6'
_chemical_formula_sum            'C37 H35 B2 P'
_chemical_formula_weight         532.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

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

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

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

_cell_length_a                   19.472(2)
_cell_length_b                   16.526(2)
_cell_length_c                   9.3359(16)
_cell_angle_alpha                90
_cell_angle_beta                 102.454(6)
_cell_angle_gamma                90
_cell_volume                     2933.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9675
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      26.72


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.119
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7050
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CMOS area detector (Photon II)'
_diffrn_detector_area_resol_mean 7.5
_diffrn_reflns_number            59270
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.142
_diffrn_reflns_theta_max         26.013
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5779
_reflns_number_gt                5652
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.38A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.38A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_refine_special_details          
;

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

The anthryl ligand was modelled as twofold disordered in a 51:49 ratio. 
ADPs within RESI 4 and 5 ANT2 were restrained with SIMU 0.01
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+7.3461P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5779
_refine_ls_number_parameters     433
_refine_ls_number_restraints     388
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.1633
_refine_ls_wR_factor_gt          0.1631
_refine_ls_goodness_of_fit_ref   1.332
_refine_ls_restrained_S_all      1.292
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1_1 B 0.29104(17) 0.5055(2) 0.8193(3) 0.0180(6) Uani 1 1 d . . . . .
H1B_1 H 0.251(2) 0.547(2) 0.723(4) 0.037(11) Uiso 1 1 d . . . . .
H1A_1 H 0.3310(19) 0.552(2) 0.861(4) 0.030(10) Uiso 1 1 d . . . . .
B2_1 B 0.19424(18) 0.5187(2) 0.6139(4) 0.0196(7) Uani 1 1 d . . . . .
H2_1 H 0.1556(16) 0.5046(19) 0.683(3) 0.014(8) Uiso 1 1 d . . . . .
P1_2 P 0.23737(4) 0.49534(5) 0.97197(8) 0.01919(18) Uani 1 1 d . . . . .
C2_2 C 0.17313(17) 0.41544(19) 0.9498(4) 0.0252(7) Uani 1 1 d . . . . .
H2A_2 H 0.147301 0.418402 1.028830 0.038 Uiso 1 1 calc R U . . .
H2B_2 H 0.196921 0.362987 0.953434 0.038 Uiso 1 1 calc R U . . .
H2C_2 H 0.140182 0.421424 0.854909 0.038 Uiso 1 1 calc R U . . .
C3_2 C 0.19270(19) 0.5891(2) 0.9923(4) 0.0302(8) Uani 1 1 d . . . . .
H3A_2 H 0.170101 0.584934 1.076160 0.045 Uiso 1 1 calc R U . . .
H3B_2 H 0.156929 0.599627 0.902940 0.045 Uiso 1 1 calc R U . . .
H3C_2 H 0.226826 0.633502 1.008697 0.045 Uiso 1 1 calc R U . . .
C1_2 C 0.29540(17) 0.4762(2) 1.1472(3) 0.0283(7) Uani 1 1 d . . . . .
H1A_2 H 0.268564 0.478339 1.224675 0.042 Uiso 1 1 calc R U . . .
H1B_2 H 0.332529 0.517261 1.165894 0.042 Uiso 1 1 calc R U . . .
H1C_2 H 0.316608 0.422437 1.146201 0.042 Uiso 1 1 calc R U . . .
C1_3 C 0.31621(15) 0.42264(17) 0.7592(3) 0.0154(6) Uani 1 1 d . . . . .
C2_3 C 0.27662(15) 0.39143(17) 0.6261(3) 0.0168(6) Uani 1 1 d . . . . .
C3_3 C 0.21833(15) 0.43763(18) 0.5450(3) 0.0178(6) Uani 1 1 d . . . . .
C4_3 C 0.18376(16) 0.40944(18) 0.4107(3) 0.0214(6) Uani 1 1 d . . . . .
H4_3 H 0.146413 0.440606 0.354827 0.026 Uiso 1 1 calc R U . . .
C5_3 C 0.20212(17) 0.33488(19) 0.3523(3) 0.0234(7) Uani 1 1 d . . . . .
H5_3 H 0.175826 0.316267 0.260435 0.028 Uiso 1 1 calc R U . . .
C6_3 C 0.25687(16) 0.29007(18) 0.4266(3) 0.0210(6) Uani 1 1 d . . . . .
H6_3 H 0.268830 0.240601 0.386196 0.025 Uiso 1 1 calc R U . . .
C7_3 C 0.29661(15) 0.31729(17) 0.5657(3) 0.0178(6) Uani 1 1 d . . . . .
C8_3 C 0.35664(16) 0.27642(18) 0.6397(3) 0.0207(6) Uani 1 1 d . . . . .
H8_3 H 0.369257 0.226538 0.601783 0.025 Uiso 1 1 calc R U . . .
C9_3 C 0.39845(16) 0.30767(18) 0.7684(3) 0.0198(6) Uani 1 1 d . . . . .
C10_3 C 0.46359(17) 0.2700(2) 0.8360(4) 0.0268(7) Uani 1 1 d . . . . .
H10_3 H 0.476806 0.220844 0.796616 0.032 Uiso 1 1 calc R U . . .
C11_3 C 0.50691(17) 0.3031(2) 0.9553(4) 0.0284(7) Uani 1 1 d . . . . .
H11_3 H 0.550125 0.277414 0.998057 0.034 Uiso 1 1 calc R U . . .
C12_3 C 0.48746(16) 0.3760(2) 1.0159(3) 0.0252(7) Uani 1 1 d . . . . .
H12_3 H 0.518042 0.399216 1.098885 0.030 Uiso 1 1 calc R U . . .
C13_3 C 0.42536(16) 0.41335(19) 0.9566(3) 0.0206(6) Uani 1 1 d . . . . .
H13_3 H 0.413034 0.461500 1.000590 0.025 Uiso 1 1 calc R U . . .
C14_3 C 0.37820(15) 0.38171(17) 0.8293(3) 0.0168(6) Uani 1 1 d . . . . .
C15_4 C 0.1854(6) 0.5966(7) 0.5078(13) 0.0132(17) Uani 0.51(2) 1 d . U P A 1
C16_4 C 0.2389(6) 0.6311(6) 0.4410(10) 0.0124(15) Uani 0.51(2) 1 d . U P A 1
C17_4 C 0.3093(6) 0.6005(8) 0.4774(14) 0.0191(18) Uani 0.51(2) 1 d . U P A 1
H17_4 H 0.320663 0.558462 0.547903 0.023 Uiso 0.51(2) 1 calc R U P A 1
C18_4 C 0.3595(6) 0.6303(7) 0.4135(12) 0.0218(17) Uani 0.51(2) 1 d . U P A 1
H18_4 H 0.405438 0.607766 0.436824 0.026 Uiso 0.51(2) 1 calc R U P A 1
C19_4 C 0.3448(6) 0.6940(6) 0.3128(10) 0.0227(16) Uani 0.51(2) 1 d . U P A 1
H19_4 H 0.381251 0.715176 0.270455 0.027 Uiso 0.51(2) 1 calc R U P A 1
C20_4 C 0.2796(7) 0.7259(5) 0.2751(8) 0.0180(15) Uani 0.51(2) 1 d . U P A 1
H20_4 H 0.270312 0.769241 0.206902 0.022 Uiso 0.51(2) 1 calc R U P A 1
C21_4 C 0.2244(6) 0.6941(5) 0.3382(9) 0.0147(14) Uani 0.51(2) 1 d . U P A 1
C22_4 C 0.1570(7) 0.7268(4) 0.2986(8) 0.0160(15) Uani 0.51(2) 1 d . U P A 1
H22_4 H 0.147997 0.769351 0.228645 0.019 Uiso 0.51(2) 1 calc R U P A 1
C23_4 C 0.1023(6) 0.6977(5) 0.3603(9) 0.0149(15) Uani 0.51(2) 1 d . U P A 1
C24_4 C 0.0326(6) 0.7292(5) 0.3180(9) 0.0212(16) Uani 0.51(2) 1 d . U P A 1
H24_4 H 0.023923 0.771707 0.247982 0.025 Uiso 0.51(2) 1 calc R U P A 1
C25_4 C -0.0219(6) 0.7013(6) 0.3731(9) 0.0230(17) Uani 0.51(2) 1 d . U P A 1
H25_4 H -0.067632 0.723315 0.340316 0.028 Uiso 0.51(2) 1 calc R U P A 1
C26_4 C -0.0101(5) 0.6388(7) 0.4804(10) 0.0212(16) Uani 0.51(2) 1 d . U P A 1
H26_4 H -0.047670 0.619746 0.521643 0.025 Uiso 0.51(2) 1 calc R U P A 1
C27_4 C 0.0574(6) 0.6055(7) 0.5249(12) 0.0181(17) Uani 0.51(2) 1 d . U P A 1
H27_4 H 0.064550 0.563598 0.596280 0.022 Uiso 0.51(2) 1 calc R U P A 1
C28_4 C 0.1168(5) 0.6322(5) 0.4664(9) 0.0111(14) Uani 0.51(2) 1 d . U P A 1
C15_5 C 0.1712(6) 0.5964(9) 0.5097(15) 0.0114(19) Uiso 0.49(2) 1 d . U P A 2
C16_5 C 0.2231(6) 0.6302(7) 0.4481(13) 0.0138(17) Uiso 0.49(2) 1 d . U P A 2
C17_5 C 0.2956(7) 0.6053(9) 0.4769(17) 0.019(2) Uiso 0.49(2) 1 d . U P A 2
H17_5 H 0.309289 0.560763 0.541102 0.022 Uiso 0.49(2) 1 calc R U P A 2
C18_5 C 0.3466(7) 0.6424(8) 0.4166(15) 0.024(2) Uiso 0.49(2) 1 d . U P A 2
H18_5 H 0.394055 0.624877 0.443674 0.029 Uiso 0.49(2) 1 calc R U P A 2
C19_5 C 0.3276(7) 0.7080(7) 0.3121(12) 0.0220(19) Uiso 0.49(2) 1 d . U P A 2
H19_5 H 0.361662 0.732174 0.266708 0.026 Uiso 0.49(2) 1 calc R U P A 2
C20_5 C 0.2593(6) 0.7340(6) 0.2808(11) 0.0199(18) Uiso 0.49(2) 1 d . U P A 2
H20_5 H 0.246889 0.777411 0.213457 0.024 Uiso 0.49(2) 1 calc R U P A 2
C21_5 C 0.2061(6) 0.6994(6) 0.3435(11) 0.0155(17) Uiso 0.49(2) 1 d . U P A 2
C22_5 C 0.1366(6) 0.7244(6) 0.3083(11) 0.0153(17) Uiso 0.49(2) 1 d . U P A 2
H22_5 H 0.124051 0.766534 0.238267 0.018 Uiso 0.49(2) 1 calc R U P A 2
