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

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

data_Me2S-BI3
_database_code_depnum_ccdc_archive 'CCDC 2106474'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            'boron trichloride dimethyl sulfide'
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H6 B I3 S'
_chemical_formula_sum            'C2 H6 B I3 S'
_chemical_formula_weight         453.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.0765(4)
_cell_length_b                   7.2293(3)
_cell_length_c                   18.9898(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.749(2)
_cell_angle_gamma                90
_cell_volume                     970.36(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9876
_cell_measurement_theta_min      4.66
_cell_measurement_theta_max      74.02

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.105
_exptl_crystal_F_000             792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.066
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.056
_exptl_absorpt_coefficient_mu    77.206
_shelx_estimated_absorpt_T_min   0.080
_shelx_estimated_absorpt_T_max   0.098
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.0409
_exptl_absorpt_correction_T_max  0.1985
_exptl_absorpt_process_details   
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37103
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.662
_diffrn_reflns_theta_max         74.732
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1973
_reflns_number_gt                1912
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0455P)²+3.8870P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00096(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1973
_refine_ls_number_parameters     67
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0787
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
I1 I 0.75386(6) 0.38940(5) 0.36928(2) 0.03811(14) Uani 1 1 d . . . . .
I2 I 0.85370(5) 0.82935(5) 0.28063(2) 0.03675(14) Uani 1 1 d . . . . .
I3 I 0.78212(6) 0.82421(5) 0.47004(2) 0.03992(15) Uani 1 1 d . . . . .
S1 S 0.43903(17) 0.72065(18) 0.34013(7) 0.0299(3) Uani 1 1 d . . . . .
C1 C 0.3909(9) 0.9647(8) 0.3469(4) 0.0410(13) Uani 1 1 d . . . . .
H1A H 0.254599 0.986161 0.339898 0.049 Uiso 1 1 calc R U . . .
H1B H 0.458065 1.031594 0.310867 0.049 Uiso 1 1 calc R U . . .
H1C H 0.433977 1.008957 0.393787 0.049 Uiso 1 1 calc R U . . .
C2 C 0.3120(9) 0.6315(11) 0.4146(4) 0.0515(17) Uani 1 1 d . . . . .
H2A H 0.177321 0.661728 0.407921 0.062 Uiso 1 1 calc R U . . .
H2B H 0.363153 0.688077 0.458326 0.062 Uiso 1 1 calc R U . . .
H2C H 0.327440 0.496953 0.417297 0.062 Uiso 1 1 calc R U . . .
B1 B 0.7051(8) 0.6944(7) 0.3671(3) 0.0230(10) 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
I1 B1 2.232(5) . ?
I2 B1 2.219(5) . ?
I3 B1 2.212(5) . ?
S1 C1 1.803(6) . ?
S1 C2 1.828(7) . ?
S1 B1 1.937(6) . ?

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 S1 C2 100.8(3) . . ?
C1 S1 B1 105.2(3) . . ?
C2 S1 B1 105.6(3) . . ?
S1 B1 I3 112.8(3) . . ?
S1 B1 I2 104.5(2) . . ?
I3 B1 I2 111.2(2) . . ?
S1 B1 I1 104.4(2) . . ?
I3 B1 I1 111.8(2) . . ?
I2 B1 I1 111.7(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
C1 S1 B1 I3 52.6(3) . . . . ?
C2 S1 B1 I3 -53.5(4) . . . . ?
C1 S1 B1 I2 -68.4(3) . . . . ?
C2 S1 B1 I2 -174.5(3) . . . . ?
C1 S1 B1 I1 174.2(3) . . . . ?
C2 S1 B1 I1 68.1(4) . . . . ?

_refine_diff_density_max         1.551
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.179


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes at -30C'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PB(NBH2)
_database_code_depnum_ccdc_archive 'CCDC 2106475'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_audit_creation_date             2021-08-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
bfrenett@ualberta.ca
erivard@ualberta.ca
_chemical_name_common            PB(NBH2)
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H42 B2 N P'
_chemical_formula_sum            'C24 H42 B2 N P'
_chemical_formula_weight         397.17
_chemical_melting_point          ?
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'

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

_cell_length_a                   11.6992(12)
_cell_length_b                   9.8865(10)
_cell_length_c                   21.0275(19)
_cell_angle_alpha                90
_cell_angle_beta                 90.527(2)
_cell_angle_gamma                90
_cell_volume                     2432.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3016
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.955
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.6965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,  J. Appl. Cryst. 48 (2015) 3-10'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             872
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 1.00 0.0990
-1.00 0.00 -1.00 0.1200
-1.00 0.00 0.00 0.1510
1.00 0.00 0.00 0.1390
1.00 0.00 -1.00 0.1610
1.00 1.00 1.00 0.0790
1.00 1.00 0.00 0.0880
1.00 1.00 -1.00 0.1080
-1.00 -1.00 1.00 0.0900
0.00 -1.00 0.00 0.0770
0.00 1.00 0.00 0.0770
0.00 -1.00 1.00 0.0550
0.00 1.00 -1.00 0.1000
1.00 -1.00 1.00 0.0970
-1.00 1.00 -1.00 0.1090
0.00 0.00 -1.00 0.2070
0.00 0.00 1.00 0.1270
-1.00 0.00 -2.00 0.1160
-2.00 0.00 1.00 0.1670
-2.00 -1.00 -2.00 0.1030
-2.00 -1.00 0.00 0.1080
-2.00 -2.00 -1.00 0.0830
-2.00 -1.00 1.00 0.1170
-1.00 -2.00 1.00 0.0500
0.00 -2.00 1.00 0.0440
0.00 -1.00 2.00 0.0780
0.00 1.00 2.00 0.1040

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes at -40C'
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.154
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15541
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.357
_diffrn_reflns_theta_min         1.937
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4547
_reflns_number_total             6374
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         6374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0630
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0943P)²+0.8630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1809
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C13(H13), C10(H10), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C14(H14A,H14B), C24(H24A,H24B), C21(H21A,H21B), C18(H18A,
 H18B), C23(H23A,H23B), C22(H22A,H22B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C5(H5)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.51063(4) 0.69520(5) 0.24034(2) 0.02491(14) Uani 1 1 d . . . . .
N1 N 0.47674(13) 0.78298(15) 0.30441(7) 0.0254(3) Uani 1 1 d . . . . .
C2 C 0.48945(14) 0.53822(18) 0.33925(9) 0.0240(4) Uani 1 1 d . . . . .
C1 C 0.50416(16) 0.52978(19) 0.27318(9) 0.0278(4) Uani 1 1 d . . . . .
C19 C 0.58538(15) 0.72298(19) 0.41696(9) 0.0264(4) Uani 1 1 d . . . . .
H19 H 0.584991 0.650141 0.449951 0.032 Uiso 1 1 calc R U . . .
C3 C 0.48938(16) 0.4142(2) 0.37190(10) 0.0303(4) Uani 1 1 d . . . . .
H3 H 0.482917 0.414229 0.416906 0.036 Uiso 1 1 calc R U . . .
C13 C 0.35284(16) 0.7139(2) 0.40506(9) 0.0294(4) Uani 1 1 d . . . . .
H13 H 0.350320 0.812391 0.415876 0.035 Uiso 1 1 calc R U . . .
C10 C 0.65677(17) 0.7312(2) 0.21477(10) 0.0332(4) Uani 1 1 d . . . . .
H10 H 0.707518 0.704592 0.251197 0.040 Uiso 1 1 calc R U . . .
C4 C 0.49848(19) 0.2920(2) 0.34026(12) 0.0396(5) Uani 1 1 d . . . . .
H4 H 0.497139 0.210038 0.363794 0.047 Uiso 1 1 calc R U . . .
C6 C 0.5132(2) 0.4065(2) 0.24068(11) 0.0390(5) Uani 1 1 d . . . . .
H6 H 0.521671 0.405055 0.195796 0.047 Uiso 1 1 calc R U . . .
C20 C 0.70301(17) 0.7138(2) 0.38604(11) 0.0369(5) Uani 1 1 d . . . . .
H20A H 0.709462 0.785854 0.353557 0.044 Uiso 1 1 calc R U . . .
H20B H 0.709700 0.625625 0.364109 0.044 Uiso 1 1 calc R U . . .
C14 C 0.34074(18) 0.6382(3) 0.46788(10) 0.0419(5) Uani 1 1 d . . . . .
H14A H 0.408323 0.657490 0.495080 0.050 Uiso 1 1 calc R U . . .
H14B H 0.339400 0.539789 0.459298 0.050 Uiso 1 1 calc R U . . .
C7 C 0.4139(2) 0.7010(3) 0.17168(11) 0.0430(5) Uani 1 1 d . . . . .
H7 H 0.436933 0.622445 0.144743 0.052 Uiso 1 1 calc R U . . .
C24 C 0.5793(2) 0.8564(2) 0.45440(12) 0.0448(6) Uani 1 1 d . . . . .
H24A H 0.582231 0.933196 0.424224 0.054 Uiso 1 1 calc R U . . .
H24B H 0.505334 0.860959 0.476823 0.054 Uiso 1 1 calc R U . . .
C21 C 0.80202(19) 0.7282(3) 0.43406(12) 0.0482(6) Uani 1 1 d . . . . .
H21A H 0.801340 0.650386 0.463690 0.058 Uiso 1 1 calc R U . . .
H21B H 0.875522 0.726907 0.411111 0.058 Uiso 1 1 calc R U . . .
C5 C 0.5095(2) 0.2876(2) 0.27470(13) 0.0462(6) Uani 1 1 d . . . . .
H5 H 0.514552 0.203061 0.253402 0.055 Uiso 1 1 calc R U . . .
B1 B 0.47570(17) 0.6889(2) 0.36970(10) 0.0239(4) Uani 1 1 d . . . . .
C18 C 0.24610(17) 0.6859(3) 0.36475(11) 0.0449(6) Uani 1 1 d . . . . .
H18A H 0.244556 0.588875 0.353039 0.054 Uiso 1 1 calc R U . . .
H18B H 0.250140 0.739138 0.324967 0.054 Uiso 1 1 calc R U . . .
C23 C 0.6767(2) 0.8706(3) 0.50290(12) 0.0509(6) Uani 1 1 d . . . . .
H23A H 0.670845 0.959441 0.524305 0.061 Uiso 1 1 calc R U . . .
H23B H 0.669285 0.799302 0.535686 0.061 Uiso 1 1 calc R U . . .
C22 C 0.7928(2) 0.8587(3) 0.47171(13) 0.0511(6) Uani 1 1 d . . . . .
H22A H 0.804429 0.936724 0.442949 0.061 Uiso 1 1 calc R U . . .
H22B H 0.853443 0.861096 0.504825 0.061 Uiso 1 1 calc R U . . .
C15 C 0.2324(2) 0.6772(3) 0.50393(11) 0.0480(6) Uani 1 1 d . . . . .
H15A H 0.228003 0.623916 0.543683 0.058 Uiso 1 1 calc R U . . .
H15B H 0.235900 0.774209 0.515550 0.058 Uiso 1 1 calc R U . . .
C11 C 0.6924(2) 0.6420(3) 0.15881(12) 0.0473(6) Uani 1 1 d . . . . .
H11A H 0.681287 0.546656 0.169913 0.071 Uiso 1 1 calc R U . . .
H11B H 0.773127 0.657953 0.149330 0.071 Uiso 1 1 calc R U . . .
H11C H 0.645539 0.664306 0.121389 0.071 Uiso 1 1 calc R U . . .
C16 C 0.1264(2) 0.6514(3) 0.46371(12) 0.0560(7) Uani 1 1 d . . . . .
H16A H 0.058285 0.684934 0.486401 0.067 Uiso 1 1 calc R U . . .
H16B H 0.117135 0.552854 0.457088 0.067 Uiso 1 1 calc R U . . .
C12 C 0.6807(2) 0.8811(2) 0.20275(13) 0.0477(6) Uani 1 1 d . . . . .
H12A H 0.633270 0.912815 0.167085 0.072 Uiso 1 1 calc R U . . .
H12B H 0.761564 0.893254 0.192500 0.072 Uiso 1 1 calc R U . . .
H12C H 0.662466 0.933315 0.240960 0.072 Uiso 1 1 calc R U . . .
C17 C 0.1347(2) 0.7216(4) 0.39962(13) 0.0683(10) Uani 1 1 d . . . . .
H17A H 0.131202 0.820741 0.406031 0.082 Uiso 1 1 calc R U . . .
H17B H 0.068499 0.695050 0.372771 0.082 Uiso 1 1 calc R U . . .
B2 B 0.4451(2) 0.9189(3) 0.30046(14) 0.0387(6) Uani 1 1 d . . . . .
C8 C 0.4207(3) 0.8216(3) 0.12820(14) 0.0669(8) Uani 1 1 d . . . . .
H8A H 0.400396 0.903530 0.151756 0.100 Uiso 1 1 calc R U . . .
H8B H 0.367375 0.809490 0.092428 0.100 Uiso 1 1 calc R U . . .
H8C H 0.498682 0.830206 0.112089 0.100 Uiso 1 1 calc R U . . .
C9 C 0.2923(2) 0.6704(5) 0.19107(14) 0.0856(13) Uani 1 1 d . . . . .
H9A H 0.291552 0.589978 0.218337 0.128 Uiso 1 1 calc R U . . .
H9B H 0.245477 0.653647 0.152994 0.128 Uiso 1 1 calc R U . . .
H9C H 0.261161 0.747602 0.214432 0.128 Uiso 1 1 calc R U . . .
H2A H 0.421(2) 0.974(2) 0.3454(12) 0.046(7) Uiso 1 1 d . . . . .
H2B H 0.443(2) 0.968(3) 0.2522(12) 0.054(7) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.6538(16) . ?
P1 C1 1.777(2) . ?
P1 C10 1.832(2) . ?
P1 C7 1.827(2) . ?
N1 B1 1.659(3) . ?
N1 B2 1.396(3) . ?
C2 C1 1.404(3) . ?
C2 C3 1.405(3) . ?
C2 B1 1.630(3) . ?
C1 C6 1.402(3) . ?
C19 H19 1.0000 . ?
C19 C20 1.530(3) . ?
C19 C24 1.538(3) . ?
C19 B1 1.650(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(3) . ?
C13 H13 1.0000 . ?
C13 C14 1.526(3) . ?
C13 B1 1.643(3) . ?
C13 C18 1.528(3) . ?
C10 H10 1.0000 . ?
C10 C11 1.531(3) . ?
C10 C12 1.530(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(4) . ?
C6 H6 0.9500 . ?
C6 C5 1.378(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.536(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.532(3) . ?
C7 H7 1.0000 . ?
C7 C8 1.505(4) . ?
C7 C9 1.515(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.529(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.518(4) . ?
C5 H5 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C17 1.542(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.518(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.516(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.520(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
B2 H2A 1.13(3) . ?
B2 H2B 1.13(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 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
N1 P1 C1 98.92(9) . . ?
N1 P1 C10 111.63(9) . . ?
N1 P1 C7 118.41(10) . . ?
C1 P1 C10 109.63(9) . . ?
C1 P1 C7 107.93(10) . . ?
C7 P1 C10 109.56(10) . . ?
P1 N1 B1 112.56(12) . . ?
B2 N1 P1 121.47(16) . . ?
B2 N1 B1 125.81(18) . . ?
C1 C2 C3 115.61(17) . . ?
C1 C2 B1 117.16(16) . . ?
C3 C2 B1 127.22(17) . . ?
C2 C1 P1 109.63(14) . . ?
C6 C1 P1 127.37(16) . . ?
C6 C1 C2 123.00(18) . . ?
C20 C19 H19 105.2 . . ?
C20 C19 C24 108.32(17) . . ?
C20 C19 B1 115.43(16) . . ?
C24 C19 H19 105.2 . . ?
C24 C19 B1 116.34(15) . . ?
B1 C19 H19 105.2 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.75(19) . . ?
C4 C3 H3 119.1 . . ?
C14 C13 H13 106.1 . . ?
C14 C13 B1 113.97(16) . . ?
C14 C13 C18 108.01(17) . . ?
B1 C13 H13 106.1 . . ?
C18 C13 H13 106.1 . . ?
C18 C13 B1 115.81(16) . . ?
P1 C10 H10 105.9 . . ?
C11 C10 P1 112.03(15) . . ?
C11 C10 H10 105.9 . . ?
C12 C10 P1 114.15(15) . . ?
C12 C10 H10 105.9 . . ?
C12 C10 C11 112.31(19) . . ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 121.0(2) . . ?
C5 C4 H4 119.5 . . ?
C1 C6 H6 120.5 . . ?
C5 C6 C1 119.1(2) . . ?
C5 C6 H6 120.5 . . ?
C19 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C19 C20 C21 113.01(18) . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C13 C14 C15 112.86(18) . . ?
H14A C14 H14B 107.8 . . ?
C15 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
P1 C7 H7 104.8 . . ?
C8 C7 P1 118.02(19) . . ?
C8 C7 H7 104.8 . . ?
C8 C7 C9 112.1(2) . . ?
C9 C7 P1 110.94(17) . . ?
C9 C7 H7 104.8 . . ?
C19 C24 H24A 109.1 . . ?
C19 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
C23 C24 C19 112.45(19) . . ?
C23 C24 H24A 109.1 . . ?
C23 C24 H24B 109.1 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 C20 111.4(2) . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.5(2) . . ?
C6 C5 H5 120.2 . . ?
C2 B1 N1 100.71(14) . . ?
C2 B1 C19 110.13(14) . . ?
C2 B1 C13 113.92(15) . . ?
C19 B1 N1 111.85(15) . . ?
C13 B1 N1 107.64(14) . . ?
C13 B1 C19 112.04(15) . . ?
C13 C18 H18A 109.1 . . ?
C13 C18 H18B 109.1 . . ?
C13 C18 C17 112.6(2) . . ?
H18A C18 H18B 107.8 . . ?
C17 C18 H18A 109.1 . . ?
C17 C18 H18B 109.1 . . ?
C24 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
H23A C23 H23B 107.9 . . ?
C22 C23 C24 111.7(2) . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
C21 C22 C23 111.03(19) . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C14 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C16 C15 C14 111.0(2) . . ?
C16 C15 H15A 109.4 . . ?
C16 C15 H15B 109.4 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C15 C16 C17 111.0(2) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
C16 C17 C18 112.2(2) . . ?
C16 C17 H17A 109.2 . . ?
C16 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
N1 B2 H2A 118.9(13) . . ?
N1 B2 H2B 118.1(13) . . ?
H2A B2 H2B 123.0(18) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 N1 B1 C2 -9.02(15) . . . . ?
P1 N1 B1 C19 107.93(15) . . . . ?
P1 N1 B1 C13 -128.57(13) . . . . ?
P1 C1 C6 C5 178.05(18) . . . . ?
N1 P1 C1 C2 -7.85(15) . . . . ?
N1 P1 C1 C6 172.86(18) . . . . ?
N1 P1 C10 C11 175.33(15) . . . . ?
N1 P1 C10 C12 -55.6(2) . . . . ?
N1 P1 C7 C8 80.4(2) . . . . ?
N1 P1 C7 C9 -51.0(3) . . . . ?
C2 C1 C6 C5 -1.2(3) . . . . ?
C2 C3 C4 C5 0.8(3) . . . . ?
C1 P1 N1 B1 10.19(13) . . . . ?
C1 P1 N1 B2 -165.48(17) . . . . ?
C1 P1 C10 C11 66.76(18) . . . . ?
C1 P1 C10 C12 -164.18(17) . . . . ?
C1 P1 C7 C8 -168.5(2) . . . . ?
C1 P1 C7 C9 60.1(3) . . . . ?
C1 C2 C3 C4 -2.6(3) . . . . ?
C1 C2 B1 N1 3.5(2) . . . . ?
C1 C2 B1 C19 -114.70(18) . . . . ?
C1 C2 B1 C13 118.44(18) . . . . ?
C1 C6 C5 C4 -0.8(3) . . . . ?
C19 C20 C21 C22 -55.7(3) . . . . ?
C19 C24 C23 C22 56.5(3) . . . . ?
C3 C2 C1 P1 -176.56(13) . . . . ?
C3 C2 C1 C6 2.8(3) . . . . ?
C3 C2 B1 N1 -177.14(16) . . . . ?
C3 C2 B1 C19 64.6(2) . . . . ?
C3 C2 B1 C13 -62.2(2) . . . . ?
C3 C4 C5 C6 1.0(4) . . . . ?
C13 C14 C15 C16 57.9(3) . . . . ?
C13 C18 C17 C16 -54.6(4) . . . . ?
C10 P1 N1 B1 -105.16(13) . . . . ?
C10 P1 N1 B2 79.17(19) . . . . ?
C10 P1 C1 C2 109.03(15) . . . . ?
C10 P1 C1 C6 -70.3(2) . . . . ?
C10 P1 C7 C8 -49.2(2) . . . . ?
C10 P1 C7 C9 179.5(2) . . . . ?
C20 C19 C24 C23 -55.3(3) . . . . ?
C20 C19 B1 N1 -54.1(2) . . . . ?
C20 C19 B1 C2 57.1(2) . . . . ?
C20 C19 B1 C13 -175.04(17) . . . . ?
C20 C21 C22 C23 53.9(3) . . . . ?
C14 C13 B1 N1 -177.57(17) . . . . ?
C14 C13 B1 C2 71.7(2) . . . . ?
C14 C13 B1 C19 -54.2(2) . . . . ?
C14 C13 C18 C17 55.0(3) . . . . ?
C14 C15 C16 C17 -54.0(3) . . . . ?
C7 P1 N1 B1 126.24(13) . . . . ?
C7 P1 N1 B2 -49.4(2) . . . . ?
C7 P1 C1 C2 -131.69(14) . . . . ?
C7 P1 C1 C6 49.0(2) . . . . ?
C7 P1 C10 C11 -51.5(2) . . . . ?
C7 P1 C10 C12 77.5(2) . . . . ?
C24 C19 C20 C21 55.1(2) . . . . ?
C24 C19 B1 N1 74.5(2) . . . . ?
C24 C19 B1 C2 -174.35(18) . . . . ?
C24 C19 B1 C13 -46.4(2) . . . . ?
C24 C23 C22 C21 -54.7(3) . . . . ?
B1 C2 C1 P1 2.9(2) . . . . ?
B1 C2 C1 C6 -177.80(17) . . . . ?
B1 C2 C3 C4 178.06(18) . . . . ?
B1 C19 C20 C21 -172.47(18) . . . . ?
B1 C19 C24 C23 172.7(2) . . . . ?
B1 C13 C14 C15 172.66(19) . . . . ?
B1 C13 C18 C17 -175.8(2) . . . . ?
C18 C13 C14 C15 -57.1(3) . . . . ?
C18 C13 B1 N1 56.2(2) . . . . ?
C18 C13 B1 C2 -54.5(2) . . . . ?
C18 C13 B1 C19 179.60(18) . . . . ?
C15 C16 C17 C18 52.8(4) . . . . ?
B2 N1 B1 C2 166.42(19) . . . . ?
B2 N1 B1 C19 -76.6(2) . . . . ?
B2 N1 B1 C13 46.9(2) . . . . ?

