# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_alldata_a
_database_code_depnum_ccdc_archive 'CCDC 1954176'
loop_
_audit_author_name
_audit_author_address
'Tom Stennett'
;Julius Maximilians Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2019-09-17 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H67 B2 P3'
_chemical_formula_sum            'C50 H67 B2 P3'
_chemical_formula_weight         782.56

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                   10.6022(5)
_cell_length_b                   10.6218(5)
_cell_length_c                   20.1023(10)
_cell_angle_alpha                94.418(2)
_cell_angle_beta                 99.288(2)
_cell_angle_gamma                100.371(2)
_cell_volume                     2184.47(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9736
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.10


_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    1.190
_exptl_crystal_F_000             844
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.170
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_T_max  0.7455
_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                   '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            57183
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.314
_diffrn_reflns_theta_max         26.022
_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             8565
_reflns_number_gt                7915
_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-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0337P)²+1.4537P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8565
_refine_ls_number_parameters     500
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0866
_refine_ls_wR_factor_gt          0.0842
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.62108(15) 0.65961(15) 0.25633(8) 0.0142(3) Uani 1 1 d . . . . .
H1 H 0.4784(15) 0.6103(15) 0.1483(8) 0.017(4) Uiso 1 1 d . . . . .
B2 B 0.47512(15) 0.66390(15) 0.19941(8) 0.0146(3) Uani 1 1 d . . . . .
P2 P 0.66084(3) 0.82945(3) 0.31426(2) 0.01520(9) Uani 1 1 d . . . . .
C2 C 0.92819(15) 0.79754(15) 0.13883(7) 0.0217(3) Uani 1 1 d . . . . .
H2 H 0.995632 0.760143 0.161549 0.026 Uiso 1 1 calc R U . . .
C4 C 0.86179(16) 0.94861(16) 0.06371(8) 0.0282(4) Uani 1 1 d . . . . .
H4 H 0.882811 1.014657 0.035753 0.034 Uiso 1 1 calc R U . . .
P3 P 0.33821(3) 0.53960(3) 0.22344(2) 0.01361(8) Uani 1 1 d . . . . .
C3 C 0.95882(16) 0.89404(16) 0.09758(8) 0.0271(4) Uani 1 1 d . . . . .
H3 H 1.046780 0.922400 0.092735 0.033 Uiso 1 1 calc R U . . .
C5 C 0.73335(16) 0.90640(16) 0.07074(8) 0.0264(3) Uani 1 1 d . . . . .
H5 H 0.666263 0.943267 0.047256 0.032 Uiso 1 1 calc R U . . .
C6 C 0.70254(15) 0.81047(14) 0.11197(8) 0.0216(3) Uani 1 1 d . . . . .
H6 H 0.614258 0.782183 0.116251 0.026 Uiso 1 1 calc R U . . .
C7 C 0.69751(13) 0.48746(14) 0.15329(7) 0.0179(3) Uani 1 1 d . . . . .
C8 C 0.64213(14) 0.48356(15) 0.08501(8) 0.0203(3) Uani 1 1 d . . . . .
H8 H 0.642658 0.561802 0.065031 0.024 Uiso 1 1 calc R U . . .
C9 C 0.58632(15) 0.36742(16) 0.04579(8) 0.0249(3) Uani 1 1 d . . . . .
H9 H 0.549786 0.367053 -0.000610 0.030 Uiso 1 1 calc R U . . .
C10 C 0.58361(15) 0.25208(15) 0.07394(8) 0.0264(3) Uani 1 1 d . . . . .
H10 H 0.544543 0.172801 0.047202 0.032 Uiso 1 1 calc R U . . .
C11 C 0.63857(15) 0.25358(15) 0.14161(8) 0.0244(3) Uani 1 1 d . . . . .
H11 H 0.636912 0.174997 0.161354 0.029 Uiso 1 1 calc R U . . .
C12 C 0.69607(14) 0.36982(15) 0.18059(8) 0.0208(3) Uani 1 1 d . . . . .
H12 H 0.735056 0.369448 0.226557 0.025 Uiso 1 1 calc R U . . .
C13 C 0.42800(13) 0.79708(14) 0.18442(7) 0.0164(3) Uani 1 1 d . . . . .
C14 C 0.36272(14) 0.81061(15) 0.11923(7) 0.0195(3) Uani 1 1 d . . . . .
H14 H 0.344420 0.739050 0.085405 0.023 Uiso 1 1 calc R U . . .
C15 C 0.32408(15) 0.92369(16) 0.10233(8) 0.0248(3) Uani 1 1 d . . . . .
H15 H 0.280652 0.928602 0.057693 0.030 Uiso 1 1 calc R U . . .
C16 C 0.34884(16) 1.02934(15) 0.15054(9) 0.0282(4) Uani 1 1 d . . . . .
H16 H 0.322631 1.107214 0.139429 0.034 Uiso 1 1 calc R U . . .
C17 C 0.41244(15) 1.02000(15) 0.21530(8) 0.0253(3) Uani 1 1 d . . . . .
H17 H 0.430096 1.092358 0.248608 0.030 Uiso 1 1 calc R U . . .
C19 C 0.51355(14) 0.89872(14) 0.30500(7) 0.0191(3) Uani 1 1 d . . . . .
H19A H 0.448767 0.846625 0.327319 0.023 Uiso 1 1 calc R U . . .
H19B H 0.535746 0.986690 0.329276 0.023 Uiso 1 1 calc R U . . .
C18 C 0.45096(13) 0.90607(14) 0.23240(7) 0.0178(3) Uani 1 1 d . . . . .
P1 P 0.77431(3) 0.63654(4) 0.20911(2) 0.01615(9) Uani 1 1 d . . . . .
C1 C 0.79950(14) 0.75488(14) 0.14730(7) 0.0180(3) Uani 1 1 d . . . . .
C20 C 0.78791(14) 0.94908(14) 0.28841(7) 0.0188(3) Uani 1 1 d . . . . .
H20 H 0.776827 0.930607 0.238046 0.023 Uiso 1 1 calc R U . . .
C21 C 0.92336(14) 0.92213(14) 0.31674(8) 0.0214(3) Uani 1 1 d . . . . .
H21A H 0.938561 0.935367 0.366906 0.026 Uiso 1 1 calc R U . . .
H21B H 0.925808 0.831216 0.302971 0.026 Uiso 1 1 calc R U . . .
C22 C 1.03187(15) 1.01047(15) 0.29098(8) 0.0250(3) Uani 1 1 d . . . . .
H22A H 1.117676 0.995224 0.312687 0.030 Uiso 1 1 calc R U . . .
H22B H 1.023060 0.989886 0.241373 0.030 Uiso 1 1 calc R U . . .
C23 C 1.02534(16) 1.15096(15) 0.30678(9) 0.0277(4) Uani 1 1 d . . . . .
H23A H 1.094454 1.205932 0.288441 0.033 Uiso 1 1 calc R U . . .
H23B H 1.041051 1.173309 0.356540 0.033 Uiso 1 1 calc R U . . .
C24 C 0.89273(16) 1.17722(15) 0.27596(9) 0.0295(4) Uani 1 1 d . . . . .
H24A H 0.879913 1.160672 0.225948 0.035 Uiso 1 1 calc R U . . .
H24B H 0.890538 1.268956 0.287690 0.035 Uiso 1 1 calc R U . . .
C25 C 0.78161(15) 1.09243(14) 0.30158(8) 0.0235(3) Uani 1 1 d . . . . .
H25A H 0.696874 1.107334 0.278158 0.028 Uiso 1 1 calc R U . . .
H25B H 0.788172 1.116046 0.350805 0.028 Uiso 1 1 calc R U . . .
C26 C 0.70192(14) 0.82775(14) 0.40774(7) 0.0182(3) Uani 1 1 d . . . . .
H26 H 0.778493 0.784526 0.416017 0.022 Uiso 1 1 calc R U . . .
C27 C 0.59105(14) 0.74431(15) 0.43523(7) 0.0208(3) Uani 1 1 d . . . . .
H27A H 0.514141 0.785877 0.430702 0.025 Uiso 1 1 calc R U . . .
H27B H 0.565391 0.658896 0.408181 0.025 Uiso 1 1 calc R U . . .
C28 C 0.63482(16) 0.72722(16) 0.50986(8) 0.0263(3) Uani 1 1 d . . . . .
H28A H 0.561869 0.675145 0.526800 0.032 Uiso 1 1 calc R U . . .
H28B H 0.707816 0.680202 0.513893 0.032 Uiso 1 1 calc R U . . .
C29 C 0.67833(18) 0.85704(18) 0.55310(8) 0.0321(4) Uani 1 1 d . . . . .
H29A H 0.602969 0.900154 0.553151 0.038 Uiso 1 1 calc R U . . .
H29B H 0.711345 0.843588 0.600448 0.038 Uiso 1 1 calc R U . . .
C30 C 0.78508(18) 0.94239(17) 0.52549(8) 0.0309(4) Uani 1 1 d . . . . .
H30A H 0.863798 0.903556 0.530381 0.037 Uiso 1 1 calc R U . . .
H30B H 0.808178 1.027805 0.552561 0.037 Uiso 1 1 calc R U . . .
C31 C 0.74261(16) 0.95980(15) 0.45052(8) 0.0255(3) Uani 1 1 d . . . . .
H31A H 0.815516 1.012769 0.433962 0.031 Uiso 1 1 calc R U . . .
H31B H 0.668485 1.005316 0.445787 0.031 Uiso 1 1 calc R U . . .
C32 C 0.62609(13) 0.54201(13) 0.30423(7) 0.0147(3) Uani 1 1 d . . . . .
C33 C 0.73840(14) 0.54443(14) 0.35312(7) 0.0181(3) Uani 1 1 d . . . . .
H33 H 0.809515 0.614632 0.356472 0.022 Uiso 1 1 calc R U . . .
C34 C 0.75109(15) 0.45035(15) 0.39656(7) 0.0212(3) Uani 1 1 d . . . . .
H34 H 0.828797 0.456978 0.428752 0.025 Uiso 1 1 calc R U . . .
C35 C 0.64898(15) 0.34654(15) 0.39242(8) 0.0228(3) Uani 1 1 d . . . . .
H35 H 0.654148 0.283008 0.422993 0.027 Uiso 1 1 calc R U . . .
C36 C 0.53913(15) 0.33693(14) 0.34291(7) 0.0200(3) Uani 1 1 d . . . . .
H36 H 0.469711 0.265044 0.339449 0.024 Uiso 1 1 calc R U . . .
C37 C 0.52766(14) 0.43030(13) 0.29785(7) 0.0159(3) Uani 1 1 d . . . . .
C38 C 0.41231(13) 0.40100(13) 0.23987(7) 0.0162(3) Uani 1 1 d . . . . .
H38A H 0.345881 0.330964 0.250536 0.019 Uiso 1 1 calc R U . . .
H38B H 0.441389 0.369867 0.198295 0.019 Uiso 1 1 calc R U . . .
C39 C 0.19871(13) 0.48509(14) 0.15330(7) 0.0167(3) Uani 1 1 d . . . . .
H39 H 0.167731 0.564107 0.139071 0.020 Uiso 1 1 calc R U . . .
C40 C 0.08001(14) 0.39415(16) 0.16934(7) 0.0227(3) Uani 1 1 d . . . . .
H40A H 0.106317 0.314320 0.183947 0.027 Uiso 1 1 calc R U . . .
H40B H 0.047496 0.436023 0.207089 0.027 Uiso 1 1 calc R U . . .
C41 C -0.02910(15) 0.36021(18) 0.10704(8) 0.0289(4) Uani 1 1 d . . . . .
H41A H -0.101874 0.297276 0.117842 0.035 Uiso 1 1 calc R U . . .
H41B H -0.062420 0.438792 0.095990 0.035 Uiso 1 1 calc R U . . .
C42 C 0.01708(15) 0.30378(17) 0.04558(8) 0.0280(4) Uani 1 1 d . . . . .
H42A H 0.039837 0.219447 0.054345 0.034 Uiso 1 1 calc R U . . .
H42B H -0.054410 0.289415 0.005841 0.034 Uiso 1 1 calc R U . . .
C43 C 0.13515(15) 0.39297(16) 0.02983(8) 0.0247(3) Uani 1 1 d . . . . .
H43A H 0.110012 0.473857 0.016147 0.030 Uiso 1 1 calc R U . . .
H43B H 0.166399 0.351498 -0.008495 0.030 Uiso 1 1 calc R U . . .
C44 C 0.24463(14) 0.42375(15) 0.09162(7) 0.0207(3) Uani 1 1 d . . . . .
H44A H 0.319452 0.483737 0.080646 0.025 Uiso 1 1 calc R U . . .
H44B H 0.274258 0.343589 0.103117 0.025 Uiso 1 1 calc R U . . .
C45 C 0.28276(14) 0.58462(13) 0.30257(7) 0.0160(3) Uani 1 1 d . . . . .
H45 H 0.363583 0.630179 0.334190 0.019 Uiso 1 1 calc R U . . .
C46 C 0.22322(15) 0.47505(14) 0.34062(7) 0.0200(3) Uani 1 1 d . . . . .
H46A H 0.138746 0.429181 0.313575 0.024 Uiso 1 1 calc R U . . .
H46B H 0.282086 0.412639 0.346529 0.024 Uiso 1 1 calc R U . . .
C47 C 0.20232(16) 0.52815(16) 0.41019(8) 0.0264(3) Uani 1 1 d . . . . .
H47A H 0.159052 0.456917 0.432603 0.032 Uiso 1 1 calc R U . . .
H47B H 0.287870 0.565504 0.438946 0.032 Uiso 1 1 calc R U . . .
C48 C 0.11904(17) 0.63103(17) 0.40379(8) 0.0289(4) Uani 1 1 d . . . . .
H48A H 0.112810 0.668053 0.449600 0.035 Uiso 1 1 calc R U . . .
H48B H 0.029896 0.591248 0.379965 0.035 Uiso 1 1 calc R U . . .
C49 C 0.17703(16) 0.73808(16) 0.36482(8) 0.0254(3) Uani 1 1 d . . . . .
H49A H 0.262486 0.783495 0.390991 0.030 Uiso 1 1 calc R U . . .
H49B H 0.118824 0.801191 0.359563 0.030 Uiso 1 1 calc R U . . .
C50 C 0.19486(14) 0.68481(14) 0.29473(7) 0.0196(3) Uani 1 1 d . . . . .
H50A H 0.234932 0.755838 0.271100 0.024 Uiso 1 1 calc R U . . .
H50B H 0.108993 0.644362 0.267165 0.024 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 C32 1.638(2) . ?
B1 B2 1.780(2) . ?
B1 P2 2.0081(16) . ?
B1 P1 2.0508(16) . ?
B2 C13 1.617(2) . ?
B2 P3 1.9283(15) . ?
B2 H1 1.144(16) . ?
P2 C19 1.8318(15) . ?
P2 C20 1.8468(14) . ?
P2 C26 1.8615(14) . ?
C2 C3 1.394(2) . ?
C2 C1 1.400(2) . ?
C2 H2 0.9500 . ?
C4 C3 1.381(2) . ?
C4 C5 1.388(2) . ?
C4 H4 0.9500 . ?
P3 C38 1.8169(14) . ?
P3 C45 1.8412(14) . ?
P3 C39 1.8449(14) . ?
C3 H3 0.9500 . ?
C5 C6 1.389(2) . ?
C5 H5 0.9500 . ?
C6 C1 1.399(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(2) . ?
C7 C12 1.402(2) . ?
C7 P1 1.8431(15) . ?
C8 C9 1.389(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.407(2) . ?
C13 C14 1.410(2) . ?
C14 C15 1.386(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.395(2) . ?
C17 H17 0.9500 . ?
C19 C18 1.517(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
P1 C1 1.8500(15) . ?
C20 C25 1.540(2) . ?
C20 C21 1.542(2) . ?
C20 H20 1.0000 . ?
C21 C22 1.533(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.518(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.525(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.533(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C31 1.539(2) . ?
C26 C27 1.544(2) . ?
C26 H26 1.0000 . ?
C27 C28 1.532(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.525(2) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.524(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.537(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.411(2) . ?
C32 C37 1.4146(19) . ?
C33 C34 1.387(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.386(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.387(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.402(2) . ?
C36 H36 0.9500 . ?
C37 C38 1.5159(19) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.5370(19) . ?
C39 C44 1.5439(19) . ?
C39 H39 1.0000 . ?
C40 C41 1.533(2) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.521(2) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.521(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.527(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C50 1.5367(19) . ?
C45 C46 1.5384(19) . ?
C45 H45 1.0000 . ?
C46 C47 1.532(2) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.524(2) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.525(2) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.531(2) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 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
C32 B1 B2 119.88(11) . . ?
C32 B1 P2 110.09(9) . . ?
B2 B1 P2 104.25(9) . . ?
C32 B1 P1 98.07(9) . . ?
B2 B1 P1 113.85(9) . . ?
P2 B1 P1 110.74(7) . . ?
C13 B2 B1 122.34(11) . . ?
C13 B2 P3 111.69(10) . . ?
B1 B2 P3 107.15(9) . . ?
C13 B2 H1 107.5(8) . . ?
B1 B2 H1 108.3(8) . . ?
P3 B2 H1 96.8(8) . . ?
C19 P2 C20 106.07(7) . . ?
C19 P2 C26 102.29(7) . . ?
C20 P2 C26 108.04(7) . . ?
C19 P2 B1 108.54(7) . . ?
C20 P2 B1 113.21(7) . . ?
C26 P2 B1 117.57(7) . . ?
C3 C2 C1 120.99(15) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C3 C4 C5 119.63(14) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C38 P3 C45 105.01(6) . . ?
C38 P3 C39 106.87(7) . . ?
C45 P3 C39 110.97(6) . . ?
C38 P3 B2 104.37(7) . . ?
C45 P3 B2 115.67(7) . . ?
C39 P3 B2 113.01(6) . . ?
C4 C3 C2 120.24(14) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C4 C5 C6 120.27(15) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 121.03(14) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C8 C7 C12 117.58(13) . . ?
C8 C7 P1 124.34(11) . . ?
C12 C7 P1 118.08(11) . . ?
C9 C8 C7 121.24(14) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C10 C9 C8 120.42(15) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 119.34(15) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C12 120.20(15) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 121.20(14) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?
C18 C13 C14 115.76(13) . . ?
C18 C13 B2 124.21(12) . . ?
C14 C13 B2 120.01(13) . . ?
C15 C14 C13 122.91(14) . . ?
C15 C14 H14 118.5 . . ?
C13 C14 H14 118.5 . . ?
C16 C15 C14 119.90(14) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 119.04(15) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C16 C17 C18 121.08(15) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C18 C19 P2 114.93(10) . . ?
C18 C19 H19A 108.5 . . ?
P2 C19 H19A 108.5 . . ?
C18 C19 H19B 108.5 . . ?
P2 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C17 C18 C13 121.31(13) . . ?
C17 C18 C19 118.90(13) . . ?
C13 C18 C19 119.75(13) . . ?
C7 P1 C1 102.04(6) . . ?
C7 P1 B1 98.98(6) . . ?
C1 P1 B1 111.41(6) . . ?
C6 C1 C2 117.84(13) . . ?
C6 C1 P1 125.53(11) . . ?
C2 C1 P1 116.50(11) . . ?
C25 C20 C21 112.11(12) . . ?
C25 C20 P2 117.76(11) . . ?
C21 C20 P2 109.38(10) . . ?
C25 C20 H20 105.5 . . ?
C21 C20 H20 105.5 . . ?
P2 C20 H20 105.5 . . ?
C22 C21 C20 111.51(12) . . ?
C22 C21 H21A 109.3 . . ?
C20 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C20 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
C23 C22 C21 110.91(13) . . ?
C23 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.0 . . ?
C22 C23 C24 110.95(13) . . ?
C22 C23 H23A 109.4 . . ?
C24 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C23 C24 C25 111.65(13) . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
C25 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 C20 110.59(13) . . ?
C24 C25 H25A 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C20 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C31 C26 C27 109.31(12) . . ?
C31 C26 P2 116.46(10) . . ?
C27 C26 P2 111.55(10) . . ?
C31 C26 H26 106.3 . . ?
C27 C26 H26 106.3 . . ?
P2 C26 H26 106.3 . . ?
C28 C27 C26 110.64(12) . . ?
C28 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C29 C28 C27 111.17(14) . . ?
C29 C28 H28A 109.4 . . ?
C27 C28 H28A 109.4 . . ?
C29 C28 H28B 109.4 . . ?
C27 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
C30 C29 C28 110.51(14) . . ?
C30 C29 H29A 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
C29 C30 C31 112.03(14) . . ?
C29 C30 H30A 109.2 . . ?
C31 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
C31 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 C26 110.12(13) . . ?
C30 C31 H31A 109.6 . . ?
C26 C31 H31A 109.6 . . ?
C30 C31 H31B 109.6 . . ?
C26 C31 H31B 109.6 . . ?
H31A C31 H31B 108.2 . . ?
C33 C32 C37 115.51(12) . . ?
C33 C32 B1 119.67(12) . . ?
C37 C32 B1 124.70(12) . . ?
C34 C33 C32 123.87(14) . . ?
C34 C33 H33 118.1 . . ?
C32 C33 H33 118.1 . . ?
C35 C34 C33 119.18(14) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C36 118.93(13) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C35 C36 C37 121.86(14) . . ?
C35 C36 H36 119.1 . . ?
C37 C36 H36 119.1 . . ?
C36 C37 C32 120.34(13) . . ?
C36 C37 C38 117.25(13) . . ?
C32 C37 C38 122.24(12) . . ?
C37 C38 P3 113.06(9) . . ?
C37 C38 H38A 109.0 . . ?
P3 C38 H38A 109.0 . . ?
C37 C38 H38B 109.0 . . ?
P3 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
C40 C39 C44 109.69(12) . . ?
C40 C39 P3 116.78(10) . . ?
C44 C39 P3 109.94(10) . . ?
C40 C39 H39 106.6 . . ?
C44 C39 H39 106.6 . . ?
P3 C39 H39 106.6 . . ?
C41 C40 C39 110.86(12) . . ?
C41 C40 H40A 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?
C42 C41 C40 112.18(13) . . ?
C42 C41 H41A 109.2 . . ?
C40 C41 H41A 109.2 . . ?
C42 C41 H41B 109.2 . . ?
C40 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
C43 C42 C41 111.25(13) . . ?
C43 C42 H42A 109.4 . . ?
C41 C42 H42A 109.4 . . ?
C43 C42 H42B 109.4 . . ?
C41 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
C42 C43 C44 110.77(13) . . ?
C42 C43 H43A 109.5 . . ?
C44 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
C43 C44 C39 111.19(12) . . ?
C43 C44 H44A 109.4 . . ?
C39 C44 H44A 109.4 . . ?
C43 C44 H44B 109.4 . . ?
C39 C44 H44B 109.4 . . ?
H44A C44 H44B 108.0 . . ?
C50 C45 C46 110.38(12) . . ?
C50 C45 P3 112.84(10) . . ?
C46 C45 P3 117.58(10) . . ?
C50 C45 H45 104.9 . . ?
C46 C45 H45 104.9 . . ?
P3 C45 H45 104.9 . . ?
C47 C46 C45 110.70(12) . . ?
C47 C46 H46A 109.5 . . ?
C45 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 108.1 . . ?
C48 C47 C46 111.30(13) . . ?
C48 C47 H47A 109.4 . . ?
C46 C47 H47A 109.4 . . ?
C48 C47 H47B 109.4 . . ?
C46 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
C47 C48 C49 111.15(13) . . ?
C47 C48 H48A 109.4 . . ?
C49 C48 H48A 109.4 . . ?
C47 C48 H48B 109.4 . . ?
C49 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C48 C49 C50 111.45(13) . . ?
C48 C49 H49A 109.3 . . ?
C50 C49 H49A 109.3 . . ?
C48 C49 H49B 109.3 . . ?
C50 C49 H49B 109.3 . . ?
H49A C49 H49B 108.0 . . ?
C49 C50 C45 109.52(12) . . ?
C49 C50 H50A 109.8 . . ?
C45 C50 H50A 109.8 . . ?
C49 C50 H50B 109.8 . . ?
C45 C50 H50B 109.8 . . ?
H50A C50 H50B 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C32 B1 B2 C13 143.43(13) . . . . ?
P2 B1 B2 C13 19.74(15) . . . . ?
P1 B1 B2 C13 -101.04(13) . . . . ?
C32 B1 B2 P3 12.64(15) . . . . ?
P2 B1 B2 P3 -111.04(8) . . . . ?
P1 B1 B2 P3 128.18(8) . . . . ?
C5 C4 C3 C2 -0.3(2) . . . . ?
C1 C2 C3 C4 -0.6(2) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
C4 C5 C6 C1 0.2(2) . . . . ?
C12 C7 C8 C9 0.7(2) . . . . ?
P1 C7 C8 C9 179.70(12) . . . . ?
C7 C8 C9 C10 0.4(2) . . . . ?
C8 C9 C10 C11 -0.7(2) . . . . ?
C9 C10 C11 C12 -0.2(2) . . . . ?
C10 C11 C12 C7 1.4(2) . . . . ?
C8 C7 C12 C11 -1.6(2) . . . . ?
P1 C7 C12 C11 179.32(11) . . . . ?
B1 B2 C13 C18 -32.5(2) . . . . ?
P3 B2 C13 C18 96.33(14) . . . . ?
B1 B2 C13 C14 145.49(13) . . . . ?
P3 B2 C13 C14 -85.65(14) . . . . ?
C18 C13 C14 C15 0.6(2) . . . . ?
B2 C13 C14 C15 -177.53(13) . . . . ?
C13 C14 C15 C16 -0.3(2) . . . . ?
C14 C15 C16 C17 0.1(2) . . . . ?
C15 C16 C17 C18 -0.3(2) . . . . ?
C20 P2 C19 C18 70.10(12) . . . . ?
C26 P2 C19 C18 -176.79(10) . . . . ?
B1 P2 C19 C18 -51.85(12) . . . . ?
C16 C17 C18 C13 0.7(2) . . . . ?
C16 C17 C18 C19 -176.67(14) . . . . ?
C14 C13 C18 C17 -0.8(2) . . . . ?
B2 C13 C18 C17 177.25(13) . . . . ?
C14 C13 C18 C19 176.50(12) . . . . ?
B2 C13 C18 C19 -5.4(2) . . . . ?
P2 C19 C18 C17 -133.79(13) . . . . ?
P2 C19 C18 C13 48.80(16) . . . . ?
C8 C7 P1 C1 -16.08(14) . . . . ?
C12 C7 P1 C1 162.89(11) . . . . ?
C8 C7 P1 B1 98.22(13) . . . . ?
C12 C7 P1 B1 -82.81(12) . . . . ?
C5 C6 C1 C2 -1.1(2) . . . . ?
C5 C6 C1 P1 174.68(12) . . . . ?
C3 C2 C1 C6 1.2(2) . . . . ?
C3 C2 C1 P1 -174.88(12) . . . . ?
C7 P1 C1 C6 76.19(14) . . . . ?
B1 P1 C1 C6 -28.58(15) . . . . ?
C7 P1 C1 C2 -108.03(12) . . . . ?
B1 P1 C1 C2 147.20(11) . . . . ?
C19 P2 C20 C25 31.44(13) . . . . ?
C26 P2 C20 C25 -77.63(12) . . . . ?
B1 P2 C20 C25 150.35(11) . . . . ?
C19 P2 C20 C21 160.94(10) . . . . ?
C26 P2 C20 C21 51.87(12) . . . . ?
B1 P2 C20 C21 -80.14(11) . . . . ?
C25 C20 C21 C22 -53.05(17) . . . . ?
P2 C20 C21 C22 174.42(10) . . . . ?
C20 C21 C22 C23 54.98(17) . . . . ?
C21 C22 C23 C24 -57.36(18) . . . . ?
C22 C23 C24 C25 57.95(19) . . . . ?
C23 C24 C25 C20 -55.14(18) . . . . ?
C21 C20 C25 C24 52.73(17) . . . . ?
P2 C20 C25 C24 -179.05(10) . . . . ?
C19 P2 C26 C31 -65.98(12) . . . . ?
C20 P2 C26 C31 45.66(13) . . . . ?
B1 P2 C26 C31 175.28(11) . . . . ?
C19 P2 C26 C27 60.43(11) . . . . ?
C20 P2 C26 C27 172.07(10) . . . . ?
B1 P2 C26 C27 -58.31(12) . . . . ?
C31 C26 C27 C28 -58.48(16) . . . . ?
P2 C26 C27 C28 171.28(11) . . . . ?
C26 C27 C28 C29 57.83(17) . . . . ?
C27 C28 C29 C30 -55.62(19) . . . . ?
C28 C29 C30 C31 55.5(2) . . . . ?
C29 C30 C31 C26 -57.05(19) . . . . ?
C27 C26 C31 C30 57.60(17) . . . . ?
P2 C26 C31 C30 -174.88(11) . . . . ?
B2 B1 C32 C33 -174.92(12) . . . . ?
P2 B1 C32 C33 -54.09(15) . . . . ?
P1 B1 C32 C33 61.54(13) . . . . ?
B2 B1 C32 C37 9.4(2) . . . . ?
P2 B1 C32 C37 130.22(12) . . . . ?
P1 B1 C32 C37 -114.14(13) . . . . ?
C37 C32 C33 C34 -4.8(2) . . . . ?
B1 C32 C33 C34 179.09(13) . . . . ?
C32 C33 C34 C35 0.4(2) . . . . ?
C33 C34 C35 C36 2.7(2) . . . . ?
C34 C35 C36 C37 -1.1(2) . . . . ?
C35 C36 C37 C32 -3.6(2) . . . . ?
C35 C36 C37 C38 171.74(13) . . . . ?
C33 C32 C37 C36 6.31(19) . . . . ?
B1 C32 C37 C36 -177.84(13) . . . . ?
C33 C32 C37 C38 -168.80(12) . . . . ?
B1 C32 C37 C38 7.0(2) . . . . ?
C36 C37 C38 P3 139.19(11) . . . . ?
C32 C37 C38 P3 -45.56(16) . . . . ?
C45 P3 C38 C37 -60.80(11) . . . . ?
C39 P3 C38 C37 -178.73(10) . . . . ?
B2 P3 C38 C37 61.32(11) . . . . ?
C38 P3 C39 C40 70.52(12) . . . . ?
C45 P3 C39 C40 -43.43(13) . . . . ?
B2 P3 C39 C40 -175.24(11) . . . . ?
C38 P3 C39 C44 -55.24(11) . . . . ?
C45 P3 C39 C44 -169.20(10) . . . . ?
B2 P3 C39 C44 58.99(12) . . . . ?
C44 C39 C40 C41 -55.68(17) . . . . ?
P3 C39 C40 C41 178.42(11) . . . . ?
C39 C40 C41 C42 55.21(19) . . . . ?
C40 C41 C42 C43 -54.9(2) . . . . ?
C41 C42 C43 C44 55.63(19) . . . . ?
C42 C43 C44 C39 -57.51(18) . . . . ?
C40 C39 C44 C43 57.42(16) . . . . ?
P3 C39 C44 C43 -172.88(10) . . . . ?
C38 P3 C45 C50 -169.43(10) . . . . ?
C39 P3 C45 C50 -54.31(12) . . . . ?
B2 P3 C45 C50 76.12(12) . . . . ?
C38 P3 C45 C46 -39.16(12) . . . . ?
C39 P3 C45 C46 75.96(12) . . . . ?
B2 P3 C45 C46 -153.61(11) . . . . ?
C50 C45 C46 C47 -57.47(16) . . . . ?
P3 C45 C46 C47 171.13(10) . . . . ?
C45 C46 C47 C48 55.59(17) . . . . ?
C46 C47 C48 C49 -54.84(18) . . . . ?
C47 C48 C49 C50 56.32(18) . . . . ?
C48 C49 C50 C45 -57.79(16) . . . . ?
C46 C45 C50 C49 58.17(15) . . . . ?
P3 C45 C50 C49 -168.00(10) . . . . ?

