# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_KB1056_0m
_database_code_depnum_ccdc_archive 'CCDC 2443592'
loop_
_audit_author_name
_audit_author_address
'Jagadeesh Babu Nanubolu'
;CSIR Indian Institute of Chemical Technology
India
;
_audit_update_record             
;
2025-04-14 deposited with the CCDC.	2025-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H29 B O4'
_chemical_formula_sum            'C23 H29 B O4'
_chemical_formula_weight         380.27

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   6.6993(11)
_cell_length_b                   14.819(2)
_cell_length_c                   21.974(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2181.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    8366
_cell_measurement_theta_min      2.307
_cell_measurement_theta_max      30.345

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.077
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6697
_exptl_absorpt_correction_T_max  0.7461
_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      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON III C7 HPAD'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19760
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.749
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4996
_reflns_number_gt                3485
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0537P)²+0.0860P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1088 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.5(4)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         4996
_refine_ls_number_parameters     331
_refine_ls_number_restraints     300
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.1022
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.124
_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
O1 O -0.0249(2) 0.26169(17) 0.41093(8) 0.0725(6) Uani 1 1 d . . . . .
O2 O 0.6397(2) 0.20005(12) 0.34375(9) 0.0558(5) Uani 1 1 d . . . . .
H2O H 0.731(5) 0.229(2) 0.3688(13) 0.082(11) Uiso 1 1 d . . . . .
C1 C 0.1159(3) 0.23614(18) 0.38124(11) 0.0451(6) Uani 1 1 d . . . . .
C2 C 0.1045(4) 0.2019(2) 0.31663(11) 0.0535(7) Uani 1 1 d . . . . .
H2A H 0.039305 0.245765 0.290618 0.064 Uiso 1 1 calc R U . . .
H2B H 0.030275 0.145736 0.314903 0.064 Uiso 1 1 calc R U . . .
C3 C 0.3206(3) 0.18711(18) 0.29646(12) 0.0503(6) Uani 1 1 d . . . . .
H3A H 0.354090 0.123434 0.297101 0.060 Uiso 1 1 calc R U . . .
H3B H 0.341381 0.210115 0.255616 0.060 Uiso 1 1 calc R U . . .
C4 C 0.4467(3) 0.23891(16) 0.34209(11) 0.0395(5) Uani 1 1 d . . . . .
C5 C 0.3321(3) 0.23544(16) 0.40328(10) 0.0400(5) Uani 1 1 d . . . . .
C6 C 0.3659(4) 0.14835(17) 0.43922(13) 0.0591(7) Uani 1 1 d . . . . .
H6A H 0.318414 0.097889 0.415957 0.089 Uiso 1 1 calc R U . . .
H6B H 0.294563 0.151430 0.477056 0.089 Uiso 1 1 calc R U . . .
H6C H 0.505847 0.141086 0.447193 0.089 Uiso 1 1 calc R U . . .
C7 C 0.3876(4) 0.32063(17) 0.43874(10) 0.0506(6) Uani 1 1 d . . . . .
H7A H 0.483010 0.306381 0.470510 0.061 Uiso 1 1 calc R U . . .
H7B H 0.269780 0.346731 0.457424 0.061 Uiso 1 1 calc R U . . .
C8 C 0.4806(3) 0.38801(16) 0.39229(10) 0.0416(6) Uani 1 1 d . . . . .
H8 H 0.623545 0.394949 0.400559 0.050 Uiso 1 1 calc R U . . .
C9 C 0.4507(4) 0.34167(15) 0.32942(10) 0.0413(6) Uani 1 1 d . . . . .
H9 H 0.317609 0.358583 0.314852 0.050 Uiso 1 1 calc R U . . .
C10 C 0.5936(4) 0.36966(16) 0.28284(11) 0.0484(6) Uani 1 1 d . . . . .
C11 C 0.7101(4) 0.39305(16) 0.24482(12) 0.0503(6) Uani 1 1 d . . . . .
C12 C 0.8545(4) 0.42033(15) 0.19989(11) 0.0468(6) Uani 1 1 d . . . . .
C13 C 0.8089(5) 0.42068(18) 0.13837(12) 0.0585(7) Uani 1 1 d . . . . .
H13 H 0.682862 0.402649 0.125467 0.070 Uiso 1 1 calc R U . . .
C14 C 0.9498(6) 0.4477(2) 0.09594(14) 0.0775(10) Uani 1 1 d . . . . .
H14 H 0.918129 0.447615 0.054729 0.093 Uiso 1 1 calc R U . . .
C15 C 1.1351(7) 0.4745(2) 0.1146(2) 0.0904(12) Uani 1 1 d . . . . .
H15 H 1.229242 0.492645 0.086027 0.109 Uiso 1 1 calc R U . . .
C16 C 1.1830(5) 0.4746(2) 0.1755(2) 0.0885(11) Uani 1 1 d . . . . .
H16 H 1.308962 0.493104 0.188123 0.106 Uiso 1 1 calc R U . . .
C17 C 1.0439(5) 0.44742(19) 0.21732(14) 0.0647(8) Uani 1 1 d . . . . .
H17 H 1.077534 0.447116 0.258386 0.078 Uiso 1 1 calc R U . . .
B1 B 0.3756(4) 0.48190(19) 0.39609(12) 0.0437(6) Uani 1 1 d . U . . .