C23_5 C 0.0848(6) 0.6914(6) 0.3695(11) 0.0159(17) Uiso 0.49(2) 1 d . U P A 2
C24_5 C 0.0133(6) 0.7187(6) 0.3291(11) 0.0180(18) Uiso 0.49(2) 1 d . U P A 2
H24_5 H 0.001148 0.761645 0.260732 0.022 Uiso 0.49(2) 1 calc R U P A 2
C25_5 C -0.0367(6) 0.6836(7) 0.3875(11) 0.0220(18) Uiso 0.49(2) 1 d . U P A 2
H25_5 H -0.083766 0.702596 0.360892 0.026 Uiso 0.49(2) 1 calc R U P A 2
C26_5 C -0.0198(5) 0.6185(7) 0.4888(11) 0.0196(18) Uiso 0.49(2) 1 d . U P A 2
H26_5 H -0.055839 0.593613 0.527696 0.023 Uiso 0.49(2) 1 calc R U P A 2
C27_5 C 0.0463(6) 0.5922(7) 0.5293(15) 0.018(2) Uiso 0.49(2) 1 d . U P A 2
H27_5 H 0.056327 0.549194 0.598084 0.021 Uiso 0.49(2) 1 calc R U P A 2
C28_5 C 0.1013(6) 0.6253(6) 0.4748(12) 0.0130(17) Uiso 0.49(2) 1 d . U P A 2
C1_6 C 0.00481(17) 0.4451(2) 0.1138(3) 0.0269(7) Uani 1 1 d . . . . .
H1_6 H 0.007765 0.407490 0.191809 0.032 Uiso 1 1 calc R U . . .
C2_6 C 0.01805(18) 0.5265(2) 0.1440(3) 0.0277(7) Uani 1 1 d . . . . .
H2_6 H 0.030757 0.544464 0.242877 0.033 Uiso 1 1 calc R U . . .
C3_6 C 0.01277(18) 0.5814(2) 0.0306(3) 0.0272(7) Uani 1 1 d . . . . .
H3_6 H 0.021179 0.637212 0.051398 0.033 Uiso 1 1 calc R U . . .
C1_7 C 0.53381(17) 0.5445(2) 0.6200(4) 0.0285(7) Uani 1 1 d . . . . .
H1_7 H 0.556854 0.575175 0.702602 0.034 Uiso 1 1 calc R U . . .
C2_7 C 0.48535(19) 0.4855(2) 0.6358(4) 0.0346(8) Uani 1 1 d . . . . .
H2_7 H 0.475384 0.475468 0.729442 0.042 Uiso 1 1 calc R U . . .
C3_7 C 0.45157(18) 0.4415(2) 0.5156(4) 0.0317(8) Uani 1 1 d . . . . .
H3_7 H 0.418151 0.401325 0.526581 0.038 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1_1 C1_3 1.597(4) . ?
B1_1 P1_2 1.948(3) . ?
B1_1 H1B_1 1.26(4) . ?
B1_1 H1A_1 1.11(4) . ?
B2_1 C3_3 1.600(4) . ?
B2_1 C15_4 1.611(13) . ?
B2_1 C15_5 1.615(15) . ?
B2_1 H1B_1 1.41(4) . ?
B2_1 H2_1 1.12(3) . ?
P1_2 C2_2 1.800(3) . ?
P1_2 C1_2 1.805(3) . ?
P1_2 C3_2 1.806(3) . ?
C2_2 H2A_2 0.9800 . ?
C2_2 H2B_2 0.9800 . ?
C2_2 H2C_2 0.9800 . ?
C3_2 H3A_2 0.9800 . ?
C3_2 H3B_2 0.9800 . ?
C3_2 H3C_2 0.9800 . ?
C1_2 H1A_2 0.9800 . ?
C1_2 H1B_2 0.9800 . ?
C1_2 H1C_2 0.9800 . ?
C1_3 C2_3 1.411(4) . ?
C1_3 C14_3 1.415(4) . ?
C2_3 C7_3 1.437(4) . ?
C2_3 C3_3 1.440(4) . ?
C3_3 C4_3 1.370(4) . ?
C4_3 C5_3 1.424(4) . ?
C4_3 H4_3 0.9500 . ?
C5_3 C6_3 1.359(4) . ?
C5_3 H5_3 0.9500 . ?
C6_3 C7_3 1.433(4) . ?
C6_3 H6_3 0.9500 . ?
C7_3 C8_3 1.397(4) . ?
C8_3 C9_3 1.397(4) . ?
C8_3 H8_3 0.9500 . ?
C9_3 C10_3 1.432(4) . ?
C9_3 C14_3 1.439(4) . ?
C10_3 C11_3 1.359(5) . ?
C10_3 H10_3 0.9500 . ?
C11_3 C12_3 1.417(5) . ?
C11_3 H11_3 0.9500 . ?
C12_3 C13_3 1.364(4) . ?
C12_3 H12_3 0.9500 . ?
C13_3 C14_3 1.434(4) . ?
C13_3 H13_3 0.9500 . ?
C15_4 C28_4 1.435(12) . ?
C15_4 C16_4 1.440(12) . ?
C16_4 C21_4 1.403(12) . ?
C16_4 C17_4 1.431(12) . ?
C17_4 C18_4 1.344(15) . ?
C17_4 H17_4 0.9500 . ?
C18_4 C19_4 1.400(14) . ?
C18_4 H18_4 0.9500 . ?
C19_4 C20_4 1.349(11) . ?
C19_4 H19_4 0.9500 . ?
C20_4 C21_4 1.432(10) . ?
C20_4 H20_4 0.9500 . ?
C21_4 C22_4 1.393(10) . ?
C22_4 C23_4 1.401(10) . ?
C22_4 H22_4 0.9500 . ?
C23_4 C24_4 1.429(10) . ?
C23_4 C28_4 1.453(11) . ?
C24_4 C25_4 1.355(12) . ?
C24_4 H24_4 0.9500 . ?
C25_4 C26_4 1.423(11) . ?
C25_4 H25_4 0.9500 . ?
C26_4 C27_4 1.404(13) . ?
C26_4 H26_4 0.9500 . ?
C27_4 C28_4 1.449(11) . ?
C27_4 H27_4 0.9500 . ?
C15_5 C16_5 1.383(14) . ?
C15_5 C28_5 1.413(13) . ?
C16_5 C17_5 1.438(13) . ?
C16_5 C21_5 1.494(16) . ?
C17_5 C18_5 1.386(19) . ?
C17_5 H17_5 0.9500 . ?
C18_5 C19_5 1.451(16) . ?
C18_5 H18_5 0.9500 . ?
C19_5 C20_5 1.368(11) . ?
C19_5 H19_5 0.9500 . ?
C20_5 C21_5 1.415(12) . ?
C20_5 H20_5 0.9500 . ?
C21_5 C22_5 1.386(11) . ?
C22_5 C23_5 1.375(11) . ?
C22_5 H22_5 0.9500 . ?
C23_5 C24_5 1.434(12) . ?
C23_5 C28_5 1.460(14) . ?
C24_5 C25_5 1.344(11) . ?
C24_5 H24_5 0.9500 . ?
C25_5 C26_5 1.424(13) . ?
C25_5 H25_5 0.9500 . ?
C26_5 C27_5 1.335(15) . ?
C26_5 H26_5 0.9500 . ?
C27_5 C28_5 1.392(13) . ?
C27_5 H27_5 0.9500 . ?
C1_6 C2_6 1.387(5) . ?
C1_6 C3_6 1.388(4) 3_565 ?
C1_6 H1_6 0.9500 . ?
C2_6 C3_6 1.382(5) . ?
C2_6 H2_6 0.9500 . ?
C3_6 H3_6 0.9500 . ?
C1_7 C3_7 1.377(5) 3_666 ?
C1_7 C2_7 1.387(5) . ?
C1_7 H1_7 0.9500 . ?
C2_7 C3_7 1.380(5) . ?
C2_7 H2_7 0.9500 . ?
C3_7 H3_7 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1_3 B1_1 P1_2 115.9(2) . . ?
C1_3 B1_1 H1B_1 113.8(18) . . ?
P1_2 B1_1 H1B_1 102.7(17) . . ?
C1_3 B1_1 H1A_1 118.5(19) . . ?
P1_2 B1_1 H1A_1 104.5(19) . . ?
H1B_1 B1_1 H1A_1 99(3) . . ?
C3_3 B2_1 C15_4 115.1(5) . . ?
C3_3 B2_1 C15_5 119.4(6) . . ?
C3_3 B2_1 H1B_1 108.4(16) . . ?
C15_4 B2_1 H1B_1 98.2(16) . . ?
C15_5 B2_1 H1B_1 104.2(17) . . ?
C3_3 B2_1 H2_1 110.5(16) . . ?
C15_4 B2_1 H2_1 121.8(17) . . ?
C15_5 B2_1 H2_1 112.4(17) . . ?
H1B_1 B2_1 H2_1 100(2) . . ?
C2_2 P1_2 C1_2 105.03(16) . . ?
C2_2 P1_2 C3_2 107.63(16) . . ?
C1_2 P1_2 C3_2 106.09(16) . . ?
C2_2 P1_2 B1_1 116.63(15) . . ?
C1_2 P1_2 B1_1 110.41(15) . . ?
C3_2 P1_2 B1_1 110.43(16) . . ?
P1_2 C2_2 H2A_2 109.5 . . ?
P1_2 C2_2 H2B_2 109.5 . . ?
H2A_2 C2_2 H2B_2 109.5 . . ?
P1_2 C2_2 H2C_2 109.5 . . ?
H2A_2 C2_2 H2C_2 109.5 . . ?
H2B_2 C2_2 H2C_2 109.5 . . ?
P1_2 C3_2 H3A_2 109.5 . . ?
P1_2 C3_2 H3B_2 109.5 . . ?
H3A_2 C3_2 H3B_2 109.5 . . ?
P1_2 C3_2 H3C_2 109.5 . . ?
H3A_2 C3_2 H3C_2 109.5 . . ?
H3B_2 C3_2 H3C_2 109.5 . . ?
P1_2 C1_2 H1A_2 109.5 . . ?
P1_2 C1_2 H1B_2 109.5 . . ?
H1A_2 C1_2 H1B_2 109.5 . . ?
P1_2 C1_2 H1C_2 109.5 . . ?
H1A_2 C1_2 H1C_2 109.5 . . ?
H1B_2 C1_2 H1C_2 109.5 . . ?
C2_3 C1_3 C14_3 118.8(3) . . ?
C2_3 C1_3 B1_1 118.2(2) . . ?
C14_3 C1_3 B1_1 122.9(3) . . ?
C1_3 C2_3 C7_3 121.0(3) . . ?
C1_3 C2_3 C3_3 119.2(3) . . ?
C7_3 C2_3 C3_3 119.7(3) . . ?
C4_3 C3_3 C2_3 118.5(3) . . ?
C4_3 C3_3 B2_1 121.6(3) . . ?
C2_3 C3_3 B2_1 119.9(3) . . ?
C3_3 C4_3 C5_3 122.0(3) . . ?
C3_3 C4_3 H4_3 119.0 . . ?
C5_3 C4_3 H4_3 119.0 . . ?
C6_3 C5_3 C4_3 120.7(3) . . ?
C6_3 C5_3 H5_3 119.7 . . ?
C4_3 C5_3 H5_3 119.7 . . ?
C5_3 C6_3 C7_3 120.1(3) . . ?
C5_3 C6_3 H6_3 119.9 . . ?
C7_3 C6_3 H6_3 119.9 . . ?
C8_3 C7_3 C6_3 121.8(3) . . ?
C8_3 C7_3 C2_3 119.1(3) . . ?
C6_3 C7_3 C2_3 119.0(3) . . ?
C7_3 C8_3 C9_3 121.1(3) . . ?
C7_3 C8_3 H8_3 119.4 . . ?
C9_3 C8_3 H8_3 119.4 . . ?
C8_3 C9_3 C10_3 121.0(3) . . ?
C8_3 C9_3 C14_3 119.7(3) . . ?
C10_3 C9_3 C14_3 119.2(3) . . ?
C11_3 C10_3 C9_3 121.4(3) . . ?
C11_3 C10_3 H10_3 119.3 . . ?
C9_3 C10_3 H10_3 119.3 . . ?
C10_3 C11_3 C12_3 119.8(3) . . ?
C10_3 C11_3 H11_3 120.1 . . ?
C12_3 C11_3 H11_3 120.1 . . ?
C13_3 C12_3 C11_3 120.8(3) . . ?
C13_3 C12_3 H12_3 119.6 . . ?
C11_3 C12_3 H12_3 119.6 . . ?
C12_3 C13_3 C14_3 121.7(3) . . ?
C12_3 C13_3 H13_3 119.2 . . ?
C14_3 C13_3 H13_3 119.2 . . ?
C1_3 C14_3 C13_3 122.6(3) . . ?
C1_3 C14_3 C9_3 120.2(3) . . ?
C13_3 C14_3 C9_3 117.1(3) . . ?
C28_4 C15_4 C16_4 116.1(9) . . ?
C28_4 C15_4 B2_1 117.5(8) . . ?
C16_4 C15_4 B2_1 126.2(7) . . ?
C21_4 C16_4 C17_4 117.7(8) . . ?
C21_4 C16_4 C15_4 122.2(8) . . ?
C17_4 C16_4 C15_4 120.1(9) . . ?
C18_4 C17_4 C16_4 121.1(11) . . ?
C18_4 C17_4 H17_4 119.4 . . ?
C16_4 C17_4 H17_4 119.4 . . ?
C17_4 C18_4 C19_4 120.7(9) . . ?
C17_4 C18_4 H18_4 119.6 . . ?
C19_4 C18_4 H18_4 119.6 . . ?
C20_4 C19_4 C18_4 120.8(8) . . ?
C20_4 C19_4 H19_4 119.6 . . ?
C18_4 C19_4 H19_4 119.6 . . ?
C19_4 C20_4 C21_4 119.9(7) . . ?
C19_4 C20_4 H20_4 120.1 . . ?
C21_4 C20_4 H20_4 120.1 . . ?
C22_4 C21_4 C16_4 120.6(7) . . ?
C22_4 C21_4 C20_4 119.8(7) . . ?
C16_4 C21_4 C20_4 119.7(7) . . ?
C21_4 C22_4 C23_4 120.9(7) . . ?
C21_4 C22_4 H22_4 119.6 . . ?
C23_4 C22_4 H22_4 119.6 . . ?
C22_4 C23_4 C24_4 121.5(7) . . ?