_olex2_date_sample_data_collection 2021-07-23
_olex2_date_sample_submission    2021-07-22
_olex2_submission_original_sample_id riv21a0
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PB(N3SiMe3)
_database_code_depnum_ccdc_archive 'CCDC 2106477'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_audit_creation_date             2021-08-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
bfrenett@ualberta.ca
michael.ferguson@ualberta.ca
erivard@ualberta.ca
_chemical_name_common            PB(N3SiMe3)
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H49 B N3 P Si'
_chemical_formula_sum            'C27 H49 B N3 P Si'
_chemical_formula_weight         485.56
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 n 1'
_space_group_name_Hall           'P -2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   9.4802(7)
_cell_length_b                   10.2175(8)
_cell_length_c                   15.3118(11)
_cell_angle_alpha                90
_cell_angle_beta                 99.8940(10)
_cell_angle_gamma                90
_cell_volume                     1461.10(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9471
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.36
_shelx_estimated_absorpt_T_max   0.971
_shelx_estimated_absorpt_T_min   0.960
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9166
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,  J. Appl. Cryst. 48 (2015) 3-10'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             532
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -1.00 0.1000
-1.00 0.00 1.00 0.1220
0.00 1.00 1.00 0.0950
-1.00 -1.00 0.00 0.0610
0.00 -1.00 1.00 0.0390
0.00 1.00 -1.00 0.0990
0.00 0.00 -1.00 0.0630
0.00 0.00 1.00 0.0980
1.00 0.00 1.00 0.1510
-1.00 0.00 -1.00 0.0820
-1.00 -1.00 -2.00 0.0250

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane at -40C'
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.192
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26386
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.993
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                6306
_reflns_number_total             6671
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.118
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 
;
 Flack x determined using 2960 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6671
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0430P)²+0.1245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0755
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C19(H19), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C18(H18A,H18B), C20(H20A,H20B), C23(H23A,H23B), C22(H22A,
 H22B), C14(H14A,H14B), C15(H15A,H15B), C21(H21A,H21B), C16(H16A,H16B),
 C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C),
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.35640(5) 0.72993(5) 0.49141(3) 0.02038(11) Uani 1 1 d . . . . .
Si1 Si 0.72164(6) 0.83987(6) 0.70108(4) 0.02896(14) Uani 1 1 d . . . . .
N2 N 0.63232(19) 0.73572(17) 0.54790(11) 0.0228(3) Uani 1 1 d . . . . .
N3 N 0.58598(19) 0.77881(17) 0.61499(11) 0.0253(4) Uani 1 1 d . . . . .
N1 N 0.52786(17) 0.70124(17) 0.48063(11) 0.0221(3) Uani 1 1 d . . . . .
C13 C 0.6520(2) 0.5202(2) 0.39173(14) 0.0261(4) Uani 1 1 d . . . . .
H13 H 0.652460 0.490829 0.329478 0.031 Uiso 1 1 calc R U . . .
C10 C 0.3139(2) 0.9019(2) 0.50943(14) 0.0264(4) Uani 1 1 d . . . . .
H10 H 0.334840 0.918188 0.574782 0.032 Uiso 1 1 calc R U . . .
C6 C 0.1396(2) 0.6616(2) 0.34736(15) 0.0287(4) Uani 1 1 d . . . . .
H6 H 0.069448 0.689356 0.380837 0.034 Uiso 1 1 calc R U . . .
C1 C 0.2853(2) 0.67393(19) 0.38206(13) 0.0224(4) Uani 1 1 d . . . . .
C19 C 0.6238(2) 0.7805(2) 0.33399(14) 0.0256(4) Uani 1 1 d . . . . .
H19 H 0.541950 0.842476 0.317497 0.031 Uiso 1 1 calc R U . . .
C3 C 0.3466(3) 0.5780(2) 0.25168(15) 0.0315(5) Uani 1 1 d . . . . .
H3 H 0.415347 0.547397 0.218110 0.038 Uiso 1 1 calc R U . . .
C7 C 0.2678(2) 0.6313(2) 0.56642(15) 0.0312(5) Uani 1 1 d . . . . .
H7 H 0.162998 0.638867 0.542955 0.037 Uiso 1 1 calc R U . . .
C2 C 0.3942(2) 0.6328(2) 0.33591(13) 0.0233(4) Uani 1 1 d . . . . .
C4 C 0.2025(3) 0.5674(2) 0.21625(15) 0.0356(5) Uani 1 1 d . . . . .
H4 H 0.174348 0.531436 0.158678 0.043 Uiso 1 1 calc R U . . .
C24 C 0.7449(2) 0.8622(2) 0.38756(15) 0.0302(5) Uani 1 1 d . . . . .
H24A H 0.713248 0.895175 0.441850 0.036 Uiso 1 1 calc R U . . .
H24B H 0.829313 0.805373 0.406039 0.036 Uiso 1 1 calc R U . . .
C12 C 0.4084(3) 0.9934(2) 0.46665(17) 0.0350(5) Uani 1 1 d . . . . .
H12A H 0.509082 0.977288 0.491832 0.052 Uiso 1 1 calc R U . . .
H12B H 0.384046 1.084383 0.477926 0.052 Uiso 1 1 calc R U . . .
H12C H 0.393052 0.977667 0.402579 0.052 Uiso 1 1 calc R U . . .
C18 C 0.5846(3) 0.4083(2) 0.43661(18) 0.0359(5) Uani 1 1 d . . . . .
H18A H 0.578762 0.434178 0.498192 0.043 Uiso 1 1 calc R U . . .
H18B H 0.485772 0.393757 0.404845 0.043 Uiso 1 1 calc R U . . .
C20 C 0.6680(3) 0.7397(2) 0.24579(16) 0.0358(5) Uani 1 1 d . . . . .
H20A H 0.747927 0.676316 0.258115 0.043 Uiso 1 1 calc R U . . .
H20B H 0.586350 0.695050 0.208651 0.043 Uiso 1 1 calc R U . . .
C5 C 0.0988(2) 0.6087(2) 0.26380(16) 0.0346(5) Uani 1 1 d . . . . .
H5 H 0.000219 0.600679 0.239082 0.041 Uiso 1 1 calc R U . . .
C9 C 0.3028(3) 0.4873(3) 0.55956(17) 0.0416(6) Uani 1 1 d . . . . .
H9A H 0.285427 0.460774 0.497117 0.062 Uiso 1 1 calc R U . . .
H9B H 0.241991 0.435522 0.592185 0.062 Uiso 1 1 calc R U . . .
H9C H 0.403654 0.472358 0.584954 0.062 Uiso 1 1 calc R U . . .
C23 C 0.7883(3) 0.9781(2) 0.33487(17) 0.0358(5) Uani 1 1 d . . . . .
H23A H 0.706604 1.039326 0.320846 0.043 Uiso 1 1 calc R U . . .
H23B H 0.868555 1.025564 0.371339 0.043 Uiso 1 1 calc R U . . .
C22 C 0.8335(3) 0.9326(2) 0.24940(18) 0.0422(6) Uani 1 1 d . . . . .
H22A H 0.857407 1.009503 0.215395 0.051 Uiso 1 1 calc R U . . .
H22B H 0.920185 0.877302 0.263420 0.051 Uiso 1 1 calc R U . . .
C11 C 0.1549(3) 0.9314(3) 0.47783(18) 0.0386(6) Uani 1 1 d . . . . .
H11A H 0.132454 0.923000 0.413176 0.058 Uiso 1 1 calc R U . . .
H11B H 0.133925 1.020827 0.494950 0.058 Uiso 1 1 calc R U . . .
H11C H 0.096743 0.869408 0.505139 0.058 Uiso 1 1 calc R U . . .
C14 C 0.8096(2) 0.5320(2) 0.4354(2) 0.0413(6) Uani 1 1 d . . . . .
H14A H 0.814469 0.563880 0.496865 0.050 Uiso 1 1 calc R U . . .
H14B H 0.856563 0.598083 0.402744 0.050 Uiso 1 1 calc R U . . .
C15 C 0.8929(3) 0.4030(3) 0.4375(2) 0.0470(7) Uani 1 1 d . . . . .
H15A H 0.897415 0.375199 0.376124 0.056 Uiso 1 1 calc R U . . .
H15B H 0.992090 0.416587 0.468955 0.056 Uiso 1 1 calc R U . . .
C21 C 0.7146(4) 0.8553(3) 0.19389(19) 0.0449(6) Uani 1 1 d . . . . .
H21A H 0.747910 0.822416 0.140116 0.054 Uiso 1 1 calc R U . . .
H21B H 0.631521 0.913497 0.174731 0.054 Uiso 1 1 calc R U . . .
C8 C 0.2864(3) 0.6769(3) 0.66266(17) 0.0445(6) Uani 1 1 d . . . . .
H8A H 0.386706 0.666339 0.690800 0.067 Uiso 1 1 calc R U . . .
H8B H 0.225245 0.624259 0.694523 0.067 Uiso 1 1 calc R U . . .
H8C H 0.259227 0.769234 0.664444 0.067 Uiso 1 1 calc R U . . .
C16 C 0.8227(3) 0.2969(3) 0.4835(2) 0.0450(7) Uani 1 1 d . . . . .
H16A H 0.826150 0.320491 0.546569 0.054 Uiso 1 1 calc R U . . .
H16B H 0.875162 0.213518 0.481197 0.054 Uiso 1 1 calc R U . . .
B1 B 0.5582(2) 0.6560(2) 0.38391(15) 0.0227(4) Uani 1 1 d . . . . .
C26 C 0.7147(3) 1.0212(3) 0.6903(2) 0.0455(6) Uani 1 1 d . . . . .
H26A H 0.743035 1.046832 0.634111 0.068 Uiso 1 1 calc R U . . .
H26B H 0.780518 1.060643 0.739667 0.068 Uiso 1 1 calc R U . . .
H26C H 0.617062 1.051626 0.691489 0.068 Uiso 1 1 calc R U . . .
C25 C 0.6689(3) 0.7808(3) 0.80578(17) 0.0465(7) Uani 1 1 d . . . . .
H25A H 0.579954 0.824067 0.814295 0.070 Uiso 1 1 calc R U . . .
H25B H 0.744890 0.801356 0.855790 0.070 Uiso 1 1 calc R U . . .
H25C H 0.653912 0.685919 0.802400 0.070 Uiso 1 1 calc R U . . .
C17 C 0.6681(3) 0.2800(3) 0.4385(2) 0.0549(8) Uani 1 1 d . . . . .
H17A H 0.621693 0.212866 0.470597 0.066 Uiso 1 1 calc R U . . .
H17B H 0.665741 0.248804 0.377090 0.066 Uiso 1 1 calc R U . . .
C27 C 0.9023(3) 0.7809(3) 0.6875(2) 0.0462(6) Uani 1 1 d . . . . .
H27A H 0.905975 0.685356 0.692998 0.069 Uiso 1 1 calc R U . . .
H27B H 0.974740 0.819928 0.733489 0.069 Uiso 1 1 calc R U . . .
H27C H 0.921213 0.806372 0.628921 0.069 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.6875(17) . ?
P1 C10 1.834(2) . ?
P1 C1 1.788(2) . ?
P1 C7 1.836(2) . ?
Si1 N3 1.7884(19) . ?
Si1 C26 1.860(3) . ?
Si1 C25 1.860(3) . ?
Si1 C27 1.860(3) . ?
N2 N3 1.264(2) . ?
N2 N1 1.347(2) . ?
N1 B1 1.624(3) . ?
C13 H13 1.0000 . ?
C13 C18 1.529(3) . ?
C13 C14 1.534(3) . ?
C13 B1 1.641(3) . ?
C10 H10 1.0000 . ?
C10 C12 1.519(3) . ?
C10 C11 1.531(3) . ?
C6 H6 0.9500 . ?
C6 C1 1.398(3) . ?
C6 C5 1.382(3) . ?
C1 C2 1.411(3) . ?
C19 H19 1.0000 . ?
C19 C24 1.537(3) . ?
C19 C20 1.539(3) . ?
C19 B1 1.659(3) . ?
C3 H3 0.9500 . ?
C3 C2 1.407(3) . ?
C3 C4 1.385(3) . ?
C7 H7 1.0000 . ?
C7 C9 1.516(4) . ?
C7 C8 1.527(3) . ?
C2 B1 1.620(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.529(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C17 1.529(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.530(3) . ?
C5 H5 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.518(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C21 1.512(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.534(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.508(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.518(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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
N1 P1 C10 114.92(9) . . ?
N1 P1 C1 93.85(9) . . ?
N1 P1 C7 121.17(10) . . ?
C10 P1 C7 107.21(10) . . ?
C1 P1 C10 112.97(10) . . ?
C1 P1 C7 105.72(10) . . ?
N3 Si1 C26 105.80(12) . . ?
N3 Si1 C25 104.84(11) . . ?
N3 Si1 C27 111.34(11) . . ?
C26 Si1 C25 112.88(14) . . ?
C26 Si1 C27 109.37(14) . . ?
C25 Si1 C27 112.35(14) . . ?
N3 N2 N1 113.58(17) . . ?
N2 N3 Si1 114.47(14) . . ?
N2 N1 P1 118.27(13) . . ?
N2 N1 B1 123.33(16) . . ?
B1 N1 P1 117.61(13) . . ?
C18 C13 H13 106.0 . . ?
C18 C13 C14 108.30(19) . . ?
C18 C13 B1 113.73(17) . . ?
C14 C13 H13 106.0 . . ?
C14 C13 B1 116.11(18) . . ?
B1 C13 H13 106.0 . . ?
P1 C10 H10 107.4 . . ?
C12 C10 P1 111.33(15) . . ?
C12 C10 H10 107.4 . . ?
C12 C10 C11 111.33(19) . . ?
C11 C10 P1 111.77(16) . . ?
C11 C10 H10 107.4 . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C5 C6 C1 119.2(2) . . ?
C6 C1 P1 124.99(16) . . ?
C6 C1 C2 122.87(19) . . ?
C2 C1 P1 111.96(15) . . ?
C24 C19 H19 105.4 . . ?
C24 C19 C20 108.91(18) . . ?
C24 C19 B1 118.36(17) . . ?
C20 C19 H19 105.4 . . ?
C20 C19 B1 112.16(17) . . ?
B1 C19 H19 105.4 . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C4 C3 C2 122.0(2) . . ?
P1 C7 H7 105.4 . . ?
C9 C7 P1 111.13(16) . . ?
C9 C7 H7 105.4 . . ?
C9 C7 C8 111.9(2) . . ?
C8 C7 P1 116.56(17) . . ?
C8 C7 H7 105.4 . . ?
C1 C2 B1 117.19(17) . . ?
C3 C2 C1 115.50(19) . . ?
C3 C2 B1 127.30(19) . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.7(2) . . ?
C5 C4 H4 119.6 . . ?
C19 C24 H24A 109.1 . . ?
C19 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
C23 C24 C19 112.53(19) . . ?
C23 C24 H24A 109.1 . . ?
C23 C24 H24B 109.1 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C18 H18A 108.9 . . ?
C13 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C17 C18 C13 113.2(2) . . ?
C17 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 C19 113.2(2) . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C6 C5 C4 119.7(2) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C22 C23 C24 111.1(2) . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C21 C22 C23 110.5(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C13 C14 C15 113.6(2) . . ?
H14A C14 H14B 107.7 . . ?
C15 C14 H14A 108.8 . . ?
C15 C14 H14B 108.8 . . ?
C14 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C16 C15 C14 111.2(2) . . ?
C16 C15 H15A 109.4 . . ?
C16 C15 H15B 109.4 . . ?
C20 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C22 C21 C20 111.4(2) . . ?
C22 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C15 C16 H16A 109.7 . . ?
C15 C16 H16B 109.7 . . ?
C15 C16 C17 109.8(2) . . ?
H16A C16 H16B 108.2 . . ?
C17 C16 H16A 109.7 . . ?
C17 C16 H16B 109.7 . . ?
N1 B1 C13 110.67(16) . . ?
N1 B1 C19 109.94(16) . . ?
C13 B1 C19 116.17(17) . . ?
C2 B1 N1 98.54(15) . . ?
C2 B1 C13 112.03(17) . . ?
C2 B1 C19 108.05(17) . . ?
Si1 C26 H26A 109.5 . . ?
Si1 C26 H26B 109.5 . . ?
Si1 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si1 C25 H25A 109.5 . . ?
Si1 C25 H25B 109.5 . . ?
Si1 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C18 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C16 C17 C18 111.6(2) . . ?
C16 C17 H17A 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
Si1 C27 H27A 109.5 . . ?
Si1 C27 H27B 109.5 . . ?
Si1 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 N1 B1 C13 -126.64(15) . . . . ?
P1 N1 B1 C19 103.70(17) . . . . ?
P1 N1 B1 C2 -9.12(19) . . . . ?
P1 C1 C2 C3 175.41(16) . . . . ?
P1 C1 C2 B1 -5.8(2) . . . . ?
N2 N1 B1 C13 63.7(2) . . . . ?
N2 N1 B1 C19 -66.0(2) . . . . ?
N2 N1 B1 C2 -178.77(17) . . . . ?
N3 N2 N1 P1 4.5(2) . . . . ?
N3 N2 N1 B1 174.09(17) . . . . ?
N1 P1 C10 C12 29.15(19) . . . . ?
N1 P1 C10 C11 154.33(16) . . . . ?
N1 P1 C1 C6 175.02(18) . . . . ?
N1 P1 C1 C2 -0.21(16) . . . . ?
N1 P1 C7 C9 -42.6(2) . . . . ?
N1 P1 C7 C8 87.2(2) . . . . ?
N1 N2 N3 Si1 -174.30(13) . . . . ?
C13 C18 C17 C16 56.5(4) . . . . ?
C13 C14 C15 C16 -56.4(3) . . . . ?
C10 P1 N1 N2 58.82(17) . . . . ?
C10 P1 N1 B1 -111.37(15) . . . . ?
C10 P1 C1 C6 -65.8(2) . . . . ?
C10 P1 C1 C2 118.94(15) . . . . ?
C10 P1 C7 C9 -177.22(17) . . . . ?
C10 P1 C7 C8 -47.5(2) . . . . ?
C6 C1 C2 C3 0.1(3) . . . . ?
C6 C1 C2 B1 178.85(19) . . . . ?
C1 P1 N1 N2 176.37(15) . . . . ?
C1 P1 N1 B1 6.19(15) . . . . ?
C1 P1 C10 C12 -76.95(18) . . . . ?
C1 P1 C10 C11 48.23(19) . . . . ?
C1 P1 C7 C9 62.01(19) . . . . ?
C1 P1 C7 C8 -168.2(2) . . . . ?
C1 C6 C5 C4 0.7(3) . . . . ?
C1 C2 B1 N1 8.9(2) . . . . ?
C1 C2 B1 C13 125.37(19) . . . . ?
C1 C2 B1 C19 -105.4(2) . . . . ?
C19 C24 C23 C22 -57.1(3) . . . . ?
C19 C20 C21 C22 55.2(3) . . . . ?
C3 C2 B1 N1 -172.5(2) . . . . ?
C3 C2 B1 C13 -56.0(3) . . . . ?
C3 C2 B1 C19 73.2(3) . . . . ?
C3 C4 C5 C6 0.3(4) . . . . ?
C7 P1 N1 N2 -72.65(18) . . . . ?
C7 P1 N1 B1 117.16(15) . . . . ?
C7 P1 C10 C12 166.99(16) . . . . ?
C7 P1 C10 C11 -67.82(18) . . . . ?
C7 P1 C1 C6 51.1(2) . . . . ?
C7 P1 C1 C2 -124.11(16) . . . . ?
C2 C3 C4 C5 -1.2(4) . . . . ?
C4 C3 C2 C1 1.0(3) . . . . ?
C4 C3 C2 B1 -177.6(2) . . . . ?
C24 C19 C20 C21 -52.9(3) . . . . ?
C24 C19 B1 N1 46.4(2) . . . . ?
C24 C19 B1 C13 -80.2(2) . . . . ?
C24 C19 B1 C2 152.95(17) . . . . ?
C24 C23 C22 C21 57.0(3) . . . . ?
C18 C13 C14 C15 52.9(3) . . . . ?
C18 C13 B1 N1 54.9(2) . . . . ?
C18 C13 B1 C19 -178.81(19) . . . . ?
C18 C13 B1 C2 -54.0(2) . . . . ?
C20 C19 C24 C23 53.8(2) . . . . ?
C20 C19 B1 N1 174.57(18) . . . . ?
C20 C19 B1 C13 47.9(3) . . . . ?
C20 C19 B1 C2 -78.9(2) . . . . ?
C5 C6 C1 P1 -175.64(17) . . . . ?
C5 C6 C1 C2 -0.9(3) . . . . ?
C23 C22 C21 C20 -55.9(3) . . . . ?
C14 C13 C18 C17 -52.8(3) . . . . ?
C14 C13 B1 N1 -71.8(2) . . . . ?
C14 C13 B1 C19 54.5(3) . . . . ?
C14 C13 B1 C2 179.33(19) . . . . ?
C14 C15 C16 C17 56.3(3) . . . . ?
C15 C16 C17 C18 -56.7(4) . . . . ?
B1 C13 C18 C17 176.5(2) . . . . ?
B1 C13 C14 C15 -177.8(2) . . . . ?
B1 C19 C24 C23 -176.59(18) . . . . ?
B1 C19 C20 C21 174.2(2) . . . . ?
C26 Si1 N3 N2 101.45(18) . . . . ?
C25 Si1 N3 N2 -139.00(17) . . . . ?
C27 Si1 N3 N2 -17.27(19) . . . . ?

_olex2_date_sample_data_collection 2021-08-11
_olex2_date_sample_submission    2021-08-11
_olex2_submission_original_sample_id riv21a7
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[PB(NLi)]2
_database_code_depnum_ccdc_archive 'CCDC 2106480'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_FORMU01_riv19a8             
;
PROBLEM: There is a discrepancy between the atom counts in the  
RESPONSE: The reported formula (and F000, mu, etc) contain the
contributions of the disordered solvent hexane molecules that were removed
from the model by use of the SQUEEZE routine of the program PLATON.
See response to PLAT869 below.
;
_vrf_PLAT869_riv19a8             
;
PROBLEM: ALERTS Related to the Use of SQUEEZE Suppressed          ! Info 
RESPONSE: Attempts to refine peaks of residual electron density as
disordered or partial-occupancy solvent hexanes carbon atoms were
unsuccessful. The data were corrected for disordered electron density through
use of the SQUEEZE procedure as implemented in PLATON (Spek, A. L. Acta
Crystallogr. 2015, C71, 9 18. PLATON - a multipurpose crystallographic tool.
Utrecht University, Utrecht, The Netherlands). A total solvent- accessible void
volume of 631 A3 with a total electron count of 139 (consistent with 1.5
molecules of solvent hexane, or 0.75 molecule per formula unit of the lithium
complex) was found in the unit cell.
;
# end Validation Reply Form  

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[PB(NLi)2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H80 B2 Li2 N2 P2, 1.5(C6 H14)'
_chemical_formula_sum            'C57 H101 B2 Li2 N2 P2'
_chemical_formula_weight         911.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.7171(3)
_cell_length_b                   16.7686(5)
_cell_length_c                   17.2773(6)
_cell_angle_alpha                68.428(2)
_cell_angle_beta                 75.826(2)
_cell_angle_gamma                77.713(2)
_cell_volume                     2773.46(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    6603
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      70.19