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.043

####################################################################### 
# 
# 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_alldata_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1954177'
loop_
_audit_author_name
_audit_author_address
'Tom Stennett'
;Julius Maximilians Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2019-09-17 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H48 B2 Br P3'
_chemical_formula_sum            'C34 H48 B2 Br P3'
_chemical_formula_weight         651.16

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'
Br Br -0.2901 2.4595 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   10.5062(8)
_cell_length_b                   17.5469(13)
_cell_length_c                   36.649(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6756.3(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9657
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      27.11


_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    1.280
_exptl_crystal_F_000             2736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    1.381
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6110
_exptl_absorpt_correction_T_max  0.7455
_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                   '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            108270
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.223
_diffrn_reflns_theta_max         26.022
_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             6644
_reflns_number_gt                5929
_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-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0326P)²+5.8314P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6644
_refine_ls_number_parameters     368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0727
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Br01 Br 0.32475(2) 0.28988(2) 0.46283(2) 0.01904(6) Uani 1 1 d . . . . .
B1 B 0.19155(19) 0.36570(12) 0.39199(5) 0.0121(4) Uani 1 1 d . . . . .
H3 H 0.084(2) 0.3781(12) 0.3855(6) 0.019(5) Uiso 1 1 d . . . . .
P002 P 0.26183(4) 0.45477(3) 0.36843(2) 0.01226(10) Uani 1 1 d . . . . .
B2 B 0.21727(19) 0.37837(12) 0.43954(5) 0.0127(4) Uani 1 1 d . . . . .
P003 P 0.21794(4) 0.26010(3) 0.37506(2) 0.01351(10) Uani 1 1 d . . . . .
P004 P 0.05126(5) 0.36107(3) 0.46201(2) 0.01614(11) Uani 1 1 d . . . . .
C005 C 0.26287(17) 0.52717(10) 0.43701(5) 0.0141(4) Uani 1 1 d . . . . .
C006 C 0.26755(17) 0.45817(10) 0.45651(5) 0.0128(4) Uani 1 1 d . . . . .
C007 C 0.30579(18) 0.59535(11) 0.45246(5) 0.0178(4) Uani 1 1 d . . . . .
H007 H 0.302729 0.641013 0.438564 0.021 Uiso 1 1 calc R U . . .
C008 C 0.31765(17) 0.46254(11) 0.49213(5) 0.0158(4) Uani 1 1 d . . . . .
H008 H 0.323443 0.417158 0.506163 0.019 Uiso 1 1 calc R U . . .
C009 C 0.35886(18) 0.53042(11) 0.50751(5) 0.0181(4) Uani 1 1 d . . . . .
H009 H 0.391349 0.530843 0.531700 0.022 Uiso 1 1 calc R U . . .
C00A C 0.38685(18) 0.24690(11) 0.36249(5) 0.0168(4) Uani 1 1 d . . . . .
C00B C 0.35284(18) 0.59719(12) 0.48786(5) 0.0203(4) Uani 1 1 d . . . . .
H00B H 0.380468 0.643837 0.498359 0.024 Uiso 1 1 calc R U . . .
C00C C 0.21076(18) 0.53157(10) 0.39854(5) 0.0162(4) Uani 1 1 d . . . . .
H00A H 0.237097 0.580745 0.387658 0.019 Uiso 1 1 calc R U . . .
H00C H 0.116629 0.531319 0.399771 0.019 Uiso 1 1 calc R U . . .
C00D C 0.13552(18) 0.24952(11) 0.33102(5) 0.0160(4) Uani 1 1 d . . . . .
C00E C 0.43533(17) 0.46341(11) 0.36274(5) 0.0154(4) Uani 1 1 d . . . . .
H00E H 0.457925 0.434131 0.340244 0.018 Uiso 1 1 calc R U . . .
C00F C 0.19459(18) 0.48633(11) 0.32437(5) 0.0168(4) Uani 1 1 d . . . . .
H00F H 0.233028 0.537267 0.319046 0.020 Uiso 1 1 calc R U . . .
C00G C 0.46352(19) 0.20483(11) 0.38619(6) 0.0205(4) Uani 1 1 d . . . . .
H00G H 0.426906 0.182880 0.407436 0.025 Uiso 1 1 calc R U . . .
C00H C 0.44333(19) 0.27661(11) 0.33101(5) 0.0196(4) Uani 1 1 d . . . . .
H00H H 0.392905 0.304706 0.314222 0.024 Uiso 1 1 calc R U . . .
C00I C 0.04946(19) 0.49849(13) 0.32613(5) 0.0232(4) Uani 1 1 d . . . . .
H00D H 0.006882 0.449262 0.331158 0.028 Uiso 1 1 calc R U . . .
H00I H 0.028912 0.533922 0.346310 0.028 Uiso 1 1 calc R U . . .
C00J C 0.01180(19) 0.27776(11) 0.32696(5) 0.0207(4) Uani 1 1 d . . . . .
H00J H -0.024724 0.307002 0.346092 0.025 Uiso 1 1 calc R U . . .
C00K C 0.48029(19) 0.54549(12) 0.35647(6) 0.0245(5) Uani 1 1 d . . . . .
H00K H 0.460147 0.576752 0.378205 0.029 Uiso 1 1 calc R U . . .
H00L H 0.434617 0.567481 0.335321 0.029 Uiso 1 1 calc R U . . .
C00L C 0.0519(2) 0.35199(12) 0.51128(5) 0.0255(5) Uani 1 1 d . . . . .
H00M H 0.090600 0.303236 0.518132 0.038 Uiso 1 1 calc R U . . .
H00N H -0.035749 0.353954 0.520404 0.038 Uiso 1 1 calc R U . . .
H00O H 0.101103 0.393872 0.521950 0.038 Uiso 1 1 calc R U . . .
C00M C -0.0346(2) 0.27869(12) 0.44560(6) 0.0226(4) Uani 1 1 d . . . . .
H00P H -0.050931 0.284290 0.419414 0.034 Uiso 1 1 calc R U . . .
H00Q H -0.115653 0.274360 0.458655 0.034 Uiso 1 1 calc R U . . .
H00R H 0.016336 0.232729 0.449835 0.034 Uiso 1 1 calc R U . . .
C00N C -0.04979(19) 0.44182(12) 0.45295(6) 0.0257(5) Uani 1 1 d . . . . .
H00S H -0.068060 0.444480 0.426762 0.039 Uiso 1 1 calc R U . . .
H00T H -0.006620 0.488637 0.460667 0.039 Uiso 1 1 calc R U . . .
H00U H -0.129678 0.436287 0.466503 0.039 Uiso 1 1 calc R U . . .
C00O C 0.50964(17) 0.42681(11) 0.39435(5) 0.0176(4) Uani 1 1 d . . . . .
H00V H 0.490286 0.454201 0.417308 0.021 Uiso 1 1 calc R U . . .
H00W H 0.482496 0.373138 0.397300 0.021 Uiso 1 1 calc R U . . .
C00P C 0.65271(18) 0.42963(13) 0.38716(6) 0.0228(4) Uani 1 1 d . . . . .
H00X H 0.698558 0.407944 0.408347 0.027 Uiso 1 1 calc R U . . .
H00Y H 0.672893 0.398054 0.365532 0.027 Uiso 1 1 calc R U . . .
C00Q C 0.22880(19) 0.43464(12) 0.29212(5) 0.0218(4) Uani 1 1 d . . . . .
H00Z H 0.322422 0.428949 0.290700 0.026 Uiso 1 1 calc R U . . .
H010 H 0.191460 0.383473 0.295993 0.026 Uiso 1 1 calc R U . . .
C00R C 0.1837(2) 0.20488(11) 0.30259(5) 0.0211(4) Uani 1 1 d . . . . .
H011 H 0.266435 0.183549 0.304755 0.025 Uiso 1 1 calc R U . . .
C00S C 0.5717(2) 0.26577(12) 0.32387(6) 0.0262(5) Uani 1 1 d . . . . .
H012 H 0.608256 0.286326 0.302302 0.031 Uiso 1 1 calc R U . . .
C00U C -0.0592(2) 0.26401(13) 0.29550(6) 0.0268(5) Uani 1 1 d . . . . .
H013 H -0.142532 0.284438 0.293250 0.032 Uiso 1 1 calc R U . . .
C00V C 0.6242(2) 0.54766(14) 0.34932(6) 0.0315(5) Uani 1 1 d . . . . .
H014 H 0.643227 0.520314 0.326331 0.038 Uiso 1 1 calc R U . . .
H015 H 0.651967 0.601232 0.346413 0.038 Uiso 1 1 calc R U . . .
C00W C 0.1127(2) 0.19101(13) 0.27113(6) 0.0279(5) Uani 1 1 d . . . . .
H016 H 0.147909 0.161013 0.252046 0.034 Uiso 1 1 calc R U . . .
C00X C 0.6981(2) 0.51092(13) 0.38061(6) 0.0283(5) Uani 1 1 d . . . . .
H017 H 0.790064 0.510522 0.374672 0.034 Uiso 1 1 calc R U . . .
H018 H 0.686246 0.541313 0.403114 0.034 Uiso 1 1 calc R U . . .
C00Y C -0.0001(2) 0.53121(13) 0.29014(6) 0.0295(5) Uani 1 1 d . . . . .
H019 H -0.093833 0.536077 0.291417 0.035 Uiso 1 1 calc R U . . .
H01A H 0.035968 0.582775 0.286471 0.035 Uiso 1 1 calc R U . . .
C00Z C 0.1790(2) 0.46785(14) 0.25628(6) 0.0293(5) Uani 1 1 d . . . . .
H01B H 0.222515 0.516793 0.251267 0.035 Uiso 1 1 calc R U . . .
H01C H 0.198822 0.432402 0.236044 0.035 Uiso 1 1 calc R U . . .
C010 C 0.5927(2) 0.19444(12) 0.37927(6) 0.0277(5) Uani 1 1 d . . . . .
H01D H 0.643661 0.166336 0.395922 0.033 Uiso 1 1 calc R U . . .
C012 C -0.0083(2) 0.22065(13) 0.26757(6) 0.0300(5) Uani 1 1 d . . . . .
H01E H -0.056381 0.211335 0.246070 0.036 Uiso 1 1 calc R U . . .
C013 C 0.6468(2) 0.22511(13) 0.34807(7) 0.0298(5) Uani 1 1 d . . . . .
H01F H 0.734986 0.218283 0.343300 0.036 Uiso 1 1 calc R U . . .
C014 C 0.0353(2) 0.48105(14) 0.25788(6) 0.0310(5) Uani 1 1 d . . . . .
H01G H 0.006772 0.505654 0.234990 0.037 Uiso 1 1 calc R U . . .
H01H H -0.008840 0.431415 0.260042 0.037 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
Br01 B2 2.101(2) . ?
B1 B2 1.777(3) . ?
B1 P002 1.932(2) . ?
B1 P003 1.974(2) . ?
B1 H3 1.18(2) . ?
P002 C00C 1.8225(19) . ?
P002 C00E 1.8411(19) . ?
P002 C00F 1.8477(18) . ?
B2 C006 1.621(3) . ?
B2 P004 1.953(2) . ?
P003 C00D 1.8411(18) . ?
P003 C00A 1.8481(19) . ?
P004 C00N 1.801(2) . ?
P004 C00M 1.807(2) . ?
P004 C00L 1.813(2) . ?
C005 C007 1.398(3) . ?
C005 C006 1.407(3) . ?
C005 C00C 1.515(2) . ?
C006 C008 1.410(2) . ?
C007 C00B 1.388(3) . ?
C007 H007 0.9500 . ?
C008 C009 1.387(3) . ?
C008 H008 0.9500 . ?
C009 C00B 1.377(3) . ?
C009 H009 0.9500 . ?
C00A C00G 1.396(3) . ?
C00A C00H 1.398(3) . ?
C00B H00B 0.9500 . ?
C00C H00A 0.9900 . ?
C00C H00C 0.9900 . ?
C00D C00R 1.398(3) . ?
C00D C00J 1.399(3) . ?
C00E C00K 1.533(3) . ?
C00E C00O 1.538(2) . ?
C00E H00E 1.0000 . ?
C00F C00Q 1.532(3) . ?
C00F C00I 1.541(3) . ?
C00F H00F 1.0000 . ?
C00G C010 1.393(3) . ?
C00G H00G 0.9500 . ?
C00H C00S 1.387(3) . ?
C00H H00H 0.9500 . ?
C00I C00Y 1.530(3) . ?
C00I H00D 0.9900 . ?
C00I H00I 0.9900 . ?
C00J C00U 1.394(3) . ?
C00J H00J 0.9500 . ?
C00K C00V 1.535(3) . ?
C00K H00K 0.9900 . ?
C00K H00L 0.9900 . ?
C00L H00M 0.9800 . ?
C00L H00N 0.9800 . ?
C00L H00O 0.9800 . ?
C00M H00P 0.9800 . ?
C00M H00Q 0.9800 . ?
C00M H00R 0.9800 . ?
C00N H00S 0.9800 . ?
C00N H00T 0.9800 . ?
C00N H00U 0.9800 . ?
C00O C00P 1.527(3) . ?
C00O H00V 0.9900 . ?
C00O H00W 0.9900 . ?
C00P C00X 1.523(3) . ?
C00P H00X 0.9900 . ?
C00P H00Y 0.9900 . ?
C00Q C00Z 1.529(3) . ?
C00Q H00Z 0.9900 . ?
C00Q H010 0.9900 . ?
C00R C00W 1.394(3) . ?
C00R H011 0.9500 . ?
C00S C013 1.385(3) . ?
C00S H012 0.9500 . ?
C00U C012 1.383(3) . ?
C00U H013 0.9500 . ?
C00V C00X 1.528(3) . ?
C00V H014 0.9900 . ?
C00V H015 0.9900 . ?
C00W C012 1.380(3) . ?
C00W H016 0.9500 . ?
C00X H017 0.9900 . ?
C00X H018 0.9900 . ?
C00Y C014 1.520(3) . ?
C00Y H019 0.9900 . ?
C00Y H01A 0.9900 . ?
C00Z C014 1.528(3) . ?
C00Z H01B 0.9900 . ?
C00Z H01C 0.9900 . ?
C010 C013 1.386(3) . ?
C010 H01D 0.9500 . ?
C012 H01E 0.9500 . ?
C013 H01F 0.9500 . ?
C014 H01G 0.9900 . ?
C014 H01H 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
B2 B1 P002 106.19(12) . . ?
B2 B1 P003 113.84(12) . . ?
P002 B1 P003 124.42(10) . . ?
B2 B1 H3 108.7(10) . . ?
P002 B1 H3 97.3(10) . . ?
P003 B1 H3 104.2(10) . . ?
C00C P002 C00E 107.41(9) . . ?
C00C P002 C00F 101.24(9) . . ?
C00E P002 C00F 104.76(8) . . ?
C00C P002 B1 102.42(9) . . ?
C00E P002 B1 119.72(9) . . ?
C00F P002 B1 119.14(9) . . ?
C006 B2 B1 122.27(15) . . ?
C006 B2 P004 105.27(12) . . ?
B1 B2 P004 104.97(12) . . ?
C006 B2 Br01 107.90(12) . . ?
B1 B2 Br01 112.82(12) . . ?
P004 B2 Br01 101.17(9) . . ?
C00D P003 C00A 102.73(9) . . ?
C00D P003 B1 107.71(9) . . ?
C00A P003 B1 109.33(8) . . ?
C00N P004 C00M 105.89(10) . . ?
C00N P004 C00L 104.76(10) . . ?
C00M P004 C00L 105.25(10) . . ?
C00N P004 B2 109.05(9) . . ?
C00M P004 B2 115.45(9) . . ?
C00L P004 B2 115.51(9) . . ?
C007 C005 C006 121.29(17) . . ?
C007 C005 C00C 116.74(17) . . ?
C006 C005 C00C 121.96(16) . . ?
C005 C006 C008 115.88(17) . . ?
C005 C006 B2 122.50(15) . . ?
C008 C006 B2 121.61(16) . . ?
C00B C007 C005 120.86(18) . . ?
C00B C007 H007 119.6 . . ?
C005 C007 H007 119.6 . . ?
C009 C008 C006 122.67(18) . . ?
C009 C008 H008 118.7 . . ?
C006 C008 H008 118.7 . . ?
C00B C009 C008 120.24(17) . . ?
C00B C009 H009 119.9 . . ?
C008 C009 H009 119.9 . . ?
C00G C00A C00H 117.76(18) . . ?
C00G C00A P003 117.72(15) . . ?
C00H C00A P003 124.52(15) . . ?
C009 C00B C007 119.04(18) . . ?
C009 C00B H00B 120.5 . . ?
C007 C00B H00B 120.5 . . ?
C005 C00C P002 114.80(13) . . ?
C005 C00C H00A 108.6 . . ?
P002 C00C H00A 108.6 . . ?
C005 C00C H00C 108.6 . . ?
P002 C00C H00C 108.6 . . ?
H00A C00C H00C 107.5 . . ?
C00R C00D C00J 117.07(17) . . ?
C00R C00D P003 122.66(15) . . ?
C00J C00D P003 119.65(14) . . ?
C00K C00E C00O 110.42(15) . . ?
C00K C00E P002 113.55(13) . . ?
C00O C00E P002 112.51(13) . . ?
C00K C00E H00E 106.6 . . ?
C00O C00E H00E 106.6 . . ?
P002 C00E H00E 106.6 . . ?
C00Q C00F C00I 110.27(16) . . ?
C00Q C00F P002 114.02(13) . . ?
C00I C00F P002 112.52(13) . . ?
C00Q C00F H00F 106.5 . . ?
C00I C00F H00F 106.5 . . ?
P002 C00F H00F 106.5 . . ?
C010 C00G C00A 121.2(2) . . ?
C010 C00G H00G 119.4 . . ?
C00A C00G H00G 119.4 . . ?
C00S C00H C00A 121.15(19) . . ?
C00S C00H H00H 119.4 . . ?
C00A C00H H00H 119.4 . . ?
C00Y C00I C00F 110.63(17) . . ?
C00Y C00I H00D 109.5 . . ?
C00F C00I H00D 109.5 . . ?
C00Y C00I H00I 109.5 . . ?
C00F C00I H00I 109.5 . . ?
H00D C00I H00I 108.1 . . ?
C00U C00J C00D 121.58(19) . . ?
C00U C00J H00J 119.2 . . ?
C00D C00J H00J 119.2 . . ?
C00E C00K C00V 110.63(18) . . ?
C00E C00K H00K 109.5 . . ?
C00V C00K H00K 109.5 . . ?
C00E C00K H00L 109.5 . . ?
C00V C00K H00L 109.5 . . ?
H00K C00K H00L 108.1 . . ?
P004 C00L H00M 109.5 . . ?
P004 C00L H00N 109.5 . . ?
H00M C00L H00N 109.5 . . ?
P004 C00L H00O 109.5 . . ?
H00M C00L H00O 109.5 . . ?
H00N C00L H00O 109.5 . . ?
P004 C00M H00P 109.5 . . ?
P004 C00M H00Q 109.5 . . ?
H00P C00M H00Q 109.5 . . ?
P004 C00M H00R 109.5 . . ?
H00P C00M H00R 109.5 . . ?
H00Q C00M H00R 109.5 . . ?
P004 C00N H00S 109.5 . . ?
P004 C00N H00T 109.5 . . ?
H00S C00N H00T 109.5 . . ?
P004 C00N H00U 109.5 . . ?
H00S C00N H00U 109.5 . . ?
H00T C00N H00U 109.5 . . ?
C00P C00O C00E 110.86(16) . . ?
C00P C00O H00V 109.5 . . ?
C00E C00O H00V 109.5 . . ?
C00P C00O H00W 109.5 . . ?
C00E C00O H00W 109.5 . . ?
H00V C00O H00W 108.1 . . ?
C00X C00P C00O 111.48(17) . . ?
C00X C00P H00X 109.3 . . ?
C00O C00P H00X 109.3 . . ?
C00X C00P H00Y 109.3 . . ?
C00O C00P H00Y 109.3 . . ?
H00X C00P H00Y 108.0 . . ?
C00Z C00Q C00F 110.89(17) . . ?
C00Z C00Q H00Z 109.5 . . ?
C00F C00Q H00Z 109.5 . . ?
C00Z C00Q H010 109.5 . . ?
C00F C00Q H010 109.5 . . ?
H00Z C00Q H010 108.0 . . ?
C00W C00R C00D 121.4(2) . . ?
C00W C00R H011 119.3 . . ?
C00D C00R H011 119.3 . . ?
C013 C00S C00H 120.3(2) . . ?
C013 C00S H012 119.9 . . ?
C00H C00S H012 119.9 . . ?
C012 C00U C00J 120.1(2) . . ?
C012 C00U H013 120.0 . . ?
C00J C00U H013 120.0 . . ?
C00X C00V C00K 111.24(18) . . ?
C00X C00V H014 109.4 . . ?
C00K C00V H014 109.4 . . ?
C00X C00V H015 109.4 . . ?
C00K C00V H015 109.4 . . ?
H014 C00V H015 108.0 . . ?
C012 C00W C00R 120.3(2) . . ?
C012 C00W H016 119.8 . . ?
C00R C00W H016 119.8 . . ?
C00P C00X C00V 110.73(17) . . ?
C00P C00X H017 109.5 . . ?
C00V C00X H017 109.5 . . ?
C00P C00X H018 109.5 . . ?
C00V C00X H018 109.5 . . ?
H017 C00X H018 108.1 . . ?
C014 C00Y C00I 111.73(18) . . ?
C014 C00Y H019 109.3 . . ?
C00I C00Y H019 109.3 . . ?
C014 C00Y H01A 109.3 . . ?
C00I C00Y H01A 109.3 . . ?
H019 C00Y H01A 107.9 . . ?
C014 C00Z C00Q 111.26(17) . . ?
C014 C00Z H01B 109.4 . . ?
C00Q C00Z H01B 109.4 . . ?
C014 C00Z H01C 109.4 . . ?
C00Q C00Z H01C 109.4 . . ?
H01B C00Z H01C 108.0 . . ?
C013 C010 C00G 120.0(2) . . ?
C013 C010 H01D 120.0 . . ?
C00G C010 H01D 120.0 . . ?
C00W C012 C00U 119.56(19) . . ?
C00W C012 H01E 120.2 . . ?
C00U C012 H01E 120.2 . . ?
C00S C013 C010 119.6(2) . . ?
C00S C013 H01F 120.2 . . ?
C010 C013 H01F 120.2 . . ?
C00Y C014 C00Z 111.05(18) . . ?
C00Y C014 H01G 109.4 . . ?
C00Z C014 H01G 109.4 . . ?
C00Y C014 H01H 109.4 . . ?
C00Z C014 H01H 109.4 . . ?
H01G C014 H01H 108.0 . . ?

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
P002 B1 B2 C006 9.5(2) . . . . ?
P003 B1 B2 C006 150.07(14) . . . . ?
P002 B1 B2 P004 128.98(10) . . . . ?
P003 B1 B2 P004 -90.50(13) . . . . ?
P002 B1 B2 Br01 -121.75(11) . . . . ?
P003 B1 B2 Br01 18.77(16) . . . . ?
C007 C005 C006 C008 0.0(3) . . . . ?
C00C C005 C006 C008 -179.62(16) . . . . ?
C007 C005 C006 B2 179.37(17) . . . . ?
C00C C005 C006 B2 -0.3(3) . . . . ?
B1 B2 C006 C005 16.8(3) . . . . ?
P004 B2 C006 C005 -102.45(17) . . . . ?
Br01 B2 C006 C005 150.14(14) . . . . ?
B1 B2 C006 C008 -163.85(16) . . . . ?
P004 B2 C006 C008 76.86(18) . . . . ?
Br01 B2 C006 C008 -30.5(2) . . . . ?
C006 C005 C007 C00B -0.9(3) . . . . ?
C00C C005 C007 C00B 178.73(17) . . . . ?
C005 C006 C008 C009 0.7(3) . . . . ?
B2 C006 C008 C009 -178.65(17) . . . . ?
C006 C008 C009 C00B -0.5(3) . . . . ?
C00D P003 C00A C00G -139.98(15) . . . . ?
B1 P003 C00A C00G 105.84(16) . . . . ?
C00D P003 C00A C00H 40.51(18) . . . . ?
B1 P003 C00A C00H -73.67(18) . . . . ?
C008 C009 C00B C007 -0.4(3) . . . . ?
C005 C007 C00B C009 1.1(3) . . . . ?
C007 C005 C00C P002 137.13(15) . . . . ?
C006 C005 C00C P002 -43.2(2) . . . . ?
C00E P002 C00C C005 -64.44(15) . . . . ?
C00F P002 C00C C005 -173.98(14) . . . . ?
B1 P002 C00C C005 62.50(15) . . . . ?
C00A P003 C00D C00R 28.41(18) . . . . ?
B1 P003 C00D C00R 143.77(16) . . . . ?
C00A P003 C00D C00J -160.89(15) . . . . ?
B1 P003 C00D C00J -45.53(17) . . . . ?
C00C P002 C00E C00K -43.66(16) . . . . ?
C00F P002 C00E C00K 63.43(15) . . . . ?
B1 P002 C00E C00K -159.67(13) . . . . ?
C00C P002 C00E C00O 82.68(15) . . . . ?
C00F P002 C00E C00O -170.23(13) . . . . ?
B1 P002 C00E C00O -33.33(17) . . . . ?
C00C P002 C00F C00Q 176.49(14) . . . . ?
C00E P002 C00F C00Q 64.91(15) . . . . ?
B1 P002 C00F C00Q -72.29(16) . . . . ?
C00C P002 C00F C00I -56.97(16) . . . . ?
C00E P002 C00F C00I -168.55(14) . . . . ?
B1 P002 C00F C00I 54.25(18) . . . . ?
C00H C00A C00G C010 1.7(3) . . . . ?
P003 C00A C00G C010 -177.88(16) . . . . ?
C00G C00A C00H C00S -1.1(3) . . . . ?
P003 C00A C00H C00S 178.43(16) . . . . ?
C00Q C00F C00I C00Y -56.5(2) . . . . ?
P002 C00F C00I C00Y 175.02(15) . . . . ?
C00R C00D C00J C00U -1.9(3) . . . . ?
P003 C00D C00J C00U -173.10(16) . . . . ?
C00O C00E C00K C00V 56.5(2) . . . . ?
P002 C00E C00K C00V -176.07(14) . . . . ?
C00K C00E C00O C00P -56.5(2) . . . . ?
P002 C00E C00O C00P 175.54(14) . . . . ?
C00E C00O C00P C00X 56.4(2) . . . . ?
C00I C00F C00Q C00Z 56.9(2) . . . . ?
P002 C00F C00Q C00Z -175.41(14) . . . . ?
C00J C00D C00R C00W 1.8(3) . . . . ?
P003 C00D C00R C00W 172.74(16) . . . . ?
C00A C00H C00S C013 -0.1(3) . . . . ?
C00D C00J C00U C012 0.9(3) . . . . ?
C00E C00K C00V C00X -56.6(2) . . . . ?
C00D C00R C00W C012 -0.8(3) . . . . ?
C00O C00P C00X C00V -56.0(2) . . . . ?
C00K C00V C00X C00P 56.0(3) . . . . ?
C00F C00I C00Y C014 56.1(2) . . . . ?
C00F C00Q C00Z C014 -56.5(2) . . . . ?
C00A C00G C010 C013 -1.0(3) . . . . ?
C00R C00W C012 C00U -0.3(3) . . . . ?
C00J C00U C012 C00W 0.2(3) . . . . ?
C00H C00S C013 C010 0.8(3) . . . . ?
C00G C010 C013 C00S -0.2(3) . . . . ?
C00I C00Y C014 C00Z -55.4(2) . . . . ?
C00Q C00Z C014 C00Y 55.4(3) . . . . ?