O3 O 0.3978(12) 0.5400(5) 0.4419(3) 0.0725(18) Uani 0.600(7) 1 d D U P A 1
O4 O 0.2401(13) 0.5102(5) 0.3535(3) 0.0600(17) Uani 0.600(7) 1 d D U P A 1
C18 C 0.1274(11) 0.5845(5) 0.3896(3) 0.0658(17) Uani 0.600(7) 1 d D U P A 1
C19 C 0.0431(18) 0.6423(7) 0.3344(5) 0.120(3) Uani 0.600(7) 1 d D U P A 1
H19A H 0.149087 0.654903 0.306241 0.180 Uiso 0.600(7) 1 calc R U P A 1
H19B H -0.060169 0.608999 0.314072 0.180 Uiso 0.600(7) 1 calc R U P A 1
H19C H -0.010646 0.698047 0.349503 0.180 Uiso 0.600(7) 1 calc R U P A 1
C20 C -0.0221(12) 0.5614(7) 0.4354(5) 0.113(3) Uani 0.600(7) 1 d D U P A 1
H20A H -0.133567 0.532439 0.416084 0.170 Uiso 0.600(7) 1 calc R U P A 1
H20B H 0.035577 0.521161 0.464793 0.170 Uiso 0.600(7) 1 calc R U P A 1
H20C H -0.066519 0.615328 0.455417 0.170 Uiso 0.600(7) 1 calc R U P A 1
C21 C 0.3186(8) 0.6318(3) 0.4124(3) 0.0553(13) Uani 0.600(7) 1 d D U P A 1
C22 C 0.4466(14) 0.6832(5) 0.3698(5) 0.124(3) Uani 0.600(7) 1 d D U P A 1
H22A H 0.558214 0.708000 0.391569 0.187 Uiso 0.600(7) 1 calc R U P A 1
H22B H 0.494156 0.643701 0.338391 0.187 Uiso 0.600(7) 1 calc R U P A 1
H22C H 0.370606 0.731272 0.351922 0.187 Uiso 0.600(7) 1 calc R U P A 1
C23 C 0.274(3) 0.6861(11) 0.4726(6) 0.099(4) Uani 0.600(7) 1 d D U P A 1
H23A H 0.190839 0.650443 0.498852 0.149 Uiso 0.600(7) 1 calc R U P A 1
H23B H 0.397260 0.699503 0.492971 0.149 Uiso 0.600(7) 1 calc R U P A 1
H23C H 0.206679 0.741346 0.462683 0.149 Uiso 0.600(7) 1 calc R U P A 1
O4D O 0.1928(18) 0.4954(7) 0.3714(5) 0.059(2) Uani 0.400(7) 1 d D U P A 2
O3D O 0.4449(14) 0.5586(7) 0.4254(5) 0.0513(19) Uani 0.400(7) 1 d D U P A 2
C18D C 0.1782(17) 0.6002(7) 0.3683(5) 0.062(2) Uani 0.400(7) 1 d D U P A 2
C19D C -0.0448(17) 0.6107(9) 0.3504(6) 0.081(3) Uani 0.400(7) 1 d D U P A 2
H19D H -0.058186 0.605742 0.307071 0.121 Uiso 0.400(7) 1 calc R U P A 2
H19E H -0.121775 0.564085 0.369718 0.121 Uiso 0.400(7) 1 calc R U P A 2
H19F H -0.092369 0.668626 0.363486 0.121 Uiso 0.400(7) 1 calc R U P A 2
C20D C 0.326(2) 0.6613(7) 0.3318(5) 0.099(3) Uani 0.400(7) 1 d D U P A 2
H20D H 0.295910 0.657497 0.289143 0.148 Uiso 0.400(7) 1 calc R U P A 2
H20E H 0.312522 0.722749 0.345068 0.148 Uiso 0.400(7) 1 calc R U P A 2
H20F H 0.460413 0.641313 0.338694 0.148 Uiso 0.400(7) 1 calc R U P A 2
C21D C 0.2255(15) 0.6062(6) 0.4352(4) 0.070(2) Uani 0.400(7) 1 d D U P A 2
C22D C 0.0363(19) 0.5690(10) 0.4708(5) 0.096(4) Uani 0.400(7) 1 d D U P A 2
H22D H 0.060781 0.571780 0.513800 0.145 Uiso 0.400(7) 1 calc R U P A 2
H22E H -0.078161 0.605177 0.460998 0.145 Uiso 0.400(7) 1 calc R U P A 2
H22F H 0.011915 0.507581 0.459090 0.145 Uiso 0.400(7) 1 calc R U P A 2
C23D C 0.303(5) 0.6978(16) 0.4558(10) 0.086(4) Uani 0.400(7) 1 d D U P A 2
H23D H 0.329738 0.696260 0.498669 0.129 Uiso 0.400(7) 1 calc R U P A 2
H23E H 0.424020 0.711686 0.434208 0.129 Uiso 0.400(7) 1 calc R U P A 2
H23F H 0.204835 0.743222 0.447322 0.129 Uiso 0.400(7) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.208(3) . ?
O2 C4 1.416(3) . ?
O2 H2O 0.93(3) . ?
C1 C2 1.510(3) . ?
C1 C5 1.527(3) . ?
C2 C3 1.530(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.519(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C9 1.548(3) . ?
C4 C5 1.549(3) . ?
C5 C7 1.529(3) . ?
C5 C6 1.530(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.558(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.556(3) . ?
C8 B1 1.561(4) . ?
C8 H8 0.9800 . ?
C9 C10 1.461(3) . ?
C9 H9 0.9800 . ?
C10 C11 1.195(3) . ?
C11 C12 1.440(4) . ?
C12 C17 1.385(4) . ?
C12 C13 1.386(4) . ?
C13 C14 1.386(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.366(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.375(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.370(4) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
B1 O3 1.332(8) . ?
B1 O4D 1.354(13) . ?
B1 O4 1.369(9) . ?
B1 O3D 1.387(11) . ?
O3 C21 1.598(8) . ?
O4 C18 1.552(11) . ?
C18 C20 1.461(11) . ?
C18 C21 1.545(10) . ?
C18 C19 1.589(11) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.480(9) . ?
C21 C23 1.576(13) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
O4D C18D 1.558(15) . ?
O3D C21D 1.644(13) . ?
C18D C21D 1.507(16) . ?
C18D C19D 1.552(15) . ?
C18D C20D 1.564(13) . ?
C19D H19D 0.9600 . ?
C19D H19E 0.9600 . ?
C19D H19F 0.9600 . ?
C20D H20D 0.9600 . ?
C20D H20E 0.9600 . ?
C20D H20F 0.9600 . ?
C21D C23D 1.52(2) . ?
C21D C22D 1.588(15) . ?
C22D H22D 0.9600 . ?
C22D H22E 0.9600 . ?
C22D H22F 0.9600 . ?
C23D H23D 0.9600 . ?
C23D H23E 0.9600 . ?
C23D H23F 0.9600 . ?

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
C4 O2 H2O 116(2) . . ?
O1 C1 C2 125.0(2) . . ?
O1 C1 C5 124.8(2) . . ?
C2 C1 C5 110.13(19) . . ?
C1 C2 C3 105.82(19) . . ?
C1 C2 H2A 110.6 . . ?
C3 C2 H2A 110.6 . . ?