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_F_000             1006
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.966
_shelx_estimated_absorpt_T_min   0.680
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.627958
_exptl_absorpt_correction_T_max  0.864356
_exptl_absorpt_process_details   
; 
 TWINABS 2012/1: Bruker AXS Inc., Madison, Wisconsin, USA 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10288
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.798
_diffrn_reflns_theta_max         70.421
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             10288
_reflns_number_gt                7944
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 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. Completness statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          'Refined as a 2-component twin.,Twin,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1239P)²+1.1647P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10288
_refine_ls_number_parameters     530
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0765
_refine_ls_wR_factor_ref         0.2176
_refine_ls_wR_factor_gt          0.2004
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.10400(9) 0.47903(6) 0.28203(6) 0.0278(2) Uani 1 1 d . . . . .
P2 P 0.52204(9) 0.17225(6) 0.27090(6) 0.0298(2) Uani 1 1 d . . . . .
N1 N 0.2428(3) 0.42201(19) 0.27811(18) 0.0249(6) Uani 1 1 d . . . . .
N2 N 0.3835(3) 0.22952(19) 0.27499(19) 0.0265(7) Uani 1 1 d . . . . .
C1 C 0.1308(4) 0.5669(3) 0.3094(2) 0.0303(8) Uani 1 1 d . . . . .
C2 C 0.2616(4) 0.5536(2) 0.3165(2) 0.0275(8) Uani 1 1 d . . . . .
C3 C 0.3024(4) 0.6174(2) 0.3359(2) 0.0350(9) Uani 1 1 d . . . . .
H3 H 0.390623 0.611899 0.340420 0.042 Uiso 1 1 calc R U . . .
C4 C 0.2178(5) 0.6874(3) 0.3485(3) 0.0442(11) Uani 1 1 d . . . . .
H4 H 0.248528 0.729347 0.361404 0.053 Uiso 1 1 calc R U . . .
C5 C 0.0873(5) 0.6978(3) 0.3427(3) 0.0484(12) Uani 1 1 d . . . . .
H5 H 0.029170 0.745910 0.352594 0.058 Uiso 1 1 calc R U . . .
C6 C 0.0432(4) 0.6373(3) 0.3224(3) 0.0421(10) Uani 1 1 d . . . . .
H6 H -0.045036 0.643596 0.317474 0.051 Uiso 1 1 calc R U . . .
C11 C 0.0411(4) 0.5218(3) 0.1831(3) 0.0453(11) Uani 1 1 d . . . . .
H11 H 0.022476 0.471338 0.172259 0.054 Uiso 1 1 calc R U . . .
C12 C 0.1434(5) 0.5640(4) 0.1094(3) 0.0596(14) Uani 1 1 d . . . . .
H12A H 0.224136 0.523451 0.108743 0.072 Uiso 1 1 calc R U . . .
H12B H 0.112506 0.579107 0.056165 0.072 Uiso 1 1 calc R U . . .
H12C H 0.159589 0.616464 0.115563 0.072 Uiso 1 1 calc R U . . .
C13 C -0.0850(5) 0.5849(4) 0.1842(4) 0.0655(16) Uani 1 1 d . . . . .
H13A H -0.156839 0.553315 0.220542 0.079 Uiso 1 1 calc DR U . . .
H13B H -0.102781 0.612763 0.126553 0.079 Uiso 1 1 calc R U . . .
H13C H -0.076143 0.629187 0.206304 0.079 Uiso 1 1 calc R U . . .
C14 C -0.0210(7) 0.4166(5) 0.3675(5) 0.0344(15) Uani 0.667(7) 1 d D . P A 1
H14 H 0.030048 0.368076 0.406380 0.041 Uiso 0.667(7) 1 calc R U P A 1
C15 C -0.102(3) 0.3729(15) 0.3372(17) 0.043(3) Uani 0.667(7) 1 d D . P A 1
H15A H -0.044168 0.336320 0.306464 0.051 Uiso 0.667(7) 1 calc R U P A 1
H15B H -0.156409 0.417297 0.299585 0.051 Uiso 0.667(7) 1 calc R U P A 1
H15C H -0.157595 0.337219 0.386145 0.051 Uiso 0.667(7) 1 calc R U P A 1
C16 C -0.1090(7) 0.4680(5) 0.4235(5) 0.0480(15) Uani 0.667(7) 1 d D . P A 1
H16A H -0.055155 0.495403 0.442148 0.058 Uiso 0.667(7) 1 calc R U P A 1
H16B H -0.169272 0.512745 0.390707 0.058 Uiso 0.667(7) 1 calc R U P A 1
H16C H -0.158373 0.428629 0.472997 0.058 Uiso 0.667(7) 1 calc R U P A 1
C14A C -0.0482(17) 0.4463(11) 0.3481(9) 0.0344(15) Uani 0.333(7) 1 d D . P A 2
H14A H -0.112081 0.500390 0.338015 0.041 Uiso 0.333(7) 1 calc DR U P A 2
C15A C -0.106(6) 0.383(3) 0.327(4) 0.043(3) Uani 0.333(7) 1 d D . P A 2
H15D H -0.107916 0.404496 0.266071 0.051 Uiso 0.333(7) 1 calc R U P A 2
H15E H -0.052629 0.326292 0.341536 0.051 Uiso 0.333(7) 1 calc R U P A 2
H15F H -0.194584 0.377869 0.359051 0.051 Uiso 0.333(7) 1 calc R U P A 2
C16A C -0.0436(15) 0.4158(10) 0.4404(8) 0.0480(15) Uani 0.333(7) 1 d D . P A 2
H16D H -0.006089 0.457471 0.452475 0.058 Uiso 0.333(7) 1 calc R U P A 2
H16E H -0.131792 0.410777 0.473384 0.058 Uiso 0.333(7) 1 calc R U P A 2
H16F H 0.010163 0.359200 0.455869 0.058 Uiso 0.333(7) 1 calc R U P A 2
C21 C 0.3999(3) 0.3977(2) 0.3869(2) 0.0247(7) Uani 1 1 d . . . . .
H21 H 0.439110 0.342592 0.375310 0.030 Uiso 1 1 calc R U . . .
C22 C 0.2899(3) 0.3751(3) 0.4647(2) 0.0297(8) Uani 1 1 d . . . . .
H22A H 0.246368 0.429143 0.475805 0.036 Uiso 1 1 calc R U . . .
H22B H 0.224780 0.350895 0.450942 0.036 Uiso 1 1 calc R U . . .
C23 C 0.3341(4) 0.3107(3) 0.5452(2) 0.0355(9) Uani 1 1 d . . . . .
H23A H 0.368001 0.254071 0.537126 0.043 Uiso 1 1 calc R U . . .
H23B H 0.258840 0.302546 0.592561 0.043 Uiso 1 1 calc R U . . .
C24 C 0.4398(4) 0.3423(3) 0.5678(3) 0.0363(9) Uani 1 1 d . . . . .
H24A H 0.403540 0.395627 0.582165 0.044 Uiso 1 1 calc R U . . .
H24B H 0.471185 0.297628 0.617768 0.044 Uiso 1 1 calc R U . . .
C25 C 0.5525(4) 0.3608(3) 0.4929(3) 0.0373(10) Uani 1 1 d . . . . .
H25A H 0.593106 0.306367 0.481673 0.045 Uiso 1 1 calc R U . . .
H25B H 0.619074 0.383529 0.506877 0.045 Uiso 1 1 calc R U . . .
C26 C 0.5051(4) 0.4271(3) 0.4134(2) 0.0375(10) Uani 1 1 d . . . . .
H26A H 0.580163 0.437751 0.365980 0.045 Uiso 1 1 calc R U . . .
H26B H 0.469826 0.482425 0.423949 0.045 Uiso 1 1 calc R U . . .
C31 C 0.4719(3) 0.4941(2) 0.2199(2) 0.0296(8) Uani 1 1 d . . . . .
H31 H 0.545897 0.490313 0.247338 0.036 Uiso 1 1 calc R U . . .
C32 C 0.5194(5) 0.4332(3) 0.1685(3) 0.0567(13) Uani 1 1 d . . . . .
H32A H 0.452592 0.438385 0.135549 0.068 Uiso 1 1 calc R U . . .
H32B H 0.529346 0.372882 0.207924 0.068 Uiso 1 1 calc R U . . .
C33 C 0.6483(7) 0.4507(4) 0.1077(4) 0.081(2) Uani 1 1 d . . . . .
H33A H 0.717516 0.440565 0.140475 0.097 Uiso 1 1 calc R U . . .
H33B H 0.672025 0.410300 0.075076 0.097 Uiso 1 1 calc R U . . .
C34 C 0.6383(6) 0.5426(4) 0.0477(3) 0.0634(15) Uani 1 1 d . . . . .
H34A H 0.579605 0.549706 0.008763 0.076 Uiso 1 1 calc R U . . .
H34B H 0.725142 0.554448 0.013315 0.076 Uiso 1 1 calc R U . . .
C35 C 0.5875(5) 0.6073(3) 0.0940(3) 0.0462(11) Uani 1 1 d . . . . .
H35A H 0.574139 0.666128 0.052334 0.055 Uiso 1 1 calc R U . . .
H35B H 0.652690 0.606645 0.126200 0.055 Uiso 1 1 calc R U . . .
C36 C 0.4595(5) 0.5868(3) 0.1548(3) 0.0478(11) Uani 1 1 d . . . . .
H36A H 0.392184 0.593004 0.121921 0.057 Uiso 1 1 calc R U . . .
H36B H 0.431030 0.629082 0.185426 0.057 Uiso 1 1 calc R U . . .
C41 C 0.4818(4) 0.0655(2) 0.2981(2) 0.0311(8) Uani 1 1 d . . . . .
C42 C 0.3463(4) 0.0715(2) 0.3112(2) 0.0274(8) Uani 1 1 d . . . . .
C43 C 0.2962(4) -0.0060(3) 0.3337(3) 0.0367(9) Uani 1 1 d . . . . .
H43 H 0.204925 -0.005188 0.342867 0.044 Uiso 1 1 calc R U . . .
C44 C 0.3780(5) -0.0852(3) 0.3429(3) 0.0472(11) Uani 1 1 d . . . . .
H44 H 0.341621 -0.137007 0.358069 0.057 Uiso 1 1 calc R U . . .
C45 C 0.5102(5) -0.0880(3) 0.3300(3) 0.0503(12) Uani 1 1 d . . . . .
H45 H 0.564998 -0.141792 0.336737 0.060 Uiso 1 1 calc R U . . .
C46 C 0.5636(5) -0.0129(3) 0.3075(3) 0.0445(11) Uani 1 1 d . . . . .
H46 H 0.655046 -0.014551 0.298355 0.053 Uiso 1 1 calc R U . . .
C51 C 0.6417(8) 0.1594(6) 0.3364(5) 0.0406(18) Uani 0.639(8) 1 d D . P B 1
H51 H 0.712880 0.114236 0.323374 0.049 Uiso 0.639(8) 1 calc R U P B 1
C52 C 0.5873(7) 0.1218(6) 0.4297(5) 0.0512(17) Uani 0.639(8) 1 d D . P B 1
H52A H 0.546295 0.071060 0.439715 0.061 Uiso 0.639(8) 1 calc R U P B 1
H52B H 0.657779 0.104569 0.461983 0.061 Uiso 0.639(8) 1 calc R U P B 1
H52C H 0.522574 0.165400 0.447817 0.061 Uiso 0.639(8) 1 calc R U P B 1
C53 C 0.707(3) 0.2380(18) 0.316(2) 0.056(3) Uani 0.639(8) 1 d D . P B 1
H53A H 0.747158 0.256818 0.256025 0.068 Uiso 0.639(8) 1 calc R U P B 1
H53B H 0.773326 0.223490 0.350868 0.068 Uiso 0.639(8) 1 calc R U P B 1
H53C H 0.641680 0.284839 0.328022 0.068 Uiso 0.639(8) 1 calc R U P B 1
C51A C 0.6005(16) 0.1759(9) 0.3582(12) 0.0406(18) Uani 0.361(8) 1 d D . P B 2
H51A H 0.529084 0.198320 0.397481 0.049 Uiso 0.361(8) 1 calc R U P B 2
C52A C 0.6599(14) 0.0876(9) 0.4119(9) 0.0512(17) Uani 0.361(8) 1 d D . P B 2
H52D H 0.596326 0.046851 0.432007 0.061 Uiso 0.361(8) 1 calc R U P B 2
H52E H 0.737408 0.066029 0.377645 0.061 Uiso 0.361(8) 1 calc R U P B 2
H52F H 0.684090 0.093420 0.460562 0.061 Uiso 0.361(8) 1 calc R U P B 2
C53A C 0.704(5) 0.235(4) 0.330(4) 0.056(3) Uani 0.361(8) 1 d D . P B 2
H53D H 0.670083 0.292633 0.294764 0.068 Uiso 0.361(8) 1 calc R U P B 2
H53E H 0.727340 0.238800 0.379363 0.068 Uiso 0.361(8) 1 calc R U P B 2
H53F H 0.780658 0.211409 0.296446 0.068 Uiso 0.361(8) 1 calc R U P B 2
C54 C 0.6305(4) 0.2041(3) 0.1680(3) 0.0448(10) Uani 1 1 d . . . . .
H54 H 0.659239 0.259385 0.162089 0.054 Uiso 1 1 calc R U . . .
C55 C 0.7546(5) 0.1404(4) 0.1591(5) 0.0772(19) Uani 1 1 d . . . . .
H55A H 0.795327 0.124519 0.208667 0.093 Uiso 1 1 calc R U . . .
H55B H 0.814997 0.167715 0.107839 0.093 Uiso 1 1 calc R U . . .
H55C H 0.732749 0.088390 0.155133 0.093 Uiso 1 1 calc R U . . .
C56 C 0.5633(5) 0.2242(5) 0.0957(3) 0.0743(18) Uani 1 1 d . . . . .
H56A H 0.484092 0.264924 0.101655 0.089 Uiso 1 1 calc R U . . .
H56B H 0.621149 0.250147 0.042445 0.089 Uiso 1 1 calc R U . . .
H56C H 0.540660 0.170723 0.095358 0.089 Uiso 1 1 calc R U . . .
C61 C 0.1691(3) 0.1761(2) 0.3867(2) 0.0280(8) Uani 1 1 d . . . . .
H61 H 0.137266 0.238986 0.376413 0.034 Uiso 1 1 calc R U . . .
C62 C 0.2383(4) 0.1444(3) 0.4630(2) 0.0309(8) Uani 1 1 d . . . . .
H62A H 0.276059 0.083068 0.472697 0.037 Uiso 1 1 calc R U . . .
H62B H 0.310971 0.178243 0.448937 0.037 Uiso 1 1 calc R U . . .
C63 C 0.1511(4) 0.1520(3) 0.5448(3) 0.0374(9) Uani 1 1 d . . . . .
H63A H 0.201391 0.126743 0.591349 0.045 Uiso 1 1 calc R U . . .
H63B H 0.122501 0.213979 0.538221 0.045 Uiso 1 1 calc R U . . .
C64 C 0.0324(4) 0.1060(3) 0.5681(3) 0.0409(10) Uani 1 1 d . . . . .
H64A H 0.060029 0.042862 0.582265 0.049 Uiso 1 1 calc R U . . .
H64B H -0.025590 0.116585 0.618566 0.049 Uiso 1 1 calc R U . . .
C65 C -0.0404(4) 0.1381(3) 0.4954(3) 0.0416(10) Uani 1 1 d . . . . .
H65A H -0.077833 0.199486 0.486335 0.050 Uiso 1 1 calc R U . . .
H65B H -0.113018 0.104182 0.509937 0.050 Uiso 1 1 calc R U . . .
C66 C 0.0480(4) 0.1303(3) 0.4138(2) 0.0379(9) Uani 1 1 d . . . . .
H66A H -0.002937 0.154601 0.367586 0.045 Uiso 1 1 calc R U . . .
H66B H 0.076117 0.068149 0.421225 0.045 Uiso 1 1 calc R U . . .
C71 C 0.1843(4) 0.1971(3) 0.2194(2) 0.0306(8) Uani 1 1 d . . . . .
H71 H 0.096004 0.180863 0.248635 0.037 Uiso 1 1 calc R U . . .
C72 C 0.1603(5) 0.2930(3) 0.1706(3) 0.0444(11) Uani 1 1 d . . . . .
H72A H 0.243833 0.312532 0.136611 0.053 Uiso 1 1 calc R U . . .
H72B H 0.127888 0.324804 0.211382 0.053 Uiso 1 1 calc R U . . .
C73 C 0.0629(6) 0.3161(3) 0.1117(3) 0.0573(14) Uani 1 1 d . . . . .
H73A H -0.023832 0.303548 0.145902 0.069 Uiso 1 1 calc R U . . .
H73B H 0.056249 0.378829 0.079257 0.069 Uiso 1 1 calc R U . . .
C74 C 0.1023(5) 0.2661(3) 0.0512(3) 0.0547(13) Uani 1 1 d . . . . .
H74A H 0.180300 0.286930 0.009781 0.066 Uiso 1 1 calc R U . . .
H74B H 0.031466 0.276871 0.019507 0.066 Uiso 1 1 calc R U . . .
C75 C 0.1314(6) 0.1703(4) 0.0962(4) 0.0607(15) Uani 1 1 d . . . . .
H75A H 0.166535 0.140631 0.053794 0.073 Uiso 1 1 calc R U . . .
H75B H 0.049717 0.147624 0.130123 0.073 Uiso 1 1 calc R U . . .
C76 C 0.2289(5) 0.1500(3) 0.1544(3) 0.0569(15) Uani 1 1 d . . . . .
H76A H 0.313506 0.166885 0.119627 0.068 Uiso 1 1 calc R U . . .
H76B H 0.241864 0.086771 0.184526 0.068 Uiso 1 1 calc R U . . .
B1 B 0.3480(4) 0.4675(3) 0.2985(3) 0.0267(9) Uani 1 1 d . . . . .
B2 B 0.2684(4) 0.1689(3) 0.2975(3) 0.0239(8) Uani 1 1 d . . . . .
Li1 Li 0.2952(8) 0.2997(5) 0.3512(4) 0.0328(12) Uani 1 1 d . . . . .
Li2 Li 0.3293(8) 0.3499(5) 0.2067(4) 0.0327(12) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.589(3) . ?
P1 C1 1.799(4) . ?
P1 C14A 1.809(18) . ?
P1 C11 1.829(4) . ?
P1 C14 1.888(8) . ?
P2 N2 1.589(3) . ?
P2 C41 1.796(4) . ?
P2 C54 1.830(5) . ?
P2 C51 1.840(8) . ?
P2 C51A 1.922(18) . ?
N1 B1 1.654(5) . ?
N1 Li2 1.975(7) . ?
N1 Li1 2.017(7) . ?
N2 B2 1.647(5) . ?
N2 Li2 1.972(8) . ?
N2 Li1 2.018(8) . ?
C1 C6 1.394(5) . ?
C1 C2 1.401(5) . ?
C2 C3 1.408(5) . ?
C2 B1 1.631(5) . ?
C3 C4 1.373(6) . ?
C4 C5 1.396(7) . ?
C5 C6 1.387(6) . ?
C11 C12 1.519(7) . ?
C11 C13 1.530(6) . ?
C14 C15 1.530(10) . ?
C14 C16 1.545(8) . ?
C14A C16A 1.495(13) . ?
C14A C15A 1.524(15) . ?
C21 C22 1.542(5) . ?
C21 C26 1.542(5) . ?
C21 B1 1.685(5) . ?
C21 Li1 2.491(9) . ?
C22 C23 1.526(5) . ?
C22 Li1 2.679(8) . ?
C23 C24 1.529(5) . ?
C24 C25 1.526(6) . ?
C25 C26 1.536(5) . ?
C31 C32 1.522(6) . ?
C31 C36 1.548(6) . ?
C31 B1 1.652(6) . ?
C32 C33 1.528(7) . ?
C32 Li2 2.531(10) . ?
C33 C34 1.507(8) . ?
C34 C35 1.512(7) . ?
C35 C36 1.527(6) . ?
C41 C46 1.395(5) . ?
C41 C42 1.401(5) . ?
C42 C43 1.397(6) . ?
C42 B2 1.629(5) . ?
C43 C44 1.404(6) . ?
C44 C45 1.373(7) . ?
C45 C46 1.379(7) . ?
C51 C53 1.509(12) . ?
C51 C52 1.511(10) . ?
C51A C53A 1.512(15) . ?
C51A C52A 1.528(13) . ?
C54 C56 1.490(7) . ?
C54 C55 1.533(6) . ?
C61 C66 1.535(6) . ?
C61 C62 1.539(4) . ?
C61 B2 1.673(6) . ?
C61 Li1 2.521(9) . ?
C62 C63 1.524(6) . ?
C62 Li1 2.699(8) . ?
C63 C64 1.522(6) . ?
C64 C65 1.510(6) . ?
C65 C66 1.527(6) . ?
C71 C72 1.514(6) . ?
C71 C76 1.532(6) . ?
C71 B2 1.674(5) . ?
C72 C73 1.528(5) . ?
C72 Li2 2.512(9) . ?
C73 C74 1.500(7) . ?
C74 C75 1.507(7) . ?
C75 C76 1.526(6) . ?
B1 Li1 2.758(9) . ?
B2 Li1 2.767(9) . ?
Li1 Li2 2.283(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C1 102.97(16) . . ?
N1 P1 C14A 127.9(5) . . ?
C1 P1 C14A 105.5(5) . . ?
N1 P1 C11 115.19(18) . . ?
C1 P1 C11 109.7(2) . . ?
C14A P1 C11 94.8(4) . . ?
N1 P1 C14 111.2(2) . . ?
C1 P1 C14 109.7(2) . . ?
C11 P1 C14 107.9(3) . . ?
N2 P2 C41 102.70(17) . . ?
N2 P2 C54 114.73(18) . . ?
C41 P2 C54 111.5(2) . . ?
N2 P2 C51 125.5(3) . . ?
C41 P2 C51 105.0(3) . . ?
C54 P2 C51 97.1(3) . . ?
N2 P2 C51A 107.8(5) . . ?
C41 P2 C51A 109.2(5) . . ?
C54 P2 C51A 110.6(6) . . ?
P1 N1 B1 110.1(2) . . ?
P1 N1 Li2 130.7(3) . . ?
B1 N1 Li2 111.8(3) . . ?
P1 N1 Li1 128.7(3) . . ?
B1 N1 Li1 96.9(3) . . ?
Li2 N1 Li1 69.8(3) . . ?
P2 N2 B2 110.1(2) . . ?
P2 N2 Li2 130.0(3) . . ?
B2 N2 Li2 111.1(3) . . ?
P2 N2 Li1 130.1(3) . . ?
B2 N2 Li1 97.5(3) . . ?
Li2 N2 Li1 69.8(3) . . ?
C6 C1 C2 123.3(4) . . ?
C6 C1 P1 129.2(3) . . ?
C2 C1 P1 107.5(3) . . ?
C1 C2 C3 115.9(3) . . ?
C1 C2 B1 115.6(3) . . ?
C3 C2 B1 128.4(3) . . ?
C4 C3 C2 121.7(4) . . ?
C3 C4 C5 121.0(4) . . ?
C6 C5 C4 119.4(4) . . ?
C5 C6 C1 118.8(4) . . ?
C12 C11 C13 109.6(4) . . ?
C12 C11 P1 110.8(3) . . ?
C13 C11 P1 115.0(4) . . ?
C15 C14 C16 110.9(13) . . ?
C15 C14 P1 115.0(12) . . ?
C16 C14 P1 114.1(5) . . ?
C16A C14A C15A 111(2) . . ?
C16A C14A P1 112.5(11) . . ?
C15A C14A P1 116(3) . . ?
C22 C21 C26 107.1(3) . . ?
C22 C21 B1 113.6(3) . . ?
C26 C21 B1 114.8(3) . . ?
C22 C21 Li1 79.5(3) . . ?
C26 C21 Li1 157.6(3) . . ?
B1 C21 Li1 80.1(2) . . ?
C23 C22 C21 114.6(3) . . ?
C23 C22 Li1 112.3(3) . . ?
C21 C22 Li1 66.1(2) . . ?
C22 C23 C24 111.3(3) . . ?
C25 C24 C23 109.7(3) . . ?
C24 C25 C26 110.7(3) . . ?
C25 C26 C21 113.3(4) . . ?
C32 C31 C36 106.2(4) . . ?
C32 C31 B1 115.7(3) . . ?
C36 C31 B1 117.7(3) . . ?
C31 C32 C33 113.7(4) . . ?
C31 C32 Li2 102.4(3) . . ?
C33 C32 Li2 143.3(4) . . ?
C34 C33 C32 110.6(5) . . ?
C33 C34 C35 112.0(4) . . ?
C34 C35 C36 111.5(4) . . ?
C35 C36 C31 112.2(4) . . ?
C46 C41 C42 122.7(4) . . ?
C46 C41 P2 129.4(3) . . ?
C42 C41 P2 107.9(3) . . ?
C43 C42 C41 116.2(4) . . ?
C43 C42 B2 128.8(4) . . ?
C41 C42 B2 115.0(3) . . ?
C42 C43 C44 121.4(4) . . ?
C45 C44 C43 120.3(4) . . ?
C44 C45 C46 120.1(4) . . ?
C45 C46 C41 119.2(4) . . ?
C53 C51 C52 112.5(14) . . ?
C53 C51 P2 115.5(15) . . ?
C52 C51 P2 111.5(6) . . ?
C53A C51A C52A 106(3) . . ?
C53A C51A P2 116(3) . . ?
C52A C51A P2 114.5(11) . . ?
C56 C54 C55 109.8(5) . . ?
C56 C54 P2 112.8(3) . . ?
C55 C54 P2 114.9(4) . . ?
C66 C61 C62 107.5(3) . . ?
C66 C61 B2 116.0(3) . . ?
C62 C61 B2 113.1(3) . . ?
C66 C61 Li1 156.5(3) . . ?
C62 C61 Li1 79.3(3) . . ?
B2 C61 Li1 79.7(3) . . ?
C63 C62 C61 114.4(3) . . ?
C63 C62 Li1 112.2(3) . . ?
C61 C62 Li1 66.6(3) . . ?
C64 C63 C62 111.8(3) . . ?
C65 C64 C63 110.5(4) . . ?
C64 C65 C66 111.6(3) . . ?
C65 C66 C61 114.6(3) . . ?
C72 C71 C76 107.2(4) . . ?
C72 C71 B2 116.3(3) . . ?
C76 C71 B2 117.8(3) . . ?
C71 C72 C73 113.7(4) . . ?
C71 C72 Li2 101.7(3) . . ?
C73 C72 Li2 143.8(4) . . ?
C74 C73 C72 111.7(4) . . ?
C73 C74 C75 111.9(4) . . ?
C74 C75 C76 112.0(4) . . ?
C75 C76 C71 112.4(4) . . ?
C2 B1 C31 110.6(3) . . ?
C2 B1 N1 103.8(3) . . ?
C31 B1 N1 113.7(3) . . ?
C2 B1 C21 110.3(3) . . ?
C31 B1 C21 110.9(3) . . ?
N1 B1 C21 107.3(3) . . ?
C2 B1 Li1 131.2(3) . . ?
C31 B1 Li1 116.8(3) . . ?
N1 B1 Li1 46.5(2) . . ?
C21 B1 Li1 62.9(2) . . ?
C42 B2 N2 104.2(3) . . ?
C42 B2 C61 111.3(3) . . ?
N2 B2 C61 108.2(3) . . ?
C42 B2 C71 109.8(3) . . ?
N2 B2 C71 112.8(3) . . ?
C61 B2 C71 110.3(3) . . ?
C42 B2 Li1 131.7(3) . . ?
N2 B2 Li1 46.3(2) . . ?
C61 B2 Li1 63.7(2) . . ?
C71 B2 Li1 116.8(3) . . ?
N1 Li1 N2 108.4(3) . . ?
N1 Li1 Li2 54.3(3) . . ?
N2 Li1 Li2 54.2(3) . . ?
N1 Li1 C21 72.4(3) . . ?
N2 Li1 C21 125.5(4) . . ?
Li2 Li1 C21 103.9(4) . . ?
N1 Li1 C61 124.1(4) . . ?
N2 Li1 C61 71.7(3) . . ?
Li2 Li1 C61 102.0(4) . . ?
C21 Li1 C61 154.1(3) . . ?
N1 Li1 C22 83.5(3) . . ?
N2 Li1 C22 153.6(4) . . ?
Li2 Li1 C22 132.2(4) . . ?
C21 Li1 C22 34.45(15) . . ?
C61 Li1 C22 121.7(3) . . ?
N1 Li1 C62 151.9(4) . . ?
N2 Li1 C62 83.2(3) . . ?
Li2 Li1 C62 130.7(4) . . ?
C21 Li1 C62 122.3(3) . . ?
C61 Li1 C62 34.07(14) . . ?
C22 Li1 C62 97.2(2) . . ?
N1 Li1 B1 36.54(17) . . ?
N2 Li1 B1 116.9(3) . . ?
Li2 Li1 B1 72.7(3) . . ?
C21 Li1 B1 37.01(16) . . ?
C61 Li1 B1 159.3(3) . . ?
C22 Li1 B1 59.6(2) . . ?
C62 Li1 B1 156.7(3) . . ?
N1 Li1 B2 116.5(3) . . ?
N2 Li1 B2 36.18(18) . . ?
Li2 Li1 B2 71.9(3) . . ?
C21 Li1 B2 160.1(3) . . ?
C61 Li1 B2 36.53(17) . . ?
C22 Li1 B2 155.8(3) . . ?
C62 Li1 B2 58.8(2) . . ?
B1 Li1 B2 144.6(3) . . ?
N2 Li2 N1 112.0(3) . . ?
N2 Li2 Li1 56.0(3) . . ?
N1 Li2 Li1 56.0(3) . . ?
N2 Li2 C72 87.2(3) . . ?
N1 Li2 C72 109.3(4) . . ?
Li1 Li2 C72 104.4(4) . . ?
N2 Li2 C32 107.8(3) . . ?
N1 Li2 C32 86.1(3) . . ?
Li1 Li2 C32 102.5(4) . . ?
C72 Li2 C32 153.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 P1 N1 B1 -0.9(3) . . . . ?
C14A P1 N1 B1 -122.7(6) . . . . ?
C11 P1 N1 B1 118.4(3) . . . . ?
C14 P1 N1 B1 -118.4(3) . . . . ?
C1 P1 N1 Li2 -147.7(4) . . . . ?
C14A P1 N1 Li2 90.6(7) . . . . ?
C11 P1 N1 Li2 -28.3(4) . . . . ?
C14 P1 N1 Li2 94.9(4) . . . . ?
C1 P1 N1 Li1 116.3(3) . . . . ?
C14A P1 N1 Li1 -5.4(7) . . . . ?
C11 P1 N1 Li1 -124.3(4) . . . . ?
C14 P1 N1 Li1 -1.1(4) . . . . ?
C41 P2 N2 B2 -2.3(3) . . . . ?
C54 P2 N2 B2 118.8(3) . . . . ?
C51 P2 N2 B2 -121.5(4) . . . . ?
C51A P2 N2 B2 -117.5(6) . . . . ?
C41 P2 N2 Li2 -146.3(3) . . . . ?
C54 P2 N2 Li2 -25.2(4) . . . . ?
C51 P2 N2 Li2 94.5(5) . . . . ?
C51A P2 N2 Li2 98.5(6) . . . . ?
C41 P2 N2 Li1 117.0(4) . . . . ?
C54 P2 N2 Li1 -121.9(4) . . . . ?
C51 P2 N2 Li1 -2.2(5) . . . . ?
C51A P2 N2 Li1 1.8(7) . . . . ?
N1 P1 C1 C6 -179.4(4) . . . . ?
C14A P1 C1 C6 -43.5(6) . . . . ?
C11 P1 C1 C6 57.5(5) . . . . ?
C14 P1 C1 C6 -61.0(5) . . . . ?
N1 P1 C1 C2 0.4(3) . . . . ?
C14A P1 C1 C2 136.2(5) . . . . ?
C11 P1 C1 C2 -122.8(3) . . . . ?
C14 P1 C1 C2 118.8(3) . . . . ?
C6 C1 C2 C3 -1.6(6) . . . . ?
P1 C1 C2 C3 178.6(3) . . . . ?
C6 C1 C2 B1 -179.8(4) . . . . ?
P1 C1 C2 B1 0.4(4) . . . . ?
C1 C2 C3 C4 1.2(6) . . . . ?
B1 C2 C3 C4 179.1(4) . . . . ?
C2 C3 C4 C5 0.2(7) . . . . ?
C3 C4 C5 C6 -1.2(7) . . . . ?
C4 C5 C6 C1 0.8(7) . . . . ?
C2 C1 C6 C5 0.6(7) . . . . ?
P1 C1 C6 C5 -179.6(4) . . . . ?
N1 P1 C11 C12 -48.5(4) . . . . ?
C1 P1 C11 C12 67.1(4) . . . . ?
C14A P1 C11 C12 175.4(6) . . . . ?
C14 P1 C11 C12 -173.4(4) . . . . ?
N1 P1 C11 C13 -173.4(4) . . . . ?
C1 P1 C11 C13 -57.8(5) . . . . ?
C14A P1 C11 C13 50.5(7) . . . . ?
C14 P1 C11 C13 61.8(5) . . . . ?
N1 P1 C14 C15 -96.0(13) . . . . ?
C1 P1 C14 C15 150.7(12) . . . . ?
C11 P1 C14 C15 31.2(13) . . . . ?
N1 P1 C14 C16 134.3(5) . . . . ?
C1 P1 C14 C16 21.1(6) . . . . ?
C11 P1 C14 C16 -98.4(6) . . . . ?
N1 P1 C14A C16A 59.8(14) . . . . ?
C1 P1 C14A C16A -60.9(12) . . . . ?
C11 P1 C14A C16A -172.9(11) . . . . ?
N1 P1 C14A C15A -70(3) . . . . ?
C1 P1 C14A C15A 170(3) . . . . ?
C11 P1 C14A C15A 58(3) . . . . ?
C26 C21 C22 C23 -53.2(4) . . . . ?
B1 C21 C22 C23 179.0(3) . . . . ?
Li1 C21 C22 C23 104.7(4) . . . . ?
C26 C21 C22 Li1 -157.9(3) . . . . ?
B1 C21 C22 Li1 74.3(3) . . . . ?
C21 C22 C23 C24 55.7(5) . . . . ?
Li1 C22 C23 C24 128.6(4) . . . . ?
C22 C23 C24 C25 -55.3(5) . . . . ?
C23 C24 C25 C26 56.8(5) . . . . ?
C24 C25 C26 C21 -58.6(5) . . . . ?
C22 C21 C26 C25 54.4(4) . . . . ?
B1 C21 C26 C25 -178.5(3) . . . . ?
Li1 C21 C26 C25 -49.8(9) . . . . ?
C36 C31 C32 C33 58.0(6) . . . . ?
B1 C31 C32 C33 -169.3(5) . . . . ?
C36 C31 C32 Li2 -114.9(3) . . . . ?
B1 C31 C32 Li2 17.8(4) . . . . ?
C31 C32 C33 C34 -57.3(8) . . . . ?
Li2 C32 C33 C34 111.2(7) . . . . ?
C32 C33 C34 C35 52.7(8) . . . . ?
C33 C34 C35 C36 -53.4(6) . . . . ?
C34 C35 C36 C31 56.8(5) . . . . ?
C32 C31 C36 C35 -57.3(5) . . . . ?
B1 C31 C36 C35 171.1(3) . . . . ?
N2 P2 C41 C46 -177.9(4) . . . . ?
C54 P2 C41 C46 58.8(4) . . . . ?
C51 P2 C41 C46 -45.3(5) . . . . ?
C51A P2 C41 C46 -63.7(7) . . . . ?
N2 P2 C41 C42 1.1(3) . . . . ?
C54 P2 C41 C42 -122.3(3) . . . . ?
C51 P2 C41 C42 133.7(4) . . . . ?
C51A P2 C41 C42 115.2(6) . . . . ?
C46 C41 C42 C43 -0.6(6) . . . . ?
P2 C41 C42 C43 -179.6(3) . . . . ?
C46 C41 C42 B2 179.7(4) . . . . ?
P2 C41 C42 B2 0.7(4) . . . . ?
C41 C42 C43 C44 0.4(6) . . . . ?
B2 C42 C43 C44 180.0(4) . . . . ?
C42 C43 C44 C45 0.1(7) . . . . ?
C43 C44 C45 C46 -0.4(7) . . . . ?
C44 C45 C46 C41 0.2(7) . . . . ?
C42 C41 C46 C45 0.4(7) . . . . ?
P2 C41 C46 C45 179.1(4) . . . . ?
N2 P2 C51 C53 -70.6(16) . . . . ?
C41 P2 C51 C53 171.3(15) . . . . ?
C54 P2 C51 C53 56.7(15) . . . . ?
N2 P2 C51 C52 59.5(8) . . . . ?
C41 P2 C51 C52 -58.6(7) . . . . ?
C54 P2 C51 C52 -173.2(6) . . . . ?
N2 P2 C54 C56 -43.3(5) . . . . ?
C41 P2 C54 C56 72.9(4) . . . . ?
C51 P2 C54 C56 -177.8(5) . . . . ?
C51A P2 C54 C56 -165.4(6) . . . . ?
N2 P2 C54 C55 -170.1(4) . . . . ?
C41 P2 C54 C55 -54.0(5) . . . . ?
C51 P2 C54 C55 55.3(5) . . . . ?
C51A P2 C54 C55 67.7(6) . . . . ?
C66 C61 C62 C63 -51.9(4) . . . . ?
B2 C61 C62 C63 178.7(3) . . . . ?
Li1 C61 C62 C63 104.8(4) . . . . ?
C66 C61 C62 Li1 -156.7(3) . . . . ?
B2 C61 C62 Li1 73.9(3) . . . . ?
C61 C62 C63 C64 55.0(5) . . . . ?
Li1 C62 C63 C64 128.5(4) . . . . ?
C62 C63 C64 C65 -54.3(5) . . . . ?
C63 C64 C65 C66 54.4(5) . . . . ?
C64 C65 C66 C61 -55.7(5) . . . . ?
C62 C61 C66 C65 52.2(4) . . . . ?
B2 C61 C66 C65 180.0(3) . . . . ?
Li1 C61 C66 C65 -51.5(9) . . . . ?
C76 C71 C72 C73 56.3(5) . . . . ?
B2 C71 C72 C73 -169.4(4) . . . . ?
C76 C71 C72 Li2 -115.9(4) . . . . ?
B2 C71 C72 Li2 18.5(4) . . . . ?
C71 C72 C73 C74 -55.3(7) . . . . ?
Li2 C72 C73 C74 111.6(6) . . . . ?
C72 C73 C74 C75 51.4(7) . . . . ?
C73 C74 C75 C76 -52.4(7) . . . . ?
C74 C75 C76 C71 56.2(7) . . . . ?
C72 C71 C76 C75 -56.4(6) . . . . ?
B2 C71 C76 C75 170.0(4) . . . . ?
C1 C2 B1 C31 121.3(4) . . . . ?
C3 C2 B1 C31 -56.6(5) . . . . ?
C1 C2 B1 N1 -1.0(4) . . . . ?
C3 C2 B1 N1 -178.9(4) . . . . ?
C1 C2 B1 C21 -115.6(4) . . . . ?
C3 C2 B1 C21 66.4(5) . . . . ?
C1 C2 B1 Li1 -44.4(5) . . . . ?
C3 C2 B1 Li1 137.6(4) . . . . ?
C32 C31 B1 C2 -151.3(4) . . . . ?
C36 C31 B1 C2 -24.1(4) . . . . ?
C32 C31 B1 N1 -34.9(5) . . . . ?
C36 C31 B1 N1 92.2(4) . . . . ?
C32 C31 B1 C21 86.0(4) . . . . ?
C36 C31 B1 C21 -146.9(3) . . . . ?
C32 C31 B1 Li1 16.7(4) . . . . ?
C36 C31 B1 Li1 143.9(3) . . . . ?
P1 N1 B1 C2 1.1(3) . . . . ?
Li2 N1 B1 C2 154.6(3) . . . . ?
Li1 N1 B1 C2 -134.5(3) . . . . ?
P1 N1 B1 C31 -119.1(3) . . . . ?
Li2 N1 B1 C31 34.3(4) . . . . ?
Li1 N1 B1 C31 105.2(3) . . . . ?
P1 N1 B1 C21 117.9(3) . . . . ?
Li2 N1 B1 C21 -88.6(3) . . . . ?
Li1 N1 B1 C21 -17.7(3) . . . . ?
P1 N1 B1 Li1 135.7(3) . . . . ?
Li2 N1 B1 Li1 -70.9(3) . . . . ?
C22 C21 B1 C2 53.0(4) . . . . ?
C26 C21 B1 C2 -70.7(4) . . . . ?
Li1 C21 B1 C2 126.8(3) . . . . ?
C22 C21 B1 C31 175.9(3) . . . . ?
C26 C21 B1 C31 52.2(4) . . . . ?
Li1 C21 B1 C31 -110.3(3) . . . . ?
C22 C21 B1 N1 -59.5(4) . . . . ?
C26 C21 B1 N1 176.8(3) . . . . ?
Li1 C21 B1 N1 14.4(3) . . . . ?
C22 C21 B1 Li1 -73.8(3) . . . . ?
C26 C21 B1 Li1 162.4(4) . . . . ?
C43 C42 B2 N2 178.3(3) . . . . ?
C41 C42 B2 N2 -2.1(4) . . . . ?
C43 C42 B2 C61 61.8(5) . . . . ?
C41 C42 B2 C61 -118.6(3) . . . . ?
C43 C42 B2 C71 -60.7(5) . . . . ?
C41 C42 B2 C71 119.0(3) . . . . ?
C43 C42 B2 Li1 135.0(4) . . . . ?
C41 C42 B2 Li1 -45.3(5) . . . . ?
P2 N2 B2 C42 2.7(3) . . . . ?
Li2 N2 B2 C42 153.9(3) . . . . ?
Li1 N2 B2 C42 -135.0(3) . . . . ?
P2 N2 B2 C61 121.3(2) . . . . ?
Li2 N2 B2 C61 -87.6(3) . . . . ?
Li1 N2 B2 C61 -16.4(3) . . . . ?
P2 N2 B2 C71 -116.3(3) . . . . ?
Li2 N2 B2 C71 34.8(4) . . . . ?
Li1 N2 B2 C71 106.0(3) . . . . ?
P2 N2 B2 Li1 137.7(3) . . . . ?
Li2 N2 B2 Li1 -71.2(3) . . . . ?
C66 C61 B2 C42 -71.4(4) . . . . ?
C62 C61 B2 C42 53.5(4) . . . . ?
Li1 C61 B2 C42 127.1(3) . . . . ?
C66 C61 B2 N2 174.6(3) . . . . ?
C62 C61 B2 N2 -60.4(4) . . . . ?
Li1 C61 B2 N2 13.2(3) . . . . ?
C66 C61 B2 C71 50.8(4) . . . . ?
C62 C61 B2 C71 175.7(3) . . . . ?
Li1 C61 B2 C71 -110.7(3) . . . . ?
C66 C61 B2 Li1 161.5(4) . . . . ?
C62 C61 B2 Li1 -73.6(3) . . . . ?
C72 C71 B2 C42 -151.9(4) . . . . ?
C76 C71 B2 C42 -22.5(5) . . . . ?
C72 C71 B2 N2 -36.1(5) . . . . ?
C76 C71 B2 N2 93.3(4) . . . . ?
C72 C71 B2 C61 85.0(4) . . . . ?
C76 C71 B2 C61 -145.6(4) . . . . ?
C72 C71 B2 Li1 15.0(5) . . . . ?
C76 C71 B2 Li1 144.4(4) . . . . ?

