# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# 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_manish20_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2024647'
loop_
_audit_author_name
_audit_author_address
'Manish Kumar jaiswal'
;IIT Delhi
India
;
_audit_update_record             
;
2020-08-21 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H35 Br N O7 P'
_chemical_formula_sum            'C32 H35 Br N O7 P'
_chemical_formula_weight         656.48

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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.4713(9)
_cell_length_b                   9.6298(12)
_cell_length_c                   48.285(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3009.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    251
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      28.319

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            WHITE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.469
_shelx_estimated_absorpt_T_min   0.970
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\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            40358
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_theta_min         2.157
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7515
_reflns_number_gt                7156
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_max     0.985
_reflns_Friedel_fraction_full    0.987

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2780 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.125(3)
_chemical_absolute_configuration S
_refine_ls_number_reflns         7515
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1214
_refine_ls_wR_factor_gt          0.1197
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.21994(6) 0.85832(4) 0.70784(2) 0.02069(12) Uani 1 1 d . . . . .
P1 P 1.07491(14) 0.56268(9) 0.57677(2) 0.00843(18) Uani 1 1 d . . . . .
O4 O 0.6795(4) 0.5704(3) 0.58370(5) 0.0109(5) Uani 1 1 d . . . . .
H4 H 0.5668 0.6075 0.5793 0.016 Uiso 1 1 calc R U . . .
O5 O 1.2666(4) 0.6459(3) 0.57747(5) 0.0138(5) Uani 1 1 d . . . . .
O3 O 0.7642(5) 0.5445(3) 0.65000(5) 0.0185(6) Uani 1 1 d . . . . .
O7 O 1.0447(4) 0.4846(3) 0.54859(5) 0.0135(5) Uani 1 1 d . . . . .
O2 O 0.6470(5) 0.4270(3) 0.69617(5) 0.0178(6) Uani 1 1 d . . . . .
O6 O 1.0644(4) 0.4432(3) 0.59927(5) 0.0118(5) Uani 1 1 d . . . . .
N1 N 0.4663(5) 0.5967(3) 0.67509(6) 0.0109(6) Uani 1 1 d . . . . .
O1 O 0.3458(6) 0.4990(4) 0.71497(7) 0.0352(9) Uani 1 1 d . . . . .
C1 C 0.6217(6) 0.6203(4) 0.65453(7) 0.0112(7) Uani 1 1 d . . . . .
C3 C 0.3764(6) 0.8047(4) 0.65468(7) 0.0111(7) Uani 1 1 d . . . . .
C22 C 0.8167(5) 0.7650(3) 0.55606(7) 0.0094(6) Uani 1 1 d . . . . .
C8 C 0.3182(6) 0.7050(3) 0.67440(7) 0.0104(7) Uani 1 1 d . . . . .
C21 C 0.8406(5) 0.6696(3) 0.58153(7) 0.0085(6) Uani 1 1 d . . . . .
C7 C 0.1387(6) 0.7159(4) 0.68994(8) 0.0140(7) Uani 1 1 d . . . . .
H7 H 0.0961 0.6446 0.7023 0.017 Uiso 1 1 calc R U . . .
C28 C 0.9511(8) 0.3493(4) 0.54447(8) 0.0238(9) Uani 1 1 d . . . . .
H28A H 0.8803 0.3199 0.5617 0.029 Uiso 1 1 calc R U . . .
H28B H 1.0598 0.2803 0.5402 0.029 Uiso 1 1 calc R U . . .
C9 C 0.4779(6) 0.5026(4) 0.69759(7) 0.0144(7) Uani 1 1 d . . . . .
C23 C 0.9548(6) 0.8739(4) 0.55185(7) 0.0137(7) Uani 1 1 d . . . . .
H23 H 1.0632 0.8891 0.5648 0.016 Uiso 1 1 calc R U . . .
C30 C 1.1984(6) 0.4443(4) 0.62326(7) 0.0142(7) Uani 1 1 d . . . . .
H30A H 1.1710 0.5274 0.6347 0.017 Uiso 1 1 calc R U . . .
H30B H 1.3450 0.4459 0.6174 0.017 Uiso 1 1 calc R U . . .
C24 C 0.9357(6) 0.9608(4) 0.52889(7) 0.0159(7) Uani 1 1 d . . . . .
H24 H 1.0298 1.0355 0.5264 0.019 Uiso 1 1 calc R U . . .
C4 C 0.2604(6) 0.9259(4) 0.65223(7) 0.0142(7) Uani 1 1 d . . . . .