C1 C2 H2B 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
C4 C3 C2 105.22(18) . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3B 110.7 . . ?
C2 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
O2 C4 C3 108.61(19) . . ?
O2 C4 C9 112.88(18) . . ?
C3 C4 C9 112.8(2) . . ?
O2 C4 C5 114.63(19) . . ?
C3 C4 C5 106.30(18) . . ?
C9 C4 C5 101.38(18) . . ?
C1 C5 C7 112.7(2) . . ?
C1 C5 C6 108.0(2) . . ?
C7 C5 C6 113.42(19) . . ?
C1 C5 C4 101.21(17) . . ?
C7 C5 C4 107.12(19) . . ?
C6 C5 C4 113.7(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 C8 107.01(18) . . ?
C5 C7 H7A 110.3 . . ?
C8 C7 H7A 110.3 . . ?
C5 C7 H7B 110.3 . . ?
C8 C7 H7B 110.3 . . ?
H7A C7 H7B 108.6 . . ?
C9 C8 C7 104.32(18) . . ?
C9 C8 B1 112.50(19) . . ?
C7 C8 B1 110.8(2) . . ?
C9 C8 H8 109.7 . . ?
C7 C8 H8 109.7 . . ?
B1 C8 H8 109.7 . . ?
C10 C9 C4 114.61(19) . . ?
C10 C9 C8 114.35(19) . . ?
C4 C9 C8 106.06(18) . . ?
C10 C9 H9 107.1 . . ?
C4 C9 H9 107.1 . . ?
C8 C9 H9 107.1 . . ?
C11 C10 C9 179.6(3) . . ?
C10 C11 C12 178.6(3) . . ?
C17 C12 C13 118.1(3) . . ?
C17 C12 C11 120.5(2) . . ?
C13 C12 C11 121.5(3) . . ?
C14 C13 C12 120.5(3) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 120.0(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 119.6(3) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C12 121.5(3) . . ?
C16 C17 H17 119.2 . . ?
C12 C17 H17 119.2 . . ?
O3 B1 O4 113.1(5) . . ?
O4D B1 O3D 111.6(7) . . ?
O3 B1 C8 124.5(4) . . ?
O4D B1 C8 121.2(5) . . ?
O4 B1 C8 122.4(4) . . ?
O3D B1 C8 127.2(5) . . ?
B1 O3 C21 102.0(5) . . ?
B1 O4 C18 101.0(6) . . ?
C20 C18 C21 116.8(7) . . ?
C20 C18 O4 121.3(7) . . ?
C21 C18 O4 94.9(6) . . ?
C20 C18 C19 114.1(7) . . ?
C21 C18 C19 107.3(8) . . ?
O4 C18 C19 99.6(7) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C18 120.6(7) . . ?
C22 C21 C23 112.2(8) . . ?
C18 C21 C23 110.3(9) . . ?
C22 C21 O3 120.1(5) . . ?
C18 C21 O3 91.1(5) . . ?
C23 C21 O3 99.1(8) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
B1 O4D C18D 102.8(9) . . ?
B1 O3D C21D 96.5(7) . . ?
C21D C18D C19D 116.3(10) . . ?
C21D C18D O4D 90.2(8) . . ?
C19D C18D O4D 99.9(10) . . ?
C21D C18D C20D 109.5(10) . . ?
C19D C18D C20D 114.9(9) . . ?
O4D C18D C20D 124.1(10) . . ?
C18D C19D H19D 109.5 . . ?
C18D C19D H19E 109.5 . . ?
H19D C19D H19E 109.5 . . ?
C18D C19D H19F 109.5 . . ?
H19D C19D H19F 109.5 . . ?
H19E C19D H19F 109.5 . . ?
C18D C20D H20D 109.5 . . ?
C18D C20D H20E 109.5 . . ?
H20D C20D H20E 109.5 . . ?
C18D C20D H20F 109.5 . . ?
H20D C20D H20F 109.5 . . ?
H20E C20D H20F 109.5 . . ?
C18D C21D C23D 114.5(12) . . ?
C18D C21D C22D 107.0(9) . . ?
C23D C21D C22D 115.9(12) . . ?
C18D C21D O3D 92.0(8) . . ?
C23D C21D O3D 96.6(15) . . ?
C22D C21D O3D 129.0(8) . . ?
C21D C22D H22D 109.5 . . ?
C21D C22D H22E 109.5 . . ?
H22D C22D H22E 109.5 . . ?
C21D C22D H22F 109.5 . . ?
H22D C22D H22F 109.5 . . ?
H22E C22D H22F 109.5 . . ?
C21D C23D H23D 109.5 . . ?
C21D C23D H23E 109.5 . . ?
H23D C23D H23E 109.5 . . ?
C21D C23D H23F 109.5 . . ?
H23D C23D H23F 109.5 . . ?
H23E C23D H23F 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
O1 C1 C2 C3 174.3(3) . . . . ?
C5 C1 C2 C3 -4.7(3) . . . . ?
C1 C2 C3 C4 -16.4(3) . . . . ?
C2 C3 C4 O2 155.3(2) . . . . ?
C2 C3 C4 C9 -78.7(3) . . . . ?
C2 C3 C4 C5 31.5(3) . . . . ?
O1 C1 C5 C7 -41.7(4) . . . . ?
C2 C1 C5 C7 137.3(2) . . . . ?
O1 C1 C5 C6 84.4(3) . . . . ?
C2 C1 C5 C6 -96.6(2) . . . . ?
O1 C1 C5 C4 -155.8(3) . . . . ?
C2 C1 C5 C4 23.2(3) . . . . ?
O2 C4 C5 C1 -153.2(2) . . . . ?
C3 C4 C5 C1 -33.2(2) . . . . ?
C9 C4 C5 C1 84.9(2) . . . . ?
O2 C4 C5 C7 88.6(2) . . . . ?
C3 C4 C5 C7 -151.5(2) . . . . ?
C9 C4 C5 C7 -33.4(2) . . . . ?
O2 C4 C5 C6 -37.6(3) . . . . ?
C3 C4 C5 C6 82.4(2) . . . . ?
C9 C4 C5 C6 -159.5(2) . . . . ?
C1 C5 C7 C8 -93.5(2) . . . . ?
C6 C5 C7 C8 143.3(2) . . . . ?