_refine_diff_density_max         0.602
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.066



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes at -40C'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PB(NH)
_database_code_depnum_ccdc_archive 'CCDC 2106479'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_audit_creation_date             2020-04-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
bfrenett@ualberta.ca
yuqiao4@ualberta.ca
erivard@ualberta.ca
_chemical_name_common            PB(NH)
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H41 B N P'
_chemical_formula_sum            'C24 H41 B N P'
_chemical_formula_weight         385.36
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.5379(3)
_cell_length_b                   9.6520(3)
_cell_length_c                   22.5624(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.7034(12)
_cell_angle_gamma                90
_cell_volume                     2292.31(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9763
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      72.763
_cell_measurement_theta_min      3.923
_shelx_estimated_absorpt_T_max   0.909
_shelx_estimated_absorpt_T_min   0.827
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.9647
_exptl_absorpt_correction_T_min  0.8844
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,  J. Appl. Cryst. 48 (2015) 3-10'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             848
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 2.00 0.0770
1.00 1.00 -2.00 0.0250
0.00 0.00 1.00 0.0640
0.00 0.00 -1.00 0.0170
1.00 2.00 -2.00 0.0370
1.00 1.00 2.00 0.0480
-1.00 -1.00 -2.00 0.0240
0.00 -1.00 1.00 0.0270
0.00 -2.00 1.00 0.0170
0.00 2.00 -1.00 0.0470
1.00 -2.00 2.00 0.0160
-1.00 2.00 -2.00 0.0670
2.00 -1.00 2.00 0.0340
0.00 2.00 1.00 0.0510
0.00 -2.00 -1.00 0.0130
2.00 -2.00 -1.00 0.0190
1.00 -2.00 -2.00 0.0120
-1.00 2.00 2.00 0.0580