C22_4 C23_4 C28_4 119.0(7) . . ?
C24_4 C23_4 C28_4 119.5(7) . . ?
C25_4 C24_4 C23_4 123.1(7) . . ?
C25_4 C24_4 H24_4 118.4 . . ?
C23_4 C24_4 H24_4 118.4 . . ?
C24_4 C25_4 C26_4 119.6(7) . . ?
C24_4 C25_4 H25_4 120.2 . . ?
C26_4 C25_4 H25_4 120.2 . . ?
C27_4 C26_4 C25_4 119.4(8) . . ?
C27_4 C26_4 H26_4 120.3 . . ?
C25_4 C26_4 H26_4 120.3 . . ?
C26_4 C27_4 C28_4 122.8(9) . . ?
C26_4 C27_4 H27_4 118.6 . . ?
C28_4 C27_4 H27_4 118.6 . . ?
C15_4 C28_4 C27_4 123.1(8) . . ?
C15_4 C28_4 C23_4 121.3(7) . . ?
C27_4 C28_4 C23_4 115.6(7) . . ?
C16_5 C15_5 C28_5 121.5(12) . . ?
C16_5 C15_5 B2_1 116.0(9) . . ?
C28_5 C15_5 B2_1 122.4(9) . . ?
C15_5 C16_5 C17_5 125.6(12) . . ?
C15_5 C16_5 C21_5 120.1(9) . . ?
C17_5 C16_5 C21_5 114.3(10) . . ?
C18_5 C17_5 C16_5 123.8(13) . . ?
C18_5 C17_5 H17_5 118.1 . . ?
C16_5 C17_5 H17_5 118.1 . . ?
C17_5 C18_5 C19_5 120.2(10) . . ?
C17_5 C18_5 H18_5 119.9 . . ?
C19_5 C18_5 H18_5 119.9 . . ?
C20_5 C19_5 C18_5 118.3(10) . . ?
C20_5 C19_5 H19_5 120.9 . . ?
C18_5 C19_5 H19_5 120.9 . . ?
C19_5 C20_5 C21_5 123.3(10) . . ?
C19_5 C20_5 H20_5 118.4 . . ?
C21_5 C20_5 H20_5 118.4 . . ?
C22_5 C21_5 C20_5 123.1(10) . . ?
C22_5 C21_5 C16_5 116.8(9) . . ?
C20_5 C21_5 C16_5 120.1(8) . . ?
C23_5 C22_5 C21_5 123.4(9) . . ?
C23_5 C22_5 H22_5 118.3 . . ?
C21_5 C22_5 H22_5 118.3 . . ?
C22_5 C23_5 C24_5 121.6(9) . . ?
C22_5 C23_5 C28_5 120.1(8) . . ?
C24_5 C23_5 C28_5 118.2(8) . . ?
C25_5 C24_5 C23_5 120.3(9) . . ?
C25_5 C24_5 H24_5 119.9 . . ?
C23_5 C24_5 H24_5 119.9 . . ?
C24_5 C25_5 C26_5 120.8(9) . . ?
C24_5 C25_5 H25_5 119.6 . . ?
C26_5 C25_5 H25_5 119.6 . . ?
C27_5 C26_5 C25_5 120.3(9) . . ?
C27_5 C26_5 H26_5 119.9 . . ?
C25_5 C26_5 H26_5 119.9 . . ?
C26_5 C27_5 C28_5 122.7(11) . . ?
C26_5 C27_5 H27_5 118.6 . . ?
C28_5 C27_5 H27_5 118.6 . . ?
C27_5 C28_5 C15_5 124.2(10) . . ?
C27_5 C28_5 C23_5 117.7(9) . . ?
C15_5 C28_5 C23_5 118.0(10) . . ?
C2_6 C1_6 C3_6 120.0(3) . 3_565 ?
C2_6 C1_6 H1_6 120.0 . . ?
C3_6 C1_6 H1_6 120.0 3_565 . ?
C3_6 C2_6 C1_6 120.0(3) . . ?
C3_6 C2_6 H2_6 120.0 . . ?
C1_6 C2_6 H2_6 120.0 . . ?
C2_6 C3_6 C1_6 120.0(3) . 3_565 ?
C2_6 C3_6 H3_6 120.0 . . ?
C1_6 C3_6 H3_6 120.0 3_565 . ?
C3_7 C1_7 C2_7 119.8(3) 3_666 . ?
C3_7 C1_7 H1_7 120.1 3_666 . ?
C2_7 C1_7 H1_7 120.1 . . ?
C3_7 C2_7 C1_7 120.1(3) . . ?
C3_7 C2_7 H2_7 120.0 . . ?
C1_7 C2_7 H2_7 120.0 . . ?
C1_7 C3_7 C2_7 120.2(3) 3_666 . ?
C1_7 C3_7 H3_7 119.9 3_666 . ?
C2_7 C3_7 H3_7 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1_2 B1_1 C1_3 C2_3 99.4(3) . . . . ?
P1_2 B1_1 C1_3 C14_3 -84.0(3) . . . . ?
C14_3 C1_3 C2_3 C7_3 3.0(4) . . . . ?
B1_1 C1_3 C2_3 C7_3 179.7(2) . . . . ?
C14_3 C1_3 C2_3 C3_3 -172.6(3) . . . . ?
B1_1 C1_3 C2_3 C3_3 4.1(4) . . . . ?
C1_3 C2_3 C3_3 C4_3 175.1(3) . . . . ?
C7_3 C2_3 C3_3 C4_3 -0.5(4) . . . . ?
C1_3 C2_3 C3_3 B2_1 -6.3(4) . . . . ?
C7_3 C2_3 C3_3 B2_1 178.0(3) . . . . ?
C15_4 B2_1 C3_3 C4_3 -51.6(6) . . . . ?
C15_5 B2_1 C3_3 C4_3 -41.5(6) . . . . ?
C15_4 B2_1 C3_3 C2_3 129.9(5) . . . . ?
C15_5 B2_1 C3_3 C2_3 140.0(5) . . . . ?
C2_3 C3_3 C4_3 C5_3 2.4(4) . . . . ?
B2_1 C3_3 C4_3 C5_3 -176.2(3) . . . . ?
C3_3 C4_3 C5_3 C6_3 -2.4(5) . . . . ?
C4_3 C5_3 C6_3 C7_3 0.4(4) . . . . ?
C5_3 C6_3 C7_3 C8_3 -174.7(3) . . . . ?
C5_3 C6_3 C7_3 C2_3 1.3(4) . . . . ?
C1_3 C2_3 C7_3 C8_3 -0.7(4) . . . . ?
C3_3 C2_3 C7_3 C8_3 174.8(3) . . . . ?
C1_3 C2_3 C7_3 C6_3 -176.9(3) . . . . ?
C3_3 C2_3 C7_3 C6_3 -1.3(4) . . . . ?
C6_3 C7_3 C8_3 C9_3 174.1(3) . . . . ?
C2_3 C7_3 C8_3 C9_3 -1.9(4) . . . . ?
C7_3 C8_3 C9_3 C10_3 -173.7(3) . . . . ?
C7_3 C8_3 C9_3 C14_3 2.3(4) . . . . ?
C8_3 C9_3 C10_3 C11_3 175.4(3) . . . . ?
C14_3 C9_3 C10_3 C11_3 -0.7(5) . . . . ?
C9_3 C10_3 C11_3 C12_3 0.6(5) . . . . ?
C10_3 C11_3 C12_3 C13_3 0.5(5) . . . . ?
C11_3 C12_3 C13_3 C14_3 -1.5(5) . . . . ?
C2_3 C1_3 C14_3 C13_3 173.6(3) . . . . ?
B1_1 C1_3 C14_3 C13_3 -3.0(4) . . . . ?
C2_3 C1_3 C14_3 C9_3 -2.6(4) . . . . ?
B1_1 C1_3 C14_3 C9_3 -179.2(3) . . . . ?
C12_3 C13_3 C14_3 C1_3 -175.0(3) . . . . ?
C12_3 C13_3 C14_3 C9_3 1.3(4) . . . . ?
C8_3 C9_3 C14_3 C1_3 0.1(4) . . . . ?
C10_3 C9_3 C14_3 C1_3 176.1(3) . . . . ?
C8_3 C9_3 C14_3 C13_3 -176.3(3) . . . . ?
C10_3 C9_3 C14_3 C13_3 -0.3(4) . . . . ?
C3_3 B2_1 C15_4 C28_4 117.9(8) . . . . ?
C3_3 B2_1 C15_4 C16_4 -57.2(11) . . . . ?
C28_4 C15_4 C16_4 C21_4 -1.8(14) . . . . ?
B2_1 C15_4 C16_4 C21_4 173.4(8) . . . . ?
C28_4 C15_4 C16_4 C17_4 179.0(9) . . . . ?
B2_1 C15_4 C16_4 C17_4 -5.8(15) . . . . ?
C21_4 C16_4 C17_4 C18_4 -1.1(16) . . . . ?
C15_4 C16_4 C17_4 C18_4 178.2(10) . . . . ?
C16_4 C17_4 C18_4 C19_4 2.1(17) . . . . ?
C17_4 C18_4 C19_4 C20_4 -1.5(15) . . . . ?
C18_4 C19_4 C20_4 C21_4 -0.2(13) . . . . ?
C17_4 C16_4 C21_4 C22_4 -179.8(9) . . . . ?
C15_4 C16_4 C21_4 C22_4 1.0(13) . . . . ?
C17_4 C16_4 C21_4 C20_4 -0.6(12) . . . . ?
C15_4 C16_4 C21_4 C20_4 -179.8(8) . . . . ?
C19_4 C20_4 C21_4 C22_4 -179.6(7) . . . . ?
C19_4 C20_4 C21_4 C16_4 1.2(12) . . . . ?
C16_4 C21_4 C22_4 C23_4 0.1(12) . . . . ?
C20_4 C21_4 C22_4 C23_4 -179.0(7) . . . . ?
C21_4 C22_4 C23_4 C24_4 -178.4(7) . . . . ?
C21_4 C22_4 C23_4 C28_4 -0.4(11) . . . . ?
C22_4 C23_4 C24_4 C25_4 178.5(8) . . . . ?
C28_4 C23_4 C24_4 C25_4 0.5(12) . . . . ?
C23_4 C24_4 C25_4 C26_4 1.3(12) . . . . ?
C24_4 C25_4 C26_4 C27_4 -1.6(12) . . . . ?
C25_4 C26_4 C27_4 C28_4 0.3(13) . . . . ?
C16_4 C15_4 C28_4 C27_4 -179.1(9) . . . . ?
B2_1 C15_4 C28_4 C27_4 5.2(13) . . . . ?
C16_4 C15_4 C28_4 C23_4 1.5(13) . . . . ?
B2_1 C15_4 C28_4 C23_4 -174.1(7) . . . . ?
C26_4 C27_4 C28_4 C15_4 -177.9(9) . . . . ?
C26_4 C27_4 C28_4 C23_4 1.4(13) . . . . ?
C22_4 C23_4 C28_4 C15_4 -0.5(12) . . . . ?
C24_4 C23_4 C28_4 C15_4 177.6(8) . . . . ?
C22_4 C23_4 C28_4 C27_4 -179.9(7) . . . . ?
C24_4 C23_4 C28_4 C27_4 -1.8(11) . . . . ?
C3_3 B2_1 C15_5 C16_5 -63.6(12) . . . . ?
C3_3 B2_1 C15_5 C28_5 112.2(11) . . . . ?
C28_5 C15_5 C16_5 C17_5 179.8(12) . . . . ?
B2_1 C15_5 C16_5 C17_5 -4.3(18) . . . . ?
C28_5 C15_5 C16_5 C21_5 0.8(18) . . . . ?
B2_1 C15_5 C16_5 C21_5 176.6(9) . . . . ?
C15_5 C16_5 C17_5 C18_5 -177.9(13) . . . . ?
C21_5 C16_5 C17_5 C18_5 1.3(19) . . . . ?
C16_5 C17_5 C18_5 C19_5 -3(2) . . . . ?
C17_5 C18_5 C19_5 C20_5 2.9(17) . . . . ?
C18_5 C19_5 C20_5 C21_5 -0.9(16) . . . . ?
C19_5 C20_5 C21_5 C22_5 -178.1(10) . . . . ?
C19_5 C20_5 C21_5 C16_5 -0.9(15) . . . . ?
C15_5 C16_5 C21_5 C22_5 -2.7(15) . . . . ?
C17_5 C16_5 C21_5 C22_5 178.1(10) . . . . ?
C15_5 C16_5 C21_5 C20_5 179.9(11) . . . . ?
C17_5 C16_5 C21_5 C20_5 0.8(15) . . . . ?
C20_5 C21_5 C22_5 C23_5 -179.6(9) . . . . ?
C16_5 C21_5 C22_5 C23_5 3.1(15) . . . . ?
C21_5 C22_5 C23_5 C24_5 -179.5(9) . . . . ?
C21_5 C22_5 C23_5 C28_5 -1.5(15) . . . . ?
C22_5 C23_5 C24_5 C25_5 178.0(10) . . . . ?
C28_5 C23_5 C24_5 C25_5 0.0(14) . . . . ?
C23_5 C24_5 C25_5 C26_5 -0.8(14) . . . . ?
C24_5 C25_5 C26_5 C27_5 1.2(15) . . . . ?
C25_5 C26_5 C27_5 C28_5 -0.9(17) . . . . ?
C26_5 C27_5 C28_5 C15_5 -176.8(12) . . . . ?
C26_5 C27_5 C28_5 C23_5 0.1(17) . . . . ?
C16_5 C15_5 C28_5 C27_5 177.8(12) . . . . ?
B2_1 C15_5 C28_5 C27_5 2.3(18) . . . . ?
C16_5 C15_5 C28_5 C23_5 0.9(18) . . . . ?
B2_1 C15_5 C28_5 C23_5 -174.7(9) . . . . ?
C22_5 C23_5 C28_5 C27_5 -177.7(10) . . . . ?
C24_5 C23_5 C28_5 C27_5 0.3(15) . . . . ?
C22_5 C23_5 C28_5 C15_5 -0.6(15) . . . . ?
C24_5 C23_5 C28_5 C15_5 177.5(10) . . . . ?
C3_6 C1_6 C2_6 C3_6 0.9(6) 3_565 . . . ?
C1_6 C2_6 C3_6 C1_6 -0.9(6) . . . 3_565 ?
C3_7 C1_7 C2_7 C3_7 -0.4(6) 3_666 . . . ?
C1_7 C2_7 C3_7 C1_7 0.4(6) . . . 3_666 ?