_refine_diff_density_max         0.635
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.055

####################################################################### 
# 
# 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_eee_a
_database_code_depnum_ccdc_archive 'CCDC 1954179'
loop_
_audit_author_name
_audit_author_address
'Tom Stennett'
;Julius Maximilians Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2019-09-17 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H48 B2 Br P3'
_chemical_formula_sum            'C34 H48 B2 Br P3'
_chemical_formula_weight         651.16

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.8091(5)
_cell_length_b                   16.5734(7)
_cell_length_c                   17.4767(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.828(2)
_cell_angle_gamma                90
_cell_volume                     3256.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9946
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      27.05


_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    1.328
_exptl_crystal_F_000             1368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    1.433
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6566
_exptl_absorpt_correction_T_max  0.7455
_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            28879
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.448
_diffrn_reflns_theta_max         26.022
_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             6411
_reflns_number_gt                5045
_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-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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6411
_refine_ls_number_parameters     368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1289
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_restrained_S_all      0.900
_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
Br1 Br 0.13630(2) 0.63828(2) 0.60087(2) 0.02395(12) Uani 1 1 d . . . . .
P1 P 0.35169(7) 0.63295(5) 0.50994(4) 0.01801(18) Uani 1 1 d . . . . .
C1 C 0.2885(2) 0.49222(18) 0.59030(15) 0.0181(6) Uani 1 1 d . . . . .
B1 B 0.3042(3) 0.5892(2) 0.60138(18) 0.0190(7) Uani 1 1 d . . . . .
P2 P 0.54307(6) 0.54034(5) 0.71298(4) 0.01697(17) Uani 1 1 d . . . . .
C2 C 0.1779(3) 0.45130(19) 0.56919(17) 0.0230(7) Uani 1 1 d . . . . .
H2 H 0.108172 0.482027 0.564327 0.028 Uiso 1 1 calc R U . . .
B2 B 0.4210(3) 0.6229(2) 0.68727(19) 0.0193(7) Uani 1 1 d . . . . .
H1 H 0.469(3) 0.6755(19) 0.6743(19) 0.025(8) Uiso 1 1 d . . . . .
C3 C 0.1659(3) 0.36956(19) 0.55533(18) 0.0251(7) Uani 1 1 d . . . . .
H3 H 0.089204 0.345502 0.540679 0.030 Uiso 1 1 calc R U . . .
P3 P 0.37439(7) 0.66853(5) 0.77503(4) 0.02003(18) Uani 1 1 d . . . . .
C4 C 0.2660(3) 0.32203(19) 0.56276(17) 0.0247(7) Uani 1 1 d . . . . .
H00M H 0.258560 0.265706 0.552365 0.030 Uiso 1 1 calc R U . . .
C6 C 0.3888(3) 0.44197(18) 0.59910(16) 0.0198(6) Uani 1 1 d . . . . .
C5 C 0.3773(3) 0.35897(18) 0.58577(17) 0.0220(6) Uani 1 1 d . . . . .
H5 H 0.446503 0.327097 0.592502 0.026 Uiso 1 1 calc R U . . .
C7 C 0.5122(2) 0.47656(18) 0.62454(17) 0.0207(6) Uani 1 1 d . . . . .
H00T H 0.523521 0.508532 0.579575 0.025 Uiso 1 1 calc R U . . .
H00U H 0.570391 0.431703 0.635680 0.025 Uiso 1 1 calc R U . . .
C9 C 0.6473(3) 0.41329(19) 0.82203(18) 0.0243(7) Uani 1 1 d . . . . .
H00P H 0.724806 0.438925 0.826442 0.029 Uiso 1 1 calc R U . . .
H00Q H 0.631232 0.372325 0.778793 0.029 Uiso 1 1 calc R U . . .
C10 C 0.6533(3) 0.3723(2) 0.9018(2) 0.0301(8) Uani 1 1 d . . . . .
H01H H 0.713224 0.328551 0.912576 0.036 Uiso 1 1 calc R U . . .
H01I H 0.679340 0.412190 0.945891 0.036 Uiso 1 1 calc R U . . .
C20 C 0.3677(3) 0.74355(18) 0.52198(16) 0.0202(6) Uani 1 1 d . . . . .
C21 C 0.4812(3) 0.77826(19) 0.53687(16) 0.0227(6) Uani 1 1 d . . . . .
H21 H 0.547866 0.744246 0.542069 0.027 Uiso 1 1 calc R U . . .
C22 C 0.4976(3) 0.86103(19) 0.54411(18) 0.0266(7) Uani 1 1 d . . . . .
H00O H 0.575376 0.882811 0.554983 0.032 Uiso 1 1 calc R U . . .
C23 C 0.4017(3) 0.91253(19) 0.53563(17) 0.0253(7) Uani 1 1 d . . . . .
H014 H 0.412826 0.969316 0.539919 0.030 Uiso 1 1 calc R U . . .
C24 C 0.2893(3) 0.8791(2) 0.52076(18) 0.0278(7) Uani 1 1 d . . . . .
H015 H 0.222930 0.913569 0.514825 0.033 Uiso 1 1 calc R U . . .
C25 C 0.2720(3) 0.79639(19) 0.51439(17) 0.0229(6) Uani 1 1 d . . . . .
H00N H 0.194181 0.775128 0.504744 0.027 Uiso 1 1 calc R U . . .
C26 C 0.2279(3) 0.62711(18) 0.41511(17) 0.0200(6) Uani 1 1 d . . . . .
C27 C 0.2398(3) 0.66928(19) 0.34821(17) 0.0214(6) Uani 1 1 d . . . . .
H27 H 0.306283 0.703806 0.354580 0.026 Uiso 1 1 calc R U . . .
C28 C 0.1557(3) 0.66134(19) 0.27260(17) 0.0234(7) Uani 1 1 d . . . . .
H28 H 0.164646 0.690981 0.228296 0.028 Uiso 1 1 calc R U . . .
C29 C 0.0592(3) 0.61046(19) 0.26194(17) 0.0235(6) Uani 1 1 d . . . . .
H29 H 0.002575 0.604351 0.210311 0.028 Uiso 1 1 calc R U . . .
C30 C 0.0460(3) 0.56849(19) 0.32724(17) 0.0236(7) Uani 1 1 d . . . . .
H30 H -0.020123 0.533546 0.320330 0.028 Uiso 1 1 calc R U . . .
C31 C 0.1293(3) 0.57724(19) 0.40313(17) 0.0223(6) Uani 1 1 d . . . . .
H31 H 0.118460 0.548574 0.447424 0.027 Uiso 1 1 calc R U . . .
C32 C 0.2706(3) 0.6147(2) 0.81458(19) 0.0279(7) Uani 1 1 d . . . . .
H00V H 0.207838 0.590574 0.770105 0.042 Uiso 1 1 calc R U . . .
H00W H 0.235090 0.652311 0.843935 0.042 Uiso 1 1 calc R U . . .
H00X H 0.312923 0.572018 0.851057 0.042 Uiso 1 1 calc R U . . .
C33 C 0.3063(3) 0.76574(19) 0.74452(18) 0.0250(7) Uani 1 1 d . . . . .
H00Y H 0.351530 0.795116 0.714879 0.037 Uiso 1 1 calc R U . . .
H00Z H 0.306035 0.796740 0.792221 0.037 Uiso 1 1 calc R U . . .
H010 H 0.224305 0.758104 0.709902 0.037 Uiso 1 1 calc R U . . .
C34 C 0.4960(3) 0.6920(2) 0.86362(18) 0.0277(7) Uani 1 1 d . . . . .
H016 H 0.552779 0.727194 0.848998 0.041 Uiso 1 1 calc R U . . .
H017 H 0.535891 0.642020 0.887251 0.041 Uiso 1 1 calc R U . . .
H018 H 0.465300 0.719617 0.902781 0.041 Uiso 1 1 calc R U . . .
C12 C 0.4349(3) 0.3992(2) 0.87537(18) 0.0280(7) Uani 1 1 d . . . . .
H01D H 0.449143 0.442169 0.916584 0.034 Uiso 1 1 calc R U . . .
H01E H 0.357692 0.373383 0.871431 0.034 Uiso 1 1 calc R U . . .
C11 C 0.5329(3) 0.3371(2) 0.9007(2) 0.0301(7) Uani 1 1 d . . . . .
H01F H 0.513301 0.290890 0.863017 0.036 Uiso 1 1 calc R U . . .
H01G H 0.538268 0.316844 0.954967 0.036 Uiso 1 1 calc R U . . .
C8 C 0.5490(2) 0.47734(18) 0.80066(17) 0.0197(6) Uani 1 1 d . . . . .
H013 H 0.566286 0.514720 0.847748 0.024 Uiso 1 1 calc R U . . .
C13 C 0.4292(3) 0.43638(19) 0.79464(18) 0.0233(7) Uani 1 1 d . . . . .
H00R H 0.364382 0.476724 0.779119 0.028 Uiso 1 1 calc R U . . .
H00S H 0.412213 0.393916 0.752814 0.028 Uiso 1 1 calc R U . . .
C14 C 0.6975(2) 0.57081(18) 0.72573(16) 0.0187(6) Uani 1 1 d . . . . .
H14 H 0.742508 0.520269 0.723267 0.022 Uiso 1 1 calc R U . . .
C15 C 0.7603(3) 0.61037(19) 0.80705(17) 0.0222(6) Uani 1 1 d . . . . .
H15 H 0.720079 0.661780 0.811516 0.027 Uiso 1 1 calc R U . . .
H00L H 0.754754 0.574407 0.851001 0.027 Uiso 1 1 calc R U . . .
C18 C 0.8394(3) 0.64217(18) 0.66546(17) 0.0212(6) Uani 1 1 d . . . . .
H011 H 0.844213 0.679648 0.622449 0.025 Uiso 1 1 calc R U . . .
H012 H 0.878611 0.591040 0.658648 0.025 Uiso 1 1 calc R U . . .
C17 C 0.9051(3) 0.6788(2) 0.74721(17) 0.0245(7) Uani 1 1 d . . . . .
H01B H 0.873440 0.733465 0.750918 0.029 Uiso 1 1 calc R U . . .
H01C H 0.990595 0.683989 0.752370 0.029 Uiso 1 1 calc R U . . .
C16 C 0.8909(3) 0.62673(19) 0.81584(18) 0.0256(7) Uani 1 1 d . . . . .
H019 H 0.932653 0.574764 0.816723 0.031 Uiso 1 1 calc R U . . .
H01A H 0.928437 0.654429 0.867610 0.031 Uiso 1 1 calc R U . . .
C19 C 0.7091(3) 0.62570(18) 0.65715(17) 0.0206(6) Uani 1 1 d . . . . .
H00B H 0.670479 0.599392 0.604784 0.025 Uiso 1 1 calc R U . . .
H19 H 0.667747 0.677430 0.658303 0.025 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
Br1 B1 2.140(3) . ?
P1 C26 1.846(3) . ?
P1 C20 1.848(3) . ?
P1 B1 1.986(3) . ?
C1 C2 1.416(4) . ?
C1 C6 1.417(4) . ?
C1 B1 1.623(5) . ?
B1 B2 1.789(5) . ?
P2 C7 1.815(3) . ?
P2 C8 1.838(3) . ?
P2 C14 1.839(3) . ?
P2 B2 1.938(3) . ?
C2 C3 1.376(4) . ?
C2 H2 0.9500 . ?
B2 P3 1.935(3) . ?
B2 H1 1.10(3) . ?
C3 C4 1.393(5) . ?
C3 H3 0.9500 . ?
P3 C34 1.802(3) . ?
P3 C33 1.807(3) . ?
P3 C32 1.815(3) . ?
C4 C5 1.392(4) . ?
C4 H00M 0.9500 . ?
C6 C5 1.395(4) . ?
C6 C7 1.502(4) . ?
C5 H5 0.9500 . ?
C7 H00T 0.9900 . ?
C7 H00U 0.9900 . ?
C9 C8 1.532(4) . ?
C9 C10 1.533(4) . ?
C9 H00P 0.9900 . ?
C9 H00Q 0.9900 . ?
C10 C11 1.532(4) . ?
C10 H01H 0.9900 . ?
C10 H01I 0.9900 . ?
C20 C25 1.403(4) . ?
C20 C21 1.408(4) . ?
C21 C22 1.386(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.389(5) . ?
C22 H00O 0.9500 . ?
C23 C24 1.388(5) . ?
C23 H014 0.9500 . ?
C24 C25 1.385(5) . ?
C24 H015 0.9500 . ?
C25 H00N 0.9500 . ?
C26 C31 1.390(4) . ?
C26 C27 1.406(4) . ?
C27 C28 1.395(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.383(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.386(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.396(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H00V 0.9800 . ?
C32 H00W 0.9800 . ?
C32 H00X 0.9800 . ?
C33 H00Y 0.9800 . ?
C33 H00Z 0.9800 . ?
C33 H010 0.9800 . ?
C34 H016 0.9800 . ?
C34 H017 0.9800 . ?
C34 H018 0.9800 . ?
C12 C11 1.510(5) . ?
C12 C13 1.522(4) . ?
C12 H01D 0.9900 . ?
C12 H01E 0.9900 . ?
C11 H01F 0.9900 . ?
C11 H01G 0.9900 . ?
C8 C13 1.543(4) . ?
C8 H013 1.0000 . ?
C13 H00R 0.9900 . ?
C13 H00S 0.9900 . ?
C14 C15 1.534(4) . ?
C14 C19 1.544(4) . ?
C14 H14 1.0000 . ?
C15 C16 1.527(4) . ?
C15 H15 0.9900 . ?
C15 H00L 0.9900 . ?
C18 C19 1.525(4) . ?
C18 C17 1.527(4) . ?
C18 H011 0.9900 . ?
C18 H012 0.9900 . ?
C17 C16 1.528(4) . ?
C17 H01B 0.9900 . ?
C17 H01C 0.9900 . ?
C16 H019 0.9900 . ?
C16 H01A 0.9900 . ?
C19 H00B 0.9900 . ?
C19 H19 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
C26 P1 C20 100.33(13) . . ?
C26 P1 B1 111.24(13) . . ?
C20 P1 B1 108.33(13) . . ?
C2 C1 C6 114.8(3) . . ?
C2 C1 B1 124.6(3) . . ?
C6 C1 B1 120.5(2) . . ?
C1 B1 B2 116.1(2) . . ?
C1 B1 P1 108.39(19) . . ?
B2 B1 P1 103.08(19) . . ?
C1 B1 Br1 107.71(19) . . ?
B2 B1 Br1 111.12(19) . . ?
P1 B1 Br1 110.34(15) . . ?
C7 P2 C8 109.01(14) . . ?
C7 P2 C14 101.30(13) . . ?
C8 P2 C14 105.76(13) . . ?
C7 P2 B2 105.82(14) . . ?
C8 P2 B2 115.49(14) . . ?
C14 P2 B2 118.29(14) . . ?
C3 C2 C1 123.7(3) . . ?
C3 C2 H2 118.2 . . ?
C1 C2 H2 118.2 . . ?
B1 B2 P3 117.0(2) . . ?
B1 B2 P2 107.6(2) . . ?
P3 B2 P2 117.65(17) . . ?
B1 B2 H1 112.8(16) . . ?
P3 B2 H1 98.2(17) . . ?
P2 B2 H1 102.3(16) . . ?
C2 C3 C4 120.1(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C34 P3 C33 103.09(15) . . ?
C34 P3 C32 103.42(15) . . ?
C33 P3 C32 105.04(15) . . ?
C34 P3 B2 114.86(14) . . ?
C33 P3 B2 108.88(14) . . ?
C32 P3 B2 119.90(15) . . ?
C5 C4 C3 118.5(3) . . ?
C5 C4 H00M 120.8 . . ?
C3 C4 H00M 120.8 . . ?
C5 C6 C1 121.7(3) . . ?
C5 C6 C7 117.5(3) . . ?
C1 C6 C7 120.7(3) . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C6 C7 P2 113.44(19) . . ?
C6 C7 H00T 108.9 . . ?
P2 C7 H00T 108.9 . . ?
C6 C7 H00U 108.9 . . ?
P2 C7 H00U 108.9 . . ?
H00T C7 H00U 107.7 . . ?
C8 C9 C10 110.4(2) . . ?
C8 C9 H00P 109.6 . . ?
C10 C9 H00P 109.6 . . ?
C8 C9 H00Q 109.6 . . ?
C10 C9 H00Q 109.6 . . ?
H00P C9 H00Q 108.1 . . ?
C11 C10 C9 111.9(3) . . ?
C11 C10 H01H 109.2 . . ?
C9 C10 H01H 109.2 . . ?
C11 C10 H01I 109.2 . . ?
C9 C10 H01I 109.2 . . ?
H01H C10 H01I 107.9 . . ?
C25 C20 C21 117.1(3) . . ?
C25 C20 P1 123.9(2) . . ?
C21 C20 P1 119.0(2) . . ?
C22 C21 C20 121.4(3) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C23 120.8(3) . . ?
C21 C22 H00O 119.6 . . ?
C23 C22 H00O 119.6 . . ?
C24 C23 C22 118.4(3) . . ?
C24 C23 H014 120.8 . . ?
C22 C23 H014 120.8 . . ?
C25 C24 C23 121.3(3) . . ?
C25 C24 H015 119.3 . . ?
C23 C24 H015 119.3 . . ?
C24 C25 C20 121.0(3) . . ?
C24 C25 H00N 119.5 . . ?
C20 C25 H00N 119.5 . . ?
C31 C26 C27 117.5(3) . . ?
C31 C26 P1 124.2(2) . . ?
C27 C26 P1 117.9(2) . . ?
C28 C27 C26 121.2(3) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C29 C28 C27 120.2(3) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 119.4(3) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C29 C30 C31 120.4(3) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C26 C31 C30 121.3(3) . . ?
C26 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
P3 C32 H00V 109.5 . . ?
P3 C32 H00W 109.5 . . ?
H00V C32 H00W 109.5 . . ?
P3 C32 H00X 109.5 . . ?
H00V C32 H00X 109.5 . . ?
H00W C32 H00X 109.5 . . ?
P3 C33 H00Y 109.5 . . ?
P3 C33 H00Z 109.5 . . ?
H00Y C33 H00Z 109.5 . . ?
P3 C33 H010 109.5 . . ?
H00Y C33 H010 109.5 . . ?
H00Z C33 H010 109.5 . . ?
P3 C34 H016 109.5 . . ?
P3 C34 H017 109.5 . . ?
H016 C34 H017 109.5 . . ?
P3 C34 H018 109.5 . . ?
H016 C34 H018 109.5 . . ?
H017 C34 H018 109.5 . . ?
C11 C12 C13 111.1(2) . . ?
C11 C12 H01D 109.4 . . ?
C13 C12 H01D 109.4 . . ?
C11 C12 H01E 109.4 . . ?
C13 C12 H01E 109.4 . . ?
H01D C12 H01E 108.0 . . ?
C12 C11 C10 111.7(3) . . ?
C12 C11 H01F 109.3 . . ?
C10 C11 H01F 109.3 . . ?
C12 C11 H01G 109.3 . . ?
C10 C11 H01G 109.3 . . ?
H01F C11 H01G 107.9 . . ?
C9 C8 C13 108.8(2) . . ?
C9 C8 P2 115.43(19) . . ?
C13 C8 P2 113.1(2) . . ?
C9 C8 H013 106.3 . . ?
C13 C8 H013 106.3 . . ?
P2 C8 H013 106.3 . . ?
C12 C13 C8 109.6(2) . . ?
C12 C13 H00R 109.7 . . ?
C8 C13 H00R 109.7 . . ?
C12 C13 H00S 109.7 . . ?
C8 C13 H00S 109.7 . . ?
H00R C13 H00S 108.2 . . ?
C15 C14 C19 109.6(2) . . ?
C15 C14 P2 114.18(19) . . ?
C19 C14 P2 112.85(19) . . ?
C15 C14 H14 106.6 . . ?
C19 C14 H14 106.6 . . ?
P2 C14 H14 106.6 . . ?
C16 C15 C14 110.8(2) . . ?
C16 C15 H15 109.5 . . ?
C14 C15 H15 109.5 . . ?
C16 C15 H00L 109.5 . . ?
C14 C15 H00L 109.5 . . ?
H15 C15 H00L 108.1 . . ?
C19 C18 C17 111.6(2) . . ?
C19 C18 H011 109.3 . . ?
C17 C18 H011 109.3 . . ?
C19 C18 H012 109.3 . . ?
C17 C18 H012 109.3 . . ?
H011 C18 H012 108.0 . . ?
C18 C17 C16 111.4(3) . . ?
C18 C17 H01B 109.4 . . ?
C16 C17 H01B 109.4 . . ?
C18 C17 H01C 109.4 . . ?
C16 C17 H01C 109.4 . . ?
H01B C17 H01C 108.0 . . ?
C15 C16 C17 111.8(2) . . ?
C15 C16 H019 109.3 . . ?
C17 C16 H019 109.3 . . ?
C15 C16 H01A 109.3 . . ?
C17 C16 H01A 109.3 . . ?
H019 C16 H01A 107.9 . . ?
C18 C19 C14 111.0(2) . . ?
C18 C19 H00B 109.4 . . ?
C14 C19 H00B 109.4 . . ?
C18 C19 H19 109.4 . . ?
C14 C19 H19 109.4 . . ?
H00B C19 H19 108.0 . . ?