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes/DCM at -40C'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.089
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            60334
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.756
_diffrn_reflns_theta_min         3.923
_diffrn_ambient_temperature      193.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           0.64
_diffrn_source_power             0.0286528
_diffrn_source_voltage           44.77
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4140
_reflns_number_total             4544
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0345
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+0.5627P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0956
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C13(H13), C19(H19), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C14(H14A,H14B), C20(H20A,H20B), C16(H16A,H16B), C24(H24A,
 H24B), C17(H17A,H17B), C15(H15A,H15B), C21(H21A,H21B), C22(H22A,H22B),
 C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P P 0.13408(3) 1.04202(3) 0.36775(2) 0.02639(10) Uani 1 1 d . . . . .
B B 0.26037(12) 0.80039(13) 0.39487(6) 0.0251(2) Uani 1 1 d . . . . .
N N 0.26610(9) 0.95796(10) 0.37011(4) 0.0277(2) Uani 1 1 d . . . . .
H H 0.3331(16) 1.0018(18) 0.3659(7) 0.047(4) Uiso 1 1 d . . . . .
C1 C 0.03286(11) 0.90113(12) 0.38522(5) 0.0271(2) Uani 1 1 d . . . . .
C2 C 0.10685(11) 0.78282(12) 0.39816(5) 0.0260(2) Uani 1 1 d . . . . .
C3 C 0.03904(12) 0.66241(12) 0.41151(5) 0.0310(3) Uani 1 1 d . . . . .
C4 C -0.09270(12) 0.66214(14) 0.41287(6) 0.0367(3) Uani 1 1 d . . . . .
C5 C -0.16242(12) 0.78183(15) 0.40044(6) 0.0384(3) Uani 1 1 d . . . . .
C6 C -0.09980(11) 0.90248(14) 0.38610(6) 0.0338(3) Uani 1 1 d . . . . .
C7 C 0.12318(12) 1.17781(12) 0.42399(6) 0.0324(3) Uani 1 1 d . . . . .
C8 C 0.00338(13) 1.26665(14) 0.41560(7) 0.0425(3) Uani 1 1 d . . . . .
C9 C 0.24286(14) 1.26732(14) 0.43124(7) 0.0443(3) Uani 1 1 d . . . . .
C10 C 0.08757(13) 1.11798(14) 0.29593(6) 0.0370(3) Uani 1 1 d . . . . .
C11 C 0.06527(17) 1.00787(18) 0.24801(6) 0.0549(4) Uani 1 1 d . . . . .
C12 C 0.18454(18) 1.22475(18) 0.27712(8) 0.0591(4) Uani 1 1 d . . . . .
C13 C 0.33639(10) 0.79060(11) 0.46016(5) 0.0264(2) Uani 1 1 d . . . . .
C14 C 0.32725(12) 0.64638(12) 0.48826(5) 0.0315(3) Uani 1 1 d . . . . .
C15 C 0.41177(13) 0.63094(14) 0.54480(6) 0.0383(3) Uani 1 1 d . . . . .
C16 C 0.38245(14) 0.74243(15) 0.59018(6) 0.0418(3) Uani 1 1 d . . . . .
C17 C 0.38666(13) 0.88743(14) 0.56337(6) 0.0372(3) Uani 1 1 d . . . . .
C18 C 0.30193(11) 0.89900(12) 0.50647(5) 0.0305(3) Uani 1 1 d . . . . .
C19 C 0.31844(11) 0.69029(12) 0.34740(5) 0.0294(2) Uani 1 1 d . . . . .
C20 C 0.46402(12) 0.68422(14) 0.34736(6) 0.0369(3) Uani 1 1 d . . . . .
C21 C 0.51226(17) 0.57357(18) 0.30536(7) 0.0529(4) Uani 1 1 d . . . . .
C22 C 0.45875(16) 0.59629(18) 0.24226(6) 0.0513(4) Uani 1 1 d . . . . .
C23 C 0.31421(16) 0.60148(16) 0.24033(6) 0.0475(4) Uani 1 1 d . . . . .
C24 C 0.26665(12) 0.71044(14) 0.28313(5) 0.0365(3) Uani 1 1 d . . . . .
H3 H 0.084354 0.579022 0.419817 0.037 Uiso 1 1 calc R U . . .
H4 H -0.135657 0.579129 0.422426 0.044 Uiso 1 1 calc R U . . .
H5 H -0.252383 0.780810 0.401772 0.046 Uiso 1 1 calc R U . . .
H6 H -0.146127 0.984809 0.377007 0.041 Uiso 1 1 calc R U . . .
H7 H 0.115568 1.128573 0.462661 0.039 Uiso 1 1 calc R U . . .
H8A H 0.010942 1.326859 0.380974 0.064 Uiso 1 1 calc R U . . .
H8B H -0.006621 1.323625 0.451028 0.064 Uiso 1 1 calc R U . . .
H8C H -0.070880 1.206337 0.409429 0.064 Uiso 1 1 calc R U . . .
H9A H 0.317946 1.207415 0.434553 0.066 Uiso 1 1 calc R U . . .
H9B H 0.238647 1.323859 0.467170 0.066 Uiso 1 1 calc R U . . .
H9C H 0.248584 1.327963 0.396633 0.066 Uiso 1 1 calc R U . . .
H10 H 0.005276 1.167607 0.300431 0.044 Uiso 1 1 calc R U . . .
H11A H 0.146110 0.963198 0.239846 0.082 Uiso 1 1 calc R U . . .
H11B H 0.029701 1.051479 0.211684 0.082 Uiso 1 1 calc R U . . .
H11C H 0.005671 0.938230 0.261733 0.082 Uiso 1 1 calc R U . . .
H12A H 0.183970 1.304365 0.304064 0.089 Uiso 1 1 calc R U . . .
H12B H 0.162598 1.255582 0.236541 0.089 Uiso 1 1 calc R U . . .
H12C H 0.269362 1.182891 0.278679 0.089 Uiso 1 1 calc R U . . .
H13 H 0.428258 0.805355 0.452826 0.032 Uiso 1 1 calc R U . . .
H14A H 0.237927 0.628482 0.497700 0.038 Uiso 1 1 calc R U . . .
H14B H 0.351990 0.575828 0.459120 0.038 Uiso 1 1 calc R U . . .
H15A H 0.398302 0.538326 0.562289 0.046 Uiso 1 1 calc R U . . .
H15B H 0.502028 0.637878 0.534822 0.046 Uiso 1 1 calc R U . . .
H16A H 0.297059 0.725600 0.605222 0.050 Uiso 1 1 calc R U . . .
H16B H 0.445072 0.736430 0.624201 0.050 Uiso 1 1 calc R U . . .
H17A H 0.475312 0.910108 0.554346 0.045 Uiso 1 1 calc R U . . .
H17B H 0.358328 0.955664 0.592724 0.045 Uiso 1 1 calc R U . . .
H18A H 0.310902 0.992819 0.489435 0.037 Uiso 1 1 calc R U . . .
H18B H 0.212063 0.886570 0.516290 0.037 Uiso 1 1 calc R U . . .
H19 H 0.289903 0.596220 0.359722 0.035 Uiso 1 1 calc R U . . .
H20A H 0.496654 0.775810 0.335501 0.044 Uiso 1 1 calc R U . . .
H20B H 0.498141 0.664692 0.388141 0.044 Uiso 1 1 calc R U . . .
H21A H 0.606211 0.576717 0.305866 0.063 Uiso 1 1 calc R U . . .
H21B H 0.486844 0.480769 0.319245 0.063 Uiso 1 1 calc R U . . .
H22A H 0.486740 0.520078 0.216571 0.062 Uiso 1 1 calc R U . . .
H22B H 0.492101 0.684318 0.226710 0.062 Uiso 1 1 calc R U . . .
H23A H 0.280650 0.509463 0.251018 0.057 Uiso 1 1 calc R U . . .
H23B H 0.282034 0.623549 0.199488 0.057 Uiso 1 1 calc R U . . .
H24A H 0.172680 0.707195 0.282307 0.044 Uiso 1 1 calc R U . . .
H24B H 0.291734 0.803396 0.269290 0.044 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P N 1.6092(10) . ?
P C1 1.7839(12) . ?
P C7 1.8318(13) . ?
P C10 1.8245(12) . ?
N B 1.6223(15) . ?
N H 0.833(17) . ?
C1 C6 1.3991(16) . ?
C2 B 1.6318(16) . ?
C2 C1 1.4056(16) . ?
C2 C3 1.4044(16) . ?
C3 C4 1.3901(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.3905(19) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C5 1.3843(18) . ?
C6 H6 0.9500 . ?
C7 C8 1.5304(17) . ?
C7 C9 1.5310(18) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.526(2) . ?
C10 C12 1.526(2) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 B 1.6461(16) . ?
C13 C14 1.5345(16) . ?
C13 H13 1.0000 . ?
C14 C15 1.5283(16) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C15 1.5269(18) . ?
C16 C17 1.5262(19) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C13 1.5343(15) . ?
C18 C17 1.5329(16) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 B 1.6472(16) . ?
C19 C24 1.5374(16) . ?
C19 H19 1.0000 . ?
C20 C19 1.5352(17) . ?
C20 C21 1.5306(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.522(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.523(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C23 1.5282(18) . ?
C24 H24A 0.9900 . ?
C24 H24B 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
N P C1 97.66(5) . . ?
N P C7 114.85(6) . . ?
N P C10 115.32(6) . . ?
C1 P C7 109.55(5) . . ?
C1 P C10 111.36(6) . . ?
C10 P C7 107.74(6) . . ?
N B C2 99.57(8) . . ?
N B C13 109.73(9) . . ?
N B C19 111.09(9) . . ?
C2 B C13 113.27(9) . . ?
C2 B C19 111.22(9) . . ?
C13 B C19 111.40(9) . . ?
P N B 115.97(7) . . ?
P N H 118.5(12) . . ?
B N H 124.1(12) . . ?
C2 C1 P 109.49(8) . . ?
C6 C1 P 127.18(9) . . ?
C6 C1 C2 123.33(11) . . ?
C1 C2 B 116.59(10) . . ?
C3 C2 B 127.68(10) . . ?
C3 C2 C1 115.72(10) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.67(12) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 120.84(12) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.53(11) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 H6 120.6 . . ?
C5 C6 C1 118.89(12) . . ?
C5 C6 H6 120.6 . . ?
P C7 H7 105.9 . . ?
C8 C7 P 113.17(9) . . ?
C8 C7 C9 111.57(11) . . ?
C8 C7 H7 105.9 . . ?
C9 C7 P 113.54(9) . . ?
C9 C7 H7 105.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P C10 H10 107.5 . . ?
C11 C10 P 112.04(9) . . ?
C11 C10 H10 107.5 . . ?
C12 C10 P 111.29(10) . . ?
C12 C10 C11 110.86(13) . . ?
C12 C10 H10 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
B C13 H13 106.1 . . ?
C14 C13 B 112.61(9) . . ?
C14 C13 H13 106.1 . . ?
C18 C13 B 116.71(9) . . ?
C18 C13 C14 108.41(9) . . ?
C18 C13 H13 106.1 . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 C13 112.82(10) . . ?
C15 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C14 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
C16 C15 C14 111.26(10) . . ?
C16 C15 H15A 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
C17 C16 C15 111.71(11) . . ?
C17 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
C16 C17 C18 111.85(11) . . ?
C16 C17 H17A 109.2 . . ?
C16 C17 H17B 109.2 . . ?
C18 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C13 C18 H18A 109.2 . . ?
C13 C18 H18B 109.2 . . ?
C17 C18 C13 111.93(9) . . ?
C17 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
B C19 H19 106.2 . . ?
C20 C19 B 115.27(10) . . ?
C20 C19 C24 108.34(10) . . ?
C20 C19 H19 106.2 . . ?
C24 C19 B 113.92(10) . . ?
C24 C19 H19 106.2 . . ?
C19 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C21 C20 C19 112.83(12) . . ?
C21 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
C22 C21 C20 111.06(12) . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C21 C22 C23 110.94(12) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.0 . . ?
C22 C23 C24 111.23(12) . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C19 C24 H24A 108.9 . . ?
C19 C24 H24B 108.9 . . ?
C23 C24 C19 113.35(11) . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P N B C2 8.74(10) . . . . ?
P N B C13 -110.35(9) . . . . ?
P N B C19 126.02(9) . . . . ?
P C1 C6 C5 179.55(10) . . . . ?
B C2 C1 P 0.37(12) . . . . ?
B C2 C1 C6 179.93(10) . . . . ?
B C2 C3 C4 179.88(11) . . . . ?
B C13 C14 C15 172.39(10) . . . . ?
B C19 C24 C23 -176.01(10) . . . . ?
N P C1 C2 4.66(9) . . . . ?
N P C1 C6 -174.88(11) . . . . ?
N P C7 C8 173.01(9) . . . . ?
N P C7 C9 44.50(11) . . . . ?
N P C10 C11 62.71(12) . . . . ?
N P C10 C12 -62.04(12) . . . . ?
C1 P N B -8.38(9) . . . . ?
C1 P C7 C8 -78.31(10) . . . . ?
C1 P C7 C9 153.18(9) . . . . ?
C1 P C10 C11 -47.37(12) . . . . ?
C1 P C10 C12 -172.13(10) . . . . ?
C1 C2 B N -5.21(12) . . . . ?
C1 C2 B C13 111.23(11) . . . . ?
C1 C2 B C19 -122.39(11) . . . . ?
C1 C2 C3 C4 -1.23(17) . . . . ?
C1 C6 C5 C4 -0.79(19) . . . . ?
C2 C1 C6 C5 0.08(18) . . . . ?
C2 C3 C4 C5 0.59(19) . . . . ?
C3 C2 B N 173.67(11) . . . . ?
C3 C2 B C13 -69.89(14) . . . . ?
C3 C2 B C19 56.49(15) . . . . ?
C3 C2 C1 P -178.64(8) . . . . ?
C3 C2 C1 C6 0.91(17) . . . . ?
C3 C4 C5 C6 0.5(2) . . . . ?
C7 P N B 107.37(9) . . . . ?
C7 P C1 C2 -115.19(9) . . . . ?
C7 P C1 C6 65.27(12) . . . . ?
C7 P C10 C11 -167.53(10) . . . . ?
C7 P C10 C12 67.71(12) . . . . ?
C10 P N B -126.42(9) . . . . ?
C10 P C1 C2 125.72(8) . . . . ?
C10 P C1 C6 -53.81(12) . . . . ?
C10 P C7 C8 42.99(11) . . . . ?
C10 P C7 C9 -85.52(11) . . . . ?
C13 C14 C15 C16 55.68(15) . . . . ?
C13 C18 C17 C16 -55.94(14) . . . . ?
C14 C13 B N 176.14(9) . . . . ?
C14 C13 B C2 65.87(12) . . . . ?
C14 C13 B C19 -60.41(12) . . . . ?
C15 C16 C17 C18 52.95(15) . . . . ?
C17 C16 C15 C14 -52.44(16) . . . . ?
C17 C18 C13 B -175.02(10) . . . . ?
C17 C18 C13 C14 56.59(13) . . . . ?
C18 C13 B N 49.81(13) . . . . ?
C18 C13 B C2 -60.46(13) . . . . ?
C18 C13 B C19 173.26(10) . . . . ?
C18 C13 C14 C15 -56.94(13) . . . . ?
C19 C20 C21 C22 56.83(17) . . . . ?
C19 C24 C23 C22 -55.49(16) . . . . ?
C20 C19 B N 78.28(12) . . . . ?
C20 C19 B C2 -171.80(10) . . . . ?
C20 C19 B C13 -44.39(13) . . . . ?
C20 C19 C24 C23 54.27(14) . . . . ?
C20 C21 C22 C23 -55.41(19) . . . . ?
C21 C20 C19 B 176.24(10) . . . . ?
C21 C20 C19 C24 -54.80(14) . . . . ?
C21 C22 C23 C24 54.69(18) . . . . ?
C24 C19 B N -47.88(13) . . . . ?
C24 C19 B C2 62.05(12) . . . . ?
C24 C19 B C13 -170.55(10) . . . . ?

_olex2_date_sample_data_collection 2019-10-23
_olex2_date_sample_submission    2019-10-23
_olex2_submission_original_sample_id RIV19A6
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_PB(NBH2)-DMAP
_database_code_depnum_ccdc_archive 'CCDC 2106476'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_audit_creation_date             2021-09-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
bfrenett@ualberta.ca
erivard@ualberta.ca
_chemical_name_common            PB(NBH2)-DMAP
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H2 Cl2, C31 H52 B2 N3 P'
_chemical_formula_sum            'C32 H54 B2 Cl2 N3 P'
_chemical_formula_weight         604.27
_chemical_melting_point          ?
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'
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'

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

_cell_length_a                   9.5926(12)
_cell_length_b                   11.0351(14)
_cell_length_c                   16.641(2)
_cell_angle_alpha                98.954(2)
_cell_angle_beta                 98.334(2)
_cell_angle_gamma                99.920(2)
_cell_volume                     1687.1(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4652
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      22.64
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   0.978
_shelx_estimated_absorpt_T_min   0.952
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9132
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,  J. Appl. Cryst. 48 (2015) 3-10'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             652
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -1.00 0.0710
0.00 -1.00 0.00 0.0430
0.00 1.00 0.00 0.0310
0.00 0.00 -1.00 0.0810
0.00 0.00 1.00 0.0720
0.00 1.00 -1.00 0.0590
0.00 -1.00 1.00 0.0480
-1.00 -1.00 0.00 0.0520
1.00 -1.00 1.00 0.0880
-1.00 1.00 -1.00 0.0920
1.00 -1.00 0.00 0.0780
-1.00 1.00 0.00 0.0770
-1.00 -1.00 1.00 0.0670
1.00 1.00 -1.00 0.0670
1.00 -1.00 -1.00 0.0680
-1.00 2.00 2.00 0.0680
-1.00 0.00 2.00 0.0940
-1.00 -2.00 2.00 0.0590
-1.00 -2.00 -2.00 0.0670
1.00 2.00 1.00 0.0570
1.00 0.00 2.00 0.0830
-1.00 -2.00 0.00 0.0510

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.086
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30383
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.179
_diffrn_reflns_theta_min         1.259
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5428
_reflns_number_total             7484
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7484
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0430
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0477P)²+0.3880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1116
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C19(H19)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C32A(H32A,H32B), C32B(H32C,H32D)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C25(H25), C26(H26), C28(H28), C29(H29)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1A Cl 0.1433(5) 0.1303(4) 0.4020(2) 0.0590(8) Uani 0.609(18) 1 d . . P A 1
Cl1B Cl 0.1375(8) 0.1621(14) 0.4064(5) 0.0883(18) Uani 0.391(18) 1 d . . P A 2
Cl2A Cl 0.4182(5) 0.2819(8) 0.3908(4) 0.0837(14) Uani 0.609(18) 1 d . . P A 1
Cl2B Cl 0.4147(9) 0.2534(10) 0.3778(6) 0.0854(19) Uani 0.391(18) 1 d . . P A 2
P1 P 0.48041(5) 0.39556(4) 0.79019(3) 0.02173(11) Uani 1 1 d . . . . .
N1 N 0.64543(14) 0.37888(12) 0.80133(8) 0.0211(3) Uani 1 1 d . . . . .
N2 N 0.87373(14) 0.56000(12) 0.86036(8) 0.0231(3) Uani 1 1 d . . . . .
N3 N 1.21034(16) 0.83834(14) 0.83415(9) 0.0325(4) Uani 1 1 d . . . . .
C1 C 0.39719(17) 0.25821(15) 0.71485(10) 0.0220(3) Uani 1 1 d . . . . .
C2 C 0.50453(17) 0.19438(15) 0.69300(9) 0.0219(3) Uani 1 1 d . . . . .
C3 C 0.45749(19) 0.08113(16) 0.63670(10) 0.0275(4) Uani 1 1 d . . . . .
H3 H 0.526220 0.034154 0.620426 0.033 Uiso 1 1 calc R U . . .
C4 C 0.3129(2) 0.03587(16) 0.60412(10) 0.0309(4) Uani 1 1 d . . . . .
H4 H 0.284253 -0.041565 0.566348 0.037 Uiso 1 1 calc R U . . .
C5 C 0.20968(19) 0.10240(17) 0.62607(11) 0.0317(4) Uani 1 1 d . . . . .
H5 H 0.111058 0.071303 0.602917 0.038 Uiso 1 1 calc R U . . .
C6 C 0.25118(18) 0.21394(17) 0.68173(10) 0.0281(4) Uani 1 1 d . . . . .
H6 H 0.181522 0.260246 0.697418 0.034 Uiso 1 1 calc R U . . .
C7 C 0.40306(18) 0.39870(16) 0.88490(10) 0.0275(4) Uani 1 1 d . . . . .
H7 H 0.454449 0.477274 0.923845 0.033 Uiso 1 1 calc R U . . .
C8 C 0.4321(2) 0.29028(19) 0.92624(12) 0.0417(5) Uani 1 1 d . . . . .
H8A H 0.387950 0.211113 0.888586 0.063 Uiso 1 1 calc R U . . .
H8B H 0.390992 0.294092 0.976957 0.063 Uiso 1 1 calc R U . . .
H8C H 0.536077 0.295543 0.939922 0.063 Uiso 1 1 calc R U . . .
C9 C 0.2430(2) 0.4030(2) 0.87204(12) 0.0433(5) Uani 1 1 d . . . . .
H9A H 0.227437 0.474800 0.846365 0.065 Uiso 1 1 calc R U . . .
H9B H 0.210888 0.411369 0.925552 0.065 Uiso 1 1 calc R U . . .
H9C H 0.188243 0.325606 0.835974 0.065 Uiso 1 1 calc R U . . .
C10 C 0.4512(2) 0.53752(16) 0.75021(11) 0.0298(4) Uani 1 1 d . . . . .
H10 H 0.524830 0.552038 0.714107 0.036 Uiso 1 1 calc R U . . .
C11 C 0.3069(2) 0.52788(19) 0.69417(13) 0.0423(5) Uani 1 1 d . . . . .
H11A H 0.292501 0.457058 0.648238 0.063 Uiso 1 1 calc R U . . .
H11B H 0.306643 0.605367 0.672323 0.063 Uiso 1 1 calc R U . . .
H11C H 0.229057 0.515051 0.726045 0.063 Uiso 1 1 calc R U . . .
C12 C 0.4858(2) 0.65481(17) 0.81800(13) 0.0450(5) Uani 1 1 d . . . . .
H12A H 0.413710 0.649321 0.854085 0.067 Uiso 1 1 calc R U . . .
H12B H 0.484739 0.729135 0.792638 0.067 Uiso 1 1 calc R U . . .
H12C H 0.581271 0.661003 0.850642 0.067 Uiso 1 1 calc R U . . .
C13 C 0.74454(18) 0.15603(16) 0.77864(10) 0.0253(4) Uani 1 1 d . . . . .
H13 H 0.734917 0.084550 0.731839 0.030 Uiso 1 1 calc R U . . .
C14 C 0.90627(19) 0.19047(18) 0.81327(12) 0.0340(4) Uani 1 1 d . . . . .
H14A H 0.957484 0.227165 0.772470 0.041 Uiso 1 1 calc R U . . .
H14B H 0.923770 0.254598 0.864272 0.041 Uiso 1 1 calc R U . . .
C15 C 0.9665(2) 0.0769(2) 0.83279(13) 0.0428(5) Uani 1 1 d . . . . .
H15A H 0.956751 0.015771 0.781010 0.051 Uiso 1 1 calc R U . . .
H15B H 1.070115 0.103627 0.856597 0.051 Uiso 1 1 calc R U . . .
C16 C 0.8884(2) 0.0144(2) 0.89340(12) 0.0426(5) Uani 1 1 d . . . . .
H16A H 0.909729 0.071159 0.947820 0.051 Uiso 1 1 calc R U . . .
H16B H 0.923524 -0.063180 0.900648 0.051 Uiso 1 1 calc R U . . .
C17 C 0.7265(2) -0.01747(18) 0.86272(12) 0.0384(5) Uani 1 1 d . . . . .
H17A H 0.677790 -0.050239 0.905694 0.046 Uiso 1 1 calc R U . . .
H17B H 0.704170 -0.083811 0.812661 0.046 Uiso 1 1 calc R U . . .
C18 C 0.66922(19) 0.09755(16) 0.84236(11) 0.0284(4) Uani 1 1 d . . . . .
H18A H 0.564703 0.072808 0.820691 0.034 Uiso 1 1 calc R U . . .
H18B H 0.683427 0.160660 0.893631 0.034 Uiso 1 1 calc R U . . .
C19 C 0.76161(18) 0.31005(16) 0.66624(10) 0.0251(4) Uani 1 1 d . . . . .
H19 H 0.849947 0.370000 0.697688 0.030 Uiso 1 1 calc R U . . .
C20 C 0.68251(19) 0.38227(17) 0.60861(10) 0.0286(4) Uani 1 1 d . . . . .
H20A H 0.596016 0.324686 0.574837 0.034 Uiso 1 1 calc R U . . .
H20B H 0.649876 0.450084 0.642709 0.034 Uiso 1 1 calc R U . . .
C21 C 0.7742(2) 0.43938(18) 0.55090(12) 0.0367(4) Uani 1 1 d . . . . .
H21A H 0.715672 0.481497 0.514335 0.044 Uiso 1 1 calc R U . . .
H21B H 0.856072 0.503186 0.584050 0.044 Uiso 1 1 calc R U . . .
C22 C 0.8309(2) 0.3396(2) 0.49846(12) 0.0388(5) Uani 1 1 d . . . . .
H22A H 0.749875 0.283389 0.458896 0.047 Uiso 1 1 calc R U . . .
H22B H 0.898481 0.379974 0.466353 0.047 Uiso 1 1 calc R U . . .
C23 C 0.9074(2) 0.2631(2) 0.55238(12) 0.0394(5) Uani 1 1 d . . . . .
H23A H 0.996608 0.317003 0.585896 0.047 Uiso 1 1 calc R U . . .
H23B H 0.934797 0.193888 0.516615 0.047 Uiso 1 1 calc R U . . .
C24 C 0.8132(2) 0.20898(18) 0.60976(11) 0.0326(4) Uani 1 1 d . . . . .
H24A H 0.868141 0.161992 0.644482 0.039 Uiso 1 1 calc R U . . .
H24B H 0.728316 0.149208 0.576007 0.039 Uiso 1 1 calc R U . . .
C25 C 0.98155(18) 0.61579(15) 0.92360(10) 0.0256(4) Uani 1 1 d . . . . .
H25 H 0.979892 0.589585 0.975253 0.031 Uiso 1 1 calc R U . . .
C26 C 1.09253(18) 0.70733(16) 0.91789(11) 0.0272(4) Uani 1 1 d . . . . .
H26 H 1.165181 0.743072 0.964809 0.033 Uiso 1 1 calc R U . . .
C27 C 1.09996(18) 0.74929(15) 0.84245(11) 0.0253(4) Uani 1 1 d . . . . .
C28 C 0.98596(19) 0.69154(16) 0.77719(11) 0.0294(4) Uani 1 1 d . . . . .
H28 H 0.984010 0.715632 0.724726 0.035 Uiso 1 1 calc R U . . .
C29 C 0.87777(19) 0.60079(16) 0.78883(10) 0.0277(4) Uani 1 1 d . . . . .
H29 H 0.801557 0.564884 0.743768 0.033 Uiso 1 1 calc R U . . .
C30 C 1.3144(2) 0.90713(18) 0.90603(13) 0.0404(5) Uani 1 1 d . . . . .
H30A H 1.264545 0.949426 0.945943 0.061 Uiso 1 1 calc R U . . .
H30B H 1.384218 0.969483 0.888916 0.061 Uiso 1 1 calc R U . . .
H30C H 1.364634 0.848855 0.931678 0.061 Uiso 1 1 calc R U . . .
C31 C 1.2198(2) 0.87815(19) 0.75556(12) 0.0386(5) Uani 1 1 d . . . . .
H31A H 1.203105 0.804391 0.711527 0.058 Uiso 1 1 calc R U . . .
H31B H 1.315643 0.928495 0.758234 0.058 Uiso 1 1 calc R U . . .
H31C H 1.147015 0.928417 0.743896 0.058 Uiso 1 1 calc R U . . .
C32A C 0.3024(14) 0.2269(10) 0.4530(6) 0.060(3) Uani 0.609(18) 1 d . . P A 1
H32A H 0.352914 0.180719 0.490502 0.072 Uiso 0.609(18) 1 calc R U P A 1
H32B H 0.279462 0.299618 0.487765 0.072 Uiso 0.609(18) 1 calc R U P A 1
C32B C 0.312(2) 0.192(2) 0.4427(13) 0.091(6) Uani 0.391(18) 1 d . . P A 2
H32C H 0.341089 0.113075 0.453523 0.109 Uiso 0.391(18) 1 calc R U P A 2
H32D H 0.331823 0.250997 0.496124 0.109 Uiso 0.391(18) 1 calc R U P A 2
B1 B 0.6699(2) 0.25975(17) 0.73609(11) 0.0224(4) Uani 1 1 d . . . . .
B2 B 0.7474(2) 0.45389(19) 0.87895(12) 0.0257(4) Uani 1 1 d . . . . .
H2A H 0.8063(18) 0.3949(15) 0.9156(10) 0.024(4) Uiso 1 1 d . . . . .
H2B H 0.6903(18) 0.5107(15) 0.9211(10) 0.023(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1A C32A 1.722(11) . ?
Cl1B C32B 1.65(2) . ?
Cl2A C32A 1.724(14) . ?
Cl2B C32B 1.70(2) . ?
P1 N1 1.6125(14) . ?
P1 C1 1.7910(16) . ?
P1 C7 1.8348(17) . ?
P1 C10 1.8431(18) . ?
N1 B1 1.643(2) . ?
N1 B2 1.527(2) . ?
N2 C25 1.349(2) . ?
N2 C29 1.340(2) . ?
N2 B2 1.633(2) . ?
N3 C27 1.354(2) . ?
N3 C30 1.454(2) . ?
N3 C31 1.453(2) . ?
C1 C2 1.403(2) . ?
C1 C6 1.400(2) . ?
C2 C3 1.401(2) . ?
C2 B1 1.633(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(2) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.516(3) . ?
C7 C9 1.529(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.530(3) . ?
C10 C12 1.532(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.534(2) . ?
C13 C18 1.529(2) . ?
C13 B1 1.647(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.527(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.520(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.524(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.532(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 1.0000 . ?
C19 C20 1.538(2) . ?
C19 C24 1.540(2) . ?
C19 B1 1.662(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.528(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.522(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.521(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.526(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25 0.9500 . ?
C25 C26 1.361(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.411(2) . ?
C27 C28 1.408(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.370(2) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32A H32A 0.9900 . ?
C32A H32B 0.9900 . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
B2 H2A 1.125(17) . ?
B2 H2B 1.130(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C1 100.21(7) . . ?
N1 P1 C7 114.34(8) . . ?
N1 P1 C10 113.73(8) . . ?
C1 P1 C7 111.40(8) . . ?
C1 P1 C10 110.45(8) . . ?
C7 P1 C10 106.71(8) . . ?
P1 N1 B1 112.84(10) . . ?
B2 N1 P1 117.34(12) . . ?
B2 N1 B1 128.42(14) . . ?
C25 N2 B2 117.31(13) . . ?
C29 N2 C25 116.51(14) . . ?
C29 N2 B2 126.11(14) . . ?
C27 N3 C30 120.54(15) . . ?
C27 N3 C31 121.41(16) . . ?
C31 N3 C30 117.69(15) . . ?
C2 C1 P1 108.46(12) . . ?
C6 C1 P1 128.85(13) . . ?
C6 C1 C2 122.68(15) . . ?
C1 C2 B1 116.60(14) . . ?
C3 C2 C1 116.15(15) . . ?
C3 C2 B1 127.25(15) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.59(17) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.76(16) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.56(16) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 H6 120.4 . . ?
C5 C6 C1 119.25(17) . . ?
C5 C6 H6 120.4 . . ?
P1 C7 H7 106.9 . . ?
C8 C7 P1 110.67(12) . . ?
C8 C7 H7 106.9 . . ?
C8 C7 C9 111.07(16) . . ?
C9 C7 P1 113.89(13) . . ?
C9 C7 H7 106.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C10 H10 105.0 . . ?
C11 C10 P1 116.43(13) . . ?
C11 C10 H10 105.0 . . ?
C11 C10 C12 111.46(16) . . ?
C12 C10 P1 112.79(13) . . ?
C12 C10 H10 105.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13 104.2 . . ?
C14 C13 B1 117.96(14) . . ?
C18 C13 H13 104.2 . . ?
C18 C13 C14 107.83(14) . . ?
C18 C13 B1 116.76(14) . . ?
B1 C13 H13 104.2 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C15 C14 C13 111.97(16) . . ?
C15 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C14 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
C16 C15 C14 111.44(16) . . ?
C16 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C15 C16 C17 111.07(16) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C16 C17 H17A 109.3 . . ?
C16 C17 H17B 109.3 . . ?
C16 C17 C18 111.41(16) . . ?
H17A C17 H17B 108.0 . . ?
C18 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C13 C18 C17 112.03(15) . . ?
C13 C18 H18A 109.2 . . ?
C13 C18 H18B 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 H19 106.6 . . ?
C20 C19 C24 106.20(14) . . ?
C20 C19 B1 114.57(14) . . ?
C24 C19 H19 106.6 . . ?
C24 C19 B1 115.77(14) . . ?
B1 C19 H19 106.6 . . ?
C19 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 C19 113.78(15) . . ?
C21 C20 H20A 108.8 . . ?
C21 C20 H20B 108.8 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 C20 111.11(16) . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 C21 110.89(16) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C22 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C22 C23 C24 111.92(16) . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C19 C24 H24A 109.0 . . ?
C19 C24 H24B 109.0 . . ?
C23 C24 C19 112.90(16) . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
N2 C25 H25 118.0 . . ?
N2 C25 C26 123.98(16) . . ?
C26 C25 H25 118.0 . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.15(16) . . ?
C27 C26 H26 119.9 . . ?
N3 C27 C26 121.70(16) . . ?
N3 C27 C28 122.92(16) . . ?
C28 C27 C26 115.38(15) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.45(16) . . ?
C29 C28 H28 119.8 . . ?
N2 C29 C28 123.51(16) . . ?
N2 C29 H29 118.2 . . ?
C28 C29 H29 118.2 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Cl1A C32A Cl2A 115.6(5) . . ?
Cl1A C32A H32A 108.4 . . ?
Cl1A C32A H32B 108.4 . . ?
Cl2A C32A H32A 108.4 . . ?
Cl2A C32A H32B 108.4 . . ?
H32A C32A H32B 107.4 . . ?
Cl1B C32B Cl2B 113.7(12) . . ?
Cl1B C32B H32C 108.8 . . ?
Cl1B C32B H32D 108.8 . . ?
Cl2B C32B H32C 108.8 . . ?
Cl2B C32B H32D 108.8 . . ?
H32C C32B H32D 107.7 . . ?
N1 B1 C13 115.22(13) . . ?
N1 B1 C19 110.35(13) . . ?
C2 B1 N1 101.40(13) . . ?
C2 B1 C13 108.49(13) . . ?
C2 B1 C19 110.40(13) . . ?
C13 B1 C19 110.57(14) . . ?
N1 B2 N2 113.79(14) . . ?
N1 B2 H2A 113.7(9) . . ?
N1 B2 H2B 112.1(9) . . ?
N2 B2 H2A 104.8(9) . . ?
N2 B2 H2B 102.9(9) . . ?
H2A B2 H2B 108.8(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 N1 B1 C2 -7.23(15) . . . . ?
P1 N1 B1 C13 -124.14(13) . . . . ?
P1 N1 B1 C19 109.77(13) . . . . ?
P1 N1 B2 N2 -114.05(14) . . . . ?
P1 C1 C2 C3 177.49(12) . . . . ?
P1 C1 C2 B1 -2.28(17) . . . . ?
P1 C1 C6 C5 -177.58(13) . . . . ?
N1 P1 C1 C2 -2.31(13) . . . . ?
N1 P1 C1 C6 176.28(15) . . . . ?
N1 P1 C7 C8 -48.96(15) . . . . ?
N1 P1 C7 C9 -174.93(13) . . . . ?
N1 P1 C10 C11 146.66(14) . . . . ?
N1 P1 C10 C12 -82.64(15) . . . . ?
N2 C25 C26 C27 -0.1(3) . . . . ?
N3 C27 C28 C29 179.23(17) . . . . ?
C1 P1 N1 B1 6.01(12) . . . . ?
C1 P1 N1 B2 -161.64(12) . . . . ?
C1 P1 C7 C8 63.77(15) . . . . ?
C1 P1 C7 C9 -62.20(16) . . . . ?
C1 P1 C10 C11 34.91(16) . . . . ?
C1 P1 C10 C12 165.61(13) . . . . ?
C1 C2 C3 C4 0.6(2) . . . . ?
C1 C2 B1 N1 5.79(18) . . . . ?
C1 C2 B1 C13 127.51(15) . . . . ?
C1 C2 B1 C19 -111.18(16) . . . . ?
C2 C1 C6 C5 0.8(3) . . . . ?
C2 C3 C4 C5 0.4(3) . . . . ?
C3 C2 B1 N1 -173.95(15) . . . . ?
C3 C2 B1 C13 -52.2(2) . . . . ?
C3 C2 B1 C19 69.1(2) . . . . ?
C3 C4 C5 C6 -0.8(3) . . . . ?
C4 C5 C6 C1 0.2(3) . . . . ?
C6 C1 C2 C3 -1.2(2) . . . . ?
C6 C1 C2 B1 179.02(15) . . . . ?
C7 P1 N1 B1 125.24(11) . . . . ?
C7 P1 N1 B2 -42.40(14) . . . . ?
C7 P1 C1 C2 -123.67(12) . . . . ?
C7 P1 C1 C6 54.92(18) . . . . ?
C7 P1 C10 C11 -86.32(15) . . . . ?
C7 P1 C10 C12 44.38(16) . . . . ?
C10 P1 N1 B1 -111.84(12) . . . . ?
C10 P1 N1 B2 80.52(14) . . . . ?
C10 P1 C1 C2 117.93(12) . . . . ?
C10 P1 C1 C6 -63.49(17) . . . . ?
C10 P1 C7 C8 -175.61(13) . . . . ?
C10 P1 C7 C9 58.42(16) . . . . ?
C13 C14 C15 C16 -57.2(2) . . . . ?
C14 C13 C18 C17 -57.63(19) . . . . ?
C14 C13 B1 N1 -74.98(19) . . . . ?
C14 C13 B1 C2 172.20(14) . . . . ?
C14 C13 B1 C19 51.00(19) . . . . ?
C14 C15 C16 C17 53.8(2) . . . . ?
C15 C16 C17 C18 -53.5(2) . . . . ?
C16 C17 C18 C13 56.8(2) . . . . ?
C18 C13 C14 C15 57.87(19) . . . . ?
C18 C13 B1 N1 56.02(19) . . . . ?
C18 C13 B1 C2 -56.80(18) . . . . ?
C18 C13 B1 C19 -178.01(14) . . . . ?
C19 C20 C21 C22 57.0(2) . . . . ?
C20 C19 C24 C23 56.59(19) . . . . ?
C20 C19 B1 N1 -65.23(17) . . . . ?
C20 C19 B1 C2 46.04(19) . . . . ?
C20 C19 B1 C13 166.11(13) . . . . ?
C20 C21 C22 C23 -52.8(2) . . . . ?
C21 C22 C23 C24 53.5(2) . . . . ?
C22 C23 C24 C19 -57.3(2) . . . . ?
C24 C19 C20 C21 -56.91(19) . . . . ?
C24 C19 B1 N1 170.61(14) . . . . ?
C24 C19 B1 C2 -78.12(18) . . . . ?
C24 C19 B1 C13 41.95(19) . . . . ?
C25 N2 C29 C28 1.9(3) . . . . ?
C25 N2 B2 N1 -169.31(15) . . . . ?
C25 C26 C27 N3 -178.63(16) . . . . ?
C25 C26 C27 C28 0.9(3) . . . . ?
C26 C27 C28 C29 -0.3(3) . . . . ?
C27 C28 C29 N2 -1.2(3) . . . . ?
C29 N2 C25 C26 -1.3(3) . . . . ?
C29 N2 B2 N1 13.5(2) . . . . ?
C30 N3 C27 C26 -9.1(3) . . . . ?
C30 N3 C27 C28 171.41(17) . . . . ?
C31 N3 C27 C26 177.93(17) . . . . ?
C31 N3 C27 C28 -1.6(3) . . . . ?
B1 N1 B2 N2 80.5(2) . . . . ?
B1 C2 C3 C4 -179.69(16) . . . . ?
B1 C13 C14 C15 -167.19(15) . . . . ?
B1 C13 C18 C17 166.82(14) . . . . ?
B1 C19 C20 C21 173.98(14) . . . . ?
B1 C19 C24 C23 -175.01(15) . . . . ?
B2 N1 B1 C2 158.73(14) . . . . ?
B2 N1 B1 C13 41.8(2) . . . . ?
B2 N1 B1 C19 -84.27(19) . . . . ?
B2 N2 C25 C26 -178.69(16) . . . . ?
B2 N2 C29 C28 179.08(17) . . . . ?