_refine_diff_density_max         0.332
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.070


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

data_test_a_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2169215'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT911_test_a              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: Reflections affected by beamstop
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        10-Mes
_chemical_name_common            BH2Mes(PMe3)
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H22 B P'
_chemical_formula_sum            'C12 H22 B P'
_chemical_formula_weight         208.07

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   13.697(2)
_cell_length_b                   13.697(2)
_cell_length_c                   28.327(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5315(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9867
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      26.71


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Bruker Kryoflex2).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_F_000             1824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.207
_exptl_absorpt_coefficient_mu    0.171
_shelx_estimated_absorpt_T_min   0.942
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6903
_exptl_absorpt_correction_T_max  0.7454
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 1.00 -1.00 0.0910
1.00 -2.00 0.00 0.0400
1.00 1.00 1.00 0.1540
-1.00 -1.00 -1.00 0.1800
1.00 -2.00 1.00 0.0280
2.00 2.00 -1.00 0.1580
-2.00 -2.00 1.00 0.1710
-2.00 -1.00 2.00 0.1580
2.00 -1.00 0.00 0.0740
0.00 1.00 -2.00 0.1420
0.00 -1.00 2.00 0.0540
-2.00 1.00 1.00 0.1290
0.00 0.00 -1.00 0.0540
0.00 0.00 1.00 0.1030

_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CMOS area detector (Photon II)'
_diffrn_detector_area_resol_mean 7.5
_diffrn_reflns_number            20912
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.548
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2614
_reflns_number_gt                2274
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          
;

 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+5.2333P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2614
_refine_ls_number_parameters     141
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0895
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.56466(9) 0.98655(10) 0.25860(5) 0.0181(3) Uani 1 1 d . . . . .
C2 C 0.57237(10) 0.97776(11) 0.30817(5) 0.0219(3) Uani 1 1 d . . . . .
C3 C 0.60089(10) 0.88990(12) 0.32902(5) 0.0256(3) Uani 1 1 d . . . . .
H3 H 0.604838 0.885995 0.362450 0.031 Uiso 1 1 calc R U . . .
C4 C 0.62357(10) 0.80835(11) 0.30235(6) 0.0259(3) Uani 1 1 d . . . . .
C5 C 0.61895(10) 0.81703(11) 0.25353(5) 0.0244(3) Uani 1 1 d . . . . .
H5 H 0.635646 0.762365 0.234534 0.029 Uiso 1 1 calc R U . . .
C6 C 0.59058(10) 0.90352(11) 0.23163(5) 0.0202(3) Uani 1 1 d . . . . .
C7 C 0.55321(12) 1.06317(13) 0.34078(5) 0.0308(4) Uani 1 1 d . . . . .
H7A H 0.556833 1.041154 0.373654 0.046 Uiso 1 1 calc R U . . .
H7B H 0.488057 1.089703 0.334480 0.046 Uiso 1 1 calc R U . . .
H7C H 0.602337 1.113946 0.335331 0.046 Uiso 1 1 calc R U . . .
C8 C 0.65137(12) 0.71255(12) 0.32505(7) 0.0374(4) Uani 1 1 d . . . . .
H8A H 0.704953 0.682631 0.307268 0.056 Uiso 1 1 calc R U . . .
H8B H 0.594888 0.668634 0.324971 0.056 Uiso 1 1 calc R U . . .
H8C H 0.672309 0.724226 0.357646 0.056 Uiso 1 1 calc R U . . .
C9 C 0.59078(11) 0.90572(12) 0.17822(5) 0.0272(3) Uani 1 1 d . . . . .
H9A H 0.608686 0.841164 0.166078 0.041 Uiso 1 1 calc R U . . .
H9B H 0.638226 0.954181 0.167196 0.041 Uiso 1 1 calc R U . . .
H9C H 0.525560 0.923254 0.166799 0.041 Uiso 1 1 calc R U . . .
C10 C 0.32100(12) 1.07817(13) 0.28408(6) 0.0324(4) Uani 1 1 d . . . . .
H10A H 0.335197 1.139052 0.300909 0.049 Uiso 1 1 calc R U . . .
H10B H 0.342452 1.022537 0.303206 0.049 Uiso 1 1 calc R U . . .
H10C H 0.250597 1.073305 0.278379 0.049 Uiso 1 1 calc R U . . .
C11 C 0.34114(11) 0.96852(11) 0.19972(6) 0.0280(3) Uani 1 1 d . . . . .
H11A H 0.358580 0.970514 0.166177 0.042 Uiso 1 1 calc R U . . .
H11B H 0.270001 0.964723 0.202910 0.042 Uiso 1 1 calc R U . . .
H11C H 0.371024 0.911096 0.214447 0.042 Uiso 1 1 calc R U . . .
C12 C 0.33197(12) 1.17750(11) 0.19591(6) 0.0297(4) Uani 1 1 d . . . . .
H12A H 0.355769 1.176152 0.163295 0.044 Uiso 1 1 calc R U . . .
H12B H 0.350671 1.239392 0.210735 0.044 Uiso 1 1 calc R U . . .
H12C H 0.260691 1.171334 0.196047 0.044 Uiso 1 1 calc R U . . .
B1 B 0.52594(12) 1.08537(12) 0.23373(6) 0.0207(3) Uani 1 1 d . . . . .
H2 H 0.5389(12) 1.1552(13) 0.2550(6) 0.032(5) Uiso 1 1 d . . . . .
H1 H 0.5499(13) 1.0974(12) 0.1960(6) 0.032(5) Uiso 1 1 d . . . . .
P1 P 0.38494(3) 1.07746(3) 0.22843(2) 0.01909(12) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.413(2) . ?
C1 C6 1.415(2) . ?
C1 B1 1.615(2) . ?
C2 C3 1.396(2) . ?
C2 C7 1.513(2) . ?
C3 C4 1.384(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(2) . ?
C4 C8 1.510(2) . ?
C5 C6 1.393(2) . ?
C5 H5 0.9500 . ?
C6 C9 1.513(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 P1 1.8036(16) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 P1 1.8022(15) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 P1 1.8035(16) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
B1 P1 1.9401(17) . ?
B1 H2 1.144(17) . ?
B1 H1 1.131(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 116.70(13) . . ?
C2 C1 B1 121.95(13) . . ?
C6 C1 B1 121.34(12) . . ?
C3 C2 C1 120.96(14) . . ?
C3 C2 C7 117.16(13) . . ?
C1 C2 C7 121.85(14) . . ?
C4 C3 C2 121.84(14) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 117.65(14) . . ?
C3 C4 C8 121.69(15) . . ?
C5 C4 C8 120.65(15) . . ?
C4 C5 C6 121.94(14) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C5 C6 C1 120.86(13) . . ?
C5 C6 C9 117.51(13) . . ?
C1 C6 C9 121.61(13) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C10 H10A 109.5 . . ?
P1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P1 C11 H11A 109.5 . . ?
P1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P1 C12 H12A 109.5 . . ?
P1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 B1 P1 108.29(10) . . ?
C1 B1 H2 114.8(9) . . ?
P1 B1 H2 104.0(9) . . ?
C1 B1 H1 116.1(9) . . ?
P1 B1 H1 102.9(9) . . ?
H2 B1 H1 109.3(12) . . ?
C11 P1 C12 105.35(8) . . ?
C11 P1 C10 103.73(8) . . ?
C12 P1 C10 104.30(8) . . ?
C11 P1 B1 114.37(7) . . ?
C12 P1 B1 113.43(7) . . ?
C10 P1 B1 114.55(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.2(2) . . . . ?
B1 C1 C2 C3 176.44(12) . . . . ?
C6 C1 C2 C7 175.93(13) . . . . ?
B1 C1 C2 C7 -5.4(2) . . . . ?
C1 C2 C3 C4 0.6(2) . . . . ?
C7 C2 C3 C4 -177.66(13) . . . . ?
C2 C3 C4 C5 1.3(2) . . . . ?
C2 C3 C4 C8 -178.08(13) . . . . ?
C3 C4 C5 C6 -1.4(2) . . . . ?
C8 C4 C5 C6 177.95(13) . . . . ?
C4 C5 C6 C1 -0.3(2) . . . . ?
C4 C5 C6 C9 178.37(13) . . . . ?
C2 C1 C6 C5 2.1(2) . . . . ?
B1 C1 C6 C5 -176.58(12) . . . . ?
C2 C1 C6 C9 -176.54(13) . . . . ?
B1 C1 C6 C9 4.8(2) . . . . ?
C2 C1 B1 P1 -88.61(14) . . . . ?
C6 C1 B1 P1 89.99(14) . . . . ?

_refine_diff_density_max         0.273
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.039


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

data_test_a_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2169209'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        8-Phen
_chemical_name_common            B2HPhen(1,10-Phen)(PMe3)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 B2 P2, 2(C6 H6)'
_chemical_formula_sum            'C46 H48 B2 P2'
_chemical_formula_weight         684.40

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'

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

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

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

_cell_length_a                   9.478(4)
_cell_length_b                   13.2148(14)
_cell_length_c                   16.397(7)
_cell_angle_alpha                83.571(10)
_cell_angle_beta                 79.41(4)
_cell_angle_gamma                71.546(5)
_cell_volume                     1911.8(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    101(2)
_cell_measurement_reflns_used    9874
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      26.73


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold 
nitrogen (Oxford Cryostream 700).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.559
_exptl_crystal_size_mid          0.436
_exptl_crystal_size_min          0.362
_exptl_absorpt_coefficient_mu    0.146
_shelx_estimated_absorpt_T_min   0.923
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6565
_exptl_absorpt_correction_T_max  0.7454
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -1.00 0.1870
-1.00 0.00 1.00 0.2070
1.00 0.00 0.00 0.1810
-1.00 0.00 0.00 0.1270
1.00 0.00 1.00 0.2840
-1.00 0.00 -1.00 0.1750
0.00 -1.00 -1.00 0.1630
0.00 1.00 1.00 0.1120
0.00 -1.00 0.00 0.1540
0.00 1.00 0.00 0.1820
0.00 -1.00 1.00 0.2570
0.00 1.00 -1.00 0.2230

_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      101(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            33407
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.265
_diffrn_reflns_theta_max         26.769
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8132
_reflns_number_gt                7041
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          
;