H4A H 0.3005 0.9965 0.6396 0.017 Uiso 1 1 calc R U . . .
C2 C 0.5648(6) 0.7565(3) 0.64065(7) 0.0112(6) Uani 1 1 d . . . . .
C27 C 0.6615(6) 0.7431(4) 0.53658(7) 0.0118(7) Uani 1 1 d . . . . .
H27 H 0.5674 0.6684 0.5390 0.014 Uiso 1 1 calc R U . . .
C6 C 0.0237(6) 0.8377(4) 0.68639(7) 0.0146(7) Uani 1 1 d . . . . .
C5 C 0.0849(6) 0.9422(4) 0.66861(7) 0.0156(7) Uani 1 1 d . . . . .
H5 H 0.0069 1.0255 0.6675 0.019 Uiso 1 1 calc R U . . .
C14 C 0.6760(6) 0.8160(3) 0.62023(7) 0.0097(6) Uani 1 1 d . . . . .
C00S C 0.8727(6) 0.7526(4) 0.60914(7) 0.0097(6) Uani 1 1 d . . . . .
H00A H 0.9307 0.6893 0.6233 0.012 Uiso 1 1 calc R U . . .
H00B H 0.9747 0.8274 0.6059 0.012 Uiso 1 1 calc R U . . .
C19 C 0.4051(7) 1.0847(4) 0.57539(8) 0.0198(8) Uani 1 1 d . . . . .
H19 H 0.3011 1.0877 0.5615 0.024 Uiso 1 1 calc R U . . .
C15 C 0.6113(6) 0.9515(4) 0.60754(7) 0.0119(7) Uani 1 1 d . . . . .
C17 C 0.6534(7) 1.2003(4) 0.60381(9) 0.0201(8) Uani 1 1 d . . . . .
H17 H 0.7188 1.2836 0.6097 0.024 Uiso 1 1 calc R U . . .
C20 C 0.4586(6) 0.9565(4) 0.58745(8) 0.0156(7) Uani 1 1 d . . . . .
H20 H 0.3903 0.8738 0.5818 0.019 Uiso 1 1 calc R U . . .
C18 C 0.5008(7) 1.2049(4) 0.58337(8) 0.0187(8) Uani 1 1 d . . . . .
H18 H 0.4638 1.2909 0.5751 0.022 Uiso 1 1 calc R U . . .
C25 C 0.7787(7) 0.9382(4) 0.50967(7) 0.0164(7) Uani 1 1 d . . . . .
H25 H 0.7652 0.9971 0.4940 0.020 Uiso 1 1 calc R U . . .
C26 C 0.6423(6) 0.8290(4) 0.51363(8) 0.0165(7) Uani 1 1 d . . . . .
H26 H 0.5351 0.8128 0.5006 0.020 Uiso 1 1 calc R U . . .
C12 C 0.5307(10) 0.2198(6) 0.72164(14) 0.0472(15) Uani 1 1 d . . . . .
H12A H 0.4004 0.2633 0.7273 0.071 Uiso 1 1 calc R U . . .
H12B H 0.5722 0.1511 0.7355 0.071 Uiso 1 1 calc R U . . .
H12C H 0.5122 0.1739 0.7037 0.071 Uiso 1 1 calc R U . . .
C31 C 1.1533(7) 0.3145(4) 0.63944(8) 0.0218(9) Uani 1 1 d . . . . .
H31A H 1.0097 0.3165 0.6459 0.033 Uiso 1 1 calc R U . . .
H31B H 1.2463 0.3092 0.6554 0.033 Uiso 1 1 calc R U . . .
H31C H 1.1744 0.2332 0.6276 0.033 Uiso 1 1 calc R U . . .
C29 C 0.7998(8) 0.3546(5) 0.52138(10) 0.0308(10) Uani 1 1 d . . . . .
H29A H 0.6855 0.4164 0.5264 0.046 Uiso 1 1 calc R U . . .
H29B H 0.7462 0.2611 0.5178 0.046 Uiso 1 1 calc R U . . .
H29C H 0.8680 0.3898 0.5047 0.046 Uiso 1 1 calc R U . . .
C16 C 0.7095(7) 1.0747(4) 0.61557(8) 0.0199(8) Uani 1 1 d . . . . .
H16 H 0.8154 1.0721 0.6292 0.024 Uiso 1 1 calc R U . . .
C10 C 0.6956(7) 0.3293(4) 0.71917(8) 0.0239(9) Uani 1 1 d . . . . .
C13 C 0.9002(8) 0.2682(5) 0.71003(11) 0.0344(12) Uani 1 1 d . . . . .