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
C2 C1 B1 B2 135.9(3) . . . . ?
C6 C1 B1 B2 -46.2(3) . . . . ?
C2 C1 B1 P1 -108.8(3) . . . . ?
C6 C1 B1 P1 69.1(3) . . . . ?
C2 C1 B1 Br1 10.6(3) . . . . ?
C6 C1 B1 Br1 -171.5(2) . . . . ?
C6 C1 C2 C3 -2.1(4) . . . . ?
B1 C1 C2 C3 175.9(3) . . . . ?
C1 B1 B2 P3 -106.9(3) . . . . ?
P1 B1 B2 P3 134.79(18) . . . . ?
Br1 B1 B2 P3 16.6(3) . . . . ?
C1 B1 B2 P2 28.2(3) . . . . ?
P1 B1 B2 P2 -90.2(2) . . . . ?
Br1 B1 B2 P2 151.66(15) . . . . ?
C1 C2 C3 C4 0.8(5) . . . . ?
C2 C3 C4 C5 1.2(4) . . . . ?
C2 C1 C6 C5 1.5(4) . . . . ?
B1 C1 C6 C5 -176.6(3) . . . . ?
C2 C1 C6 C7 -177.6(2) . . . . ?
B1 C1 C6 C7 4.4(4) . . . . ?
C3 C4 C5 C6 -1.7(4) . . . . ?
C1 C6 C5 C4 0.3(4) . . . . ?
C7 C6 C5 C4 179.4(3) . . . . ?
C5 C6 C7 P2 -129.4(2) . . . . ?
C1 C6 C7 P2 49.7(3) . . . . ?
C8 P2 C7 C6 68.8(2) . . . . ?
C14 P2 C7 C6 -180.0(2) . . . . ?
B2 P2 C7 C6 -56.0(2) . . . . ?
C8 C9 C10 C11 54.8(4) . . . . ?
C26 P1 C20 C25 48.1(3) . . . . ?
B1 P1 C20 C25 -68.5(3) . . . . ?
C26 P1 C20 C21 -129.5(2) . . . . ?
B1 P1 C20 C21 113.8(2) . . . . ?
C25 C20 C21 C22 0.3(4) . . . . ?
P1 C20 C21 C22 178.1(2) . . . . ?
C20 C21 C22 C23 -1.0(4) . . . . ?
C21 C22 C23 C24 0.8(4) . . . . ?
C22 C23 C24 C25 0.0(4) . . . . ?
C23 C24 C25 C20 -0.7(4) . . . . ?
C21 C20 C25 C24 0.5(4) . . . . ?
P1 C20 C25 C24 -177.2(2) . . . . ?
C20 P1 C26 C31 -133.3(3) . . . . ?
B1 P1 C26 C31 -18.8(3) . . . . ?
C20 P1 C26 C27 53.7(3) . . . . ?
B1 P1 C26 C27 168.1(2) . . . . ?
C31 C26 C27 C28 0.0(4) . . . . ?
P1 C26 C27 C28 173.5(2) . . . . ?
C26 C27 C28 C29 -0.9(5) . . . . ?
C27 C28 C29 C30 1.0(5) . . . . ?
C28 C29 C30 C31 -0.1(5) . . . . ?
C27 C26 C31 C30 0.9(4) . . . . ?
P1 C26 C31 C30 -172.2(2) . . . . ?
C29 C30 C31 C26 -0.8(5) . . . . ?
C13 C12 C11 C10 54.9(4) . . . . ?
C9 C10 C11 C12 -52.6(4) . . . . ?
C10 C9 C8 C13 -58.8(3) . . . . ?
C10 C9 C8 P2 172.8(2) . . . . ?
C7 P2 C8 C9 62.4(2) . . . . ?
C14 P2 C8 C9 -45.9(3) . . . . ?
B2 P2 C8 C9 -178.7(2) . . . . ?
C7 P2 C8 C13 -63.9(2) . . . . ?
C14 P2 C8 C13 -172.1(2) . . . . ?
B2 P2 C8 C13 55.0(3) . . . . ?
C11 C12 C13 C8 -59.6(3) . . . . ?
C9 C8 C13 C12 61.2(3) . . . . ?
P2 C8 C13 C12 -169.1(2) . . . . ?
C7 P2 C14 C15 -166.9(2) . . . . ?
C8 P2 C14 C15 -53.3(2) . . . . ?
B2 P2 C14 C15 78.0(2) . . . . ?
C7 P2 C14 C19 67.1(2) . . . . ?
C8 P2 C14 C19 -179.2(2) . . . . ?
B2 P2 C14 C19 -48.0(3) . . . . ?
C19 C14 C15 C16 -57.5(3) . . . . ?
P2 C14 C15 C16 174.8(2) . . . . ?
C19 C18 C17 C16 53.9(3) . . . . ?
C14 C15 C16 C17 56.4(3) . . . . ?
C18 C17 C16 C15 -54.1(3) . . . . ?
C17 C18 C19 C14 -56.1(3) . . . . ?
C15 C14 C19 C18 57.6(3) . . . . ?
P2 C14 C19 C18 -174.02(19) . . . . ?

_refine_diff_density_max         0.372
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_hhhh_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1954178'
loop_
_audit_author_name
_audit_author_address
'Tom Stennett'
;Julius Maximilians Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2019-09-17 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H55 B2 N2 P2, Br'
_chemical_formula_sum            'C40 H55 B2 Br N2 P2'
_chemical_formula_weight         727.33

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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   28.3736(16)
_cell_length_b                   57.198(3)
_cell_length_c                   10.0055(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16237.9(16)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8484
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.08


_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    1.190
_exptl_crystal_F_000             6144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    1.120
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6841
_exptl_absorpt_correction_T_max  0.7455
_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            24574
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -70
_diffrn_reflns_limit_k_max       73
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.408
_diffrn_reflns_theta_max         27.205
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8889
_reflns_number_gt                7660
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    1.000

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

_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. Refined as a 2-component inversion 
twin.The structure was refined using TWIN keyword 
(matrix: TWIN

).
 The BASF parameter was refined to 0°.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0202P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.034(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8889
_refine_ls_number_parameters     434
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0701
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br01 Br 0.66871(2) 0.29014(2) 0.85902(5) 0.04230(14) Uani 1 1 d . . . . .
B1 B 0.64126(13) 0.43404(7) 0.4246(4) 0.0149(8) Uani 1 1 d . . . . .
P1 P 0.74318(3) 0.43333(2) 0.51109(8) 0.01482(18) Uani 1 1 d . . . . .
P003 P 0.63707(3) 0.41816(2) 0.59647(9) 0.01609(18) Uani 1 1 d . . . . .
N005 N 0.55217(9) 0.44749(5) 0.3738(3) 0.0183(6) Uani 1 1 d . . . . .
N006 N 0.60620(9) 0.47251(5) 0.3285(3) 0.0174(6) Uani 1 1 d . . . . .
C008 C 0.72234(12) 0.39686(6) 0.1840(4) 0.0210(8) Uani 1 1 d . . . . .
H008 H 0.752169 0.389316 0.184922 0.025 Uiso 1 1 calc R U . . .
C009 C 0.63645(12) 0.37286(6) 0.4946(4) 0.0209(8) Uani 1 1 d . . . . .
H009 H 0.623383 0.379588 0.416102 0.025 Uiso 1 1 calc R U . . .
C00A C 0.78518(11) 0.42932(6) 0.6508(3) 0.0188(7) Uani 1 1 d . . . . .
H00A H 0.809442 0.441932 0.643272 0.023 Uiso 1 1 calc R U . . .
C00B C 0.81660(11) 0.44577(6) 0.3356(4) 0.0214(8) Uani 1 1 d . . . . .
H00B H 0.812823 0.430314 0.292395 0.026 Uiso 1 1 calc R U . . .
H00C H 0.839512 0.444073 0.409587 0.026 Uiso 1 1 calc R U . . .
C00C C 0.70618(11) 0.40750(6) 0.3003(3) 0.0147(7) Uani 1 1 d . . . . .
C00D C 0.66185(11) 0.41926(6) 0.3013(3) 0.0154(7) Uani 1 1 d . . . . .
C00E C 0.77353(13) 0.47832(6) 0.4529(4) 0.0216(8) Uani 1 1 d . . . . .
H00D H 0.742274 0.483581 0.485036 0.026 Uiso 1 1 calc R U . . .
H00E H 0.795099 0.477719 0.530585 0.026 Uiso 1 1 calc R U . . .
C00F C 0.59623(11) 0.42542(7) 0.7293(3) 0.0188(8) Uani 1 1 d . . . . .
C00G C 0.73798(11) 0.40575(6) 0.4217(3) 0.0170(7) Uani 1 1 d . . . . .
H00F H 0.769713 0.400622 0.392812 0.020 Uiso 1 1 calc R U . . .
H00G H 0.725301 0.393725 0.483134 0.020 Uiso 1 1 calc R U . . .
C00H C 0.56445(12) 0.48189(6) 0.2832(4) 0.0222(8) Uani 1 1 d . . . . .
H00H H 0.560441 0.496566 0.240293 0.027 Uiso 1 1 calc R U . . .
C00I C 0.64510(12) 0.34882(6) 0.4994(4) 0.0230(8) Uani 1 1 d . . . . .
H00I H 0.638631 0.339317 0.423763 0.028 Uiso 1 1 calc R U . . .
C00J C 0.63673(12) 0.41899(6) 0.1810(3) 0.0197(8) Uani 1 1 d . . . . .
H00J H 0.606995 0.426603 0.177823 0.024 Uiso 1 1 calc R U . . .
C00K C 0.66460(12) 0.37657(7) 0.7208(3) 0.0206(8) Uani 1 1 d . . . . .
H00K H 0.671561 0.385976 0.796485 0.025 Uiso 1 1 calc R U . . .
C00L C 0.69647(12) 0.39691(7) 0.0674(4) 0.0261(9) Uani 1 1 d . . . . .
H00L H 0.708114 0.389407 -0.010648 0.031 Uiso 1 1 calc R U . . .
C00M C 0.65491(12) 0.50750(6) 0.3675(5) 0.0305(9) Uani 1 1 d . . . . .
H00M H 0.687311 0.513404 0.364478 0.046 Uiso 1 1 calc R U . . .
H00N H 0.644200 0.506843 0.460548 0.046 Uiso 1 1 calc R U . . .
H00O H 0.634298 0.517958 0.316478 0.046 Uiso 1 1 calc R U . . .
C00N C 0.76903(11) 0.45383(6) 0.3918(3) 0.0170(7) Uani 1 1 d . . . . .
H00P H 0.746729 0.455062 0.314748 0.020 Uiso 1 1 calc R U . . .
C00O C 0.59921(11) 0.45121(6) 0.3828(3) 0.0160(7) Uani 1 1 d . . . . .
C00P C 0.52591(12) 0.42659(7) 0.4174(4) 0.0246(8) Uani 1 1 d . . . . .
H00Q H 0.548818 0.415549 0.459721 0.030 Uiso 1 1 calc R U . . .
C00Q C 0.65312(13) 0.40813(7) 0.0660(3) 0.0254(8) Uani 1 1 d . . . . .
H00R H 0.634729 0.408380 -0.013303 0.030 Uiso 1 1 calc R U . . .
C00R C 0.66496(13) 0.48258(7) 0.1589(4) 0.0288(9) Uani 1 1 d . . . . .
H00S H 0.662185 0.466534 0.125580 0.043 Uiso 1 1 calc R U . . .
H00T H 0.697270 0.488164 0.145423 0.043 Uiso 1 1 calc R U . . .
H00U H 0.643018 0.492711 0.110246 0.043 Uiso 1 1 calc R U . . .
C00S C 0.82088(14) 0.40622(8) 0.8950(4) 0.0315(10) Uani 1 1 d . . . . .
H00V H 0.844235 0.405313 0.968339 0.038 Uiso 1 1 calc R U . . .
H00W H 0.798113 0.393265 0.906702 0.038 Uiso 1 1 calc R U . . .
C00T C 0.53055(12) 0.46634(7) 0.3114(4) 0.0233(8) Uani 1 1 d . . . . .
H00X H 0.497907 0.467915 0.292372 0.028 Uiso 1 1 calc R U . . .
C00U C 0.56411(12) 0.40859(7) 0.7740(4) 0.0270(9) Uani 1 1 d . . . . .
H00Y H 0.563118 0.393645 0.732624 0.032 Uiso 1 1 calc R U . . .
C00V C 0.81121(13) 0.40589(7) 0.6454(4) 0.0298(9) Uani 1 1 d . . . . .
H00Z H 0.828635 0.404684 0.559911 0.036 Uiso 1 1 calc R U . . .
H010 H 0.788066 0.392957 0.648871 0.036 Uiso 1 1 calc R U . . .
C00W C 0.84578(14) 0.40356(9) 0.7621(4) 0.0391(11) Uani 1 1 d . . . . .
H011 H 0.861265 0.388068 0.758186 0.047 Uiso 1 1 calc R U . . .
H012 H 0.870534 0.415685 0.754121 0.047 Uiso 1 1 calc R U . . .
C00X C 0.79245(12) 0.49588(6) 0.3502(4) 0.0247(8) Uani 1 1 d . . . . .
H013 H 0.769380 0.497611 0.276651 0.030 Uiso 1 1 calc R U . . .
H014 H 0.796399 0.511330 0.393335 0.030 Uiso 1 1 calc R U . . .
C00Y C 0.65321(11) 0.48312(6) 0.3070(4) 0.0217(8) Uani 1 1 d . . . . .
H015 H 0.676952 0.473254 0.354658 0.026 Uiso 1 1 calc R U . . .
C00Z C 0.67194(12) 0.35270(7) 0.7256(4) 0.0227(8) Uani 1 1 d . . . . .
H016 H 0.683137 0.345726 0.805693 0.027 Uiso 1 1 calc R U . . .
C010 C 0.76063(13) 0.43238(7) 0.7865(3) 0.0267(9) Uani 1 1 d . . . . .
H01A H 0.746263 0.448135 0.791029 0.032 Uiso 1 1 calc R U . . .
H01B H 0.735040 0.420704 0.794923 0.032 Uiso 1 1 calc R U . . .
C011 C 0.59697(13) 0.44709(7) 0.7913(4) 0.0297(9) Uani 1 1 d . . . . .
H01C H 0.618932 0.458628 0.763247 0.036 Uiso 1 1 calc R U . . .
C012 C 0.83555(13) 0.46339(7) 0.2333(4) 0.0275(9) Uani 1 1 d . . . . .
H01D H 0.867018 0.458269 0.202204 0.033 Uiso 1 1 calc R U . . .
H01E H 0.814261 0.463833 0.154942 0.033 Uiso 1 1 calc R U . . .
C013 C 0.66319(11) 0.33888(6) 0.6152(4) 0.0247(8) Uani 1 1 d . . . . .
H01F H 0.669532 0.322583 0.618443 0.030 Uiso 1 1 calc R U . . .
C014 C 0.53410(14) 0.43530(9) 0.9371(4) 0.0383(11) Uani 1 1 d . . . . .
H01G H 0.512560 0.438760 1.007043 0.046 Uiso 1 1 calc R U . . .
C015 C 0.56559(15) 0.45199(9) 0.8946(4) 0.0396(11) Uani 1 1 d . . . . .
H01H H 0.565949 0.466946 0.935863 0.047 Uiso 1 1 calc R U . . .
C016 C 0.53387(13) 0.41364(8) 0.8781(4) 0.0374(11) Uani 1 1 d . . . . .
H01I H 0.512670 0.401993 0.909290 0.045 Uiso 1 1 calc R U . . .
C017 C 0.83934(13) 0.48790(7) 0.2935(4) 0.0277(9) Uani 1 1 d . . . . .
H01J H 0.863323 0.487858 0.365401 0.033 Uiso 1 1 calc R U . . .
H01K H 0.849744 0.499028 0.223715 0.033 Uiso 1 1 calc R U . . .
C018 C 0.79504(14) 0.42942(8) 0.9023(4) 0.0314(9) Uani 1 1 d . . . . .
H01L H 0.818262 0.442334 0.900574 0.038 Uiso 1 1 calc R U . . .
H01M H 0.777585 0.430346 0.987806 0.038 Uiso 1 1 calc R U . . .
C019 C 0.48962(13) 0.43340(9) 0.5225(4) 0.0424(12) Uani 1 1 d . . . . .
H01N H 0.465362 0.443261 0.481472 0.064 Uiso 1 1 calc R U . . .
H01O H 0.505167 0.442064 0.594584 0.064 Uiso 1 1 calc R U . . .
H01P H 0.474980 0.419262 0.559045 0.064 Uiso 1 1 calc R U . . .
C01A C 0.50383(14) 0.41429(7) 0.2969(4) 0.0362(10) Uani 1 1 d . . . . .
H01Q H 0.481673 0.424909 0.252723 0.054 Uiso 1 1 calc R U . . .
H01R H 0.487021 0.400276 0.327039 0.054 Uiso 1 1 calc R U . . .
H01S H 0.528669 0.409793 0.233906 0.054 Uiso 1 1 calc R U . . .
B01B B 0.68102(13) 0.44245(7) 0.5525(4) 0.0176(8) Uani 1 1 d . . . . .
H1 H 0.6767(11) 0.4585(6) 0.615(4) 0.023(9) Uiso 1 1 d . . . . .
C2 C 0.64675(10) 0.38695(6) 0.6032(4) 0.0162(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C00O 1.601(5) . ?
B1 C00D 1.606(5) . ?
B1 B01B 1.772(5) . ?
B1 P003 1.948(4) . ?
P1 C00G 1.819(3) . ?
P1 C00N 1.827(3) . ?
P1 C00A 1.851(3) . ?
P1 B01B 1.885(4) . ?
P003 C2 1.807(3) . ?
P003 C00F 1.812(3) . ?
P003 B01B 1.918(4) . ?
N005 C00O 1.355(4) . ?
N005 C00T 1.388(4) . ?
N005 C00P 1.475(4) . ?
N006 C00O 1.349(4) . ?
N006 C00H 1.377(4) . ?
N006 C00Y 1.481(4) . ?
C008 C00L 1.378(5) . ?
C008 C00C 1.392(5) . ?
C008 H008 0.9500 . ?
C009 C2 1.384(5) . ?
C009 C00I 1.397(5) . ?
C009 H009 0.9500 . ?
C00A C00V 1.531(5) . ?
C00A C010 1.536(5) . ?
C00A H00A 1.0000 . ?
C00B C00N 1.533(5) . ?
C00B C012 1.534(5) . ?
C00B H00B 0.9900 . ?
C00B H00C 0.9900 . ?
C00C C00D 1.427(4) . ?
C00C C00G 1.516(4) . ?
C00D C00J 1.399(5) . ?
C00E C00X 1.534(5) . ?
C00E C00N 1.534(5) . ?
C00E H00D 0.9900 . ?
C00E H00E 0.9900 . ?
C00F C011 1.386(5) . ?
C00F C00U 1.399(5) . ?
C00G H00F 0.9900 . ?
C00G H00G 0.9900 . ?
C00H C00T 1.340(5) . ?
C00H H00H 0.9500 . ?
C00I C013 1.389(5) . ?
C00I H00I 0.9500 . ?
C00J C00Q 1.387(5) . ?
C00J H00J 0.9500 . ?
C00K C00Z 1.382(5) . ?
C00K C2 1.412(5) . ?
C00K H00K 0.9500 . ?
C00L C00Q 1.388(5) . ?
C00L H00L 0.9500 . ?
C00M C00Y 1.521(5) . ?
C00M H00M 0.9800 . ?
C00M H00N 0.9800 . ?
C00M H00O 0.9800 . ?
C00N H00P 1.0000 . ?
C00P C019 1.522(5) . ?
C00P C01A 1.530(5) . ?
C00P H00Q 1.0000 . ?
C00Q H00R 0.9500 . ?
C00R C00Y 1.519(5) . ?
C00R H00S 0.9800 . ?
C00R H00T 0.9800 . ?
C00R H00U 0.9800 . ?
C00S C00W 1.513(6) . ?
C00S C018 1.518(6) . ?
C00S H00V 0.9900 . ?
C00S H00W 0.9900 . ?
C00T H00X 0.9500 . ?
C00U C016 1.380(5) . ?
C00U H00Y 0.9500 . ?
C00V C00W 1.531(5) . ?
C00V H00Z 0.9900 . ?
C00V H010 0.9900 . ?
C00W H011 0.9900 . ?
C00W H012 0.9900 . ?
C00X C017 1.516(5) . ?
C00X H013 0.9900 . ?
C00X H014 0.9900 . ?
C00Y H015 1.0000 . ?
C00Z C013 1.381(5) . ?
C00Z H016 0.9500 . ?
C010 C018 1.524(5) . ?
C010 H01A 0.9900 . ?
C010 H01B 0.9900 . ?
C011 C015 1.392(6) . ?
C011 H01C 0.9500 . ?
C012 C017 1.530(5) . ?
C012 H01D 0.9900 . ?
C012 H01E 0.9900 . ?
C013 H01F 0.9500 . ?
C014 C016 1.373(6) . ?
C014 C015 1.375(6) . ?
C014 H01G 0.9500 . ?
C015 H01H 0.9500 . ?
C016 H01I 0.9500 . ?
C017 H01J 0.9900 . ?
C017 H01K 0.9900 . ?
C018 H01L 0.9900 . ?
C018 H01M 0.9900 . ?
C019 H01N 0.9800 . ?
C019 H01O 0.9800 . ?
C019 H01P 0.9800 . ?
C01A H01Q 0.9800 . ?
C01A H01R 0.9800 . ?
C01A H01S 0.9800 . ?
B01B H1 1.12(4) . ?