C4 C5 C7 C8 16.9(2) . . . . ?
C5 C7 C8 C9 6.6(2) . . . . ?
C5 C7 C8 B1 127.9(2) . . . . ?
O2 C4 C9 C10 41.6(3) . . . . ?
C3 C4 C9 C10 -82.0(2) . . . . ?
C5 C4 C9 C10 164.70(18) . . . . ?
O2 C4 C9 C8 -85.6(2) . . . . ?
C3 C4 C9 C8 150.84(18) . . . . ?
C5 C4 C9 C8 37.6(2) . . . . ?
C7 C8 C9 C10 -155.1(2) . . . . ?
B1 C8 C9 C10 84.7(3) . . . . ?
C7 C8 C9 C4 -27.8(2) . . . . ?
B1 C8 C9 C4 -148.0(2) . . . . ?
C17 C12 C13 C14 -0.2(4) . . . . ?
C11 C12 C13 C14 179.6(2) . . . . ?
C12 C13 C14 C15 -0.1(5) . . . . ?
C13 C14 C15 C16 0.1(6) . . . . ?
C14 C15 C16 C17 0.3(6) . . . . ?
C15 C16 C17 C12 -0.6(5) . . . . ?
C13 C12 C17 C16 0.6(4) . . . . ?
C11 C12 C17 C16 -179.2(3) . . . . ?
C9 C8 B1 O3 -171.6(5) . . . . ?
C7 C8 B1 O3 72.1(5) . . . . ?
C9 C8 B1 O4D 40.1(6) . . . . ?
C7 C8 B1 O4D -76.3(6) . . . . ?
C9 C8 B1 O4 12.6(5) . . . . ?
C7 C8 B1 O4 -103.8(4) . . . . ?
C9 C8 B1 O3D -142.8(5) . . . . ?
C7 C8 B1 O3D 100.8(5) . . . . ?
O4 B1 O3 C21 -21.2(6) . . . . ?
C8 B1 O3 C21 162.6(4) . . . . ?
O3 B1 O4 C18 -16.9(6) . . . . ?
C8 B1 O4 C18 159.4(4) . . . . ?
B1 O4 C18 C20 -77.1(8) . . . . ?
B1 O4 C18 C21 48.4(6) . . . . ?
B1 O4 C18 C19 156.9(6) . . . . ?
C20 C18 C21 C22 -160.4(7) . . . . ?
O4 C18 C21 C22 70.7(6) . . . . ?
C19 C18 C21 C22 -30.9(8) . . . . ?
C20 C18 C21 C23 -27.0(11) . . . . ?
O4 C18 C21 C23 -155.9(8) . . . . ?
C19 C18 C21 C23 102.5(10) . . . . ?
C20 C18 C21 O3 73.1(7) . . . . ?
O4 C18 C21 O3 -55.8(6) . . . . ?
C19 C18 C21 O3 -157.4(6) . . . . ?
B1 O3 C21 C22 -77.4(7) . . . . ?
B1 O3 C21 C18 49.5(7) . . . . ?
B1 O3 C21 C23 160.3(8) . . . . ?
O3D B1 O4D C18D 19.0(9) . . . . ?
C8 B1 O4D C18D -163.5(6) . . . . ?
O4D B1 O3D C21D 21.3(8) . . . . ?
C8 B1 O3D C21D -156.1(5) . . . . ?
B1 O4D C18D C21D -54.0(9) . . . . ?
B1 O4D C18D C19D -170.8(8) . . . . ?
B1 O4D C18D C20D 59.9(13) . . . . ?
C19D C18D C21D C23D -99.3(18) . . . . ?
O4D C18D C21D C23D 159.6(16) . . . . ?
C20D C18D C21D C23D 33.1(18) . . . . ?
C19D C18D C21D C22D 30.6(12) . . . . ?
O4D C18D C21D C22D -70.5(9) . . . . ?
C20D C18D C21D C22D 162.9(9) . . . . ?
C19D C18D C21D O3D 162.5(9) . . . . ?
O4D C18D C21D O3D 61.4(9) . . . . ?
C20D C18D C21D O3D -65.1(9) . . . . ?
B1 O3D C21D C18D -54.5(8) . . . . ?
B1 O3D C21D C23D -169.4(10) . . . . ?
B1 O3D C21D C22D 59.3(12) . . . . ?

_refine_diff_density_max         0.164
_refine_diff_density_min         -0.123
_refine_diff_density_rms         0.026


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Isopropanol and Dichloromethane'
####################################################################### 
# 
# 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_KB1112_0m
_database_code_depnum_ccdc_archive 'CCDC 2443593'
loop_
_audit_author_name
_audit_author_address
'Jagadeesh Babu Nanubolu'
;CSIR Indian Institute of Chemical Technology
India
;
_audit_update_record             
;
2025-04-14 deposited with the CCDC.	2025-07-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H32 B Br O4'
_chemical_formula_sum            'C29 H32 B Br O4'
_chemical_formula_weight         535.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   6.661(2)
_cell_length_b                   19.722(5)
_cell_length_c                   20.481(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2690.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    8684
_cell_measurement_theta_min      2.862
_cell_measurement_theta_max      19.934

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.560
_shelx_estimated_absorpt_T_min   0.696
_shelx_estimated_absorpt_T_max   0.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5721
_exptl_absorpt_correction_T_max  0.7461
_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      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON III C7 HPAD'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32534
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.868
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6169
_reflns_number_gt                3313
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0552P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1055 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(5)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         6169
_refine_ls_number_parameters     401
_refine_ls_number_restraints     279
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1278
_refine_ls_wR_factor_gt          0.1034
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.020
_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
Br1 Br 0.53509(13) 0.38657(3) 0.61348(3) 0.0988(3) Uani 1 1 d . . . . .
O1 O 1.0977(5) 0.70366(18) 0.59039(15) 0.0607(10) Uani 1 1 d . . . . .
O2 O 0.4307(4) 0.63520(16) 0.64206(15) 0.0458(8) Uani 1 1 d D . . . .
H2O H 0.346(7) 0.657(3) 0.618(2) 0.08(2) Uiso 1 1 d D . . . .
C1 C 0.9554(6) 0.6754(2) 0.6157(2) 0.0407(10) Uani 1 1 d . . . . .
C2 C 0.9653(6) 0.6295(2) 0.6732(2) 0.0454(11) Uani 1 1 d . . . . .
