# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_LuZaPB_1_a
_database_code_depnum_ccdc_archive 'CCDC 2231981'
loop_
_audit_author_name
_audit_author_address
'Maik Finze'
;University of Wuerzburg
Germany
;
_audit_update_record             
;
2022-12-21 deposited with the CCDC.	2023-02-06 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT089_LuZaPB_1_a          
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       2.41 Note  
RESPONSE: Due to the disorder of the whole molecule sveral restraints have to
          be applied to ensure a stable refinement.
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 B P'
_chemical_formula_sum            'C36 H30 B P'
_chemical_formula_weight         504.38

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

_space_group_crystal_system      hexagonal
_space_group_IT_number           185
_space_group_name_H-M_alt        'P 63 c m'
_space_group_name_Hall           'P 6c -2'

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

_cell_length_a                   9.8279(7)
_cell_length_b                   9.8279(7)
_cell_length_c                   8.0179(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     670.68(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1054
_cell_measurement_theta_min      5.1980
_cell_measurement_theta_max      70.7590

_exptl_crystal_description       needle
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_F_000             266
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.028
_exptl_absorpt_coefficient_mu    1.070
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.802
_oxdiff_exptl_absorpt_empirical_full_max 1.396
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      99.97(12)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            4248
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.197
_diffrn_reflns_theta_max         74.962
_diffrn_reflns_theta_full        72.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             500
_reflns_number_gt                384
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_max     0.936
_reflns_Friedel_fraction_full    0.968

_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       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          
;
 The whole molecule is disordered over several positions and symmetry elements. 
 The P-B distance was fixed at 214.9 pm with the DFIX command. The phenyl groups were restrained
 with SADI, FLAT, SIMU, RIGU, and SAME commands to ensure a stable refinement.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0796P)²+0.0880P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 126 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         500
_refine_ls_number_parameters     116
_refine_ls_number_restraints     327
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1562
_refine_ls_wR_factor_gt          0.1434
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      0.896
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.000000 0.000000 0.322(2) 0.0465(12) Uani 0.255(6) 6 d DS TU P . .
B11 B 0.000000 0.000000 -0.004(2) 0.0465(12) Uani 0.245(6) 6 d DS TU P A .
P1 P 0.000000 0.000000 0.2621(13) 0.0465(12) Uani 0.245(6) 6 d DS TU P . .
P11 P 0.000000 0.000000 0.0561(12) 0.0465(12) Uani 0.255(6) 6 d DS TU P A .
C1_3 C 0.164(2) 0.168(2) 0.3533(17) 0.054(3) Uani 0.255(6) 1 d D U P A -2
C2_3 C 0.212(2) 0.322(2) 0.304(2) 0.054(4) Uani 0.255(6) 1 d D U P A -2
H2_3 H 0.150067 0.341228 0.227918 0.064 Uiso 0.255(6) 1 calc R U P A -2
C3_3 C 0.350(2) 0.445(2) 0.365(3) 0.057(4) Uani 0.255(6) 1 d D U P A -2
H3_3 H 0.381350 0.548774 0.328466 0.068 Uiso 0.255(6) 1 calc R U P A -2
C4_3 C 0.445(2) 0.425(2) 0.478(2) 0.060(4) Uani 0.255(6) 1 d D U P A -2
H4_3 H 0.537950 0.512059 0.520058 0.073 Uiso 0.255(6) 1 calc R U P A -2
C5_3 C 0.399(2) 0.274(2) 0.526(3) 0.063(4) Uani 0.255(6) 1 d D U P A -2
H5_3 H 0.462852 0.255361 0.601536 0.075 Uiso 0.255(6) 1 calc R U P A -2
C6_3 C 0.261(3) 0.150(2) 0.466(3) 0.060(4) Uani 0.255(6) 1 d D U P A -2
H6_3 H 0.230436 0.046719 0.503418 0.072 Uiso 0.255(6) 1 calc R U P A -2
C1_1 C 0.167(2) 0.164(2) 0.4513(19) 0.051(3) Uani 0.245(6) 1 d D U P A -1
C2_1 C 0.277(2) 0.156(2) 0.348(2) 0.049(3) Uani 0.245(6) 1 d D U P A -1
H2_1 H 0.260833 0.057284 0.309850 0.059 Uiso 0.245(6) 1 calc R U P A -1
C3_1 C 0.410(2) 0.294(2) 0.303(3) 0.058(4) Uani 0.245(6) 1 d D U P A -1
H3_1 H 0.483607 0.289381 0.229827 0.070 Uiso 0.245(6) 1 calc R U P A -1
C4_1 C 0.438(3) 0.439(2) 0.360(2) 0.060(3) Uani 0.245(6) 1 d D U P A -1
H4_1 H 0.532865 0.531405 0.331911 0.072 Uiso 0.245(6) 1 calc R U P A -1
C5_1 C 0.327(2) 0.447(2) 0.460(3) 0.052(3) Uani 0.245(6) 1 d D U P A -1
H5_1 H 0.343506 0.546125 0.498144 0.063 Uiso 0.245(6) 1 calc R U P A -1
C6_1 C 0.191(2) 0.309(2) 0.503(3) 0.051(4) Uani 0.245(6) 1 d D U P A -1
H6_1 H 0.114025 0.314443 0.569808 0.061 Uiso 0.245(6) 1 calc R U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 B11 1.40(2) 4 ?
B1 C1_3 1.653(13) . ?
B1 P11 1.880(17) 4 ?
B1 C1_1 1.927(19) . ?
B1 P11 2.129(17) . ?
B11 P1 1.877(17) 4_554 ?
B11 P1 2.132(17) . ?
P1 P11 1.651(8) . ?
P1 C1_3 1.790(13) . ?
P1 C1_1 2.222(18) . ?
P1 P11 2.358(8) 4 ?
C1_3 C6_3 1.39(2) . ?
C1_3 C2_3 1.391(19) . ?
C2_3 C3_3 1.383(17) . ?
C3_3 C4_3 1.379(19) . ?
C4_3 C5_3 1.372(18) . ?
C5_3 C6_3 1.387(16) . ?
C1_1 C6_1 1.39(2) . ?
C1_1 C2_1 1.397(19) . ?
C2_1 C3_1 1.380(17) . ?
C3_1 C4_1 1.39(2) . ?
C4_1 C5_1 1.39(2) . ?
C5_1 C6_1 1.389(18) . ?