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
C00O B1 C00D 113.2(3) . . ?
C00O B1 B01B 119.8(3) . . ?
C00D B1 B01B 117.8(3) . . ?
C00O B1 P003 118.1(2) . . ?
C00D B1 P003 117.0(2) . . ?
B01B B1 P003 61.86(18) . . ?
C00G P1 C00N 105.54(16) . . ?
C00G P1 C00A 108.42(16) . . ?
C00N P1 C00A 108.33(15) . . ?
C00G P1 B01B 105.80(17) . . ?
C00N P1 B01B 109.96(17) . . ?
C00A P1 B01B 118.07(17) . . ?
C2 P003 C00F 107.23(16) . . ?
C2 P003 B01B 128.70(16) . . ?
C00F P003 B01B 114.71(18) . . ?
C2 P003 B1 118.97(17) . . ?
C00F P003 B1 125.41(16) . . ?
B01B P003 B1 54.55(16) . . ?
C00O N005 C00T 110.1(3) . . ?
C00O N005 C00P 127.2(3) . . ?
C00T N005 C00P 122.6(3) . . ?
C00O N006 C00H 111.0(3) . . ?
C00O N006 C00Y 124.1(3) . . ?
C00H N006 C00Y 124.6(3) . . ?
C00L C008 C00C 122.1(3) . . ?
C00L C008 H008 118.9 . . ?
C00C C008 H008 118.9 . . ?
C2 C009 C00I 120.6(3) . . ?
C2 C009 H009 119.7 . . ?
C00I C009 H009 119.7 . . ?
C00V C00A C010 110.5(3) . . ?
C00V C00A P1 113.1(2) . . ?
C010 C00A P1 111.2(2) . . ?
C00V C00A H00A 107.3 . . ?
C010 C00A H00A 107.3 . . ?
P1 C00A H00A 107.3 . . ?
C00N C00B C012 110.9(3) . . ?
C00N C00B H00B 109.5 . . ?
C012 C00B H00B 109.5 . . ?
C00N C00B H00C 109.5 . . ?
C012 C00B H00C 109.5 . . ?
H00B C00B H00C 108.1 . . ?
C008 C00C C00D 120.2(3) . . ?
C008 C00C C00G 116.4(3) . . ?
C00D C00C C00G 123.4(3) . . ?
C00J C00D C00C 116.0(3) . . ?
C00J C00D B1 118.8(3) . . ?
C00C C00D B1 125.0(3) . . ?
C00X C00E C00N 111.1(3) . . ?
C00X C00E H00D 109.4 . . ?
C00N C00E H00D 109.4 . . ?
C00X C00E H00E 109.4 . . ?
C00N C00E H00E 109.4 . . ?
H00D C00E H00E 108.0 . . ?
C011 C00F C00U 118.8(3) . . ?
C011 C00F P003 121.6(3) . . ?
C00U C00F P003 119.6(3) . . ?
C00C C00G P1 112.6(2) . . ?
C00C C00G H00F 109.1 . . ?
P1 C00G H00F 109.1 . . ?
C00C C00G H00G 109.1 . . ?
P1 C00G H00G 109.1 . . ?
H00F C00G H00G 107.8 . . ?
C00T C00H N006 106.8(3) . . ?
C00T C00H H00H 126.6 . . ?
N006 C00H H00H 126.6 . . ?
C013 C00I C009 119.8(4) . . ?
C013 C00I H00I 120.1 . . ?
C009 C00I H00I 120.1 . . ?
C00Q C00J C00D 123.2(3) . . ?
C00Q C00J H00J 118.4 . . ?
C00D C00J H00J 118.4 . . ?
C00Z C00K C2 119.9(3) . . ?
C00Z C00K H00K 120.0 . . ?
C2 C00K H00K 120.0 . . ?
C008 C00L C00Q 118.8(3) . . ?
C008 C00L H00L 120.6 . . ?
C00Q C00L H00L 120.6 . . ?
C00Y C00M H00M 109.5 . . ?
C00Y C00M H00N 109.5 . . ?
H00M C00M H00N 109.5 . . ?
C00Y C00M H00O 109.5 . . ?
H00M C00M H00O 109.5 . . ?
H00N C00M H00O 109.5 . . ?
C00B C00N C00E 110.3(3) . . ?
C00B C00N P1 113.6(2) . . ?
C00E C00N P1 111.1(2) . . ?
C00B C00N H00P 107.2 . . ?
C00E C00N H00P 107.2 . . ?
P1 C00N H00P 107.2 . . ?
N006 C00O N005 105.1(3) . . ?
N006 C00O B1 123.3(3) . . ?
N005 C00O B1 131.0(3) . . ?
N005 C00P C019 109.8(3) . . ?
N005 C00P C01A 110.3(3) . . ?
C019 C00P C01A 112.6(3) . . ?
N005 C00P H00Q 108.0 . . ?
C019 C00P H00Q 108.0 . . ?
C01A C00P H00Q 108.0 . . ?
C00J C00Q C00L 119.8(3) . . ?
C00J C00Q H00R 120.1 . . ?
C00L C00Q H00R 120.1 . . ?
C00Y C00R H00S 109.5 . . ?
C00Y C00R H00T 109.5 . . ?
H00S C00R H00T 109.5 . . ?
C00Y C00R H00U 109.5 . . ?
H00S C00R H00U 109.5 . . ?
H00T C00R H00U 109.5 . . ?
C00W C00S C018 110.8(3) . . ?
C00W C00S H00V 109.5 . . ?
C018 C00S H00V 109.5 . . ?
C00W C00S H00W 109.5 . . ?
C018 C00S H00W 109.5 . . ?
H00V C00S H00W 108.1 . . ?
C00H C00T N005 107.0(3) . . ?
C00H C00T H00X 126.5 . . ?
N005 C00T H00X 126.5 . . ?
C016 C00U C00F 120.2(4) . . ?
C016 C00U H00Y 119.9 . . ?
C00F C00U H00Y 119.9 . . ?
C00A C00V C00W 111.0(3) . . ?
C00A C00V H00Z 109.4 . . ?
C00W C00V H00Z 109.4 . . ?
C00A C00V H010 109.4 . . ?
C00W C00V H010 109.4 . . ?
H00Z C00V H010 108.0 . . ?
C00S C00W C00V 111.3(3) . . ?
C00S C00W H011 109.4 . . ?
C00V C00W H011 109.4 . . ?
C00S C00W H012 109.4 . . ?
C00V C00W H012 109.4 . . ?
H011 C00W H012 108.0 . . ?
C017 C00X C00E 111.2(3) . . ?
C017 C00X H013 109.4 . . ?
C00E C00X H013 109.4 . . ?
C017 C00X H014 109.4 . . ?
C00E C00X H014 109.4 . . ?
H013 C00X H014 108.0 . . ?
N006 C00Y C00R 109.3(3) . . ?
N006 C00Y C00M 110.3(3) . . ?
C00R C00Y C00M 113.6(3) . . ?
N006 C00Y H015 107.8 . . ?
C00R C00Y H015 107.8 . . ?
C00M C00Y H015 107.8 . . ?
C013 C00Z C00K 120.7(3) . . ?
C013 C00Z H016 119.6 . . ?
C00K C00Z H016 119.6 . . ?
C018 C010 C00A 111.6(3) . . ?
C018 C010 H01A 109.3 . . ?
C00A C010 H01A 109.3 . . ?
C018 C010 H01B 109.3 . . ?
C00A C010 H01B 109.3 . . ?
H01A C010 H01B 108.0 . . ?
C00F C011 C015 120.2(4) . . ?
C00F C011 H01C 119.9 . . ?
C015 C011 H01C 119.9 . . ?
C017 C012 C00B 111.3(3) . . ?
C017 C012 H01D 109.4 . . ?
C00B C012 H01D 109.4 . . ?
C017 C012 H01E 109.4 . . ?
C00B C012 H01E 109.4 . . ?
H01D C012 H01E 108.0 . . ?
C00Z C013 C00I 120.0(3) . . ?
C00Z C013 H01F 120.0 . . ?
C00I C013 H01F 120.0 . . ?
C016 C014 C015 119.8(4) . . ?
C016 C014 H01G 120.1 . . ?
C015 C014 H01G 120.1 . . ?
C014 C015 C011 120.4(4) . . ?
C014 C015 H01H 119.8 . . ?
C011 C015 H01H 119.8 . . ?
C014 C016 C00U 120.7(4) . . ?
C014 C016 H01I 119.7 . . ?
C00U C016 H01I 119.7 . . ?
C00X C017 C012 111.2(3) . . ?
C00X C017 H01J 109.4 . . ?
C012 C017 H01J 109.4 . . ?
C00X C017 H01K 109.4 . . ?
C012 C017 H01K 109.4 . . ?
H01J C017 H01K 108.0 . . ?
C00S C018 C010 111.7(3) . . ?
C00S C018 H01L 109.3 . . ?
C010 C018 H01L 109.3 . . ?
C00S C018 H01M 109.3 . . ?
C010 C018 H01M 109.3 . . ?
H01L C018 H01M 107.9 . . ?
C00P C019 H01N 109.5 . . ?
C00P C019 H01O 109.5 . . ?
H01N C019 H01O 109.5 . . ?
C00P C019 H01P 109.5 . . ?
H01N C019 H01P 109.5 . . ?
H01O C019 H01P 109.5 . . ?
C00P C01A H01Q 109.5 . . ?
C00P C01A H01R 109.5 . . ?
H01Q C01A H01R 109.5 . . ?
C00P C01A H01S 109.5 . . ?
H01Q C01A H01S 109.5 . . ?
H01R C01A H01S 109.5 . . ?
B1 B01B P1 111.2(2) . . ?
B1 B01B P003 63.59(18) . . ?
P1 B01B P003 117.3(2) . . ?
B1 B01B H1 123.8(18) . . ?
P1 B01B H1 117.0(16) . . ?
P003 B01B H1 113.2(18) . . ?
C009 C2 C00K 119.0(3) . . ?
C009 C2 P003 120.9(3) . . ?
C00K C2 P003 120.1(3) . . ?

_refine_diff_density_max         0.329
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.051



####################################################################### 
# 
# 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_tobr060_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1954180'
loop_
_audit_author_name
_audit_author_address
'Tom Stennett'
;Julius Maximilians Universitaet Wuerzburg
Germany
;
_audit_update_record             
;
2019-09-17 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H71 B2 N4 P'
_chemical_formula_sum            'C58 H71 B2 N4 P'
_chemical_formula_weight         876.77

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

_space_group_crystal_system      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                   11.3635(4)
_cell_length_b                   13.0900(5)
_cell_length_c                   19.2394(6)
_cell_angle_alpha                89.9680(10)
_cell_angle_beta                 76.3530(10)
_cell_angle_gamma                70.1810(10)
_cell_volume                     2606.41(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    107(2)
_cell_measurement_reflns_used    9907
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      26.70


_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            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.201
_exptl_absorpt_coefficient_mu    0.093
_shelx_estimated_absorpt_T_min   0.962
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7154
_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 0.1440
1.00 1.00 1.00 0.0990
1.00 1.00 -1.00 0.1180
-1.00 -1.00 1.00 0.0980
0.00 1.00 -1.00 0.1620
0.00 -1.00 1.00 0.0770
0.00 -1.00 0.00 0.0780
0.00 1.00 0.00 0.1230
0.00 -1.00 -1.00 0.0820
0.00 1.00 1.00 0.1000
1.00 -1.00 1.00 0.1100
-1.00 1.00 0.00 0.1470
1.00 -1.00 -1.00 0.1120
-1.00 1.00 1.00 0.1180
-1.00 0.00 -1.00 0.1870
-1.00 0.00 0.00 0.1510
-1.00 0.00 1.00 0.1300
0.00 0.00 1.00 0.1240
1.00 0.00 1.00 0.1090
0.00 0.00 -1.00 0.1220
1.00 0.00 -1.00 0.1210
1.00 0.00 0.00 0.1180