_olex2_date_sample_data_collection 2021-07-20
_olex2_date_sample_submission    2021-07-20
_olex2_exptl_crystal_mounting_method 
'A suitable crystal was coated in Paratone oil and mounted on a loop.'
_olex2_submission_original_sample_id riv21a1
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes/DCM at -40C'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PB(H2BNH2)
_database_code_depnum_ccdc_archive 'CCDC 2106482'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            PB(H2BNH2)
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H44 B2 N P'
_chemical_formula_sum            'C24 H44 B2 N P'
_chemical_formula_weight         399.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   19.7455(6)
_cell_length_b                   10.9680(3)
_cell_length_c                   23.1511(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.217(2)
_cell_angle_gamma                90
_cell_volume                     4900.3(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8759
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      73.82

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_F_000             1760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.096
_exptl_absorpt_coefficient_mu    1.032
_shelx_estimated_absorpt_T_min   0.755
_shelx_estimated_absorpt_T_max   0.907
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8018
_exptl_absorpt_correction_T_max  0.9920
_exptl_absorpt_process_details   'SADABS (version 2016/2)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            112848
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.289
_diffrn_reflns_theta_max         74.212
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9929
_reflns_number_gt                7806
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (version 2014/5)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+1.5907P] 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         9929
_refine_ls_number_parameters     545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1175
_refine_ls_wR_factor_gt          0.1068
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
P1A P 0.12777(2) 0.39101(3) 0.76168(2) 0.02643(10) Uani 1 1 d . . . . .
N1A N 0.18823(7) 0.53916(12) 0.68413(6) 0.0281(3) Uani 1 1 d . . . . .
H1NA H 0.2256(11) 0.5510(18) 0.6650(9) 0.043(5) Uiso 1 1 d . . . . .
H2NA H 0.1838(11) 0.612(2) 0.7016(9) 0.045(6) Uiso 1 1 d . . . . .
C1A C 0.04895(8) 0.42831(14) 0.70963(7) 0.0269(3) Uani 1 1 d . . . . .
C2A C 0.05163(8) 0.49307(13) 0.65730(6) 0.0255(3) Uani 1 1 d . . . . .
C3A C -0.01361(8) 0.51935(15) 0.62142(7) 0.0313(3) Uani 1 1 d . . . . .
H3A H -0.015060 0.566148 0.586651 0.038 Uiso 1 1 calc R U . . .
C4A C -0.07581(9) 0.48104(16) 0.63381(7) 0.0345(4) Uani 1 1 d . . . . .
H4A H -0.118166 0.500262 0.607342 0.041 Uiso 1 1 calc R U . . .
C5A C -0.07658(9) 0.41464(15) 0.68473(8) 0.0345(4) Uani 1 1 d . . . . .
H5A H -0.119039 0.387483 0.693359 0.041 Uiso 1 1 calc R U . . .
C6A C -0.01414(9) 0.38899(15) 0.72256(7) 0.0320(3) Uani 1 1 d . . . . .
H6A H -0.013740 0.344240 0.757760 0.038 Uiso 1 1 calc R U . . .
C11A C 0.11285(8) 0.64897(14) 0.59193(7) 0.0288(3) Uani 1 1 d . . . . .
H11A H 0.070200 0.639265 0.560138 0.035 Uiso 1 1 calc R U . . .
C12A C 0.10003(10) 0.76148(15) 0.62817(8) 0.0373(4) Uani 1 1 d . . . . .
H12A H 0.058445 0.746507 0.644686 0.045 Uiso 1 1 calc R U . . .
H12B H 0.139985 0.771673 0.661764 0.045 Uiso 1 1 calc R U . . .
C13A C 0.08959(10) 0.88039(15) 0.59229(9) 0.0422(4) Uani 1 1 d . . . . .
H13A H 0.045930 0.875254 0.562088 0.051 Uiso 1 1 calc R U . . .
H13B H 0.085406 0.949311 0.618926 0.051 Uiso 1 1 calc R U . . .
C14A C 0.14922(12) 0.90426(17) 0.56217(11) 0.0555(6) Uani 1 1 d . . . . .
H14A H 0.192051 0.918880 0.592392 0.067 Uiso 1 1 calc R U . . .
H14B H 0.139418 0.978274 0.537332 0.067 Uiso 1 1 calc R U . . .
C15A C 0.15996(13) 0.79664(18) 0.52400(11) 0.0571(6) Uani 1 1 d . . . . .
H15A H 0.200487 0.812462 0.506184 0.069 Uiso 1 1 calc R U . . .
H15B H 0.118750 0.787084 0.491500 0.069 Uiso 1 1 calc R U . . .
C16A C 0.17187(11) 0.67831(16) 0.56019(9) 0.0444(4) Uani 1 1 d . . . . .
H16A H 0.215799 0.685313 0.589952 0.053 Uiso 1 1 calc R U . . .
H16B H 0.176846 0.609858 0.533522 0.053 Uiso 1 1 calc R U . . .
C21A C 0.13469(8) 0.39534(13) 0.59468(6) 0.0251(3) Uani 1 1 d . . . . .
H21A H 0.126337 0.325806 0.620234 0.030 Uiso 1 1 calc R U . . .
C22A C 0.08264(9) 0.37899(15) 0.53568(7) 0.0320(3) Uani 1 1 d . . . . .
H22A H 0.035009 0.386003 0.542619 0.038 Uiso 1 1 calc R U . . .
H22B H 0.089335 0.445315 0.508428 0.038 Uiso 1 1 calc R U . . .
C23A C 0.09027(9) 0.25627(16) 0.50648(8) 0.0363(4) Uani 1 1 d . . . . .
H23A H 0.078762 0.189800 0.531695 0.044 Uiso 1 1 calc R U . . .
H23B H 0.057182 0.252164 0.467885 0.044 Uiso 1 1 calc R U . . .
C24A C 0.16365(9) 0.23800(15) 0.49709(7) 0.0360(4) Uani 1 1 d . . . . .
H24A H 0.167944 0.155389 0.481003 0.043 Uiso 1 1 calc R U . . .
H24B H 0.173214 0.298183 0.467957 0.043 Uiso 1 1 calc R U . . .
C25A C 0.21623(9) 0.25306(15) 0.55482(8) 0.0347(4) Uani 1 1 d . . . . .
H25A H 0.263583 0.246433 0.547222 0.042 Uiso 1 1 calc R U . . .
H25B H 0.210084 0.186741 0.582262 0.042 Uiso 1 1 calc R U . . .
C26A C 0.20819(8) 0.37624(15) 0.58361(7) 0.0305(3) Uani 1 1 d . . . . .
H26A H 0.218731 0.442255 0.557700 0.037 Uiso 1 1 calc R U . . .
H26B H 0.242131 0.381611 0.621695 0.037 Uiso 1 1 calc R U . . .
C31A C 0.12787(9) 0.22720(14) 0.77726(7) 0.0333(3) Uani 1 1 d . . . . .
H31A H 0.088200 0.208817 0.796481 0.040 Uiso 1 1 calc R U . . .
C32A C 0.11825(11) 0.15408(15) 0.71970(8) 0.0423(4) Uani 1 1 d . . . . .
H32A H 0.074149 0.176616 0.693670 0.063 Uiso 1 1 calc R U . . .
H32B H 0.118043 0.066762 0.728628 0.063 Uiso 1 1 calc R U . . .
H32C H 0.156401 0.172112 0.699985 0.063 Uiso 1 1 calc R U . . .
C33A C 0.19542(10) 0.19309(17) 0.82033(8) 0.0423(4) Uani 1 1 d . . . . .
H33A H 0.196844 0.232727 0.858509 0.063 Uiso 1 1 calc R U . . .
H33B H 0.235013 0.220297 0.804313 0.063 Uiso 1 1 calc R U . . .
H33C H 0.197591 0.104444 0.825714 0.063 Uiso 1 1 calc R U . . .
C34A C 0.12849(9) 0.47128(16) 0.83151(7) 0.0338(4) Uani 1 1 d . . . . .
H34A H 0.174202 0.453525 0.858274 0.041 Uiso 1 1 calc R U . . .
C35A C 0.12588(11) 0.60889(17) 0.82046(8) 0.0446(4) Uani 1 1 d . . . . .
H35A H 0.162853 0.632050 0.800277 0.067 Uiso 1 1 calc R U . . .
H35B H 0.132265 0.652006 0.858308 0.067 Uiso 1 1 calc R U . . .
H35C H 0.080849 0.630751 0.795736 0.067 Uiso 1 1 calc R U . . .
C36A C 0.07274(11) 0.4336(2) 0.86450(8) 0.0499(5) Uani 1 1 d . . . . .
H36A H 0.073763 0.344953 0.869781 0.075 Uiso 1 1 calc R U . . .
H36B H 0.027172 0.458281 0.841691 0.075 Uiso 1 1 calc R U . . .
H36C H 0.081422 0.473468 0.903266 0.075 Uiso 1 1 calc R U . . .
B1A B 0.20936(9) 0.43749(17) 0.73254(8) 0.0293(4) Uani 1 1 d . . . . .
H1BA H 0.2510(10) 0.4710(19) 0.7734(9) 0.046(6) Uiso 1 1 d . . . . .
H2BA H 0.2311(10) 0.3537(18) 0.7154(8) 0.040(5) Uiso 1 1 d . . . . .
B2A B 0.12097(9) 0.52071(15) 0.63032(7) 0.0251(3) Uani 1 1 d . . . . .
P1B P 0.37394(2) 0.64349(3) 0.24971(2) 0.02672(10) Uani 1 1 d . . . . .
N1B N 0.31486(7) 0.79505(12) 0.32697(6) 0.0281(3) Uani 1 1 d . . . . .
H1NB H 0.2792(11) 0.8060(19) 0.3446(9) 0.046(6) Uiso 1 1 d . . . . .
H2NB H 0.3203(11) 0.864(2) 0.3091(10) 0.049(6) Uiso 1 1 d . . . . .
C1B C 0.45331(8) 0.68405(13) 0.30026(7) 0.0264(3) Uani 1 1 d . . . . .
C2B C 0.45149(8) 0.75103(13) 0.35235(6) 0.0249(3) Uani 1 1 d . . . . .
C3B C 0.51729(8) 0.78211(15) 0.38602(7) 0.0303(3) Uani 1 1 d . . . . .
H3B H 0.519437 0.829239 0.420794 0.036 Uiso 1 1 calc R U . . .
C4B C 0.57905(9) 0.74791(16) 0.37136(8) 0.0348(4) Uani 1 1 d . . . . .
H4B H 0.621854 0.771711 0.395925 0.042 Uiso 1 1 calc R U . . .
C5B C 0.57879(9) 0.67913(16) 0.32106(8) 0.0358(4) Uani 1 1 d . . . . .
H5B H 0.621005 0.654176 0.311186 0.043 Uiso 1 1 calc R U . . .
C6B C 0.51589(9) 0.64779(15) 0.28570(7) 0.0332(3) Uani 1 1 d . . . . .
H6B H 0.514835 0.601006 0.250981 0.040 Uiso 1 1 calc R U . . .
C11B C 0.37010(8) 0.65852(13) 0.41890(6) 0.0259(3) Uani 1 1 d . . . . .
H11B H 0.381630 0.586747 0.396132 0.031 Uiso 1 1 calc R U . . .
C12B C 0.29622(8) 0.63446(15) 0.42863(7) 0.0311(3) Uani 1 1 d . . . . .
H12C H 0.282886 0.700949 0.452928 0.037 Uiso 1 1 calc R U . . .
H12D H 0.263159 0.634719 0.389968 0.037 Uiso 1 1 calc R U . . .
C13B C 0.29140(9) 0.51250(16) 0.45940(8) 0.0358(4) Uani 1 1 d . . . . .
H13C H 0.243606 0.500585 0.465247 0.043 Uiso 1 1 calc R U . . .
H13D H 0.302074 0.445334 0.434176 0.043 Uiso 1 1 calc R U . . .
C14B C 0.34201(9) 0.50895(18) 0.51899(8) 0.0394(4) Uani 1 1 d . . . . .
H14C H 0.339804 0.427977 0.537395 0.047 Uiso 1 1 calc R U . . .
H14D H 0.328559 0.571127 0.545460 0.047 Uiso 1 1 calc R U . . .
C15B C 0.41585(9) 0.53327(17) 0.51207(8) 0.0388(4) Uani 1 1 d . . . . .
H15C H 0.431471 0.465124 0.490052 0.047 Uiso 1 1 calc R U . . .
H15D H 0.446995 0.537180 0.551620 0.047 Uiso 1 1 calc R U . . .
C16B C 0.42074(8) 0.65282(15) 0.47915(7) 0.0301(3) Uani 1 1 d . . . . .
H16C H 0.468620 0.662590 0.473151 0.036 Uiso 1 1 calc R U . . .
H16D H 0.411061 0.721652 0.503863 0.036 Uiso 1 1 calc R U . . .
C21B C 0.39161(8) 0.90937(14) 0.41706(7) 0.0293(3) Uani 1 1 d . . . . .
H21B H 0.433439 0.898882 0.449609 0.035 Uiso 1 1 calc R U . . .
C22B C 0.40673(10) 1.02106(15) 0.38160(8) 0.0393(4) Uani 1 1 d . . . . .
H22C H 0.447005 1.003036 0.363802 0.047 Uiso 1 1 calc R U . . .
H22D H 0.366305 1.036517 0.349011 0.047 Uiso 1 1 calc R U . . .
C23B C 0.42201(11) 1.13619(16) 0.41979(9) 0.0474(5) Uani 1 1 d . . . . .
H23C H 0.465507 1.124462 0.449620 0.057 Uiso 1 1 calc R U . . .
H23D H 0.428699 1.206056 0.394502 0.057 Uiso 1 1 calc R U . . .
C24B C 0.36316(12) 1.16493(17) 0.45108(10) 0.0552(6) Uani 1 1 d . . . . .
H24C H 0.376539 1.234915 0.478087 0.066 Uiso 1 1 calc R U . . .
H24D H 0.321321 1.188352 0.421410 0.066 Uiso 1 1 calc R U . . .
C25B C 0.34656(11) 1.05618(17) 0.48605(10) 0.0495(5) Uani 1 1 d . . . . .
H25C H 0.305581 1.075192 0.502751 0.059 Uiso 1 1 calc R U . . .
H25D H 0.386116 1.040359 0.519364 0.059 Uiso 1 1 calc R U . . .
C26B C 0.33188(10) 0.94161(16) 0.44762(9) 0.0407(4) Uani 1 1 d . . . . .
H26C H 0.289068 0.954379 0.417120 0.049 Uiso 1 1 calc R U . . .
H26D H 0.323751 0.872138 0.472595 0.049 Uiso 1 1 calc R U . . .
C31B C 0.37462(9) 0.47926(14) 0.23575(7) 0.0324(3) Uani 1 1 d . . . . .
H31B H 0.413769 0.460766 0.215913 0.039 Uiso 1 1 calc R U . . .
C32B C 0.38593(11) 0.40760(15) 0.29388(8) 0.0426(4) Uani 1 1 d . . . . .
H32D H 0.430150 0.431757 0.319251 0.064 Uiso 1 1 calc R U . . .
H32E H 0.386772 0.320100 0.285486 0.064 Uiso 1 1 calc R U . . .
H32F H 0.348115 0.425145 0.314052 0.064 Uiso 1 1 calc R U . . .
C33B C 0.30661(10) 0.44244(17) 0.19397(9) 0.0452(4) Uani 1 1 d . . . . .
H33D H 0.304372 0.479468 0.155092 0.068 Uiso 1 1 calc R U . . .
H33E H 0.267351 0.470840 0.210130 0.068 Uiso 1 1 calc R U . . .
H33F H 0.304636 0.353481 0.190007 0.068 Uiso 1 1 calc R U . . .
C34B C 0.37117(10) 0.72111(17) 0.17897(7) 0.0395(4) Uani 1 1 d . . . . .
H34B H 0.323363 0.708860 0.154722 0.047 Uiso 1 1 calc R U . . .
C35B C 0.37990(12) 0.85841(17) 0.18988(8) 0.0486(5) Uani 1 1 d . . . . .
H35D H 0.346923 0.886285 0.213287 0.073 Uiso 1 1 calc R U . . .
H35E H 0.371121 0.901433 0.151927 0.073 Uiso 1 1 calc R U . . .
H35F H 0.427256 0.875423 0.211424 0.073 Uiso 1 1 calc R U . . .
C36B C 0.42095(14) 0.6750(2) 0.14195(9) 0.0636(6) Uani 1 1 d . . . . .
H36D H 0.416440 0.586352 0.137538 0.095 Uiso 1 1 calc R U . . .
H36E H 0.468565 0.695544 0.161587 0.095 Uiso 1 1 calc R U . . .
H36F H 0.409920 0.713480 0.102874 0.095 Uiso 1 1 calc R U . . .
B1B B 0.29303(10) 0.69173(17) 0.27947(8) 0.0298(4) Uani 1 1 d . . . . .
H1BB H 0.2727(10) 0.6072(17) 0.2993(8) 0.037(5) Uiso 1 1 d . . . . .
H2BB H 0.2520(10) 0.7235(18) 0.2401(8) 0.041(5) Uiso 1 1 d . . . . .
B2B B 0.38282(9) 0.77981(15) 0.38014(7) 0.0250(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1A C1A 1.8022(16) . ?
P1A C31A 1.8324(16) . ?
P1A C34A 1.8383(16) . ?
P1A B1A 1.9418(19) . ?
N1A B1A 1.573(2) . ?
N1A B2A 1.630(2) . ?
C1A C6A 1.409(2) . ?
C1A C2A 1.415(2) . ?
C2A C3A 1.407(2) . ?
C2A B2A 1.649(2) . ?
C3A C4A 1.384(2) . ?
C4A C5A 1.389(2) . ?
C5A C6A 1.382(2) . ?
C11A C16A 1.538(2) . ?
C11A C12A 1.543(2) . ?
C11A B2A 1.654(2) . ?
C12A C13A 1.537(2) . ?
C13A C14A 1.513(3) . ?
C14A C15A 1.516(3) . ?
C15A C16A 1.536(2) . ?
C21A C22A 1.536(2) . ?
C21A C26A 1.541(2) . ?
C21A B2A 1.655(2) . ?
C22A C23A 1.528(2) . ?
C23A C24A 1.523(2) . ?
C24A C25A 1.518(2) . ?
C25A C26A 1.529(2) . ?
C31A C32A 1.532(2) . ?
C31A C33A 1.533(2) . ?
C34A C36A 1.524(2) . ?
C34A C35A 1.530(2) . ?
P1B C1B 1.8019(16) . ?
P1B C31B 1.8306(16) . ?
P1B C34B 1.8363(17) . ?
P1B B1B 1.9425(19) . ?
N1B B1B 1.574(2) . ?
N1B B2B 1.626(2) . ?
C1B C6B 1.405(2) . ?
C1B C2B 1.419(2) . ?
C2B C3B 1.408(2) . ?
C2B B2B 1.650(2) . ?
C3B C4B 1.385(2) . ?
C4B C5B 1.387(2) . ?
C5B C6B 1.379(2) . ?
C11B C16B 1.536(2) . ?
C11B C12B 1.545(2) . ?
C11B B2B 1.653(2) . ?
C12B C13B 1.528(2) . ?
C13B C14B 1.523(2) . ?
C14B C15B 1.524(2) . ?
C15B C16B 1.530(2) . ?
C21B C22B 1.539(2) . ?
C21B C26B 1.539(2) . ?
C21B B2B 1.648(2) . ?
C22B C23B 1.534(2) . ?
C23B C24B 1.527(3) . ?
C24B C25B 1.516(3) . ?
C25B C26B 1.531(2) . ?
C31B C32B 1.533(2) . ?
C31B C33B 1.534(2) . ?
C34B C36B 1.521(3) . ?
C34B C35B 1.531(3) . ?