H2A H 1.033699 0.651589 0.709238 0.054 Uiso 1 1 calc R U . . .
H2B H 1.037369 0.588274 0.662324 0.054 Uiso 1 1 calc R U . . .
C3 C 0.7494(6) 0.6133(2) 0.69174(19) 0.0406(10) Uani 1 1 d . . . . .
H3A H 0.715460 0.567143 0.679587 0.049 Uiso 1 1 calc R U . . .
H3B H 0.729181 0.618623 0.738361 0.049 Uiso 1 1 calc R U . . .
C4 C 0.6222(6) 0.6637(2) 0.6539(2) 0.0358(10) Uani 1 1 d . . . . .
C5 C 0.7400(6) 0.6828(2) 0.59207(18) 0.0347(10) Uani 1 1 d . . . . .
C6 C 0.7090(7) 0.6361(2) 0.5314(2) 0.0470(12) Uani 1 1 d . . . . .
H6A H 0.567633 0.636958 0.520074 0.056 Uiso 1 1 calc R U . . .
H6B H 0.781922 0.655860 0.495049 0.056 Uiso 1 1 calc R U . . .
C7 C 0.7721(8) 0.5633(2) 0.5375(2) 0.0498(12) Uani 1 1 d . . . . .
C8 C 0.9622(9) 0.5431(3) 0.5187(2) 0.0717(15) Uani 1 1 d . . . . .
H8 H 1.050790 0.574409 0.500788 0.086 Uiso 1 1 calc R U . . .
C9 C 1.0220(11) 0.4752(4) 0.5266(3) 0.096(2) Uani 1 1 d . . . . .
H9 H 1.149112 0.461502 0.513154 0.115 Uiso 1 1 calc R U . . .
C10 C 0.8943(12) 0.4295(3) 0.5539(3) 0.090(2) Uani 1 1 d . . . . .
H10 H 0.934546 0.384800 0.559974 0.108 Uiso 1 1 calc R U . . .
C11 C 0.7089(9) 0.4495(3) 0.5721(2) 0.0614(14) Uani 1 1 d . . . . .
C12 C 0.6427(8) 0.5156(2) 0.5640(2) 0.0518(13) Uani 1 1 d . . . . .
H12 H 0.513216 0.527749 0.576313 0.062 Uiso 1 1 calc R U . . .
C13 C 0.6858(7) 0.7559(2) 0.5750(2) 0.0454(11) Uani 1 1 d . . . . .
H13A H 0.592014 0.756909 0.538814 0.055 Uiso 1 1 calc R U . . .
H13B H 0.805322 0.780886 0.562575 0.055 Uiso 1 1 calc R U . . .
C14 C 0.5887(7) 0.7884(2) 0.6369(2) 0.0427(11) Uani 1 1 d . . . . .
H14 H 0.445889 0.796810 0.628695 0.051 Uiso 1 1 calc R U . . .
C15 C 0.6114(6) 0.7325(2) 0.68967(19) 0.0394(11) Uani 1 1 d . . . . .
H15 H 0.742976 0.739499 0.709998 0.047 Uiso 1 1 calc R U . . .
C16 C 0.4651(7) 0.7331(2) 0.7423(2) 0.0476(11) Uani 1 1 d . . . . .
C17 C 0.3482(7) 0.7303(2) 0.7859(2) 0.0502(12) Uani 1 1 d . . . . .
C18 C 0.2042(8) 0.7255(2) 0.8380(2) 0.0491(12) Uani 1 1 d . . . . .
C19 C 0.2587(8) 0.6939(3) 0.8963(3) 0.0671(15) Uani 1 1 d . . . . .
H19 H 0.388722 0.677562 0.901575 0.081 Uiso 1 1 calc R U . . .
C20 C 0.1227(11) 0.6867(3) 0.9458(3) 0.0822(19) Uani 1 1 d . . . . .
H20 H 0.161066 0.665465 0.984367 0.099 Uiso 1 1 calc R U . . .
C21 C -0.0632(12) 0.7096(3) 0.9393(3) 0.088(2) Uani 1 1 d . . . . .
H21 H -0.154435 0.703687 0.973227 0.106 Uiso 1 1 calc R U . . .
C22 C -0.1240(8) 0.7425(3) 0.8825(4) 0.0850(19) Uani 1 1 d . . . . .
H22 H -0.254613 0.758572 0.878558 0.102 Uiso 1 1 calc R U . . .
C23 C 0.0127(8) 0.7510(3) 0.8314(2) 0.0643(14) Uani 1 1 d . . . . .
H23 H -0.024991 0.773681 0.793510 0.077 Uiso 1 1 calc R U . . .