_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      107(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            74317
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.187
_diffrn_reflns_theta_max         26.021
_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             10258
_reflns_number_gt                8426
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-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)+(0.0440P)²+2.0461P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10258
_refine_ls_number_parameters     598
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1270
_refine_ls_wR_factor_gt          0.1174
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 0.52096(19) 0.67410(16) 0.74683(10) 0.0215(4) Uani 1 1 d . . . . .
N1_1 N 0.47123(13) 0.58800(12) 0.63858(7) 0.0207(3) Uani 1 1 d . . . . .
P1_1 P 0.58127(4) 0.55726(4) 0.80643(2) 0.02216(11) Uani 1 1 d . . . . .
C1_1 C 0.45154(16) 0.67371(14) 0.68637(9) 0.0202(4) Uani 1 1 d . . . . .
B2_1 B 0.53138(19) 0.78175(17) 0.77585(11) 0.0231(4) Uani 1 1 d . . . . .
H1_1 H 0.487(2) 0.8628(18) 0.7603(12) 0.041(6) Uiso 1 1 d . . . . .
N2_1 N 0.35578(15) 0.75983(12) 0.67099(8) 0.0255(3) Uani 1 1 d . . . . .
C2_1 C 0.38297(19) 0.61644(16) 0.59095(11) 0.0321(4) Uani 1 1 d . . . . .
H2A_1 H 0.326298 0.572192 0.598415 0.039 Uiso 1 1 calc R U . . .
H2AB_1 H 0.431821 0.604832 0.539942 0.039 Uiso 1 1 calc R U . . .
N3_1 N 0.73117(14) 0.75003(12) 0.83433(8) 0.0230(3) Uani 1 1 d . . . . .
C3_1 C 0.3059(2) 0.73427(16) 0.61198(10) 0.0322(4) Uani 1 1 d . . . . .
H3A_1 H 0.320300 0.779019 0.571527 0.039 Uiso 1 1 calc R U . . .
H3AB_1 H 0.212474 0.746359 0.628328 0.039 Uiso 1 1 calc R U . . .
N4_1 N 0.54279(14) 0.86487(12) 0.89386(8) 0.0242(3) Uani 1 1 d . . . . .
C5_1 C 0.3371(2) 0.95009(16) 0.67695(11) 0.0350(5) Uani 1 1 d . . . . .
C6_1 C 0.2676(2) 1.05670(18) 0.70669(13) 0.0442(6) Uani 1 1 d . . . . .
H6_1 H 0.296146 1.113921 0.688217 0.053 Uiso 1 1 calc R U . . .
C7_1 C 0.1581(2) 1.08085(19) 0.76251(13) 0.0495(7) Uani 1 1 d . . . . .
H7_1 H 0.112621 1.154008 0.782438 0.059 Uiso 1 1 calc R U . . .
C8_1 C 0.1145(2) 0.9990(2) 0.78935(13) 0.0499(6) Uani 1 1 d . . . . .
H8_1 H 0.038381 1.016675 0.827376 0.060 Uiso 1 1 calc R U . . .
C9_1 C 0.1802(2) 0.89009(18) 0.76170(11) 0.0400(5) Uani 1 1 d . . . . .
C10_1 C 0.1303(2) 0.8019(2) 0.79141(13) 0.0519(6) Uani 1 1 d . . . . .
H10A_1 H 0.045819 0.814475 0.780573 0.062 Uiso 1 1 calc R U . . .
H10B_1 H 0.190796 0.730794 0.766499 0.062 Uiso 1 1 calc R U . . .
C11_1 C 0.1143(3) 0.7958(3) 0.87010(14) 0.0736(9) Uani 1 1 d . . . . .
H11A_1 H 0.083331 0.735910 0.885179 0.110 Uiso 1 1 calc R U . . .
H11B_1 H 0.051422 0.864606 0.895496 0.110 Uiso 1 1 calc R U . . .
H11C_1 H 0.197554 0.782727 0.881471 0.110 Uiso 1 1 calc R U . . .
C12_1 C 0.4583(2) 0.92117(17) 0.61665(12) 0.0413(5) Uani 1 1 d . . . . .
H12A_1 H 0.439647 0.896788 0.573057 0.050 Uiso 1 1 calc R U . . .
H12B_1 H 0.525393 0.858448 0.629438 0.050 Uiso 1 1 calc R U . . .
C13_1 C 0.5138(3) 1.0105(2) 0.59809(16) 0.0633(7) Uani 1 1 d . . . . .
H13A_1 H 0.594275 0.981861 0.560248 0.095 Uiso 1 1 calc R U . . .
H13B_1 H 0.531585 1.036738 0.640847 0.095 Uiso 1 1 calc R U . . .
H13C_1 H 0.451595 1.070943 0.581166 0.095 Uiso 1 1 calc R U . . .
C14_1 C 0.58941(17) 0.49853(15) 0.60989(9) 0.0228(4) Uani 1 1 d . . . . .
C15_1 C 0.5886(2) 0.39251(15) 0.61552(10) 0.0295(4) Uani 1 1 d . . . . .
C16_1 C 0.6985(2) 0.30669(16) 0.57853(11) 0.0392(5) Uani 1 1 d . . . . .
H16_1 H 0.700881 0.233735 0.582614 0.047 Uiso 1 1 calc R U . . .
C17_1 C 0.8033(2) 0.32636(18) 0.53633(11) 0.0412(6) Uani 1 1 d . . . . .
H17_1 H 0.876367 0.267236 0.510742 0.049 Uiso 1 1 calc R U . . .
C18_1 C 0.80251(19) 0.43165(18) 0.53107(10) 0.0346(5) Uani 1 1 d . . . . .
H18_1 H 0.875722 0.444079 0.502066 0.042 Uiso 1 1 calc R U . . .
C19_1 C 0.69622(17) 0.52033(16) 0.56753(9) 0.0256(4) Uani 1 1 d . . . . .
C20_1 C 0.69446(18) 0.63571(16) 0.56268(10) 0.0294(4) Uani 1 1 d . . . . .
H20A_1 H 0.685251 0.666440 0.611491 0.035 Uiso 1 1 calc R U . . .
H20B_1 H 0.616587 0.678959 0.547025 0.035 Uiso 1 1 calc R U . . .
C21_1 C 0.8116(2) 0.6515(2) 0.51250(12) 0.0484(6) Uani 1 1 d . . . . .
H21A_1 H 0.798961 0.729361 0.512754 0.073 Uiso 1 1 calc R U . . .
H21B_1 H 0.821886 0.622317 0.463665 0.073 Uiso 1 1 calc R U . . .
H21C_1 H 0.889218 0.612884 0.528832 0.073 Uiso 1 1 calc R U . . .
C22_1 C 0.60365(17) 0.79493(14) 0.83438(9) 0.0234(4) Uani 1 1 d . . . . .
C23_1 C 0.76020(18) 0.79907(17) 0.89451(10) 0.0312(4) Uani 1 1 d . . . . .
H23A_1 H 0.810862 0.846491 0.877100 0.037 Uiso 1 1 calc R U . . .
H23B_1 H 0.808781 0.742116 0.921262 0.037 Uiso 1 1 calc R U . . .
C24_1 C 0.62792(18) 0.86474(17) 0.94076(10) 0.0308(4) Uani 1 1 d . . . . .
H24A_1 H 0.606369 0.829560 0.985195 0.037 Uiso 1 1 calc R U . . .
H24B_1 H 0.622280 0.939733 0.953726 0.037 Uiso 1 1 calc R U . . .
C25_1 C 0.40982(17) 0.93584(15) 0.91397(9) 0.0241(4) Uani 1 1 d . . . . .
C26_1 C 0.31939(18) 0.90170(16) 0.96151(10) 0.0281(4) Uani 1 1 d . . . . .
C27_1 C 0.19404(18) 0.97739(17) 0.98528(11) 0.0325(4) Uani 1 1 d . . . . .
H27_1 H 0.130173 0.957315 1.017820 0.039 Uiso 1 1 calc R U . . .
C28_1 C 0.16174(19) 1.08080(17) 0.96218(10) 0.0334(5) Uani 1 1 d . . . . .
H28_1 H 0.076049 1.130976 0.979086 0.040 Uiso 1 1 calc R U . . .
C29_1 C 0.25241(19) 1.11223(16) 0.91482(10) 0.0325(4) Uani 1 1 d . . . . .
H29_1 H 0.228425 1.183457 0.899014 0.039 Uiso 1 1 calc R U . . .
C30_1 C 0.37906(18) 1.04003(16) 0.89003(10) 0.0286(4) Uani 1 1 d . . . . .
C31_1 C 0.4817(2) 1.07225(18) 0.83931(12) 0.0410(5) Uani 1 1 d . . . . .
H31A_1 H 0.552947 1.063451 0.862687 0.049 Uiso 1 1 calc R U . . .
H31B_1 H 0.517097 1.020290 0.795850 0.049 Uiso 1 1 calc R U . . .
C32_1 C 0.4407(3) 1.1853(2) 0.81594(15) 0.0558(7) Uani 1 1 d . . . . .
H32A_1 H 0.514215 1.196005 0.782279 0.084 Uiso 1 1 calc R U . . .
H32B_1 H 0.410661 1.238275 0.857943 0.084 Uiso 1 1 calc R U . . .
H32C_1 H 0.370497 1.195648 0.792282 0.084 Uiso 1 1 calc R U . . .
C33_1 C 0.3580(2) 0.78734(17) 0.98498(12) 0.0374(5) Uani 1 1 d . . . . .
H33A_1 H 0.426050 0.778229 1.010908 0.045 Uiso 1 1 calc R U . . .
H33B_1 H 0.396917 0.735517 0.941428 0.045 Uiso 1 1 calc R U . . .
C34_1 C 0.2512(2) 0.7555(2) 1.03254(14) 0.0499(6) Uani 1 1 d . . . . .
H34A_1 H 0.286972 0.680205 1.044367 0.075 Uiso 1 1 calc R U . . .
H34B_1 H 0.184180 0.761474 1.007123 0.075 Uiso 1 1 calc R U . . .
H34C_1 H 0.213442 0.804288 1.076833 0.075 Uiso 1 1 calc R U . . .
C35_1 C 0.83807(17) 0.68504(15) 0.77754(9) 0.0231(4) Uani 1 1 d . . . . .
C36_1 C 0.91714(17) 0.58356(15) 0.79262(9) 0.0240(4) Uani 1 1 d . . . . .
C37_1 C 1.02780(17) 0.52488(16) 0.73948(10) 0.0274(4) Uani 1 1 d . . . . .
H37_1 H 1.083170 0.456281 0.748656 0.033 Uiso 1 1 calc R U . . .
C38_1 C 1.05774(18) 0.56527(17) 0.67381(10) 0.0305(4) Uani 1 1 d . . . . .
H38_1 H 1.133225 0.524382 0.638244 0.037 Uiso 1 1 calc R U . . .
C39_1 C 0.97836(18) 0.66470(16) 0.65979(10) 0.0293(4) Uani 1 1 d . . . . .
H39_1 H 0.999431 0.690967 0.614161 0.035 Uiso 1 1 calc R U . . .
C40_1 C 0.86781(18) 0.72766(15) 0.71107(10) 0.0262(4) Uani 1 1 d . . . . .
C41_1 C 0.7898(2) 0.83831(16) 0.69285(11) 0.0345(5) Uani 1 1 d . . . . .
H41A_1 H 0.802615 0.836907 0.640099 0.041 Uiso 1 1 calc R U . . .
H41B_1 H 0.697054 0.851861 0.714367 0.041 Uiso 1 1 calc R U . . .
C42_1 C 0.8227(3) 0.9318(2) 0.71803(15) 0.0538(6) Uani 1 1 d . . . . .
H42A_1 H 0.770655 0.999674 0.702211 0.081 Uiso 1 1 calc R U . . .
H42B_1 H 0.914601 0.918919 0.697693 0.081 Uiso 1 1 calc R U . . .
H42C_1 H 0.804226 0.937544 0.770556 0.081 Uiso 1 1 calc R U . . .
C43_1 C 0.88334(18) 0.53720(16) 0.86359(10) 0.0292(4) Uani 1 1 d . . . . .
H43A_1 H 0.788154 0.558596 0.879230 0.035 Uiso 1 1 calc R U . . .
H43B_1 H 0.910683 0.571824 0.899627 0.035 Uiso 1 1 calc R U . . .
C44_1 C 0.9420(2) 0.41407(17) 0.86446(11) 0.0339(5) Uani 1 1 d . . . . .
H44A_1 H 0.907833 0.392662 0.911650 0.051 Uiso 1 1 calc R U . . .
H44B_1 H 1.036140 0.392177 0.854881 0.051 Uiso 1 1 calc R U . . .
H44C_1 H 0.919640 0.378119 0.827415 0.051 Uiso 1 1 calc R U . . .
C45_1 C 0.44527(18) 0.51690(15) 0.85394(9) 0.0243(4) Uani 1 1 d . . . . .
C46_1 C 0.4500(2) 0.47199(17) 0.91975(10) 0.0328(4) Uani 1 1 d . . . . .
H46_1 H 0.524241 0.461342 0.937422 0.039 Uiso 1 1 calc R U . . .
C47_1 C 0.3501(2) 0.44259(18) 0.95989(11) 0.0396(5) Uani 1 1 d . . . . .
H47_1 H 0.356934 0.411075 1.003904 0.048 Uiso 1 1 calc R U . . .
C48_1 C 0.2403(2) 0.45924(19) 0.93573(11) 0.0413(5) Uani 1 1 d . . . . .
H48_1 H 0.171002 0.439818 0.963148 0.050 Uiso 1 1 calc R U . . .
C49_1 C 0.2322(2) 0.50453(19) 0.87115(11) 0.0385(5) Uani 1 1 d . . . . .
H49_1 H 0.156887 0.516252 0.854285 0.046 Uiso 1 1 calc R U . . .
C50_1 C 0.33326(19) 0.53287(17) 0.83097(10) 0.0300(4) Uani 1 1 d . . . . .
H50_1 H 0.326009 0.563830 0.786819 0.036 Uiso 1 1 calc R U . . .
C51_1 C 0.69582(17) 0.42598(15) 0.76047(9) 0.0242(4) Uani 1 1 d . . . . .
C52_1 C 0.6920(2) 0.32484(16) 0.78204(11) 0.0319(4) Uani 1 1 d . . . . .
H52_1 H 0.619152 0.321808 0.817208 0.038 Uiso 1 1 calc R U . . .
C53_1 C 0.7930(2) 0.22868(17) 0.75292(12) 0.0397(5) Uani 1 1 d . . . . .
H53_1 H 0.788607 0.160778 0.768280 0.048 Uiso 1 1 calc R U . . .
C54_1 C 0.9000(2) 0.23161(18) 0.70151(12) 0.0414(5) Uani 1 1 d . . . . .
H54_1 H 0.968988 0.165925 0.681560 0.050 Uiso 1 1 calc R U . . .
C55_1 C 0.90556(19) 0.33045(18) 0.67956(11) 0.0357(5) Uani 1 1 d . . . . .
H55_1 H 0.978835 0.332833 0.644467 0.043 Uiso 1 1 calc R U . . .
C56_1 C 0.80478(17) 0.42653(16) 0.70843(10) 0.0271(4) Uani 1 1 d . . . . .
H56_1 H 0.809890 0.493978 0.692537 0.033 Uiso 1 1 calc R U . . .
C57_1 C 0.4740(2) 0.36853(18) 0.65944(11) 0.0409(5) Uani 1 1 d . . . . .
H57A_1 H 0.411578 0.436226 0.687945 0.049 Uiso 1 1 calc R U . . .
H57B_1 H 0.503187 0.314589 0.693461 0.049 Uiso 1 1 calc R U . . .
C58_1 C 0.4061(3) 0.3246(2) 0.61405(14) 0.0493(6) Uani 1 1 d . . . . .
H58A_1 H 0.334447 0.308200 0.645470 0.074 Uiso 1 1 calc R U . . .
H58B_1 H 0.467517 0.257947 0.585257 0.074 Uiso 1 1 calc R U . . .
H58C_1 H 0.372474 0.379317 0.582138 0.074 Uiso 1 1 calc R U . . .
C4_1 C 0.29224(19) 0.86838(16) 0.70586(10) 0.0307(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1_1 C1_1 1.553(2) . ?
B1_1 B2_1 1.567(3) . ?
B1_1 P1_1 1.945(2) . ?
N1_1 C1_1 1.374(2) . ?
N1_1 C14_1 1.437(2) . ?
N1_1 C2_1 1.471(2) . ?
P1_1 C51_1 1.8361(18) . ?
P1_1 C45_1 1.8410(19) . ?
C1_1 N2_1 1.365(2) . ?
B2_1 C22_1 1.583(3) . ?
B2_1 H1_1 1.08(2) . ?
N2_1 C4_1 1.438(2) . ?
N2_1 C3_1 1.468(2) . ?
C2_1 C3_1 1.492(3) . ?
C2_1 H2A_1 0.9900 . ?
C2_1 H2AB_1 0.9900 . ?
N3_1 C22_1 1.366(2) . ?
N3_1 C35_1 1.438(2) . ?
N3_1 C23_1 1.479(2) . ?
C3_1 H3A_1 0.9900 . ?
C3_1 H3AB_1 0.9900 . ?
N4_1 C22_1 1.351(2) . ?
N4_1 C25_1 1.438(2) . ?
N4_1 C24_1 1.470(2) . ?
C5_1 C6_1 1.392(3) . ?
C5_1 C4_1 1.396(3) . ?
C5_1 C12_1 1.509(3) . ?
C6_1 C7_1 1.380(4) . ?
C6_1 H6_1 0.9500 . ?
C7_1 C8_1 1.378(4) . ?