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
C1A P1A C31A 108.60(7) . . ?
C1A P1A C34A 108.91(7) . . ?
C31A P1A C34A 107.28(8) . . ?
C1A P1A B1A 111.76(7) . . ?
C31A P1A B1A 111.06(8) . . ?
C34A P1A B1A 109.10(8) . . ?
B1A N1A B2A 120.45(12) . . ?
C6A C1A C2A 122.03(14) . . ?
C6A C1A P1A 117.76(12) . . ?
C2A C1A P1A 120.19(12) . . ?
C3A C2A C1A 114.39(14) . . ?
C3A C2A B2A 117.95(13) . . ?
C1A C2A B2A 126.95(13) . . ?
C4A C3A C2A 123.86(15) . . ?
C3A C4A C5A 120.31(15) . . ?
C6A C5A C4A 118.44(15) . . ?
C5A C6A C1A 120.90(15) . . ?
C16A C11A C12A 108.71(14) . . ?
C16A C11A B2A 115.97(13) . . ?
C12A C11A B2A 113.36(13) . . ?
C13A C12A C11A 113.80(14) . . ?
C14A C13A C12A 111.57(16) . . ?
C13A C14A C15A 110.64(16) . . ?
C14A C15A C16A 111.35(18) . . ?
C15A C16A C11A 113.18(15) . . ?
C22A C21A C26A 108.22(12) . . ?
C22A C21A B2A 113.02(12) . . ?
C26A C21A B2A 117.08(12) . . ?
C23A C22A C21A 112.72(13) . . ?
C24A C23A C22A 111.40(14) . . ?
C25A C24A C23A 110.73(14) . . ?
C24A C25A C26A 111.41(13) . . ?
C25A C26A C21A 112.39(13) . . ?
C32A C31A C33A 111.64(15) . . ?
C32A C31A P1A 110.32(11) . . ?
C33A C31A P1A 109.38(12) . . ?
C36A C34A C35A 110.41(16) . . ?
C36A C34A P1A 116.06(13) . . ?
C35A C34A P1A 109.38(11) . . ?
N1A B1A P1A 108.61(11) . . ?
N1A B2A C2A 109.94(12) . . ?
N1A B2A C11A 106.01(12) . . ?
C2A B2A C11A 111.48(12) . . ?
N1A B2A C21A 106.93(12) . . ?
C2A B2A C21A 105.83(12) . . ?
C11A B2A C21A 116.51(12) . . ?
C1B P1B C31B 108.65(7) . . ?
C1B P1B C34B 108.81(8) . . ?
C31B P1B C34B 107.38(8) . . ?
C1B P1B B1B 111.71(7) . . ?
C31B P1B B1B 111.59(8) . . ?
C34B P1B B1B 108.57(8) . . ?
B1B N1B B2B 120.98(12) . . ?
C6B C1B C2B 122.14(14) . . ?
C6B C1B P1B 117.54(12) . . ?
C2B C1B P1B 120.32(12) . . ?
C3B C2B C1B 114.18(14) . . ?
C3B C2B B2B 118.42(13) . . ?
C1B C2B B2B 126.95(13) . . ?
C4B C3B C2B 123.76(15) . . ?
C3B C4B C5B 120.42(16) . . ?
C6B C5B C4B 118.49(16) . . ?
C5B C6B C1B 120.95(15) . . ?
C16B C11B C12B 108.29(12) . . ?
C16B C11B B2B 112.41(12) . . ?
C12B C11B B2B 118.23(12) . . ?
C13B C12B C11B 111.79(13) . . ?
C14B C13B C12B 110.54(14) . . ?
C13B C14B C15B 111.06(14) . . ?
C14B C15B C16B 111.41(14) . . ?
C15B C16B C11B 112.93(13) . . ?
C22B C21B C26B 108.44(14) . . ?
C22B C21B B2B 114.88(13) . . ?
C26B C21B B2B 115.44(13) . . ?
C23B C22B C21B 112.61(15) . . ?
C24B C23B C22B 111.51(17) . . ?
C25B C24B C23B 111.30(16) . . ?
C24B C25B C26B 111.78(17) . . ?
C25B C26B C21B 112.72(15) . . ?
C32B C31B C33B 111.35(15) . . ?
C32B C31B P1B 110.76(11) . . ?
C33B C31B P1B 109.41(12) . . ?
C36B C34B C35B 110.88(18) . . ?
C36B C34B P1B 116.59(14) . . ?
C35B C34B P1B 109.14(12) . . ?
N1B B1B P1B 108.64(11) . . ?
N1B B2B C21B 106.46(12) . . ?
N1B B2B C2B 109.83(12) . . ?
C21B B2B C2B 111.24(12) . . ?
N1B B2B C11B 107.32(12) . . ?
C21B B2B C11B 115.06(12) . . ?
C2B B2B C11B 106.83(12) . . ?

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
C31A P1A C1A C6A 51.13(14) . . . . ?
C34A P1A C1A C6A -65.39(14) . . . . ?
B1A P1A C1A C6A 174.00(12) . . . . ?
C31A P1A C1A C2A -127.76(13) . . . . ?
C34A P1A C1A C2A 115.72(13) . . . . ?
B1A P1A C1A C2A -4.89(15) . . . . ?
C6A C1A C2A C3A 2.9(2) . . . . ?
P1A C1A C2A C3A -178.22(11) . . . . ?
C6A C1A C2A B2A -167.07(14) . . . . ?
P1A C1A C2A B2A 11.8(2) . . . . ?
C1A C2A C3A C4A -3.0(2) . . . . ?
B2A C2A C3A C4A 167.96(15) . . . . ?
C2A C3A C4A C5A 1.4(3) . . . . ?
C3A C4A C5A C6A 0.5(3) . . . . ?
C4A C5A C6A C1A -0.5(2) . . . . ?
C2A C1A C6A C5A -1.3(2) . . . . ?
P1A C1A C6A C5A 179.82(13) . . . . ?
C16A C11A C12A C13A 51.7(2) . . . . ?
B2A C11A C12A C13A -177.76(14) . . . . ?
C11A C12A C13A C14A -54.5(2) . . . . ?
C12A C13A C14A C15A 55.4(2) . . . . ?
C13A C14A C15A C16A -56.4(3) . . . . ?
C14A C15A C16A C11A 56.5(3) . . . . ?
C12A C11A C16A C15A -52.6(2) . . . . ?
B2A C11A C16A C15A 178.34(16) . . . . ?
C26A C21A C22A C23A 55.30(18) . . . . ?
B2A C21A C22A C23A -173.36(14) . . . . ?
C21A C22A C23A C24A -56.32(19) . . . . ?
C22A C23A C24A C25A 54.83(19) . . . . ?
C23A C24A C25A C26A -55.18(19) . . . . ?
C24A C25A C26A C21A 56.86(19) . . . . ?
C22A C21A C26A C25A -55.45(17) . . . . ?
B2A C21A C26A C25A 175.45(13) . . . . ?
C1A P1A C31A C32A 55.45(14) . . . . ?
C34A P1A C31A C32A 173.02(12) . . . . ?
B1A P1A C31A C32A -67.83(14) . . . . ?
C1A P1A C31A C33A 178.62(12) . . . . ?
C34A P1A C31A C33A -63.81(14) . . . . ?
B1A P1A C31A C33A 55.33(14) . . . . ?
C1A P1A C34A C36A 65.02(15) . . . . ?
C31A P1A C34A C36A -52.35(16) . . . . ?
B1A P1A C34A C36A -172.75(14) . . . . ?
C1A P1A C34A C35A -60.68(14) . . . . ?
C31A P1A C34A C35A -178.05(13) . . . . ?
B1A P1A C34A C35A 61.55(15) . . . . ?
B2A N1A B1A P1A -49.50(17) . . . . ?
B1A N1A B2A C2A 55.70(18) . . . . ?
B1A N1A B2A C11A 176.32(13) . . . . ?
B1A N1A B2A C21A -58.74(17) . . . . ?
C3A C2A B2A N1A 156.60(13) . . . . ?
C1A C2A B2A N1A -33.7(2) . . . . ?
C3A C2A B2A C11A 39.34(18) . . . . ?
C1A C2A B2A C11A -150.97(14) . . . . ?
C3A C2A B2A C21A -88.25(16) . . . . ?
C1A C2A B2A C21A 81.44(17) . . . . ?
C16A C11A B2A N1A 65.46(17) . . . . ?
C12A C11A B2A N1A -61.33(17) . . . . ?
C16A C11A B2A C2A -174.92(14) . . . . ?
C12A C11A B2A C2A 58.28(17) . . . . ?
C16A C11A B2A C21A -53.34(19) . . . . ?
C12A C11A B2A C21A 179.87(13) . . . . ?
C22A C21A B2A N1A -168.82(12) . . . . ?
C26A C21A B2A N1A -42.05(17) . . . . ?
C22A C21A B2A C2A 73.99(15) . . . . ?
C26A C21A B2A C2A -159.23(12) . . . . ?
C22A C21A B2A C11A -50.53(18) . . . . ?
C26A C21A B2A C11A 76.25(17) . . . . ?
C31B P1B C1B C6B 52.77(14) . . . . ?
C34B P1B C1B C6B -63.84(14) . . . . ?
B1B P1B C1B C6B 176.30(12) . . . . ?
C31B P1B C1B C2B -127.73(12) . . . . ?
C34B P1B C1B C2B 115.66(13) . . . . ?
B1B P1B C1B C2B -4.20(15) . . . . ?
C6B C1B C2B C3B 2.8(2) . . . . ?
P1B C1B C2B C3B -176.68(11) . . . . ?
C6B C1B C2B B2B -169.30(14) . . . . ?
P1B C1B C2B B2B 11.2(2) . . . . ?
C1B C2B C3B C4B -1.9(2) . . . . ?
B2B C2B C3B C4B 170.88(15) . . . . ?
C2B C3B C4B C5B 0.0(3) . . . . ?
C3B C4B C5B C6B 1.2(2) . . . . ?
C4B C5B C6B C1B -0.3(2) . . . . ?
C2B C1B C6B C5B -1.8(2) . . . . ?
P1B C1B C6B C5B 177.68(13) . . . . ?
C16B C11B C12B C13B -56.80(17) . . . . ?
B2B C11B C12B C13B 173.91(13) . . . . ?
C11B C12B C13B C14B 58.63(18) . . . . ?
C12B C13B C14B C15B -56.4(2) . . . . ?
C13B C14B C15B C16B 54.4(2) . . . . ?
C14B C15B C16B C11B -54.9(2) . . . . ?
C12B C11B C16B C15B 54.94(17) . . . . ?
B2B C11B C16B C15B -172.59(13) . . . . ?
C26B C21B C22B C23B 55.3(2) . . . . ?
B2B C21B C22B C23B -173.92(15) . . . . ?
C21B C22B C23B C24B -55.8(2) . . . . ?
C22B C23B C24B C25B 53.8(2) . . . . ?
C23B C24B C25B C26B -53.8(2) . . . . ?
C24B C25B C26B C21B 55.8(2) . . . . ?
C22B C21B C26B C25B -55.2(2) . . . . ?
B2B C21B C26B C25B 174.31(15) . . . . ?
C1B P1B C31B C32B 55.49(14) . . . . ?
C34B P1B C31B C32B 173.02(13) . . . . ?
B1B P1B C31B C32B -68.12(14) . . . . ?
C1B P1B C31B C33B 178.61(12) . . . . ?
C34B P1B C31B C33B -63.86(15) . . . . ?
B1B P1B C31B C33B 55.00(14) . . . . ?
C1B P1B C34B C36B 71.16(18) . . . . ?
C31B P1B C34B C36B -46.26(18) . . . . ?
B1B P1B C34B C36B -167.05(16) . . . . ?
C1B P1B C34B C35B -55.39(16) . . . . ?
C31B P1B C34B C35B -172.82(14) . . . . ?
B1B P1B C34B C35B 66.40(16) . . . . ?
B2B N1B B1B P1B -48.99(17) . . . . ?
B1B N1B B2B C21B 175.88(14) . . . . ?
B1B N1B B2B C2B 55.34(18) . . . . ?
B1B N1B B2B C11B -60.43(18) . . . . ?
C22B C21B B2B N1B -63.91(17) . . . . ?
C26B C21B B2B N1B 63.44(17) . . . . ?
C22B C21B B2B C2B 55.71(18) . . . . ?
C26B C21B B2B C2B -176.94(13) . . . . ?
C22B C21B B2B C11B 177.35(14) . . . . ?
C26B C21B B2B C11B -55.30(18) . . . . ?
C3B C2B B2B N1B 154.95(13) . . . . ?
C1B C2B B2B N1B -33.24(19) . . . . ?
C3B C2B B2B C21B 37.36(18) . . . . ?
C1B C2B B2B C21B -150.84(14) . . . . ?
C3B C2B B2B C11B -88.96(15) . . . . ?
C1B C2B B2B C11B 82.84(17) . . . . ?
C16B C11B B2B N1B -164.97(12) . . . . ?
C12B C11B B2B N1B -37.62(17) . . . . ?
C16B C11B B2B C21B -46.72(18) . . . . ?
C12B C11B B2B C21B 80.64(17) . . . . ?
C16B C11B B2B C2B 77.28(15) . . . . ?
C12B C11B B2B C2B -155.36(13) . . . . ?

_refine_diff_density_max         0.390
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.044


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes at -40C'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PB(HBNH)
_database_code_depnum_ccdc_archive 'CCDC 2106478'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            PB(HBNH)
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H42 B2 N P'
_chemical_formula_sum            'C24 H42 B2 N P'
_chemical_formula_weight         397.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.1624(4)
_cell_length_b                   9.3546(3)
_cell_length_c                   23.6269(8)
_cell_angle_alpha                90
_cell_angle_beta                 99.5776(19)
_cell_angle_gamma                90
_cell_volume                     2432.73(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9878
_cell_measurement_theta_min      4.02
_cell_measurement_theta_max      72.70

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_F_000             872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.127
_exptl_absorpt_coefficient_mu    1.039
_shelx_estimated_absorpt_T_min   0.765
_shelx_estimated_absorpt_T_max   0.879
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7494
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_process_details   
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            92836
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.794
_diffrn_reflns_theta_max         72.777
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             4766
_reflns_number_gt                4438
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0566P)²+1.7782P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4766
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1376
_refine_ls_wR_factor_gt          0.1340
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.45179(4) 0.20073(5) 0.37039(2) 0.02831(14) Uani 1 1 d . . . . .
N1 N 0.67987(15) 0.11092(17) 0.42373(7) 0.0339(4) Uani 1 1 d . . . . .
H1 H 0.727(2) 0.046(3) 0.4432(12) 0.059(8) Uiso 1 1 d . . . . .
C1 C 0.52175(16) 0.37397(18) 0.37707(7) 0.0280(4) Uani 1 1 d . . . . .
C2 C 0.64843(16) 0.38442(19) 0.39384(7) 0.0286(4) Uani 1 1 d . . . . .
C3 C 0.69276(19) 0.5261(2) 0.39594(8) 0.0360(4) Uani 1 1 d . . . . .
H3 H 0.777861 0.540563 0.406149 0.043 Uiso 1 1 calc R U . . .
C4 C 0.6193(2) 0.6448(2) 0.38399(9) 0.0417(5) Uani 1 1 d . . . . .
H4 H 0.654466 0.737541 0.386405 0.050 Uiso 1 1 calc R U . . .
C5 C 0.4953(2) 0.6296(2) 0.36858(10) 0.0453(5) Uani 1 1 d . . . . .
H5 H 0.444331 0.711042 0.360745 0.054 Uiso 1 1 calc R U . . .
C6 C 0.44672(19) 0.4936(2) 0.36478(9) 0.0392(4) Uani 1 1 d . . . . .
H6 H 0.361588 0.481024 0.353723 0.047 Uiso 1 1 calc R U . . .
C11 C 0.41599(19) 0.1581(2) 0.29312(9) 0.0395(4) Uani 1 1 d . . . . .
H11 H 0.484913 0.197847 0.275904 0.047 Uiso 1 1 calc R U . . .
C12 C 0.3026(2) 0.2331(3) 0.26217(9) 0.0526(6) Uani 1 1 d . . . . .
H12A H 0.307234 0.335255 0.271449 0.063 Uiso 1 1 calc R U . . .
H12B H 0.297202 0.220512 0.220639 0.063 Uiso 1 1 calc R U . . .
H12C H 0.230508 0.191761 0.274498 0.063 Uiso 1 1 calc R U . . .
C13 C 0.4151(2) -0.0015(3) 0.28066(11) 0.0538(6) Uani 1 1 d . . . . .
H13A H 0.489482 -0.045033 0.301408 0.065 Uiso 1 1 calc R U . . .
H13B H 0.344251 -0.045489 0.293203 0.065 Uiso 1 1 calc R U . . .
H13C H 0.410945 -0.016738 0.239344 0.065 Uiso 1 1 calc R U . . .
C14 C 0.31230(18) 0.2085(2) 0.40227(9) 0.0380(4) Uani 1 1 d . . . . .
H14 H 0.256482 0.280335 0.380381 0.046 Uiso 1 1 calc R U . . .
C15 C 0.2471(2) 0.0640(3) 0.39815(12) 0.0552(6) Uani 1 1 d . . . . .
H15A H 0.228121 0.034617 0.357844 0.066 Uiso 1 1 calc R U . . .
H15B H 0.299735 -0.007623 0.419999 0.066 Uiso 1 1 calc R U . . .
H15C H 0.171626 0.072632 0.413972 0.066 Uiso 1 1 calc R U . . .
C16 C 0.3441(2) 0.2596(3) 0.46438(10) 0.0555(6) Uani 1 1 d . . . . .
H16A H 0.385606 0.352053 0.465420 0.067 Uiso 1 1 calc R U . . .
H16B H 0.269446 0.269812 0.480768 0.067 Uiso 1 1 calc R U . . .
H16C H 0.397556 0.189557 0.486794 0.067 Uiso 1 1 calc R U . . .
C21 C 0.82564(18) 0.2182(2) 0.36011(8) 0.0364(4) Uani 1 1 d . . . . .
H21 H 0.877726 0.134107 0.373898 0.044 Uiso 1 1 calc R U . . .
C22 C 0.9133(2) 0.3367(3) 0.34893(10) 0.0490(5) Uani 1 1 d . . . . .
H22A H 0.865650 0.422106 0.334211 0.059 Uiso 1 1 calc R U . . .
H22B H 0.964674 0.363264 0.385702 0.059 Uiso 1 1 calc R U . . .
C23 C 0.9950(2) 0.2941(3) 0.30618(11) 0.0610(7) Uani 1 1 d . . . . .
H23A H 1.046408 0.376393 0.299271 0.073 Uiso 1 1 calc R U . . .
H23B H 1.049156 0.215175 0.322378 0.073 Uiso 1 1 calc R U . . .
C24 C 0.9207(3) 0.2471(4) 0.25035(11) 0.0719(9) Uani 1 1 d . . . . .
H24A H 0.975564 0.212672 0.224374 0.086 Uiso 1 1 calc R U . . .
H24B H 0.874517 0.329642 0.231766 0.086 Uiso 1 1 calc R U . . .
C25 C 0.8327(2) 0.1284(4) 0.25947(11) 0.0697(8) Uani 1 1 d . . . . .
H25A H 0.879025 0.041526 0.273440 0.084 Uiso 1 1 calc R U . . .
H25B H 0.780774 0.105082 0.222462 0.084 Uiso 1 1 calc R U . . .
C26 C 0.7523(2) 0.1737(3) 0.30322(9) 0.0473(5) Uani 1 1 d . . . . .
H26B H 0.700066 0.254464 0.287236 0.057 Uiso 1 1 calc R U . . .
H26A H 0.698716 0.093066 0.309553 0.057 Uiso 1 1 calc R U . . .
C31 C 0.83731(17) 0.2968(2) 0.47210(8) 0.0311(4) Uani 1 1 d . . . . .
H31 H 0.877535 0.388648 0.464445 0.037 Uiso 1 1 calc R U . . .
C32 C 0.77131(19) 0.3252(2) 0.52283(9) 0.0396(5) Uani 1 1 d . . . . .
H32A H 0.730956 0.236276 0.532373 0.048 Uiso 1 1 calc R U . . .
H32B H 0.707575 0.398260 0.511618 0.048 Uiso 1 1 calc R U . . .
C33 C 0.8581(2) 0.3772(3) 0.57614(9) 0.0517(6) Uani 1 1 d . . . . .
H33A H 0.890592 0.472201 0.568134 0.062 Uiso 1 1 calc R U . . .
H33B H 0.812420 0.388030 0.608402 0.062 Uiso 1 1 calc R U . . .
C34 C 0.9633(2) 0.2742(3) 0.59358(9) 0.0483(5) Uani 1 1 d . . . . .
H34A H 1.021566 0.316661 0.625280 0.058 Uiso 1 1 calc R U . . .
H34B H 0.932108 0.184256 0.607789 0.058 Uiso 1 1 calc R U . . .
C35 C 1.02825(19) 0.2410(3) 0.54382(9) 0.0441(5) Uani 1 1 d . . . . .
H35A H 1.090383 0.166511 0.555562 0.053 Uiso 1 1 calc R U . . .
H35B H 1.070381 0.328041 0.533566 0.053 Uiso 1 1 calc R U . . .
C36 C 0.94001(18) 0.1892(2) 0.49135(9) 0.0383(4) Uani 1 1 d . . . . .
H36A H 0.904253 0.096934 0.500534 0.046 Uiso 1 1 calc R U . . .
H36B H 0.985331 0.172564 0.459316 0.046 Uiso 1 1 calc R U . . .
B1 B 0.74631(18) 0.2541(2) 0.41177(9) 0.0294(4) Uani 1 1 d . . . . .
B2 B 0.5642(2) 0.0647(2) 0.41101(10) 0.0349(5) Uani 1 1 d . . . . .
H2 H 0.528(2) -0.043(3) 0.4212(10) 0.045(6) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.7945(18) . ?
P1 C14 1.840(2) . ?
P1 C11 1.846(2) . ?
P1 B2 1.927(2) . ?
N1 B2 1.347(3) . ?
N1 B1 1.579(3) . ?
C1 C6 1.399(3) . ?
C1 C2 1.407(3) . ?
C2 C3 1.413(3) . ?
C2 B1 1.645(3) . ?
C3 C4 1.381(3) . ?
C4 C5 1.379(3) . ?
C5 C6 1.380(3) . ?
C11 C13 1.521(3) . ?
C11 C12 1.523(3) . ?
C14 C16 1.528(3) . ?
C14 C15 1.530(3) . ?
C21 C26 1.511(3) . ?
C21 C22 1.530(3) . ?
C21 B1 1.657(3) . ?
C22 C23 1.523(3) . ?
C23 C24 1.502(4) . ?
C24 C25 1.521(4) . ?
C25 C26 1.537(3) . ?
C31 C32 1.531(3) . ?
C31 C36 1.536(3) . ?
C31 B1 1.656(3) . ?
C32 C33 1.534(3) . ?
C33 C34 1.522(3) . ?
C34 C35 1.512(3) . ?
C35 C36 1.528(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 C14 108.29(9) . . ?
C1 P1 C11 107.55(9) . . ?
C14 P1 C11 110.76(10) . . ?
C1 P1 B2 108.35(9) . . ?
C14 P1 B2 110.33(9) . . ?
C11 P1 B2 111.44(10) . . ?
B2 N1 B1 133.91(17) . . ?
C6 C1 C2 122.81(17) . . ?
C6 C1 P1 117.86(14) . . ?
C2 C1 P1 119.33(13) . . ?
C1 C2 C3 113.88(16) . . ?
C1 C2 B1 127.91(15) . . ?
C3 C2 B1 118.20(16) . . ?
C4 C3 C2 123.67(19) . . ?
C5 C4 C3 120.47(19) . . ?
C4 C5 C6 118.55(19) . . ?
C5 C6 C1 120.60(19) . . ?
C13 C11 C12 112.4(2) . . ?
C13 C11 P1 113.38(16) . . ?
C12 C11 P1 113.64(15) . . ?
C16 C14 C15 111.66(19) . . ?
C16 C14 P1 109.17(15) . . ?
C15 C14 P1 111.41(15) . . ?
C26 C21 C22 108.23(18) . . ?
C26 C21 B1 115.74(16) . . ?
C22 C21 B1 114.56(16) . . ?
C23 C22 C21 113.3(2) . . ?
C24 C23 C22 110.8(2) . . ?
C23 C24 C25 111.4(2) . . ?
C24 C25 C26 110.9(2) . . ?
C21 C26 C25 112.57(19) . . ?
C32 C31 C36 108.35(16) . . ?
C32 C31 B1 114.19(15) . . ?
C36 C31 B1 114.68(15) . . ?
C31 C32 C33 112.18(17) . . ?
C34 C33 C32 112.01(19) . . ?
C35 C34 C33 111.56(18) . . ?
C34 C35 C36 111.59(18) . . ?
C35 C36 C31 112.37(17) . . ?
N1 B1 C2 111.29(14) . . ?
N1 B1 C31 106.83(15) . . ?
C2 B1 C31 109.22(15) . . ?
N1 B1 C21 106.52(15) . . ?
C2 B1 C21 111.96(15) . . ?
C31 B1 C21 110.88(15) . . ?
N1 B2 P1 114.80(15) . . ?