O3 O 0.6764(12) 0.9145(3) 0.6264(3) 0.0794(19) Uani 0.755(7) 1 d . U P A 1
O4 O 0.8217(10) 0.8578(3) 0.7094(3) 0.0663(16) Uani 0.755(7) 1 d . U P A 1
C24 C 0.7932(13) 0.9649(4) 0.6621(4) 0.073(2) Uani 0.755(7) 1 d D U P A 1
C25 C 0.9320(19) 1.0070(6) 0.6142(6) 0.108(4) Uani 0.755(7) 1 d D U P A 1
H25A H 1.010901 0.976409 0.588231 0.162 Uiso 0.755(7) 1 calc R U P A 1
H25B H 1.019399 1.035737 0.639097 0.162 Uiso 0.755(7) 1 calc R U P A 1
H25C H 0.849775 1.034307 0.586050 0.162 Uiso 0.755(7) 1 calc R U P A 1
C26 C 0.6466(14) 1.0064(5) 0.6989(6) 0.102(3) Uani 0.755(7) 1 d D U P A 1
H26A H 0.570745 1.033758 0.668943 0.153 Uiso 0.755(7) 1 calc R U P A 1
H26B H 0.716802 1.035301 0.728947 0.153 Uiso 0.755(7) 1 calc R U P A 1
H26C H 0.557284 0.977229 0.722576 0.153 Uiso 0.755(7) 1 calc R U P A 1
C27 C 0.9343(13) 0.9208(4) 0.7035(4) 0.0633(18) Uani 0.755(7) 1 d . U P A 1
C28 C 0.9924(18) 0.9432(6) 0.7706(5) 0.096(3) Uani 0.755(7) 1 d . U P A 1
H28A H 1.104596 0.916816 0.785458 0.144 Uiso 0.755(7) 1 calc R U P A 1
H28B H 0.881055 0.936807 0.799721 0.144 Uiso 0.755(7) 1 calc R U P A 1
H28C H 1.028741 0.990252 0.769664 0.144 Uiso 0.755(7) 1 calc R U P A 1
C29 C 1.1312(15) 0.8968(7) 0.6732(6) 0.110(4) Uani 0.755(7) 1 d . U P A 1
H29A H 1.103253 0.868637 0.636148 0.165 Uiso 0.755(7) 1 calc R U P A 1
H29B H 1.206020 0.871412 0.704957 0.165 Uiso 0.755(7) 1 calc R U P A 1
H29C H 1.208401 0.935446 0.659614 0.165 Uiso 0.755(7) 1 calc R U P A 1
O3D O 0.800(3) 0.8988(9) 0.6130(9) 0.071(3) Uani 0.245(7) 1 d . U P A 2
O4D O 0.717(3) 0.8768(10) 0.7149(10) 0.070(3) Uani 0.245(7) 1 d . U P A 2
C24D C 0.909(4) 0.9510(12) 0.6525(15) 0.076(3) Uani 0.245(7) 1 d D U P A 2
C25D C 0.835(6) 1.0209(14) 0.629(2) 0.098(6) Uani 0.245(7) 1 d D U P A 2
H25D H 0.777162 1.016786 0.586649 0.148 Uiso 0.245(7) 1 calc R U P A 2
H25E H 0.945335 1.052031 0.628072 0.148 Uiso 0.245(7) 1 calc R U P A 2
H25F H 0.734766 1.037460 0.659259 0.148 Uiso 0.245(7) 1 calc R U P A 2
C27D C 0.816(4) 0.9425(12) 0.7149(13) 0.071(3) Uani 0.245(7) 1 d D U P A 2
C26D C 1.109(4) 0.9197(17) 0.6389(17) 0.090(6) Uani 0.245(7) 1 d D U P A 2
H26D H 1.096371 0.871192 0.638820 0.134 Uiso 0.245(7) 1 calc R U P A 2
H26E H 1.202851 0.933061 0.672141 0.134 Uiso 0.245(7) 1 calc R U P A 2
H26F H 1.156766 0.934632 0.597095 0.134 Uiso 0.245(7) 1 calc R U P A 2
C29D C 0.648(4) 0.9851(15) 0.7402(16) 0.085(4) Uani 0.245(7) 1 d D U P A 2
H29D H 0.701302 1.023183 0.763561 0.128 Uiso 0.245(7) 1 calc R U P A 2
H29E H 0.565405 0.958527 0.768970 0.128 Uiso 0.245(7) 1 calc R U P A 2
H29F H 0.567781 1.000981 0.704263 0.128 Uiso 0.245(7) 1 calc R U P A 2
C28D C 0.908(5) 0.957(2) 0.7793(15) 0.080(4) Uani 0.245(7) 1 d D U P A 2
H28D H 0.952111 0.915289 0.798915 0.119 Uiso 0.245(7) 1 calc R U P A 2
H28E H 0.811388 0.978421 0.807198 0.119 Uiso 0.245(7) 1 calc R U P A 2
H28F H 1.021422 0.986538 0.773549 0.119 Uiso 0.245(7) 1 calc R U P A 2
B1 B 0.6917(8) 0.8550(3) 0.6568(3) 0.0455(13) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C11 1.897(6) . ?
O1 C1 1.216(5) . ?
O2 C4 1.415(5) . ?
O2 H2O 0.86(3) . ?
C1 C2 1.487(6) . ?
C1 C5 1.522(6) . ?
C2 C3 1.521(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.518(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.537(6) . ?
C4 C15 1.544(6) . ?
C5 C13 1.528(6) . ?
C5 C6 1.560(6) . ?
C6 C7 1.500(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.383(8) . ?
C7 C12 1.388(7) . ?
C8 C9 1.407(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.359(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.349(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.559(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 B1 1.538(7) . ?
C14 C15 1.552(6) . ?
C14 H14 0.9800 . ?
C15 C16 1.453(6) . ?
C15 H15 0.9800 . ?
C16 C17 1.186(6) . ?
C17 C18 1.438(7) . ?
C18 C23 1.378(7) . ?
C18 C19 1.396(7) . ?
C19 C20 1.366(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.325(9) . ?
C20 H20 0.9300 . ?
C21 C22 1.392(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.397(7) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
O3 B1 1.333(7) . ?
O3 C24 1.458(9) . ?
O4 B1 1.383(8) . ?
O4 C27 1.455(8) . ?
C24 C26 1.480(9) . ?
C24 C27 1.535(13) . ?
C24 C25 1.584(9) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.495(11) . ?
C27 C29 1.525(13) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
O3D B1 1.44(2) . ?
O3D C24D 1.50(3) . ?
O4D B1 1.28(2) . ?
O4D C27D 1.45(3) . ?
C24D C27D 1.43(5) . ?
C24D C26D 1.494(14) . ?
C24D C25D 1.540(13) . ?
C25D H25D 0.9600 . ?
C25D H25E 0.9600 . ?
C25D H25F 0.9600 . ?
C27D C28D 1.484(14) . ?
C27D C29D 1.492(13) . ?
C26D H26D 0.9600 . ?
C26D H26E 0.9600 . ?
C26D H26F 0.9600 . ?
C29D C28D 1.99(4) . ?
C29D H29D 0.9600 . ?
C29D H29E 0.9600 . ?
C29D H29F 0.9600 . ?
C28D H28D 0.9600 . ?
C28D H28E 0.9600 . ?
C28D H28F 0.9600 . ?

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
C4 O2 H2O 119(4) . . ?
O1 C1 C2 125.7(4) . . ?
O1 C1 C5 123.7(4) . . ?
C2 C1 C5 110.6(4) . . ?
C1 C2 C3 106.5(3) . . ?
C1 C2 H2A 110.4 . . ?
C3 C2 H2A 110.4 . . ?
C1 C2 H2B 110.4 . . ?
C3 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
C4 C3 C2 105.2(3) . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3B 110.7 . . ?
C2 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
O2 C4 C3 109.3(3) . . ?