C7_1 H7_1 0.9500 . ?
C8_1 C9_1 1.401(3) . ?
C8_1 H8_1 0.9500 . ?
C9_1 C4_1 1.402(3) . ?
C9_1 C10_1 1.506(4) . ?
C10_1 C11_1 1.487(4) . ?
C10_1 H10A_1 0.9900 . ?
C10_1 H10B_1 0.9900 . ?
C11_1 H11A_1 0.9800 . ?
C11_1 H11B_1 0.9800 . ?
C11_1 H11C_1 0.9800 . ?
C12_1 C13_1 1.513(3) . ?
C12_1 H12A_1 0.9900 . ?
C12_1 H12B_1 0.9900 . ?
C13_1 H13A_1 0.9800 . ?
C13_1 H13B_1 0.9800 . ?
C13_1 H13C_1 0.9800 . ?
C14_1 C15_1 1.395(3) . ?
C14_1 C19_1 1.410(3) . ?
C15_1 C16_1 1.399(3) . ?
C15_1 C57_1 1.505(3) . ?
C16_1 C17_1 1.376(3) . ?
C16_1 H16_1 0.9500 . ?
C17_1 C18_1 1.379(3) . ?
C17_1 H17_1 0.9500 . ?
C18_1 C19_1 1.396(3) . ?
C18_1 H18_1 0.9500 . ?
C19_1 C20_1 1.507(3) . ?
C20_1 C21_1 1.525(3) . ?
C20_1 H20A_1 0.9900 . ?
C20_1 H20B_1 0.9900 . ?
C21_1 H21A_1 0.9800 . ?
C21_1 H21B_1 0.9800 . ?
C21_1 H21C_1 0.9800 . ?
C23_1 C24_1 1.511(3) . ?
C23_1 H23A_1 0.9900 . ?
C23_1 H23B_1 0.9900 . ?
C24_1 H24A_1 0.9900 . ?
C24_1 H24B_1 0.9900 . ?
C25_1 C30_1 1.395(3) . ?
C25_1 C26_1 1.400(3) . ?
C26_1 C27_1 1.399(3) . ?
C26_1 C33_1 1.512(3) . ?
C27_1 C28_1 1.380(3) . ?
C27_1 H27_1 0.9500 . ?
C28_1 C29_1 1.380(3) . ?
C28_1 H28_1 0.9500 . ?
C29_1 C30_1 1.395(3) . ?
C29_1 H29_1 0.9500 . ?
C30_1 C31_1 1.512(3) . ?
C31_1 C32_1 1.497(3) . ?
C31_1 H31A_1 0.9900 . ?
C31_1 H31B_1 0.9900 . ?
C32_1 H32A_1 0.9800 . ?
C32_1 H32B_1 0.9800 . ?
C32_1 H32C_1 0.9800 . ?
C33_1 C34_1 1.518(3) . ?
C33_1 H33A_1 0.9900 . ?
C33_1 H33B_1 0.9900 . ?
C34_1 H34A_1 0.9800 . ?
C34_1 H34B_1 0.9800 . ?
C34_1 H34C_1 0.9800 . ?
C35_1 C36_1 1.403(3) . ?
C35_1 C40_1 1.409(3) . ?
C36_1 C37_1 1.398(2) . ?
C36_1 C43_1 1.513(3) . ?
C37_1 C38_1 1.382(3) . ?
C37_1 H37_1 0.9500 . ?
C38_1 C39_1 1.378(3) . ?
C38_1 H38_1 0.9500 . ?
C39_1 C40_1 1.395(3) . ?
C39_1 H39_1 0.9500 . ?
C40_1 C41_1 1.511(3) . ?
C41_1 C42_1 1.506(3) . ?
C41_1 H41A_1 0.9900 . ?
C41_1 H41B_1 0.9900 . ?
C42_1 H42A_1 0.9800 . ?
C42_1 H42B_1 0.9800 . ?
C42_1 H42C_1 0.9800 . ?
C43_1 C44_1 1.523(3) . ?
C43_1 H43A_1 0.9900 . ?
C43_1 H43B_1 0.9900 . ?
C44_1 H44A_1 0.9800 . ?
C44_1 H44B_1 0.9800 . ?
C44_1 H44C_1 0.9800 . ?
C45_1 C50_1 1.394(3) . ?
C45_1 C46_1 1.401(3) . ?
C46_1 C47_1 1.384(3) . ?
C46_1 H46_1 0.9500 . ?
C47_1 C48_1 1.381(3) . ?
C47_1 H47_1 0.9500 . ?
C48_1 C49_1 1.386(3) . ?
C48_1 H48_1 0.9500 . ?
C49_1 C50_1 1.387(3) . ?
C49_1 H49_1 0.9500 . ?
C50_1 H50_1 0.9500 . ?
C51_1 C52_1 1.399(3) . ?
C51_1 C56_1 1.399(3) . ?
C52_1 C53_1 1.390(3) . ?
C52_1 H52_1 0.9500 . ?
C53_1 C54_1 1.387(3) . ?
C53_1 H53_1 0.9500 . ?
C54_1 C55_1 1.378(3) . ?
C54_1 H54_1 0.9500 . ?
C55_1 C56_1 1.388(3) . ?
C55_1 H55_1 0.9500 . ?
C56_1 H56_1 0.9500 . ?
C57_1 C58_1 1.520(3) . ?
C57_1 H57A_1 0.9900 . ?
C57_1 H57B_1 0.9900 . ?
C58_1 H58A_1 0.9800 . ?
C58_1 H58B_1 0.9800 . ?
C58_1 H58C_1 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1_1 B1_1 B2_1 121.30(16) . . ?
C1_1 B1_1 P1_1 128.01(14) . . ?
B2_1 B1_1 P1_1 110.05(13) . . ?
C1_1 N1_1 C14_1 127.53(14) . . ?
C1_1 N1_1 C2_1 112.69(14) . . ?
C14_1 N1_1 C2_1 114.26(13) . . ?
C51_1 P1_1 C45_1 100.95(8) . . ?
C51_1 P1_1 B1_1 117.36(8) . . ?
C45_1 P1_1 B1_1 109.65(8) . . ?
N2_1 C1_1 N1_1 106.00(14) . . ?
N2_1 C1_1 B1_1 126.15(15) . . ?
N1_1 C1_1 B1_1 127.84(15) . . ?
B1_1 B2_1 C22_1 127.46(17) . . ?
B1_1 B2_1 H1_1 126.0(12) . . ?
C22_1 B2_1 H1_1 106.6(12) . . ?
C1_1 N2_1 C4_1 130.23(15) . . ?
C1_1 N2_1 C3_1 113.93(14) . . ?
C4_1 N2_1 C3_1 115.74(14) . . ?
N1_1 C2_1 C3_1 104.22(14) . . ?
N1_1 C2_1 H2A_1 110.9 . . ?
C3_1 C2_1 H2A_1 110.9 . . ?
N1_1 C2_1 H2AB_1 110.9 . . ?
C3_1 C2_1 H2AB_1 110.9 . . ?
H2A_1 C2_1 H2AB_1 108.9 . . ?
C22_1 N3_1 C35_1 128.69(14) . . ?
C22_1 N3_1 C23_1 111.62(14) . . ?
C35_1 N3_1 C23_1 117.92(14) . . ?
N2_1 C3_1 C2_1 103.12(14) . . ?
N2_1 C3_1 H3A_1 111.1 . . ?
C2_1 C3_1 H3A_1 111.1 . . ?
N2_1 C3_1 H3AB_1 111.1 . . ?
C2_1 C3_1 H3AB_1 111.1 . . ?
H3A_1 C3_1 H3AB_1 109.1 . . ?
C22_1 N4_1 C25_1 127.44(15) . . ?
C22_1 N4_1 C24_1 113.04(15) . . ?
C25_1 N4_1 C24_1 119.52(14) . . ?
C6_1 C5_1 C4_1 117.6(2) . . ?
C6_1 C5_1 C12_1 122.4(2) . . ?
C4_1 C5_1 C12_1 120.06(18) . . ?
C7_1 C6_1 C5_1 121.3(2) . . ?
C7_1 C6_1 H6_1 119.4 . . ?
C5_1 C6_1 H6_1 119.4 . . ?
C8_1 C7_1 C6_1 120.1(2) . . ?
C8_1 C7_1 H7_1 120.0 . . ?
C6_1 C7_1 H7_1 120.0 . . ?
C7_1 C8_1 C9_1 121.3(2) . . ?
C7_1 C8_1 H8_1 119.3 . . ?
C9_1 C8_1 H8_1 119.3 . . ?
C8_1 C9_1 C4_1 117.0(2) . . ?
C8_1 C9_1 C10_1 120.5(2) . . ?
C4_1 C9_1 C10_1 122.51(19) . . ?
C11_1 C10_1 C9_1 114.3(2) . . ?
C11_1 C10_1 H10A_1 108.7 . . ?
C9_1 C10_1 H10A_1 108.7 . . ?
C11_1 C10_1 H10B_1 108.7 . . ?
C9_1 C10_1 H10B_1 108.7 . . ?
H10A_1 C10_1 H10B_1 107.6 . . ?
C10_1 C11_1 H11A_1 109.5 . . ?
C10_1 C11_1 H11B_1 109.5 . . ?
H11A_1 C11_1 H11B_1 109.5 . . ?
C10_1 C11_1 H11C_1 109.5 . . ?
H11A_1 C11_1 H11C_1 109.5 . . ?
H11B_1 C11_1 H11C_1 109.5 . . ?
C5_1 C12_1 C13_1 116.4(2) . . ?
C5_1 C12_1 H12A_1 108.2 . . ?
C13_1 C12_1 H12A_1 108.2 . . ?
C5_1 C12_1 H12B_1 108.2 . . ?
C13_1 C12_1 H12B_1 108.2 . . ?
H12A_1 C12_1 H12B_1 107.3 . . ?
C12_1 C13_1 H13A_1 109.5 . . ?
C12_1 C13_1 H13B_1 109.5 . . ?
H13A_1 C13_1 H13B_1 109.5 . . ?
C12_1 C13_1 H13C_1 109.5 . . ?
H13A_1 C13_1 H13C_1 109.5 . . ?
H13B_1 C13_1 H13C_1 109.5 . . ?
C15_1 C14_1 C19_1 121.72(17) . . ?
C15_1 C14_1 N1_1 118.66(16) . . ?
C19_1 C14_1 N1_1 118.87(16) . . ?
C14_1 C15_1 C16_1 118.14(19) . . ?
C14_1 C15_1 C57_1 122.12(18) . . ?
C16_1 C15_1 C57_1 119.74(19) . . ?
C17_1 C16_1 C15_1 121.0(2) . . ?
C17_1 C16_1 H16_1 119.5 . . ?
C15_1 C16_1 H16_1 119.5 . . ?
C16_1 C17_1 C18_1 120.19(19) . . ?
C16_1 C17_1 H17_1 119.9 . . ?
C18_1 C17_1 H17_1 119.9 . . ?
C17_1 C18_1 C19_1 121.3(2) . . ?
C17_1 C18_1 H18_1 119.4 . . ?
C19_1 C18_1 H18_1 119.4 . . ?
C18_1 C19_1 C14_1 117.64(18) . . ?
C18_1 C19_1 C20_1 121.83(18) . . ?
C14_1 C19_1 C20_1 120.53(16) . . ?
C19_1 C20_1 C21_1 116.62(17) . . ?
C19_1 C20_1 H20A_1 108.1 . . ?
C21_1 C20_1 H20A_1 108.1 . . ?
C19_1 C20_1 H20B_1 108.1 . . ?
C21_1 C20_1 H20B_1 108.1 . . ?
H20A_1 C20_1 H20B_1 107.3 . . ?
C20_1 C21_1 H21A_1 109.5 . . ?
C20_1 C21_1 H21B_1 109.5 . . ?
H21A_1 C21_1 H21B_1 109.5 . . ?
C20_1 C21_1 H21C_1 109.5 . . ?
H21A_1 C21_1 H21C_1 109.5 . . ?
H21B_1 C21_1 H21C_1 109.5 . . ?
N4_1 C22_1 N3_1 107.75(15) . . ?
N4_1 C22_1 B2_1 121.97(16) . . ?
N3_1 C22_1 B2_1 130.10(15) . . ?
N3_1 C23_1 C24_1 103.32(14) . . ?
N3_1 C23_1 H23A_1 111.1 . . ?
C24_1 C23_1 H23A_1 111.1 . . ?
N3_1 C23_1 H23B_1 111.1 . . ?
C24_1 C23_1 H23B_1 111.1 . . ?
H23A_1 C23_1 H23B_1 109.1 . . ?
N4_1 C24_1 C23_1 102.64(14) . . ?
N4_1 C24_1 H24A_1 111.2 . . ?
C23_1 C24_1 H24A_1 111.2 . . ?
N4_1 C24_1 H24B_1 111.2 . . ?
C23_1 C24_1 H24B_1 111.2 . . ?
H24A_1 C24_1 H24B_1 109.2 . . ?
C30_1 C25_1 C26_1 122.76(17) . . ?
C30_1 C25_1 N4_1 117.94(17) . . ?
C26_1 C25_1 N4_1 119.04(17) . . ?
C27_1 C26_1 C25_1 117.10(18) . . ?
C27_1 C26_1 C33_1 122.51(18) . . ?
C25_1 C26_1 C33_1 120.38(17) . . ?
C28_1 C27_1 C26_1 120.99(19) . . ?
C28_1 C27_1 H27_1 119.5 . . ?
C26_1 C27_1 H27_1 119.5 . . ?
C27_1 C28_1 C29_1 120.81(18) . . ?
C27_1 C28_1 H28_1 119.6 . . ?
C29_1 C28_1 H28_1 119.6 . . ?
C28_1 C29_1 C30_1 120.39(19) . . ?
C28_1 C29_1 H29_1 119.8 . . ?
C30_1 C29_1 H29_1 119.8 . . ?
C29_1 C30_1 C25_1 117.94(18) . . ?
C29_1 C30_1 C31_1 121.91(19) . . ?
C25_1 C30_1 C31_1 120.15(17) . . ?
C32_1 C31_1 C30_1 116.8(2) . . ?
C32_1 C31_1 H31A_1 108.1 . . ?
C30_1 C31_1 H31A_1 108.1 . . ?
C32_1 C31_1 H31B_1 108.1 . . ?
C30_1 C31_1 H31B_1 108.1 . . ?
H31A_1 C31_1 H31B_1 107.3 . . ?
C31_1 C32_1 H32A_1 109.5 . . ?
C31_1 C32_1 H32B_1 109.5 . . ?
H32A_1 C32_1 H32B_1 109.5 . . ?
C31_1 C32_1 H32C_1 109.5 . . ?
H32A_1 C32_1 H32C_1 109.5 . . ?
H32B_1 C32_1 H32C_1 109.5 . . ?
C26_1 C33_1 C34_1 116.48(18) . . ?
C26_1 C33_1 H33A_1 108.2 . . ?
C34_1 C33_1 H33A_1 108.2 . . ?
C26_1 C33_1 H33B_1 108.2 . . ?
C34_1 C33_1 H33B_1 108.2 . . ?
H33A_1 C33_1 H33B_1 107.3 . . ?
C33_1 C34_1 H34A_1 109.5 . . ?
C33_1 C34_1 H34B_1 109.5 . . ?
H34A_1 C34_1 H34B_1 109.5 . . ?
C33_1 C34_1 H34C_1 109.5 . . ?
H34A_1 C34_1 H34C_1 109.5 . . ?
H34B_1 C34_1 H34C_1 109.5 . . ?
C36_1 C35_1 C40_1 121.67(16) . . ?
C36_1 C35_1 N3_1 118.11(16) . . ?
C40_1 C35_1 N3_1 119.98(16) . . ?
C37_1 C36_1 C35_1 118.06(17) . . ?
C37_1 C36_1 C43_1 120.50(17) . . ?
C35_1 C36_1 C43_1 121.43(16) . . ?
C38_1 C37_1 C36_1 120.94(18) . . ?
C38_1 C37_1 H37_1 119.5 . . ?
C36_1 C37_1 H37_1 119.5 . . ?
C39_1 C38_1 C37_1 120.15(17) . . ?
C39_1 C38_1 H38_1 119.9 . . ?
C37_1 C38_1 H38_1 119.9 . . ?
C38_1 C39_1 C40_1 121.50(18) . . ?
C38_1 C39_1 H39_1 119.3 . . ?
C40_1 C39_1 H39_1 119.3 . . ?
C39_1 C40_1 C35_1 117.67(17) . . ?
C39_1 C40_1 C41_1 118.19(17) . . ?
C35_1 C40_1 C41_1 124.11(17) . . ?
C42_1 C41_1 C40_1 114.80(19) . . ?
C42_1 C41_1 H41A_1 108.6 . . ?
C40_1 C41_1 H41A_1 108.6 . . ?
C42_1 C41_1 H41B_1 108.6 . . ?
C40_1 C41_1 H41B_1 108.6 . . ?
H41A_1 C41_1 H41B_1 107.5 . . ?
C41_1 C42_1 H42A_1 109.5 . . ?
C41_1 C42_1 H42B_1 109.5 . . ?
H42A_1 C42_1 H42B_1 109.5 . . ?
C41_1 C42_1 H42C_1 109.5 . . ?
H42A_1 C42_1 H42C_1 109.5 . . ?
H42B_1 C42_1 H42C_1 109.5 . . ?
C36_1 C43_1 C44_1 116.55(16) . . ?
C36_1 C43_1 H43A_1 108.2 . . ?
C44_1 C43_1 H43A_1 108.2 . . ?
C36_1 C43_1 H43B_1 108.2 . . ?
C44_1 C43_1 H43B_1 108.2 . . ?
H43A_1 C43_1 H43B_1 107.3 . . ?
C43_1 C44_1 H44A_1 109.5 . . ?
C43_1 C44_1 H44B_1 109.5 . . ?
H44A_1 C44_1 H44B_1 109.5 . . ?
C43_1 C44_1 H44C_1 109.5 . . ?
H44A_1 C44_1 H44C_1 109.5 . . ?
H44B_1 C44_1 H44C_1 109.5 . . ?
C50_1 C45_1 C46_1 116.74(17) . . ?
C50_1 C45_1 P1_1 124.62(14) . . ?
C46_1 C45_1 P1_1 118.56(14) . . ?
C47_1 C46_1 C45_1 122.18(19) . . ?
C47_1 C46_1 H46_1 118.9 . . ?
C45_1 C46_1 H46_1 118.9 . . ?
C48_1 C47_1 C46_1 119.79(19) . . ?
C48_1 C47_1 H47_1 120.1 . . ?
C46_1 C47_1 H47_1 120.1 . . ?
C47_1 C48_1 C49_1 119.4(2) . . ?
C47_1 C48_1 H48_1 120.3 . . ?
C49_1 C48_1 H48_1 120.3 . . ?
C48_1 C49_1 C50_1 120.4(2) . . ?
C48_1 C49_1 H49_1 119.8 . . ?
C50_1 C49_1 H49_1 119.8 . . ?
C49_1 C50_1 C45_1 121.46(18) . . ?
C49_1 C50_1 H50_1 119.3 . . ?
C45_1 C50_1 H50_1 119.3 . . ?
C52_1 C51_1 C56_1 117.47(17) . . ?
C52_1 C51_1 P1_1 123.82(15) . . ?
C56_1 C51_1 P1_1 117.90(14) . . ?
C53_1 C52_1 C51_1 121.1(2) . . ?
C53_1 C52_1 H52_1 119.4 . . ?
C51_1 C52_1 H52_1 119.4 . . ?
C54_1 C53_1 C52_1 120.2(2) . . ?
C54_1 C53_1 H53_1 119.9 . . ?
C52_1 C53_1 H53_1 119.9 . . ?
C55_1 C54_1 C53_1 119.53(19) . . ?
C55_1 C54_1 H54_1 120.2 . . ?
C53_1 C54_1 H54_1 120.2 . . ?
C54_1 C55_1 C56_1 120.4(2) . . ?
C54_1 C55_1 H55_1 119.8 . . ?
C56_1 C55_1 H55_1 119.8 . . ?
C55_1 C56_1 C51_1 121.27(19) . . ?
C55_1 C56_1 H56_1 119.4 . . ?
C51_1 C56_1 H56_1 119.4 . . ?
C15_1 C57_1 C58_1 113.13(18) . . ?
C15_1 C57_1 H57A_1 109.0 . . ?
C58_1 C57_1 H57A_1 109.0 . . ?
C15_1 C57_1 H57B_1 109.0 . . ?
C58_1 C57_1 H57B_1 109.0 . . ?
H57A_1 C57_1 H57B_1 107.8 . . ?
C57_1 C58_1 H58A_1 109.5 . . ?
C57_1 C58_1 H58B_1 109.5 . . ?
H58A_1 C58_1 H58B_1 109.5 . . ?
C57_1 C58_1 H58C_1 109.5 . . ?
H58A_1 C58_1 H58C_1 109.5 . . ?
H58B_1 C58_1 H58C_1 109.5 . . ?
C5_1 C4_1 C9_1 122.73(19) . . ?
C5_1 C4_1 N2_1 117.86(18) . . ?
C9_1 C4_1 N2_1 119.00(19) . . ?