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 P1 C1 C6 -43.26(17) . . . . ?
C11 P1 C1 C6 76.49(17) . . . . ?
B2 P1 C1 C6 -162.93(15) . . . . ?
C14 P1 C1 C2 137.21(15) . . . . ?
C11 P1 C1 C2 -103.05(15) . . . . ?
B2 P1 C1 C2 17.53(17) . . . . ?
C6 C1 C2 C3 -1.2(3) . . . . ?
P1 C1 C2 C3 178.30(13) . . . . ?
C6 C1 C2 B1 177.53(18) . . . . ?
P1 C1 C2 B1 -3.0(2) . . . . ?
C1 C2 C3 C4 1.4(3) . . . . ?
B1 C2 C3 C4 -177.52(18) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
C3 C4 C5 C6 -0.7(3) . . . . ?
C4 C5 C6 C1 0.8(3) . . . . ?
C2 C1 C6 C5 0.2(3) . . . . ?
P1 C1 C6 C5 -179.35(17) . . . . ?
C1 P1 C11 C13 151.94(16) . . . . ?
C14 P1 C11 C13 -89.90(18) . . . . ?
B2 P1 C11 C13 33.3(2) . . . . ?
C1 P1 C11 C12 -78.10(18) . . . . ?
C14 P1 C11 C12 40.1(2) . . . . ?
B2 P1 C11 C12 163.29(17) . . . . ?
C1 P1 C14 C16 -56.27(17) . . . . ?
C11 P1 C14 C16 -173.98(16) . . . . ?
B2 P1 C14 C16 62.15(18) . . . . ?
C1 P1 C14 C15 179.95(15) . . . . ?
C11 P1 C14 C15 62.24(18) . . . . ?
B2 P1 C14 C15 -61.63(18) . . . . ?
C26 C21 C22 C23 -55.8(3) . . . . ?
B1 C21 C22 C23 173.43(19) . . . . ?
C21 C22 C23 C24 56.3(3) . . . . ?
C22 C23 C24 C25 -54.6(4) . . . . ?
C23 C24 C25 C26 54.7(3) . . . . ?
C22 C21 C26 C25 55.4(3) . . . . ?
B1 C21 C26 C25 -174.5(2) . . . . ?
C24 C25 C26 C21 -56.3(3) . . . . ?
C36 C31 C32 C33 55.9(2) . . . . ?
B1 C31 C32 C33 -174.91(17) . . . . ?
C31 C32 C33 C34 -55.2(3) . . . . ?
C32 C33 C34 C35 52.8(3) . . . . ?
C33 C34 C35 C36 -53.2(3) . . . . ?
C34 C35 C36 C31 56.5(3) . . . . ?
C32 C31 C36 C35 -56.8(2) . . . . ?
B1 C31 C36 C35 174.36(17) . . . . ?
B2 N1 B1 C2 16.9(3) . . . . ?
B2 N1 B1 C31 136.1(2) . . . . ?
B2 N1 B1 C21 -105.4(2) . . . . ?
C1 C2 B1 N1 -14.5(2) . . . . ?
C3 C2 B1 N1 164.17(16) . . . . ?
C1 C2 B1 C31 -132.24(18) . . . . ?
C3 C2 B1 C31 46.5(2) . . . . ?
C1 C2 B1 C21 104.6(2) . . . . ?
C3 C2 B1 C21 -76.7(2) . . . . ?
C32 C31 B1 N1 -61.8(2) . . . . ?
C36 C31 B1 N1 64.1(2) . . . . ?
C32 C31 B1 C2 58.7(2) . . . . ?
C36 C31 B1 C2 -175.42(15) . . . . ?
C32 C31 B1 C21 -177.48(16) . . . . ?
C36 C31 B1 C21 -51.6(2) . . . . ?
C26 C21 B1 N1 62.5(2) . . . . ?
C22 C21 B1 N1 -170.47(17) . . . . ?
C26 C21 B1 C2 -59.4(2) . . . . ?
C22 C21 B1 C2 67.7(2) . . . . ?
C26 C21 B1 C31 178.38(18) . . . . ?
C22 C21 B1 C31 -54.6(2) . . . . ?
B1 N1 B2 P1 -1.2(3) . . . . ?

_refine_diff_density_max         0.605
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.048


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes at -40C'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PB(HIBNH2)
_database_code_depnum_ccdc_archive 'CCDC 2106481'
loop_
_audit_author_name
_audit_author_address
'Michael J. Ferguson'
;University of Alberta
Canada
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_FORMU01_riv1990             
;
PROBLEM: There is a discrepancy between the atom counts in the
			_chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE: _chemical_formula_sum includes the contributions of the partially
 occupied or disordered solvent hexane atoms, which were corrected by the use of
 the SQUEEZE procedure of the program PLATON.  For more details, please refer to
 SQUEEZE RESULTS in the CIF. This response also applies to CELLZ01, PLAT041,
 PLAT051 and PLAT068.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            PB(HIBNH2)
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H43 B2 I N P, 0.5 (C6 H14)'
_chemical_formula_sum            'C27 H50 B2 I N P'
_chemical_formula_weight         568.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   18.2679(5)
_cell_length_b                   11.4128(4)
_cell_length_c                   14.6131(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.048(2)
_cell_angle_gamma                90
_cell_volume                     2912.78(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3676
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      64.26

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_F_000             1188
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    9.241
_shelx_estimated_absorpt_T_min   0.406
_shelx_estimated_absorpt_T_max   0.709
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.1563
_exptl_absorpt_correction_T_max  0.2912
_exptl_absorpt_process_details   'SADABS (version 2016/2)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38652
_diffrn_reflns_av_unetI/netI     0.0999
_diffrn_reflns_av_R_equivalents  0.1170
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.530
_diffrn_reflns_theta_max         73.950
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             5714
_reflns_number_gt                4015
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (version 2014/5)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+0.3809P] 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     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00181(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5714
_refine_ls_number_parameters     276
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1380
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I I 0.43523(2) 0.56142(3) 0.87661(2) 0.04280(15) Uani 1 1 d . . . . .
P P 0.36766(7) 0.72845(12) 0.66897(10) 0.0373(3) Uani 1 1 d . . . . .
N N 0.2853(3) 0.5311(4) 0.7038(4) 0.0411(11) Uani 1 1 d D . . . .
H1N H 0.263(3) 0.569(5) 0.733(4) 0.062 Uiso 1 1 d D U . . .
H2N H 0.289(3) 0.462(3) 0.711(4) 0.062 Uiso 1 1 d D U . . .
C1 C 0.3651(3) 0.8405(5) 0.7576(4) 0.0446(13) Uani 1 1 d . . . . .
H1 H 0.410231 0.825718 0.814709 0.053 Uiso 1 1 calc R U . . .
C2 C 0.2937(3) 0.8252(5) 0.7908(4) 0.0506(14) Uani 1 1 d . . . . .
H2A H 0.294183 0.883315 0.840411 0.076 Uiso 1 1 calc R U . . .
H2B H 0.293280 0.746248 0.817002 0.076 Uiso 1 1 calc R U . . .
H2C H 0.247821 0.836331 0.736377 0.076 Uiso 1 1 calc R U . . .
C3 C 0.3725(4) 0.9668(5) 0.7261(5) 0.0572(16) Uani 1 1 d . . . . .
H3A H 0.376939 1.019854 0.780184 0.086 Uiso 1 1 calc R U . . .
H3B H 0.327009 0.987440 0.673617 0.086 Uiso 1 1 calc R U . . .
H3C H 0.418179 0.973842 0.704346 0.086 Uiso 1 1 calc R U . . .
C4 C 0.4519(3) 0.7538(4) 0.6276(4) 0.0395(12) Uani 1 1 d . . . . .
H4 H 0.445818 0.832801 0.596766 0.047 Uiso 1 1 calc R U . . .
C5 C 0.4557(3) 0.6641(5) 0.5516(4) 0.0551(15) Uani 1 1 d . . . . .
H5A H 0.497693 0.684427 0.525387 0.083 Uiso 1 1 calc R U . . .
H5B H 0.407242 0.664340 0.500012 0.083 Uiso 1 1 calc R U . . .
H5C H 0.464666 0.585926 0.580491 0.083 Uiso 1 1 calc R U . . .
C6 C 0.5256(3) 0.7564(5) 0.7116(5) 0.0557(16) Uani 1 1 d . . . . .
H6A H 0.569731 0.767012 0.687149 0.084 Uiso 1 1 calc R U . . .
H6B H 0.531004 0.682339 0.746967 0.084 Uiso 1 1 calc R U . . .
H6C H 0.523335 0.821444 0.754472 0.084 Uiso 1 1 calc R U . . .
C11 C 0.2837(3) 0.7438(4) 0.5669(4) 0.0369(11) Uani 1 1 d . . . . .
C12 C 0.2262(3) 0.6570(5) 0.5444(4) 0.0374(12) Uani 1 1 d . . . . .
C13 C 0.1633(3) 0.6845(5) 0.4644(4) 0.0432(13) Uani 1 1 d . . . . .
H13 H 0.122776 0.629132 0.445615 0.052 Uiso 1 1 calc R U . . .
C14 C 0.1568(3) 0.7865(5) 0.4118(4) 0.0470(14) Uani 1 1 d . . . . .
H14 H 0.112855 0.800072 0.358907 0.056 Uiso 1 1 calc R U . . .
C15 C 0.2143(3) 0.8678(5) 0.4364(4) 0.0481(14) Uani 1 1 d . . . . .
H15 H 0.210186 0.938312 0.400626 0.058 Uiso 1 1 calc R U . . .
C16 C 0.2779(3) 0.8479(5) 0.5124(4) 0.0427(13) Uani 1 1 d . . . . .
H16 H 0.318047 0.903990 0.528612 0.051 Uiso 1 1 calc R U . . .
C21 C 0.1410(3) 0.5021(5) 0.6073(4) 0.0440(13) Uani 1 1 d . . . . .
H21 H 0.105040 0.492343 0.541435 0.053 Uiso 1 1 calc R U . . .
C22 C 0.1346(3) 0.3889(6) 0.6620(5) 0.0621(17) Uani 1 1 d . . . . .
H22A H 0.151034 0.321626 0.629990 0.075 Uiso 1 1 calc R U . . .
H22B H 0.169929 0.394185 0.727808 0.075 Uiso 1 1 calc R U . . .
C23 C 0.0531(4) 0.3661(7) 0.6675(5) 0.071(2) Uani 1 1 d . . . . .
H23A H 0.018283 0.352829 0.602214 0.085 Uiso 1 1 calc R U . . .
H23B H 0.052784 0.294599 0.705744 0.085 Uiso 1 1 calc R U . . .
C24 C 0.0245(4) 0.4697(8) 0.7130(6) 0.083(3) Uani 1 1 d . . . . .
H24A H -0.029047 0.455259 0.712392 0.100 Uiso 1 1 calc R U . . .
H24B H 0.056091 0.477525 0.780459 0.100 Uiso 1 1 calc R U . . .
C25 C 0.0284(3) 0.5818(7) 0.6602(5) 0.068(2) Uani 1 1 d . . . . .
H25A H 0.013039 0.648191 0.694181 0.082 Uiso 1 1 calc R U . . .
H25B H -0.008108 0.577643 0.595131 0.082 Uiso 1 1 calc R U . . .
C26 C 0.1096(3) 0.6041(6) 0.6526(4) 0.0543(15) Uani 1 1 d . . . . .
H26A H 0.108861 0.675550 0.613985 0.065 Uiso 1 1 calc R U . . .
H26B H 0.144618 0.618708 0.717523 0.065 Uiso 1 1 calc R U . . .
C31 C 0.2607(3) 0.4321(4) 0.5343(4) 0.0456(13) Uani 1 1 d . . . . .
H31 H 0.305403 0.471568 0.521071 0.055 Uiso 1 1 calc R U . . .
C32 C 0.2924(3) 0.3163(5) 0.5840(5) 0.0547(15) Uani 1 1 d . . . . .
H32A H 0.330325 0.334031 0.646371 0.066 Uiso 1 1 calc DR U . . .
H32B H 0.250052 0.271645 0.596911 0.066 Uiso 1 1 calc R U . . .
C33 C 0.3306(4) 0.2399(6) 0.5247(5) 0.0658(18) Uani 1 1 d . . . . .
H33A H 0.376085 0.280967 0.516791 0.079 Uiso 1 1 calc R U . . .
H33B H 0.347990 0.165484 0.559045 0.079 Uiso 1 1 calc R U . . .
C34 C 0.2755(4) 0.2137(6) 0.4273(5) 0.072(2) Uani 1 1 d . . . . .
H34A H 0.302464 0.169140 0.388860 0.087 Uiso 1 1 calc R U . . .
H34B H 0.233177 0.164269 0.435144 0.087 Uiso 1 1 calc R U . . .
C35 C 0.2432(4) 0.3233(6) 0.3754(5) 0.072(2) Uani 1 1 d . . . . .
H35A H 0.204511 0.302542 0.314380 0.086 Uiso 1 1 calc R U . . .
H35B H 0.284592 0.367570 0.359925 0.086 Uiso 1 1 calc R U . . .
C36 C 0.2058(4) 0.4012(6) 0.4346(5) 0.0601(16) Uani 1 1 d . . . . .
H36A H 0.160416 0.360360 0.443083 0.072 Uiso 1 1 calc R U . . .
H36B H 0.187975 0.474550 0.398931 0.072 Uiso 1 1 calc R U . . .
B1 B 0.3676(3) 0.5700(6) 0.7177(5) 0.0414(14) Uani 1 1 d . . . . .
H1B H 0.397(3) 0.515(5) 0.685(4) 0.050 Uiso 1 1 d . U . . .
B2 B 0.2263(3) 0.5284(6) 0.5935(5) 0.0398(14) 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
I B1 2.290(7) . ?
P C11 1.807(5) . ?
P C1 1.831(6) . ?
P C4 1.833(5) . ?
P B1 1.944(7) . ?
N B1 1.523(7) . ?
N B2 1.657(8) . ?
C1 C2 1.530(7) . ?
C1 C3 1.530(8) . ?
C4 C5 1.528(7) . ?
C4 C6 1.534(7) . ?
C11 C12 1.411(7) . ?
C11 C16 1.416(7) . ?
C12 C13 1.413(7) . ?
C12 B2 1.633(8) . ?
C13 C14 1.381(8) . ?
C14 C15 1.369(8) . ?
C15 C16 1.370(7) . ?
C21 C26 1.531(8) . ?
C21 C22 1.542(8) . ?
C21 B2 1.656(8) . ?
C22 C23 1.538(8) . ?
C23 C24 1.522(11) . ?
C24 C25 1.507(10) . ?
C25 C26 1.541(8) . ?
C31 C32 1.538(8) . ?
C31 C36 1.547(8) . ?
C31 B2 1.634(8) . ?
C32 C33 1.534(8) . ?
C33 C34 1.513(9) . ?
C34 C35 1.492(9) . ?
C35 C36 1.533(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 P C1 109.0(2) . . ?
C11 P C4 107.7(2) . . ?
C1 P C4 108.7(2) . . ?
C11 P B1 107.5(3) . . ?
C1 P B1 112.8(3) . . ?
C4 P B1 111.0(2) . . ?
B1 N B2 118.1(4) . . ?
C2 C1 C3 111.2(5) . . ?
C2 C1 P 110.2(4) . . ?
C3 C1 P 115.0(4) . . ?
C5 C4 C6 112.2(4) . . ?
C5 C4 P 110.9(4) . . ?
C6 C4 P 111.4(4) . . ?
C12 C11 C16 122.0(5) . . ?
C12 C11 P 121.2(4) . . ?
C16 C11 P 116.8(4) . . ?
C11 C12 C13 114.0(5) . . ?
C11 C12 B2 128.6(4) . . ?
C13 C12 B2 117.3(4) . . ?
C14 C13 C12 124.3(5) . . ?
C15 C14 C13 119.5(5) . . ?
C14 C15 C16 120.2(5) . . ?
C15 C16 C11 120.1(5) . . ?
C26 C21 C22 108.6(5) . . ?
C26 C21 B2 113.6(5) . . ?
C22 C21 B2 115.6(5) . . ?
C23 C22 C21 113.0(5) . . ?
C24 C23 C22 110.6(6) . . ?
C25 C24 C23 111.3(6) . . ?
C24 C25 C26 111.6(6) . . ?
C21 C26 C25 113.3(5) . . ?
C32 C31 C36 107.4(5) . . ?
C32 C31 B2 118.5(5) . . ?
C36 C31 B2 114.1(4) . . ?
C33 C32 C31 113.1(5) . . ?
C34 C33 C32 110.9(5) . . ?
C35 C34 C33 111.6(6) . . ?
C34 C35 C36 112.0(6) . . ?
C35 C36 C31 113.0(5) . . ?
N B1 P 109.2(4) . . ?
N B1 I 109.9(4) . . ?
P B1 I 110.7(3) . . ?
C12 B2 C31 108.8(4) . . ?
C12 B2 C21 109.7(4) . . ?
C31 B2 C21 117.7(5) . . ?
C12 B2 N 109.1(4) . . ?
C31 B2 N 106.7(4) . . ?
C21 B2 N 104.5(4) . . ?

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
C11 P C1 C2 60.6(4) . . . . ?
C4 P C1 C2 177.7(4) . . . . ?
B1 P C1 C2 -58.7(5) . . . . ?
C11 P C1 C3 -66.0(5) . . . . ?
C4 P C1 C3 51.1(5) . . . . ?
B1 P C1 C3 174.7(4) . . . . ?
C11 P C4 C5 -60.8(4) . . . . ?
C1 P C4 C5 -178.7(4) . . . . ?
B1 P C4 C5 56.7(4) . . . . ?
C11 P C4 C6 173.5(4) . . . . ?
C1 P C4 C6 55.6(4) . . . . ?
B1 P C4 C6 -69.0(4) . . . . ?
C1 P C11 C12 -113.0(4) . . . . ?
C4 P C11 C12 129.3(4) . . . . ?
B1 P C11 C12 9.6(5) . . . . ?
C1 P C11 C16 65.6(4) . . . . ?
C4 P C11 C16 -52.1(4) . . . . ?
B1 P C11 C16 -171.8(4) . . . . ?
C16 C11 C12 C13 -0.6(7) . . . . ?
P C11 C12 C13 177.9(4) . . . . ?
C16 C11 C12 B2 174.8(5) . . . . ?
P C11 C12 B2 -6.7(7) . . . . ?
C11 C12 C13 C14 -0.2(7) . . . . ?
B2 C12 C13 C14 -176.2(5) . . . . ?
C12 C13 C14 C15 0.4(8) . . . . ?
C13 C14 C15 C16 0.2(8) . . . . ?
C14 C15 C16 C11 -1.1(8) . . . . ?
C12 C11 C16 C15 1.3(8) . . . . ?
P C11 C16 C15 -177.3(4) . . . . ?
C26 C21 C22 C23 54.3(7) . . . . ?
B2 C21 C22 C23 -176.7(5) . . . . ?
C21 C22 C23 C24 -56.6(8) . . . . ?
C22 C23 C24 C25 55.8(8) . . . . ?
C23 C24 C25 C26 -55.0(7) . . . . ?
C22 C21 C26 C25 -53.2(6) . . . . ?
B2 C21 C26 C25 176.8(5) . . . . ?
C24 C25 C26 C21 54.9(7) . . . . ?
C36 C31 C32 C33 55.1(6) . . . . ?
B2 C31 C32 C33 -173.8(5) . . . . ?
C31 C32 C33 C34 -56.9(7) . . . . ?
C32 C33 C34 C35 55.0(8) . . . . ?
C33 C34 C35 C36 -54.6(8) . . . . ?
C34 C35 C36 C31 55.4(8) . . . . ?
C32 C31 C36 C35 -53.9(7) . . . . ?
B2 C31 C36 C35 172.5(5) . . . . ?
B2 N B1 P 59.5(6) . . . . ?
B2 N B1 I -179.0(4) . . . . ?
C11 P B1 N -34.0(5) . . . . ?
C1 P B1 N 86.1(5) . . . . ?
C4 P B1 N -151.6(4) . . . . ?
C11 P B1 I -155.2(2) . . . . ?
C1 P B1 I -35.0(3) . . . . ?
C4 P B1 I 87.3(3) . . . . ?
C11 C12 B2 C31 -91.4(6) . . . . ?
C13 C12 B2 C31 83.8(5) . . . . ?
C11 C12 B2 C21 138.5(5) . . . . ?
C13 C12 B2 C21 -46.2(6) . . . . ?
C11 C12 B2 N 24.6(7) . . . . ?
C13 C12 B2 N -160.2(4) . . . . ?
C32 C31 B2 C12 159.2(5) . . . . ?
C36 C31 B2 C12 -72.7(6) . . . . ?
C32 C31 B2 C21 -75.3(6) . . . . ?
C36 C31 B2 C21 52.8(7) . . . . ?
C32 C31 B2 N 41.7(6) . . . . ?
C36 C31 B2 N 169.7(5) . . . . ?
C26 C21 B2 C12 -47.8(6) . . . . ?
C22 C21 B2 C12 -174.2(5) . . . . ?
C26 C21 B2 C31 -172.8(5) . . . . ?
C22 C21 B2 C31 60.7(7) . . . . ?
C26 C21 B2 N 69.1(6) . . . . ?
C22 C21 B2 N -57.4(6) . . . . ?
B1 N B2 C12 -54.6(6) . . . . ?
B1 N B2 C31 62.8(6) . . . . ?
B1 N B2 C21 -171.9(5) . . . . ?

_refine_diff_density_max         1.238
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.120



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexanes at -40C'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