O2 C4 C5 114.5(3) . . ?
C3 C4 C5 107.2(3) . . ?
O2 C4 C15 112.9(3) . . ?
C3 C4 C15 111.1(3) . . ?
C5 C4 C15 101.5(3) . . ?
C1 C5 C13 112.7(4) . . ?
C1 C5 C4 101.2(3) . . ?
C13 C5 C4 107.4(3) . . ?
C1 C5 C6 108.8(3) . . ?
C13 C5 C6 110.1(3) . . ?
C4 C5 C6 116.4(3) . . ?
C7 C6 C5 117.4(3) . . ?
C7 C6 H6A 107.9 . . ?
C5 C6 H6A 107.9 . . ?
C7 C6 H6B 107.9 . . ?
C5 C6 H6B 107.9 . . ?
H6A C6 H6B 107.2 . . ?
C8 C7 C12 118.8(5) . . ?
C8 C7 C6 120.6(5) . . ?
C12 C7 C6 120.6(4) . . ?
C7 C8 C9 120.2(6) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 120.1(6) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 119.6(6) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 122.2(6) . . ?
C10 C11 Br1 119.4(5) . . ?
C12 C11 Br1 118.3(5) . . ?
C11 C12 C7 119.2(5) . . ?
C11 C12 H12 120.4 . . ?
C7 C12 H12 120.4 . . ?
C5 C13 C14 107.5(3) . . ?
C5 C13 H13A 110.2 . . ?
C14 C13 H13A 110.2 . . ?
C5 C13 H13B 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
B1 C14 C15 112.2(4) . . ?
B1 C14 C13 112.4(4) . . ?
C15 C14 C13 103.5(3) . . ?
B1 C14 H14 109.5 . . ?
C15 C14 H14 109.5 . . ?
C13 C14 H14 109.5 . . ?
C16 C15 C4 113.0(4) . . ?
C16 C15 C14 116.5(4) . . ?
C4 C15 C14 107.4(3) . . ?
C16 C15 H15 106.5 . . ?
C4 C15 H15 106.5 . . ?
C14 C15 H15 106.5 . . ?
C17 C16 C15 176.7(5) . . ?
C16 C17 C18 178.6(5) . . ?
C23 C18 C19 119.2(5) . . ?
C23 C18 C17 121.4(5) . . ?
C19 C18 C17 119.4(5) . . ?
C20 C19 C18 120.6(5) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C21 C20 C19 120.7(6) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 120.9(6) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C21 C22 C23 119.6(6) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C18 C23 C22 119.0(5) . . ?
C18 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
B1 O3 C24 108.9(5) . . ?
B1 O4 C27 106.9(5) . . ?
O3 C24 C26 106.3(7) . . ?
O3 C24 C27 102.5(6) . . ?
C26 C24 C27 115.9(8) . . ?
O3 C24 C25 110.9(8) . . ?
C26 C24 C25 114.2(8) . . ?
C27 C24 C25 106.4(9) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O4 C27 C28 107.9(7) . . ?
O4 C27 C29 102.3(7) . . ?
C28 C27 C29 104.0(8) . . ?
O4 C27 C24 102.4(6) . . ?
C28 C27 C24 119.8(7) . . ?
C29 C27 C24 118.6(8) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
B1 O3D C24D 108.6(16) . . ?
B1 O4D C27D 111.1(17) . . ?
C27D C24D C26D 120(2) . . ?
C27D C24D O3D 101(2) . . ?
C26D C24D O3D 93(2) . . ?
C27D C24D C25D 104(3) . . ?
C26D C24D C25D 127(3) . . ?
O3D C24D C25D 107(2) . . ?
C24D C25D H25D 109.5 . . ?
C24D C25D H25E 109.5 . . ?
H25D C25D H25E 109.5 . . ?
C24D C25D H25F 109.5 . . ?
H25D C25D H25F 109.5 . . ?
H25E C25D H25F 109.5 . . ?
C24D C27D O4D 107.5(19) . . ?
C24D C27D C28D 126(3) . . ?
O4D C27D C28D 111(2) . . ?
C24D C27D C29D 125(2) . . ?
O4D C27D C29D 99(2) . . ?
C28D C27D C29D 84(2) . . ?
C24D C26D H26D 109.5 . . ?
C24D C26D H26E 109.5 . . ?
H26D C26D H26E 109.5 . . ?
C24D C26D H26F 109.5 . . ?
H26D C26D H26F 109.5 . . ?
H26E C26D H26F 109.5 . . ?
C27D C29D C28D 47.8(11) . . ?
C27D C29D H29D 109.5 . . ?
C28D C29D H29D 72.1 . . ?
C27D C29D H29E 109.5 . . ?
C28D C29D H29E 95.6 . . ?
H29D C29D H29E 109.5 . . ?
C27D C29D H29F 109.5 . . ?
C28D C29D H29F 151.9 . . ?
H29D C29D H29F 109.5 . . ?
H29E C29D H29F 109.5 . . ?
C27D C28D C29D 48.2(11) . . ?
C27D C28D H28D 109.5 . . ?
C29D C28D H28D 132.2 . . ?
C27D C28D H28E 109.5 . . ?
C29D C28D H28E 62.0 . . ?
H28D C28D H28E 109.5 . . ?
C27D C28D H28F 109.5 . . ?
C29D C28D H28F 117.7 . . ?
H28D C28D H28F 109.5 . . ?
H28E C28D H28F 109.5 . . ?
O3 B1 O4 112.1(5) . . ?
O4D B1 O3D 108.2(12) . . ?
O4D B1 C14 126.5(10) . . ?
O3 B1 C14 126.4(5) . . ?
O4 B1 C14 121.4(5) . . ?
O3D B1 C14 124.8(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 173.6(4) . . . . ?
C5 C1 C2 C3 -6.4(5) . . . . ?
C1 C2 C3 C4 -13.0(5) . . . . ?
C2 C3 C4 O2 152.3(4) . . . . ?
C2 C3 C4 C5 27.6(4) . . . . ?
C2 C3 C4 C15 -82.5(4) . . . . ?
O1 C1 C5 C13 -43.0(6) . . . . ?
C2 C1 C5 C13 136.9(4) . . . . ?
O1 C1 C5 C4 -157.5(4) . . . . ?
C2 C1 C5 C4 22.4(4) . . . . ?