 Refinement of F² against ALL reflections. The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based on F, 
with F set to zero for negative F². The threshold expression of F² > 
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not 
relevant to the choice of reflections for refinement. R-factors based on F² 
are statistically about twice as large as those based on F, and R-factors 
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0475P)²+0.8574P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8132
_refine_ls_number_parameters     461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0967
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1_1 P 0.37169(4) 0.49138(3) 0.18673(2) 0.01340(9) Uani 1 1 d . . . . .
C1_1 C 0.25680(16) 0.57708(11) 0.11397(9) 0.0201(3) Uani 1 1 d . . . . .
H1A_1 H 0.150498 0.595788 0.139320 0.030 Uiso 1 1 calc R U . . .
H1B_1 H 0.271469 0.539429 0.063410 0.030 Uiso 1 1 calc R U . . .
H1C_1 H 0.286311 0.642367 0.099840 0.030 Uiso 1 1 calc R U . . .
C2_1 C 0.33381(16) 0.57064(11) 0.27560(9) 0.0211(3) Uani 1 1 d . . . . .
H2A_1 H 0.386187 0.527484 0.319922 0.032 Uiso 1 1 calc R U . . .
H2B_1 H 0.225169 0.594364 0.295550 0.032 Uiso 1 1 calc R U . . .
H2C_1 H 0.369517 0.633098 0.259557 0.032 Uiso 1 1 calc R U . . .
P2_1 P 0.88922(4) 0.29284(3) 0.15712(2) 0.01581(9) Uani 1 1 d . . . . .
C3_1 C 0.27815(16) 0.39028(11) 0.22088(10) 0.0219(3) Uani 1 1 d . . . . .
H3A_1 H 0.320271 0.347377 0.268414 0.033 Uiso 1 1 calc R U . . .
H3B_1 H 0.293488 0.343906 0.175339 0.033 Uiso 1 1 calc R U . . .
H3C_1 H 0.170094 0.424877 0.237353 0.033 Uiso 1 1 calc R U . . .
C4_1 C 0.88827(17) 0.19658(13) 0.08613(10) 0.0272(3) Uani 1 1 d . . . . .
H4A_1 H 0.987598 0.172497 0.051779 0.041 Uiso 1 1 calc R U . . .
H4B_1 H 0.811960 0.230298 0.050290 0.041 Uiso 1 1 calc R U . . .
H4C_1 H 0.864726 0.135129 0.118100 0.041 Uiso 1 1 calc R U . . .
C5_1 C 1.02583(16) 0.21572(12) 0.22229(9) 0.0240(3) Uani 1 1 d . . . . .
H5A_1 H 1.120841 0.180843 0.187214 0.036 Uiso 1 1 calc R U . . .
H5B_1 H 0.987512 0.161332 0.256289 0.036 Uiso 1 1 calc R U . . .
H5C_1 H 1.042998 0.263298 0.258601 0.036 Uiso 1 1 calc R U . . .
C6_1 C 0.98332(16) 0.37679(12) 0.08756(9) 0.0226(3) Uani 1 1 d . . . . .
H6A_1 H 1.077415 0.331895 0.057417 0.034 Uiso 1 1 calc R U . . .
H6B_1 H 1.005669 0.426267 0.119915 0.034 Uiso 1 1 calc R U . . .
H6C_1 H 0.917667 0.417531 0.047804 0.034 Uiso 1 1 calc R U . . .
C1_4 C 0.7726(2) 0.13338(14) 0.71617(11) 0.0341(4) Uani 1 1 d . . . . .
H1_4 H 0.724610 0.148582 0.668255 0.041 Uiso 1 1 calc R U . . .
C2_4 C 0.92812(19) 0.09429(13) 0.70771(10) 0.0303(3) Uani 1 1 d . . . . .
H2_4 H 0.986857 0.083004 0.654070 0.036 Uiso 1 1 calc R U . . .
C3_4 C 0.99757(18) 0.07177(13) 0.77748(10) 0.0288(3) Uani 1 1 d . . . . .
H3_4 H 1.104202 0.044498 0.771920 0.035 Uiso 1 1 calc R U . . .
C4_4 C 0.91155(19) 0.08901(13) 0.85572(10) 0.0295(3) Uani 1 1 d . . . . .
H4_4 H 0.959395 0.073838 0.903683 0.035 Uiso 1 1 calc R U . . .
C5_4 C 0.75615(18) 0.12826(12) 0.86398(10) 0.0278(3) Uani 1 1 d . . . . .
H5_4 H 0.697306 0.139972 0.917552 0.033 Uiso 1 1 calc R U . . .
C6_4 C 0.68684(18) 0.15035(13) 0.79421(11) 0.0308(4) Uani 1 1 d . . . . .
H6_4 H 0.580185 0.177223 0.799781 0.037 Uiso 1 1 calc R U . . .
C1_5 C 0.0756(2) 0.39494(18) 0.48303(11) 0.0451(5) Uani 1 1 d . . . . .
H1_5 H 0.127601 0.322615 0.471143 0.054 Uiso 1 1 calc R U . . .
C4_5 C 0.1531(2) 0.46870(19) 0.47390(11) 0.0467(5) Uani 1 1 d . . . . .
H4_5 H 0.258879 0.447018 0.456058 0.056 Uiso 1 1 calc R U . . .
C3_5 C -0.0783(2) 0.42641(19) 0.50957(11) 0.0440(5) Uani 1 1 d . . . . .
H3_5 H -0.132129 0.375637 0.516349 0.053 Uiso 1 1 calc R U . . .
C1_6 C 0.84487(18) 0.03050(14) 0.50765(11) 0.0328(4) Uani 1 1 d . . . . .
H1_6 H 0.738190 0.051358 0.512955 0.039 Uiso 1 1 calc R U . . .
C2_6 C 0.92184(19) -0.06729(14) 0.54265(11) 0.0340(4) Uani 1 1 d . . . . .
H2_6 H 0.868023 -0.113374 0.571915 0.041 Uiso 1 1 calc R U . . .
C3_6 C 1.07732(18) -0.09761(13) 0.53485(10) 0.0318(4) Uani 1 1 d . . . . .
H3_6 H 1.130366 -0.164573 0.558743 0.038 Uiso 1 1 calc R U . . .
C1 C 0.62779(14) 0.55339(10) 0.11907(8) 0.0127(2) Uani 1 1 d . . . . .
B1 B 0.58378(16) 0.44336(11) 0.14153(9) 0.0126(3) Uani 1 1 d . . . . .
H1 H 0.5865(19) 0.3976(13) 0.0854(10) 0.025(4) Uiso 1 1 d . . . . .
C2 C 0.71467(14) 0.56784(10) 0.17844(7) 0.0124(2) Uani 1 1 d . . . . .
B2 B 0.69857(16) 0.38052(11) 0.21980(9) 0.0131(3) Uani 1 1 d . . . . .
C3 C 0.75429(14) 0.48019(10) 0.23766(8) 0.0131(2) Uani 1 1 d . . . . .
C4 C 0.84281(14) 0.48851(11) 0.29388(8) 0.0152(3) Uani 1 1 d . . . . .
H4 H 0.872340 0.431444 0.333992 0.018 Uiso 1 1 calc R U . . .
C5 C 0.88953(14) 0.57958(11) 0.29259(8) 0.0168(3) Uani 1 1 d . . . . .
H5 H 0.947712 0.583725 0.332797 0.020 Uiso 1 1 calc R U . . .
C6 C 0.85253(15) 0.66321(11) 0.23404(8) 0.0159(3) Uani 1 1 d . . . . .
H6 H 0.886562 0.723606 0.233692 0.019 Uiso 1 1 calc R U . . .
C7 C 0.76405(14) 0.65899(10) 0.17461(8) 0.0138(3) Uani 1 1 d . . . . .
C8 C 0.72512(14) 0.74082(10) 0.10830(8) 0.0143(3) Uani 1 1 d . . . . .
C9 C 0.76473(15) 0.83614(11) 0.09978(8) 0.0184(3) Uani 1 1 d . . . . .
H9 H 0.816142 0.849603 0.139964 0.022 Uiso 1 1 calc R U . . .
C10 C 0.73066(16) 0.91028(11) 0.03452(9) 0.0206(3) Uani 1 1 d . . . . .
H10 H 0.758959 0.973757 0.030132 0.025 Uiso 1 1 calc R U . . .
C11 C 0.65437(15) 0.89228(11) -0.02538(9) 0.0193(3) Uani 1 1 d . . . . .
H11 H 0.632088 0.942885 -0.070764 0.023 Uiso 1 1 calc R U . . .
C12 C 0.61208(15) 0.80093(11) -0.01797(8) 0.0168(3) Uani 1 1 d . . . . .
H12 H 0.559736 0.789373 -0.058485 0.020 Uiso 1 1 calc R U . . .
C13 C 0.64460(14) 0.72368(10) 0.04853(8) 0.0141(3) Uani 1 1 d . . . . .
C14 C 0.59774(14) 0.62934(10) 0.05591(8) 0.0139(3) Uani 1 1 d . . . . .
H14 H 0.544001 0.619585 0.015398 0.017 Uiso 1 1 calc R U . . .
C21_1 C 0.63660(14) 0.31566(10) 0.30117(8) 0.0132(2) Uani 1 1 d . . . . .
C16 C 0.58581(14) 0.22336(10) 0.29571(8) 0.0143(3) Uani 1 1 d . . . . .
C17 C 0.59264(15) 0.18520(11) 0.21752(8) 0.0172(3) Uani 1 1 d . . . . .
H17 H 0.628343 0.221608 0.168767 0.021 Uiso 1 1 calc R U . . .
C18 C 0.54948(17) 0.09726(11) 0.20944(9) 0.0213(3) Uani 1 1 d . . . . .
H18 H 0.557731 0.072690 0.155973 0.026 Uiso 1 1 calc R U . . .
C19 C 0.49327(18) 0.04416(11) 0.28058(10) 0.0255(3) Uani 1 1 d . . . . .
H19 H 0.465545 -0.017731 0.275747 0.031 Uiso 1 1 calc R U . . .
C20 C 0.47842(17) 0.08201(11) 0.35739(9) 0.0221(3) Uani 1 1 d . . . . .
H20 H 0.437605 0.046575 0.405110 0.027 Uiso 1 1 calc R U . . .
C21 C 0.52202(15) 0.17196(10) 0.36750(8) 0.0159(3) Uani 1 1 d . . . . .
C22 C 0.50085(15) 0.21414(10) 0.44838(8) 0.0157(3) Uani 1 1 d . . . . .
C23 C 0.42915(16) 0.17268(11) 0.52202(9) 0.0198(3) Uani 1 1 d . . . . .
H23 H 0.393195 0.113834 0.519533 0.024 Uiso 1 1 calc R U . . .
C24 C 0.41077(16) 0.21614(12) 0.59693(9) 0.0213(3) Uani 1 1 d . . . . .
H24 H 0.361738 0.187395 0.645504 0.026 Uiso 1 1 calc R U . . .
C25 C 0.46359(15) 0.30239(11) 0.60239(8) 0.0196(3) Uani 1 1 d . . . . .
H25 H 0.451430 0.331692 0.654481 0.023 Uiso 1 1 calc R U . . .
C26 C 0.53327(15) 0.34444(11) 0.53176(8) 0.0172(3) Uani 1 1 d . . . . .
H26 H 0.569510 0.402751 0.535643 0.021 Uiso 1 1 calc R U . . .
C27 C 0.55192(14) 0.30245(10) 0.45353(8) 0.0144(3) Uani 1 1 d . . . . .
C28 C 0.61832(14) 0.34992(10) 0.37932(8) 0.0144(3) Uani 1 1 d . . . . .
H28 H 0.651767 0.409038 0.384875 0.017 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1_1 C2_1 1.8058(15) . ?
P1_1 C3_1 1.8123(14) . ?
P1_1 C1_1 1.8128(16) . ?
P1_1 B1 1.9348(17) . ?
C1_1 H1A_1 0.9800 . ?
C1_1 H1B_1 0.9800 . ?
C1_1 H1C_1 0.9800 . ?
C2_1 H2A_1 0.9800 . ?
C2_1 H2B_1 0.9800 . ?
C2_1 H2C_1 0.9800 . ?
P2_1 C5_1 1.8128(16) . ?
P2_1 C6_1 1.8155(15) . ?
P2_1 C4_1 1.8211(15) . ?
P2_1 B2 1.9806(17) . ?
C3_1 H3A_1 0.9800 . ?
C3_1 H3B_1 0.9800 . ?
C3_1 H3C_1 0.9800 . ?
C4_1 H4A_1 0.9800 . ?
C4_1 H4B_1 0.9800 . ?
C4_1 H4C_1 0.9800 . ?
C5_1 H5A_1 0.9800 . ?
C5_1 H5B_1 0.9800 . ?
C5_1 H5C_1 0.9800 . ?
C6_1 H6A_1 0.9800 . ?
C6_1 H6B_1 0.9800 . ?
C6_1 H6C_1 0.9800 . ?
C1_4 C6_4 1.384(3) . ?
C1_4 C2_4 1.385(2) . ?
C1_4 H1_4 0.9500 . ?
C2_4 C3_4 1.381(2) . ?
C2_4 H2_4 0.9500 . ?
C3_4 C4_4 1.388(2) . ?
C3_4 H3_4 0.9500 . ?
C4_4 C5_4 1.384(2) . ?
C4_4 H4_4 0.9500 . ?
C5_4 C6_4 1.380(2) . ?
C5_4 H5_4 0.9500 . ?
C6_4 H6_4 0.9500 . ?
C1_5 C4_5 1.375(3) . ?
C1_5 C3_5 1.383(3) . ?
C1_5 H1_5 0.9500 . ?
C4_5 C3_5 1.374(3) 2_566 ?
C4_5 H4_5 0.9500 . ?
C3_5 H3_5 0.9500 . ?
C1_6 C3_6 1.379(2) 2_756 ?
C1_6 C2_6 1.387(2) . ?
C1_6 H1_6 0.9500 . ?
C2_6 C3_6 1.385(2) . ?
C2_6 H2_6 0.9500 . ?
C3_6 H3_6 0.9500 . ?
C1 C14 1.3622(18) . ?
C1 C2 1.4484(18) . ?
C1 B1 1.6221(18) . ?
B1 B2 1.795(2) . ?
B1 H1 1.148(17) . ?
C2 C7 1.4152(17) . ?
C2 C3 1.4257(18) . ?
B2 C21_1 1.6230(19) . ?
B2 C3 1.6381(18) . ?
C3 C4 1.3896(18) . ?
C4 C5 1.4047(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.4135(19) . ?
C6 H6 0.9500 . ?
C7 C8 1.4557(19) . ?
C8 C9 1.4099(18) . ?
C8 C13 1.4241(19) . ?
C9 C10 1.379(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.402(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.3742(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.4146(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.4364(18) . ?
C14 H14 0.9500 . ?
C21_1 C28 1.3696(18) . ?