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
C14_1 N1_1 C1_1 N2_1 150.13(17) . . . . ?
C2_1 N1_1 C1_1 N2_1 -1.9(2) . . . . ?
C14_1 N1_1 C1_1 B1_1 -30.9(3) . . . . ?
C2_1 N1_1 C1_1 B1_1 177.14(17) . . . . ?
B2_1 B1_1 C1_1 N2_1 -26.2(3) . . . . ?
P1_1 B1_1 C1_1 N2_1 143.68(16) . . . . ?
B2_1 B1_1 C1_1 N1_1 154.97(17) . . . . ?
P1_1 B1_1 C1_1 N1_1 -35.2(3) . . . . ?
C1_1 B1_1 B2_1 C22_1 -177.10(16) . . . . ?
P1_1 B1_1 B2_1 C22_1 11.4(2) . . . . ?
N1_1 C1_1 N2_1 C4_1 176.77(18) . . . . ?
B1_1 C1_1 N2_1 C4_1 -2.3(3) . . . . ?
N1_1 C1_1 N2_1 C3_1 0.7(2) . . . . ?
B1_1 C1_1 N2_1 C3_1 -178.33(17) . . . . ?
C1_1 N1_1 C2_1 C3_1 2.3(2) . . . . ?
C14_1 N1_1 C2_1 C3_1 -153.64(16) . . . . ?
C1_1 N2_1 C3_1 C2_1 0.7(2) . . . . ?
C4_1 N2_1 C3_1 C2_1 -176.01(17) . . . . ?
N1_1 C2_1 C3_1 N2_1 -1.6(2) . . . . ?
C4_1 C5_1 C6_1 C7_1 -0.3(3) . . . . ?
C12_1 C5_1 C6_1 C7_1 -179.06(19) . . . . ?
C5_1 C6_1 C7_1 C8_1 -0.8(3) . . . . ?
C6_1 C7_1 C8_1 C9_1 0.8(3) . . . . ?
C7_1 C8_1 C9_1 C4_1 0.3(3) . . . . ?
C7_1 C8_1 C9_1 C10_1 -179.5(2) . . . . ?
C8_1 C9_1 C10_1 C11_1 -56.4(3) . . . . ?
C4_1 C9_1 C10_1 C11_1 123.8(3) . . . . ?
C6_1 C5_1 C12_1 C13_1 9.9(3) . . . . ?
C4_1 C5_1 C12_1 C13_1 -168.8(2) . . . . ?
C1_1 N1_1 C14_1 C15_1 126.95(18) . . . . ?
C2_1 N1_1 C14_1 C15_1 -81.4(2) . . . . ?
C1_1 N1_1 C14_1 C19_1 -62.8(2) . . . . ?
C2_1 N1_1 C14_1 C19_1 88.84(19) . . . . ?
C19_1 C14_1 C15_1 C16_1 0.9(3) . . . . ?
N1_1 C14_1 C15_1 C16_1 170.90(15) . . . . ?
C19_1 C14_1 C15_1 C57_1 -178.75(16) . . . . ?
N1_1 C14_1 C15_1 C57_1 -8.8(2) . . . . ?
C14_1 C15_1 C16_1 C17_1 -1.6(3) . . . . ?
C57_1 C15_1 C16_1 C17_1 178.12(18) . . . . ?
C15_1 C16_1 C17_1 C18_1 1.4(3) . . . . ?
C16_1 C17_1 C18_1 C19_1 -0.5(3) . . . . ?
C17_1 C18_1 C19_1 C14_1 -0.1(3) . . . . ?
C17_1 C18_1 C19_1 C20_1 179.55(17) . . . . ?
C15_1 C14_1 C19_1 C18_1 -0.1(2) . . . . ?
N1_1 C14_1 C19_1 C18_1 -170.06(15) . . . . ?
C15_1 C14_1 C19_1 C20_1 -179.78(16) . . . . ?
N1_1 C14_1 C19_1 C20_1 10.3(2) . . . . ?
C18_1 C19_1 C20_1 C21_1 3.4(3) . . . . ?
C14_1 C19_1 C20_1 C21_1 -176.96(17) . . . . ?
C25_1 N4_1 C22_1 N3_1 175.61(17) . . . . ?
C24_1 N4_1 C22_1 N3_1 -4.0(2) . . . . ?
C25_1 N4_1 C22_1 B2_1 0.0(3) . . . . ?
C24_1 N4_1 C22_1 B2_1 -179.63(17) . . . . ?
C35_1 N3_1 C22_1 N4_1 -169.05(17) . . . . ?
C23_1 N3_1 C22_1 N4_1 -4.8(2) . . . . ?
C35_1 N3_1 C22_1 B2_1 6.1(3) . . . . ?
C23_1 N3_1 C22_1 B2_1 170.36(19) . . . . ?
B1_1 B2_1 C22_1 N4_1 -124.8(2) . . . . ?
B1_1 B2_1 C22_1 N3_1 60.7(3) . . . . ?
C22_1 N3_1 C23_1 C24_1 11.0(2) . . . . ?
C35_1 N3_1 C23_1 C24_1 177.19(16) . . . . ?
C22_1 N4_1 C24_1 C23_1 10.6(2) . . . . ?
C25_1 N4_1 C24_1 C23_1 -169.08(17) . . . . ?
N3_1 C23_1 C24_1 N4_1 -12.1(2) . . . . ?
C22_1 N4_1 C25_1 C30_1 -89.1(2) . . . . ?
C24_1 N4_1 C25_1 C30_1 90.5(2) . . . . ?
C22_1 N4_1 C25_1 C26_1 96.5(2) . . . . ?
C24_1 N4_1 C25_1 C26_1 -83.8(2) . . . . ?
C30_1 C25_1 C26_1 C27_1 -0.4(3) . . . . ?
N4_1 C25_1 C26_1 C27_1 173.69(16) . . . . ?
C30_1 C25_1 C26_1 C33_1 179.36(17) . . . . ?
N4_1 C25_1 C26_1 C33_1 -6.6(3) . . . . ?
C25_1 C26_1 C27_1 C28_1 0.4(3) . . . . ?
C33_1 C26_1 C27_1 C28_1 -179.33(19) . . . . ?
C26_1 C27_1 C28_1 C29_1 0.1(3) . . . . ?
C27_1 C28_1 C29_1 C30_1 -0.7(3) . . . . ?
C28_1 C29_1 C30_1 C25_1 0.7(3) . . . . ?
C28_1 C29_1 C30_1 C31_1 -178.76(18) . . . . ?
C26_1 C25_1 C30_1 C29_1 -0.2(3) . . . . ?
N4_1 C25_1 C30_1 C29_1 -174.30(15) . . . . ?
C26_1 C25_1 C30_1 C31_1 179.30(17) . . . . ?
N4_1 C25_1 C30_1 C31_1 5.2(2) . . . . ?
C29_1 C30_1 C31_1 C32_1 -0.8(3) . . . . ?
C25_1 C30_1 C31_1 C32_1 179.8(2) . . . . ?
C27_1 C26_1 C33_1 C34_1 3.7(3) . . . . ?
C25_1 C26_1 C33_1 C34_1 -175.99(19) . . . . ?
C22_1 N3_1 C35_1 C36_1 -126.48(19) . . . . ?
C23_1 N3_1 C35_1 C36_1 70.1(2) . . . . ?
C22_1 N3_1 C35_1 C40_1 59.1(3) . . . . ?
C23_1 N3_1 C35_1 C40_1 -104.4(2) . . . . ?
C40_1 C35_1 C36_1 C37_1 0.1(3) . . . . ?
N3_1 C35_1 C36_1 C37_1 -174.24(15) . . . . ?
C40_1 C35_1 C36_1 C43_1 -178.81(16) . . . . ?
N3_1 C35_1 C36_1 C43_1 6.9(2) . . . . ?
C35_1 C36_1 C37_1 C38_1 -0.6(3) . . . . ?
C43_1 C36_1 C37_1 C38_1 178.34(17) . . . . ?
C36_1 C37_1 C38_1 C39_1 0.1(3) . . . . ?
C37_1 C38_1 C39_1 C40_1 0.9(3) . . . . ?
C38_1 C39_1 C40_1 C35_1 -1.4(3) . . . . ?
C38_1 C39_1 C40_1 C41_1 176.86(18) . . . . ?
C36_1 C35_1 C40_1 C39_1 0.9(3) . . . . ?
N3_1 C35_1 C40_1 C39_1 175.07(16) . . . . ?
C36_1 C35_1 C40_1 C41_1 -177.27(17) . . . . ?
N3_1 C35_1 C40_1 C41_1 -3.1(3) . . . . ?
C39_1 C40_1 C41_1 C42_1 -94.4(2) . . . . ?
C35_1 C40_1 C41_1 C42_1 83.8(2) . . . . ?
C37_1 C36_1 C43_1 C44_1 -21.6(3) . . . . ?
C35_1 C36_1 C43_1 C44_1 157.24(17) . . . . ?
C51_1 P1_1 C45_1 C50_1 -100.72(17) . . . . ?
B1_1 P1_1 C45_1 C50_1 23.76(18) . . . . ?
C51_1 P1_1 C45_1 C46_1 82.74(16) . . . . ?
B1_1 P1_1 C45_1 C46_1 -152.78(15) . . . . ?
C50_1 C45_1 C46_1 C47_1 1.2(3) . . . . ?
P1_1 C45_1 C46_1 C47_1 178.01(16) . . . . ?
C45_1 C46_1 C47_1 C48_1 -1.2(3) . . . . ?
C46_1 C47_1 C48_1 C49_1 0.5(3) . . . . ?
C47_1 C48_1 C49_1 C50_1 0.1(3) . . . . ?
C48_1 C49_1 C50_1 C45_1 0.0(3) . . . . ?
C46_1 C45_1 C50_1 C49_1 -0.6(3) . . . . ?
P1_1 C45_1 C50_1 C49_1 -177.21(16) . . . . ?
C45_1 P1_1 C51_1 C52_1 -21.23(17) . . . . ?
B1_1 P1_1 C51_1 C52_1 -140.29(15) . . . . ?
C45_1 P1_1 C51_1 C56_1 169.44(13) . . . . ?
B1_1 P1_1 C51_1 C56_1 50.37(16) . . . . ?
C56_1 C51_1 C52_1 C53_1 0.2(3) . . . . ?
P1_1 C51_1 C52_1 C53_1 -169.21(15) . . . . ?
C51_1 C52_1 C53_1 C54_1 0.0(3) . . . . ?
C52_1 C53_1 C54_1 C55_1 0.0(3) . . . . ?
C53_1 C54_1 C55_1 C56_1 -0.2(3) . . . . ?
C54_1 C55_1 C56_1 C51_1 0.3(3) . . . . ?
C52_1 C51_1 C56_1 C55_1 -0.3(3) . . . . ?
P1_1 C51_1 C56_1 C55_1 169.70(14) . . . . ?
C14_1 C15_1 C57_1 C58_1 111.9(2) . . . . ?
C16_1 C15_1 C57_1 C58_1 -67.8(2) . . . . ?
C6_1 C5_1 C4_1 C9_1 1.4(3) . . . . ?
C12_1 C5_1 C4_1 C9_1 -179.80(18) . . . . ?
C6_1 C5_1 C4_1 N2_1 174.02(16) . . . . ?
C12_1 C5_1 C4_1 N2_1 -7.2(3) . . . . ?
C8_1 C9_1 C4_1 C5_1 -1.4(3) . . . . ?
C10_1 C9_1 C4_1 C5_1 178.4(2) . . . . ?
C8_1 C9_1 C4_1 N2_1 -173.93(17) . . . . ?
C10_1 C9_1 C4_1 N2_1 5.8(3) . . . . ?
C1_1 N2_1 C4_1 C5_1 96.6(2) . . . . ?
C3_1 N2_1 C4_1 C5_1 -87.4(2) . . . . ?
C1_1 N2_1 C4_1 C9_1 -90.5(2) . . . . ?
C3_1 N2_1 C4_1 C9_1 85.5(2) . . . . ?

_refine_diff_density_max         0.670
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.046