O1 C1 C5 C6 79.4(5) . . . . ?
C2 C1 C5 C6 -100.7(4) . . . . ?
O2 C4 C5 C1 -151.8(4) . . . . ?
C3 C4 C5 C1 -30.3(4) . . . . ?
C15 C4 C5 C1 86.3(4) . . . . ?
O2 C4 C5 C13 89.9(4) . . . . ?
C3 C4 C5 C13 -148.6(4) . . . . ?
C15 C4 C5 C13 -32.0(4) . . . . ?
O2 C4 C5 C6 -34.0(5) . . . . ?
C3 C4 C5 C6 87.4(4) . . . . ?
C15 C4 C5 C6 -155.9(3) . . . . ?
C1 C5 C6 C7 50.9(5) . . . . ?
C13 C5 C6 C7 174.8(4) . . . . ?
C4 C5 C6 C7 -62.6(5) . . . . ?
C5 C6 C7 C8 -92.7(5) . . . . ?
C5 C6 C7 C12 85.2(5) . . . . ?
C12 C7 C8 C9 0.0(8) . . . . ?
C6 C7 C8 C9 177.9(5) . . . . ?
C7 C8 C9 C10 -1.2(9) . . . . ?
C8 C9 C10 C11 1.3(10) . . . . ?
C9 C10 C11 C12 -0.1(9) . . . . ?
C9 C10 C11 Br1 -177.4(5) . . . . ?
C10 C11 C12 C7 -1.1(8) . . . . ?
Br1 C11 C12 C7 176.1(3) . . . . ?
C8 C7 C12 C11 1.2(7) . . . . ?
C6 C7 C12 C11 -176.8(4) . . . . ?
C1 C5 C13 C14 -93.6(4) . . . . ?
C4 C5 C13 C14 17.0(4) . . . . ?
C6 C5 C13 C14 144.7(4) . . . . ?
C5 C13 C14 B1 126.6(4) . . . . ?
C5 C13 C14 C15 5.3(4) . . . . ?
O2 C4 C15 C16 42.5(5) . . . . ?
C3 C4 C15 C16 -80.7(4) . . . . ?
C5 C4 C15 C16 165.6(3) . . . . ?
O2 C4 C15 C14 -87.3(4) . . . . ?
C3 C4 C15 C14 149.5(3) . . . . ?
C5 C4 C15 C14 35.8(4) . . . . ?
B1 C14 C15 C16 84.9(5) . . . . ?
C13 C14 C15 C16 -153.6(4) . . . . ?
B1 C14 C15 C4 -147.3(4) . . . . ?
C13 C14 C15 C4 -25.8(4) . . . . ?
C23 C18 C19 C20 1.7(8) . . . . ?
C17 C18 C19 C20 -177.9(5) . . . . ?
C18 C19 C20 C21 -0.1(10) . . . . ?
C19 C20 C21 C22 -1.0(11) . . . . ?
C20 C21 C22 C23 0.3(10) . . . . ?
C19 C18 C23 C22 -2.3(8) . . . . ?
C17 C18 C23 C22 177.3(5) . . . . ?
C21 C22 C23 C18 1.3(9) . . . . ?
B1 O3 C24 C26 -103.3(9) . . . . ?
B1 O3 C24 C27 18.8(9) . . . . ?
B1 O3 C24 C25 132.0(9) . . . . ?
B1 O4 C27 C28 151.6(7) . . . . ?
B1 O4 C27 C29 -99.1(8) . . . . ?
B1 O4 C27 C24 24.2(8) . . . . ?
O3 C24 C27 O4 -25.6(8) . . . . ?
C26 C24 C27 O4 89.7(8) . . . . ?
C25 C24 C27 O4 -142.1(8) . . . . ?
O3 C24 C27 C28 -144.9(8) . . . . ?
C26 C24 C27 C28 -29.6(11) . . . . ?
C25 C24 C27 C28 98.6(11) . . . . ?
O3 C24 C27 C29 86.0(9) . . . . ?
C26 C24 C27 C29 -158.6(9) . . . . ?
C25 C24 C27 C29 -30.5(10) . . . . ?
B1 O3D C24D C27D -13(2) . . . . ?
B1 O3D C24D C26D 109(2) . . . . ?
B1 O3D C24D C25D -121(3) . . . . ?
C26D C24D C27D O4D -82(3) . . . . ?
O3D C24D C27D O4D 18(2) . . . . ?
C25D C24D C27D O4D 129(2) . . . . ?
C26D C24D C27D C28D 52(4) . . . . ?
O3D C24D C27D C28D 152(3) . . . . ?
C25D C24D C27D C28D -97(3) . . . . ?
C26D C24D C27D C29D 163(3) . . . . ?
O3D C24D C27D C29D -97(3) . . . . ?
C25D C24D C27D C29D 14(4) . . . . ?
B1 O4D C27D C24D -19(3) . . . . ?
B1 O4D C27D C28D -160(2) . . . . ?
B1 O4D C27D C29D 113(2) . . . . ?
C24D C27D C29D C28D -130(3) . . . . ?
O4D C27D C29D C28D 110(2) . . . . ?
C24D C27D C28D C29D 129(3) . . . . ?
O4D C27D C28D C29D -98(2) . . . . ?
C27D O4D B1 O3D 10(2) . . . . ?
C27D O4D B1 C14 -178.4(12) . . . . ?
C24 O3 B1 O4 -4.0(8) . . . . ?
C24 O3 B1 C14 178.5(6) . . . . ?
C27 O4 B1 O3 -13.8(8) . . . . ?
C27 O4 B1 C14 163.9(5) . . . . ?
C24D O3D B1 O4D 2.5(19) . . . . ?
C24D O3D B1 C14 -169.7(12) . . . . ?
C15 C14 B1 O4D -29.3(14) . . . . ?
C13 C14 B1 O4D -145.5(13) . . . . ?
C15 C14 B1 O3 -170.4(6) . . . . ?
C13 C14 B1 O3 73.3(7) . . . . ?
C15 C14 B1 O4 12.3(7) . . . . ?
C13 C14 B1 O4 -104.0(6) . . . . ?
C15 C14 B1 O3D 141.5(12) . . . . ?
C13 C14 B1 O3D 25.3(13) . . . . ?

_refine_diff_density_max         0.360
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.050


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Isopropanol and Dichloromethane'