C21_1 C16 1.4627(17) . ?
C16 C17 1.4128(19) . ?
C16 C21 1.4254(19) . ?
C17 C18 1.3750(19) . ?
C17 H17 0.9500 . ?
C18 C19 1.401(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.374(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.4112(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.4516(19) . ?
C22 C27 1.4134(18) . ?
C22 C23 1.4163(19) . ?
C23 C24 1.373(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.399(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.376(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.4137(19) . ?
C26 H26 0.9500 . ?
C27 C28 1.4380(18) . ?
C28 H28 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2_1 P1_1 C3_1 104.76(7) . . ?
C2_1 P1_1 C1_1 104.49(7) . . ?
C3_1 P1_1 C1_1 103.04(7) . . ?
C2_1 P1_1 B1 112.39(7) . . ?
C3_1 P1_1 B1 117.57(7) . . ?
C1_1 P1_1 B1 113.27(7) . . ?
P1_1 C1_1 H1A_1 109.5 . . ?
P1_1 C1_1 H1B_1 109.5 . . ?
H1A_1 C1_1 H1B_1 109.5 . . ?
P1_1 C1_1 H1C_1 109.5 . . ?
H1A_1 C1_1 H1C_1 109.5 . . ?
H1B_1 C1_1 H1C_1 109.5 . . ?
P1_1 C2_1 H2A_1 109.5 . . ?
P1_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
P1_1 C2_1 H2C_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
C5_1 P2_1 C6_1 105.16(7) . . ?
C5_1 P2_1 C4_1 103.59(8) . . ?
C6_1 P2_1 C4_1 100.90(8) . . ?
C5_1 P2_1 B2 113.88(7) . . ?
C6_1 P2_1 B2 110.84(7) . . ?
C4_1 P2_1 B2 120.71(7) . . ?
P1_1 C3_1 H3A_1 109.5 . . ?
P1_1 C3_1 H3B_1 109.5 . . ?
H3A_1 C3_1 H3B_1 109.5 . . ?
P1_1 C3_1 H3C_1 109.5 . . ?
H3A_1 C3_1 H3C_1 109.5 . . ?
H3B_1 C3_1 H3C_1 109.5 . . ?
P2_1 C4_1 H4A_1 109.5 . . ?
P2_1 C4_1 H4B_1 109.5 . . ?
H4A_1 C4_1 H4B_1 109.5 . . ?
P2_1 C4_1 H4C_1 109.5 . . ?
H4A_1 C4_1 H4C_1 109.5 . . ?
H4B_1 C4_1 H4C_1 109.5 . . ?
P2_1 C5_1 H5A_1 109.5 . . ?
P2_1 C5_1 H5B_1 109.5 . . ?
H5A_1 C5_1 H5B_1 109.5 . . ?
P2_1 C5_1 H5C_1 109.5 . . ?
H5A_1 C5_1 H5C_1 109.5 . . ?
H5B_1 C5_1 H5C_1 109.5 . . ?
P2_1 C6_1 H6A_1 109.5 . . ?
P2_1 C6_1 H6B_1 109.5 . . ?
H6A_1 C6_1 H6B_1 109.5 . . ?
P2_1 C6_1 H6C_1 109.5 . . ?
H6A_1 C6_1 H6C_1 109.5 . . ?
H6B_1 C6_1 H6C_1 109.5 . . ?
C6_4 C1_4 C2_4 120.20(16) . . ?
C6_4 C1_4 H1_4 119.9 . . ?
C2_4 C1_4 H1_4 119.9 . . ?
C3_4 C2_4 C1_4 119.80(16) . . ?
C3_4 C2_4 H2_4 120.1 . . ?
C1_4 C2_4 H2_4 120.1 . . ?
C2_4 C3_4 C4_4 119.98(15) . . ?
C2_4 C3_4 H3_4 120.0 . . ?
C4_4 C3_4 H3_4 120.0 . . ?
C5_4 C4_4 C3_4 120.09(16) . . ?
C5_4 C4_4 H4_4 120.0 . . ?
C3_4 C4_4 H4_4 120.0 . . ?
C6_4 C5_4 C4_4 119.87(16) . . ?
C6_4 C5_4 H5_4 120.1 . . ?
C4_4 C5_4 H5_4 120.1 . . ?
C5_4 C6_4 C1_4 120.06(16) . . ?
C5_4 C6_4 H6_4 120.0 . . ?
C1_4 C6_4 H6_4 120.0 . . ?
C4_5 C1_5 C3_5 119.8(2) . . ?
C4_5 C1_5 H1_5 120.1 . . ?
C3_5 C1_5 H1_5 120.1 . . ?
C3_5 C4_5 C1_5 120.37(18) 2_566 . ?
C3_5 C4_5 H4_5 119.8 2_566 . ?
C1_5 C4_5 H4_5 119.8 . . ?
C4_5 C3_5 C1_5 119.9(2) 2_566 . ?
C4_5 C3_5 H3_5 120.1 2_566 . ?
C1_5 C3_5 H3_5 120.1 . . ?
C3_6 C1_6 C2_6 120.22(16) 2_756 . ?
C3_6 C1_6 H1_6 119.9 2_756 . ?
C2_6 C1_6 H1_6 119.9 . . ?
C3_6 C2_6 C1_6 119.83(16) . . ?
C3_6 C2_6 H2_6 120.1 . . ?
C1_6 C2_6 H2_6 120.1 . . ?
C1_6 C3_6 C2_6 119.95(16) 2_756 . ?
C1_6 C3_6 H3_6 120.0 2_756 . ?
C2_6 C3_6 H3_6 120.0 . . ?
C14 C1 C2 118.02(12) . . ?
C14 C1 B1 131.12(11) . . ?
C2 C1 B1 110.86(11) . . ?
C1 B1 B2 101.23(10) . . ?
C1 B1 P1_1 103.69(9) . . ?
B2 B1 P1_1 112.33(9) . . ?
C1 B1 H1 115.2(8) . . ?
B2 B1 H1 120.5(8) . . ?
P1_1 B1 H1 103.0(8) . . ?
C7 C2 C3 122.72(11) . . ?
C7 C2 C1 122.48(12) . . ?
C3 C2 C1 114.69(11) . . ?
C21_1 B2 C3 116.11(10) . . ?
C21_1 B2 B1 121.57(11) . . ?
C3 B2 B1 100.12(10) . . ?
C21_1 B2 P2_1 112.59(9) . . ?
C3 B2 P2_1 98.95(8) . . ?
B1 B2 P2_1 104.41(9) . . ?
C4 C3 C2 116.82(12) . . ?
C4 C3 B2 131.23(12) . . ?
C2 C3 B2 111.62(11) . . ?
C3 C4 C5 121.33(12) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 121.29(12) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 120.04(12) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C2 117.75(12) . . ?
C6 C7 C8 123.99(12) . . ?
C2 C7 C8 118.22(11) . . ?
C9 C8 C13 118.19(12) . . ?
C9 C8 C7 123.12(12) . . ?
C13 C8 C7 118.69(12) . . ?
C10 C9 C8 121.60(13) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 120.20(13) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 119.54(13) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C13 121.58(13) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C8 118.86(12) . . ?
C12 C13 C14 120.83(12) . . ?
C8 C13 C14 120.31(12) . . ?
C1 C14 C13 122.19(12) . . ?
C1 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C28 C21_1 C16 115.92(11) . . ?
C28 C21_1 B2 121.16(11) . . ?
C16 C21_1 B2 122.75(11) . . ?
C17 C16 C21 117.69(12) . . ?
C17 C16 C21_1 120.31(12) . . ?
C21 C16 C21_1 121.94(12) . . ?
C18 C17 C16 122.37(13) . . ?
C18 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
C17 C18 C19 119.54(13) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 119.68(13) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 121.94(13) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C16 118.62(12) . . ?
C20 C21 C22 121.77(12) . . ?
C16 C21 C22 119.60(12) . . ?
C27 C22 C23 118.39(12) . . ?
C27 C22 C21 118.22(12) . . ?
C23 C22 C21 123.38(12) . . ?
C24 C23 C22 121.08(13) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 120.60(13) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C26 C25 C24 119.52(13) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C27 121.21(13) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C22 C27 C26 119.18(12) . . ?
C22 C27 C28 119.83(12) . . ?
C26 C27 C28 120.97(12) . . ?
C21_1 C28 C27 124.42(12) . . ?
C21_1 C28 H28 117.8 . . ?
C27 C28 H28 117.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6_4 C1_4 C2_4 C3_4 0.3(3) . . . . ?
C1_4 C2_4 C3_4 C4_4 -0.4(2) . . . . ?
C2_4 C3_4 C4_4 C5_4 0.3(2) . . . . ?
C3_4 C4_4 C5_4 C6_4 -0.1(2) . . . . ?
C4_4 C5_4 C6_4 C1_4 -0.1(2) . . . . ?
C2_4 C1_4 C6_4 C5_4 -0.1(3) . . . . ?
C3_5 C1_5 C4_5 C3_5 -0.5(3) . . . 2_566 ?
C4_5 C1_5 C3_5 C4_5 0.5(3) . . . 2_566 ?
C3_6 C1_6 C2_6 C3_6 0.0(3) 2_756 . . . ?
C1_6 C2_6 C3_6 C1_6 0.0(3) . . . 2_756 ?
C14 C1 B1 B2 168.77(13) . . . . ?
C2 C1 B1 B2 -10.70(12) . . . . ?
C14 C1 B1 P1_1 -74.68(15) . . . . ?
C2 C1 B1 P1_1 105.86(11) . . . . ?
C14 C1 C2 C7 2.26(18) . . . . ?
B1 C1 C2 C7 -178.19(11) . . . . ?
C14 C1 C2 C3 -174.02(11) . . . . ?
B1 C1 C2 C3 5.52(15) . . . . ?
C1 B1 B2 C21_1 140.71(11) . . . . ?
P1_1 B1 B2 C21_1 30.68(14) . . . . ?
C1 B1 B2 C3 11.35(11) . . . . ?
P1_1 B1 B2 C3 -98.68(10) . . . . ?
C1 B1 B2 P2_1 -90.72(9) . . . . ?
P1_1 B1 B2 P2_1 159.25(7) . . . . ?
C7 C2 C3 C4 1.23(18) . . . . ?
C1 C2 C3 C4 177.51(11) . . . . ?
C7 C2 C3 B2 -172.94(11) . . . . ?
C1 C2 C3 B2 3.34(15) . . . . ?
C21_1 B2 C3 C4 44.68(19) . . . . ?
B1 B2 C3 C4 177.49(13) . . . . ?
P2_1 B2 C3 C4 -76.01(15) . . . . ?
C21_1 B2 C3 C2 -142.24(11) . . . . ?
B1 B2 C3 C2 -9.43(12) . . . . ?
P2_1 B2 C3 C2 97.07(11) . . . . ?
C2 C3 C4 C5 0.57(18) . . . . ?
B2 C3 C4 C5 173.36(12) . . . . ?
C3 C4 C5 C6 -1.69(19) . . . . ?
C4 C5 C6 C7 0.99(19) . . . . ?
C5 C6 C7 C2 0.76(18) . . . . ?
C5 C6 C7 C8 -177.11(12) . . . . ?
C3 C2 C7 C6 -1.90(18) . . . . ?
C1 C2 C7 C6 -177.89(11) . . . . ?
C3 C2 C7 C8 176.09(11) . . . . ?
C1 C2 C7 C8 0.10(18) . . . . ?
C6 C7 C8 C9 -3.9(2) . . . . ?
C2 C7 C8 C9 178.23(12) . . . . ?
C6 C7 C8 C13 175.40(12) . . . . ?
C2 C7 C8 C13 -2.46(17) . . . . ?
C13 C8 C9 C10 -1.63(19) . . . . ?
C7 C8 C9 C10 177.68(12) . . . . ?
C8 C9 C10 C11 0.2(2) . . . . ?
C9 C10 C11 C12 0.9(2) . . . . ?
C10 C11 C12 C13 -0.5(2) . . . . ?
C11 C12 C13 C8 -0.95(19) . . . . ?
C11 C12 C13 C14 179.15(12) . . . . ?
C9 C8 C13 C12 1.96(18) . . . . ?
C7 C8 C13 C12 -177.38(11) . . . . ?
C9 C8 C13 C14 -178.14(11) . . . . ?
C7 C8 C13 C14 2.52(18) . . . . ?
C2 C1 C14 C13 -2.25(18) . . . . ?
B1 C1 C14 C13 178.32(12) . . . . ?
C12 C13 C14 C1 179.79(12) . . . . ?
C8 C13 C14 C1 -0.11(19) . . . . ?
C3 B2 C21_1 C28 6.37(17) . . . . ?
B1 B2 C21_1 C28 -115.68(14) . . . . ?
P2_1 B2 C21_1 C28 119.43(12) . . . . ?
C3 B2 C21_1 C16 -178.66(11) . . . . ?
B1 B2 C21_1 C16 59.29(16) . . . . ?
P2_1 B2 C21_1 C16 -65.60(14) . . . . ?
C28 C21_1 C16 C17 176.77(12) . . . . ?
B2 C21_1 C16 C17 1.56(18) . . . . ?
C28 C21_1 C16 C21 -0.35(18) . . . . ?
B2 C21_1 C16 C21 -175.56(12) . . . . ?
C21 C16 C17 C18 -4.3(2) . . . . ?
C21_1 C16 C17 C18 178.45(12) . . . . ?
C16 C17 C18 C19 1.5(2) . . . . ?
C17 C18 C19 C20 1.6(2) . . . . ?
C18 C19 C20 C21 -1.7(2) . . . . ?
C19 C20 C21 C16 -1.2(2) . . . . ?
C19 C20 C21 C22 177.61(13) . . . . ?
C17 C16 C21 C20 4.06(19) . . . . ?
C21_1 C16 C21 C20 -178.75(12) . . . . ?
C17 C16 C21 C22 -174.76(12) . . . . ?
C21_1 C16 C21 C22 2.43(19) . . . . ?
C20 C21 C22 C27 178.04(12) . . . . ?
C16 C21 C22 C27 -3.18(18) . . . . ?
C20 C21 C22 C23 -3.2(2) . . . . ?
C16 C21 C22 C23 175.57(12) . . . . ?
C27 C22 C23 C24 -0.7(2) . . . . ?
C21 C22 C23 C24 -179.42(13) . . . . ?
C22 C23 C24 C25 -0.4(2) . . . . ?
C23 C24 C25 C26 0.6(2) . . . . ?
C24 C25 C26 C27 0.3(2) . . . . ?
C23 C22 C27 C26 1.56(18) . . . . ?
C21 C22 C27 C26 -179.63(12) . . . . ?
C23 C22 C27 C28 -176.87(12) . . . . ?
C21 C22 C27 C28 1.94(18) . . . . ?
C25 C26 C27 C22 -1.4(2) . . . . ?
C25 C26 C27 C28 177.00(12) . . . . ?
C16 C21_1 C28 C27 -0.98(19) . . . . ?
B2 C21_1 C28 C27 174.32(12) . . . . ?
C22 C27 C28 C21_1 0.2(2) . . . . ?
C26 C27 C28 C21_1 -178.24(12) . . . . ?