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
B11 B1 C1_3 81.2(9) 4 . ?
B11 B1 P11 0.000(2) 4 4 ?
C1_3 B1 P11 81.2(9) . 4 ?
B11 B1 C1_1 57.4(7) 4 . ?
P11 B1 C1_1 57.4(7) 4 . ?
B11 B1 P11 180.0 4 . ?
C1_3 B1 P11 98.8(9) . . ?
P11 B1 P11 180.0 4 . ?
C1_1 B1 P11 122.6(7) . . ?
B1 B11 P1 0.000(1) 4_554 4_554 ?
B1 B11 P1 180.0 4_554 . ?
P1 B11 P1 180.0 4_554 . ?
P11 P1 C1_3 114.1(6) . . ?
P11 P1 B11 180.0 . 4 ?
P11 P1 B11 0.0 . . ?
C1_3 P1 B11 114.1(6) . . ?
B11 P1 B11 180.0 4 . ?
P11 P1 C1_1 133.1(4) . . ?
B11 P1 C1_1 46.9(4) 4 . ?
B11 P1 C1_1 133.1(4) . . ?
P11 P1 P11 180.0 . 4 ?
C1_3 P1 P11 65.9(6) . 4 ?
B11 P1 P11 0.000(2) 4 4 ?
B11 P1 P11 180.0 . 4 ?
C1_1 P1 P11 46.9(4) . 4 ?
P1 P11 B1 180.0 . 4_554 ?
P1 P11 B1 0.000(1) . . ?
B1 P11 B1 180.0 4_554 . ?
P1 P11 P1 180.0 . 4_554 ?
B1 P11 P1 0.000(1) 4_554 4_554 ?
B1 P11 P1 180.0 . 4_554 ?
C6_3 C1_3 C2_3 116.2(14) . . ?
C6_3 C1_3 B1 111.0(16) . . ?
C2_3 C1_3 B1 132.3(19) . . ?
C6_3 C1_3 P1 120.3(17) . . ?
C2_3 C1_3 P1 123.1(16) . . ?
B1 C1_3 P1 15.3(6) . . ?
C3_3 C2_3 C1_3 120.4(15) . . ?
C4_3 C3_3 C2_3 122.6(15) . . ?
C5_3 C4_3 C3_3 117.6(13) . . ?
C4_3 C5_3 C6_3 119.9(16) . . ?
C5_3 C6_3 C1_3 123.2(17) . . ?
C6_1 C1_1 C2_1 119.6(14) . . ?
C6_1 C1_1 B1 131(2) . . ?
C2_1 C1_1 B1 89.6(13) . . ?
C6_1 C1_1 P1 129.5(19) . . ?
C2_1 C1_1 P1 82.3(12) . . ?
B1 C1_1 P1 10.4(5) . . ?
C3_1 C2_1 C1_1 118.7(16) . . ?
C2_1 C3_1 C4_1 121.8(15) . . ?
C3_1 C4_1 C5_1 119.7(14) . . ?
C6_1 C5_1 C4_1 118.8(15) . . ?
C5_1 C6_1 C1_1 121.3(15) . . ?

_refine_diff_density_max         0.080
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.023