_refine_diff_density_max         0.433
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.047


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

data_test_a_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2169214'
loop_
_audit_author_name
_audit_author_address
'Merle Arrowsmith'
;Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-06-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT601_test_a              
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .         31 Ang**3
RESPONSE: no other solvent molecules found in residual electron density
;
_vrf_PLAT911_test_a              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: boron-bound H atom freely refined
;


_audit_creation_method           'CIF-fill 1.2r (K.Radacki 2005-21)'
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        6-Phen
_chemical_name_common            B2(Phen)2Cl2(PMe3)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 B2 Cl2 P2, C4 H8 O'
_chemical_formula_sum            'C38 H44 B2 Cl2 O P2'
_chemical_formula_weight         671.24

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

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

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

_cell_length_a                   14.3363(13)
_cell_length_b                   14.3363(13)
_cell_length_c                   17.508(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3598.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9977
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      26.31


_exptl_special_details           
;
The crystal was immersed in a film of perfluoropolyether oil, mounted on a 
polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800).
;
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.222
_exptl_absorpt_coefficient_mu    0.299
_shelx_estimated_absorpt_T_min   0.923
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -3.00 1.00 0.1040
0.00 1.00 0.00 0.1110
0.00 3.00 2.00 0.1040
0.00 -3.00 -2.00 0.0890
-1.00 -2.00 3.00 0.1120
1.00 3.00 -2.00 0.1280
0.00 1.00 2.00 0.0880
0.00 -1.00 -2.00 0.1210
2.00 3.00 -3.00 0.1310
1.00 2.00 1.00 0.1300
-1.00 -2.00 -1.00 0.0590
-3.00 -3.00 2.00 0.0960
3.00 3.00 -2.00 0.1430
-3.00 -2.00 1.00 0.0990
2.00 1.00 1.00 0.1240
-2.00 -1.00 -1.00 0.1360
-1.00 0.00 -2.00 0.1330
1.00 0.00 2.00 0.0780
2.00 -1.00 -2.00 0.0880
-2.00 1.00 2.00 0.1330

_exptl_absorpt_special_details   ?
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector                 CPA
_diffrn_detector_type            'Photon II'
_diffrn_detector_area_resol_mean 7.5
_diffrn_reflns_number            55828
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.836
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3540
_reflns_number_gt                2881
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BIS 6.2.14 / APEX3 ver. 2019.1 (Bruker AXS)'
_computing_cell_refinement       'Saint+ ver. V8.40A (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.40A (Bruker AXS)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          
;
The asymmetric unit contains half a twofold disordered THF molecule placed on 
a fourfold rotoinversion axis, modelled with PARTs -1 and -2 and refined to a 
64:36 ratio.  The displacement parameters of all atoms of residues RESI 3 THF 
and RESI 4 THF were restrained to the same value with similarity restraint SIMU.

The 1-2 and 1-3 distances in RESI 3 THF and RESI 4 THF were restrained to the 
same values with SAME.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0360P)²+1.6805P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         3540
_refine_ls_number_parameters     275
_refine_ls_number_restraints     160
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0838
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1_1 B 0.28040(13) 0.69604(12) 0.52351(10) 0.0163(4) Uani 1 1 d . . . . .
P1_1 P 0.38957(3) 0.68479(3) 0.59357(2) 0.01934(12) Uani 1 1 d . . . . .
Cl1_1 Cl 0.20288(3) 0.60140(3) 0.57500(2) 0.01983(11) Uani 1 1 d . . . . .
C2_1 C 0.42986(14) 0.56504(13) 0.59213(11) 0.0292(4) Uani 1 1 d . . . . .
H2A_1 H 0.482838 0.558193 0.627057 0.044 Uiso 1 1 calc R U . . .
H2B_1 H 0.449366 0.548491 0.540219 0.044 Uiso 1 1 calc R U . . .
H2C_1 H 0.379183 0.523649 0.608327 0.044 Uiso 1 1 calc R U . . .
C3_1 C 0.49369(13) 0.75059(14) 0.57144(11) 0.0294(4) Uani 1 1 d . . . . .
H3A_1 H 0.541994 0.736866 0.609420 0.044 Uiso 1 1 calc R U . . .
H3B_1 H 0.479347 0.817414 0.572361 0.044 Uiso 1 1 calc R U . . .
H3C_1 H 0.516171 0.733149 0.520545 0.044 Uiso 1 1 calc R U . . .
C1_1 C 0.36650(13) 0.70906(12) 0.69284(10) 0.0249(4) Uani 1 1 d . . . . .
H1A_1 H 0.422553 0.696057 0.723060 0.037 Uiso 1 1 calc R U . . .
H1B_1 H 0.315185 0.669513 0.710687 0.037 Uiso 1 1 calc R U . . .
H1C_1 H 0.349237 0.774812 0.698727 0.037 Uiso 1 1 calc R U . . .
C1_2 C 0.31867(11) 0.65335(11) 0.44316(9) 0.0165(3) Uani 1 1 d . . . . .
C2_2 C 0.37984(11) 0.70676(11) 0.39255(9) 0.0174(3) Uani 1 1 d . . . . .
C3_2 C 0.40355(12) 0.80025(12) 0.40924(9) 0.0199(3) Uani 1 1 d . . . . .
H3_2 H 0.376986 0.829133 0.452965 0.024 Uiso 1 1 calc R U . . .
C4_2 C 0.46366(12) 0.85065(13) 0.36436(10) 0.0241(4) Uani 1 1 d . . . . .
H4_2 H 0.478704 0.913117 0.377617 0.029 Uiso 1 1 calc R U . . .
C5_2 C 0.50289(13) 0.81015(13) 0.29903(10) 0.0271(4) Uani 1 1 d . . . . .
H5_2 H 0.544631 0.844813 0.267876 0.032 Uiso 1 1 calc R U . . .
C6_2 C 0.48047(12) 0.72000(13) 0.28049(10) 0.0247(4) Uani 1 1 d . . . . .
H6_2 H 0.506815 0.693030 0.235863 0.030 Uiso 1 1 calc R U . . .
C7_2 C 0.41944(11) 0.66609(12) 0.32571(9) 0.0193(4) Uani 1 1 d . . . . .
C8_2 C 0.39763(11) 0.57016(12) 0.30647(9) 0.0198(4) Uani 1 1 d . . . . .
C9_2 C 0.43416(12) 0.52415(13) 0.24127(10) 0.0248(4) Uani 1 1 d . . . . .
H9_2 H 0.472404 0.557651 0.206474 0.030 Uiso 1 1 calc R U . . .
C10_2 C 0.41488(13) 0.43161(14) 0.22782(10) 0.0282(4) Uani 1 1 d . . . . .
H10_2 H 0.440605 0.401625 0.184262 0.034 Uiso 1 1 calc R U . . .
C11_2 C 0.35779(13) 0.38137(13) 0.27768(11) 0.0283(4) Uani 1 1 d . . . . .
H11_2 H 0.345617 0.317207 0.268466 0.034 Uiso 1 1 calc R U . . .
C12_2 C 0.31916(12) 0.42500(13) 0.34022(10) 0.0248(4) Uani 1 1 d . . . . .
H12_2 H 0.279335 0.390963 0.373438 0.030 Uiso 1 1 calc R U . . .
C13_2 C 0.33820(11) 0.51987(12) 0.35544(9) 0.0194(3) Uani 1 1 d . . . . .
C14_2 C 0.30021(11) 0.56366(11) 0.42225(9) 0.0184(3) Uani 1 1 d . . . . .
H14_2 H 0.259772 0.527996 0.453796 0.022 Uiso 1 1 calc R U . . .
O1_3 O 0.2374(10) 0.2405(9) 0.5008(4) 0.045(2) Uani 0.321(6) 1 d D U P A -1
C1_3 C 0.2290(12) 0.3338(13) 0.5521(8) 0.050(3) Uani 0.321(6) 1 d D U P A -1
H1A_3 H 0.261322 0.387421 0.528226 0.059 Uiso 0.321(6) 1 calc R U P A -1
H1B_3 H 0.163243 0.350473 0.562531 0.059 Uiso 0.321(6) 1 calc R U P A -1
C2_3 C 0.2779(14) 0.3010(15) 0.6220(9) 0.046(3) Uani 0.321(6) 1 d D U P A -1
H2A_3 H 0.258491 0.337549 0.667254 0.055 Uiso 0.321(6) 1 calc R U P A -1
H2B_3 H 0.346372 0.305717 0.616059 0.055 Uiso 0.321(6) 1 calc R U P A -1
C3_3 C 0.2473(16) 0.1991(14) 0.6292(9) 0.041(3) Uani 0.321(6) 1 d D U P A -1
H3A_3 H 0.291436 0.161964 0.660327 0.049 Uiso 0.321(6) 1 calc R U P A -1
H3B_3 H 0.183609 0.193331 0.650681 0.049 Uiso 0.321(6) 1 calc R U P A -1
C4_3 C 0.2507(13) 0.1721(11) 0.5450(8) 0.043(3) Uani 0.321(6) 1 d D U P A -1
H4A_3 H 0.312244 0.144118 0.533594 0.051 Uiso 0.321(6) 1 calc R U P A -1
H4B_3 H 0.202473 0.124166 0.534908 0.051 Uiso 0.321(6) 1 calc R U P A -1
O1_4 O 0.2823(13) 0.2350(12) 0.5058(8) 0.047(3) Uani 0.179(6) 1 d D U P A -2
C1_4 C 0.3112(12) 0.3180(10) 0.5649(9) 0.044(3) Uani 0.179(6) 1 d D U P A -2
H1A_4 H 0.379544 0.321492 0.572739 0.053 Uiso 0.179(6) 1 calc R U P A -2
H1B_4 H 0.287386 0.379605 0.548280 0.053 Uiso 0.179(6) 1 calc R U P A -2
C2_4 C 0.261(3) 0.2824(16) 0.6340(12) 0.045(3) Uani 0.179(6) 1 d D U P A -2
H2A_4 H 0.200332 0.313876 0.639855 0.054 Uiso 0.179(6) 1 calc R U P A -2
H2B_4 H 0.298900 0.293877 0.680580 0.054 Uiso 0.179(6) 1 calc R U P A -2
C3_4 C 0.248(3) 0.1788(15) 0.6217(11) 0.043(3) Uani 0.179(6) 1 d D U P A -2
H3A_4 H 0.196587 0.153547 0.653264 0.052 Uiso 0.179(6) 1 calc R U P A -2
H3B_4 H 0.305883 0.143241 0.631740 0.052 Uiso 0.179(6) 1 calc R U P A -2
C4_4 C 0.2233(19) 0.1800(16) 0.5373(11) 0.046(3) Uani 0.179(6) 1 d D U P A -2
H4A_4 H 0.228195 0.116563 0.515293 0.055 Uiso 0.179(6) 1 calc R U P A -2
H4B_4 H 0.158902 0.203103 0.529684 0.055 Uiso 0.179(6) 1 calc R U P A -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1_1 C1_2 1.629(2) . ?
B1_1 B1_1 1.776(4) 2_565 ?
B1_1 Cl1_1 1.9719(19) . ?
B1_1 P1_1 1.9950(19) . ?
P1_1 C1_1 1.8030(18) . ?
P1_1 C3_1 1.808(2) . ?
P1_1 C2_1 1.8116(18) . ?
C2_1 H2A_1 0.9800 . ?
C2_1 H2B_1 0.9800 . ?
C2_1 H2C_1 0.9800 . ?
C3_1 H3A_1 0.9800 . ?
C3_1 H3B_1 0.9800 . ?
C3_1 H3C_1 0.9800 . ?
C1_1 H1A_1 0.9800 . ?
C1_1 H1B_1 0.9800 . ?
C1_1 H1C_1 0.9800 . ?
C1_2 C14_2 1.363(2) . ?
C1_2 C2_2 1.463(2) . ?
C2_2 C3_2 1.413(2) . ?
C2_2 C7_2 1.425(2) . ?
C3_2 C4_2 1.372(2) . ?
C3_2 H3_2 0.9500 . ?
C4_2 C5_2 1.401(3) . ?
C4_2 H4_2 0.9500 . ?
C5_2 C6_2 1.371(3) . ?
C5_2 H5_2 0.9500 . ?
C6_2 C7_2 1.411(2) . ?
C6_2 H6_2 0.9500 . ?
C7_2 C8_2 1.450(2) . ?
C8_2 C13_2 1.407(2) . ?
C8_2 C9_2 1.419(2) . ?
C9_2 C10_2 1.375(3) . ?
C9_2 H9_2 0.9500 . ?
C10_2 C11_2 1.397(3) . ?
C10_2 H10_2 0.9500 . ?
C11_2 C12_2 1.377(3) . ?
C11_2 H11_2 0.9500 . ?
C12_2 C13_2 1.413(2) . ?
C12_2 H12_2 0.9500 . ?
C13_2 C14_2 1.435(2) . ?
C14_2 H14_2 0.9500 . ?
O1_3 C4_3 1.263(16) . ?
O1_3 C1_3 1.615(18) . ?
C1_3 C2_3 1.49(2) . ?
C1_3 H1A_3 0.9900 . ?
C1_3 H1B_3 0.9900 . ?
C2_3 C3_3 1.531(10) . ?
C2_3 H2A_3 0.9900 . ?
C2_3 H2B_3 0.9900 . ?
C3_3 C4_3 1.53(2) . ?
C3_3 H3A_3 0.9900 . ?
C3_3 H3B_3 0.9900 . ?
C4_3 H4A_3 0.9900 . ?
C4_3 H4B_3 0.9900 . ?
O1_4 C4_4 1.28(2) . ?
O1_4 C1_4 1.631(19) . ?
C1_4 C2_4 1.50(2) . ?
C1_4 H1A_4 0.9900 . ?
C1_4 H1B_4 0.9900 . ?
C2_4 C3_4 1.513(15) . ?
C2_4 H2A_4 0.9900 . ?
C2_4 H2B_4 0.9900 . ?
C3_4 C4_4 1.52(2) . ?
C3_4 H3A_4 0.9900 . ?
C3_4 H3B_4 0.9900 . ?
C4_4 H4A_4 0.9900 . ?
C4_4 H4B_4 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1_2 B1_1 B1_1 119.51(8) . 2_565 ?
C1_2 B1_1 Cl1_1 109.03(11) . . ?
B1_1 B1_1 Cl1_1 108.83(13) 2_565 . ?
C1_2 B1_1 P1_1 103.67(11) . . ?
B1_1 B1_1 P1_1 117.10(11) 2_565 . ?
Cl1_1 B1_1 P1_1 96.05(8) . . ?
C1_1 P1_1 C3_1 104.91(9) . . ?
C1_1 P1_1 C2_1 104.76(9) . . ?
C3_1 P1_1 C2_1 103.19(9) . . ?
C1_1 P1_1 B1_1 115.67(8) . . ?
C3_1 P1_1 B1_1 118.28(8) . . ?
C2_1 P1_1 B1_1 108.55(8) . . ?
P1_1 C2_1 H2A_1 109.5 . . ?
P1_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
P1_1 C2_1 H2C_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
P1_1 C3_1 H3A_1 109.5 . . ?
P1_1 C3_1 H3B_1 109.5 . . ?
H3A_1 C3_1 H3B_1 109.5 . . ?
P1_1 C3_1 H3C_1 109.5 . . ?
H3A_1 C3_1 H3C_1 109.5 . . ?
H3B_1 C3_1 H3C_1 109.5 . . ?
P1_1 C1_1 H1A_1 109.5 . . ?
P1_1 C1_1 H1B_1 109.5 . . ?
H1A_1 C1_1 H1B_1 109.5 . . ?
P1_1 C1_1 H1C_1 109.5 . . ?
H1A_1 C1_1 H1C_1 109.5 . . ?
H1B_1 C1_1 H1C_1 109.5 . . ?
C14_2 C1_2 C2_2 116.58(14) . . ?
C14_2 C1_2 B1_1 121.39(15) . . ?
C2_2 C1_2 B1_1 121.89(14) . . ?
C3_2 C2_2 C7_2 117.52(15) . . ?
C3_2 C2_2 C1_2 121.01(14) . . ?
C7_2 C2_2 C1_2 121.46(15) . . ?
C4_2 C3_2 C2_2 122.14(16) . . ?
C4_2 C3_2 H3_2 118.9 . . ?
C2_2 C3_2 H3_2 118.9 . . ?
C3_2 C4_2 C5_2 120.11(17) . . ?
C3_2 C4_2 H4_2 119.9 . . ?
C5_2 C4_2 H4_2 119.9 . . ?
C6_2 C5_2 C4_2 119.34(17) . . ?
C6_2 C5_2 H5_2 120.3 . . ?
C4_2 C5_2 H5_2 120.3 . . ?
C5_2 C6_2 C7_2 121.94(16) . . ?
C5_2 C6_2 H6_2 119.0 . . ?
C7_2 C6_2 H6_2 119.0 . . ?
C6_2 C7_2 C2_2 118.93(16) . . ?
C6_2 C7_2 C8_2 121.53(15) . . ?
C2_2 C7_2 C8_2 119.53(15) . . ?
C13_2 C8_2 C9_2 118.39(16) . . ?
C13_2 C8_2 C7_2 118.35(15) . . ?
C9_2 C8_2 C7_2 123.26(17) . . ?
C10_2 C9_2 C8_2 120.80(18) . . ?
C10_2 C9_2 H9_2 119.6 . . ?
C8_2 C9_2 H9_2 119.6 . . ?
C9_2 C10_2 C11_2 120.55(17) . . ?
C9_2 C10_2 H10_2 119.7 . . ?
C11_2 C10_2 H10_2 119.7 . . ?
C12_2 C11_2 C10_2 119.88(17) . . ?
C12_2 C11_2 H11_2 120.1 . . ?
C10_2 C11_2 H11_2 120.1 . . ?
C11_2 C12_2 C13_2 120.65(18) . . ?
C11_2 C12_2 H12_2 119.7 . . ?
C13_2 C12_2 H12_2 119.7 . . ?
C8_2 C13_2 C12_2 119.68(15) . . ?
C8_2 C13_2 C14_2 120.15(15) . . ?
C12_2 C13_2 C14_2 120.12(16) . . ?
C1_2 C14_2 C13_2 123.92(16) . . ?
C1_2 C14_2 H14_2 118.0 . . ?
C13_2 C14_2 H14_2 118.0 . . ?
C4_3 O1_3 C1_3 108.3(6) . . ?
C2_3 C1_3 O1_3 99.2(13) . . ?
C2_3 C1_3 H1A_3 111.9 . . ?
O1_3 C1_3 H1A_3 111.9 . . ?
C2_3 C1_3 H1B_3 111.9 . . ?
O1_3 C1_3 H1B_3 111.9 . . ?
H1A_3 C1_3 H1B_3 109.6 . . ?
C1_3 C2_3 C3_3 103.6(16) . . ?
C1_3 C2_3 H2A_3 111.0 . . ?
C3_3 C2_3 H2A_3 111.0 . . ?
C1_3 C2_3 H2B_3 111.0 . . ?
C3_3 C2_3 H2B_3 111.0 . . ?
H2A_3 C2_3 H2B_3 109.0 . . ?
C4_3 C3_3 C2_3 98.8(14) . . ?
C4_3 C3_3 H3A_3 112.0 . . ?
C2_3 C3_3 H3A_3 112.0 . . ?
C4_3 C3_3 H3B_3 112.0 . . ?
C2_3 C3_3 H3B_3 112.0 . . ?
H3A_3 C3_3 H3B_3 109.7 . . ?
O1_3 C4_3 C3_3 112.9(13) . . ?
O1_3 C4_3 H4A_3 109.0 . . ?
C3_3 C4_3 H4A_3 109.0 . . ?
O1_3 C4_3 H4B_3 109.0 . . ?
C3_3 C4_3 H4B_3 109.0 . . ?
H4A_3 C4_3 H4B_3 107.8 . . ?
C4_4 O1_4 C1_4 110.2(12) . . ?
C2_4 C1_4 O1_4 98.2(13) . . ?
C2_4 C1_4 H1A_4 112.1 . . ?
O1_4 C1_4 H1A_4 112.1 . . ?
C2_4 C1_4 H1B_4 112.1 . . ?
O1_4 C1_4 H1B_4 112.1 . . ?
H1A_4 C1_4 H1B_4 109.8 . . ?
C1_4 C2_4 C3_4 106.3(19) . . ?
C1_4 C2_4 H2A_4 110.5 . . ?
C3_4 C2_4 H2A_4 110.5 . . ?
C1_4 C2_4 H2B_4 110.5 . . ?
C3_4 C2_4 H2B_4 110.5 . . ?
H2A_4 C2_4 H2B_4 108.7 . . ?
C2_4 C3_4 C4_4 99.1(17) . . ?
C2_4 C3_4 H3A_4 112.0 . . ?
C4_4 C3_4 H3A_4 112.0 . . ?
C2_4 C3_4 H3B_4 112.0 . . ?
C4_4 C3_4 H3B_4 112.0 . . ?
H3A_4 C3_4 H3B_4 109.6 . . ?
O1_4 C4_4 C3_4 105.8(18) . . ?
O1_4 C4_4 H4A_4 110.6 . . ?
C3_4 C4_4 H4A_4 110.6 . . ?
O1_4 C4_4 H4B_4 110.6 . . ?
C3_4 C4_4 H4B_4 110.6 . . ?
H4A_4 C4_4 H4B_4 108.7 . . ?

_refine_diff_density_max         0.259
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.045


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