H13A H 0.8849 0.2271 0.6916 0.052 Uiso 1 1 calc R U . . .
H13B H 0.9432 0.1964 0.7232 0.052 Uiso 1 1 calc R U . . .
H13C H 1.0049 0.3417 0.7094 0.052 Uiso 1 1 calc R U . . .
C11 C 0.7217(12) 0.4112(7) 0.74586(10) 0.0515(17) Uani 1 1 d . . . . .
H11A H 0.8109 0.4916 0.7425 0.077 Uiso 1 1 calc R U . . .
H11B H 0.7847 0.3518 0.7600 0.077 Uiso 1 1 calc R U . . .
H11C H 0.5862 0.4431 0.7523 0.077 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C6 1.897(4) . ?
P1 O5 1.477(3) . ?
P1 O7 1.567(3) . ?
P1 O6 1.584(3) . ?
P1 C21 1.847(3) . ?
O4 C21 1.418(4) . ?
O4 H4 0.8400 . ?
O3 C1 1.196(5) . ?
O7 C28 1.450(5) . ?
O2 C9 1.317(5) . ?
O2 C10 1.489(4) . ?
O6 C30 1.447(4) . ?
N1 C9 1.417(4) . ?
N1 C8 1.417(4) . ?
N1 C1 1.431(4) . ?
O1 C9 1.198(5) . ?
C1 C2 1.518(5) . ?
C3 C4 1.393(5) . ?
C3 C8 1.403(5) . ?
C3 C2 1.470(5) . ?
C22 C27 1.392(5) . ?
C22 C23 1.393(5) . ?
C22 C21 1.542(4) . ?
C8 C7 1.386(5) . ?
C21 C00S 1.568(5) . ?
C7 C6 1.400(5) . ?
C7 H7 0.9500 . ?
C28 C29 1.485(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C23 C24 1.395(5) . ?
C23 H23 0.9500 . ?
C30 C31 1.502(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C24 C25 1.393(6) . ?
C24 H24 0.9500 . ?
C4 C5 1.392(5) . ?
C4 H4A 0.9500 . ?
C2 C14 1.349(5) . ?
C27 C26 1.388(5) . ?
C27 H27 0.9500 . ?
C6 C5 1.380(5) . ?
C5 H5 0.9500 . ?
C14 C15 1.501(5) . ?
C14 C00S 1.510(5) . ?
C00S H00A 0.9900 . ?
C00S H00B 0.9900 . ?
C19 C18 1.369(6) . ?
C19 C20 1.408(5) . ?
C19 H19 0.9500 . ?
C15 C20 1.385(5) . ?
C15 C16 1.401(5) . ?
C17 C16 1.385(5) . ?
C17 C18 1.397(6) . ?
C17 H17 0.9500 . ?
C20 H20 0.9500 . ?
C18 H18 0.9500 . ?
C25 C26 1.386(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C12 C10 1.504(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C16 H16 0.9500 . ?
C10 C13 1.514(6) . ?
C10 C11 1.521(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
O5 P1 O7 112.64(15) . . ?
O5 P1 O6 114.49(14) . . ?
O7 P1 O6 103.99(14) . . ?
O5 P1 C21 112.58(15) . . ?
O7 P1 C21 105.85(16) . . ?
O6 P1 C21 106.52(15) . . ?
C21 O4 H4 109.5 . . ?
C28 O7 P1 127.0(2) . . ?
C9 O2 C10 119.1(3) . . ?
C30 O6 P1 121.2(2) . . ?
C9 N1 C8 121.7(3) . . ?
C9 N1 C1 126.6(3) . . ?
C8 N1 C1 110.0(3) . . ?
O3 C1 N1 124.9(3) . . ?
O3 C1 C2 129.3(3) . . ?
N1 C1 C2 105.8(3) . . ?
C4 C3 C8 119.1(3) . . ?
C4 C3 C2 132.2(3) . . ?
C8 C3 C2 108.6(3) . . ?
C27 C22 C23 118.6(3) . . ?
C27 C22 C21 121.4(3) . . ?
C23 C22 C21 120.0(3) . . ?
C7 C8 C3 122.7(3) . . ?
C7 C8 N1 127.5(3) . . ?
C3 C8 N1 109.7(3) . . ?
O4 C21 C22 112.7(3) . . ?
O4 C21 C00S 112.2(3) . . ?
C22 C21 C00S 112.8(3) . . ?
O4 C21 P1 103.7(2) . . ?
C22 C21 P1 108.4(2) . . ?
C00S C21 P1 106.3(2) . . ?
C8 C7 C6 116.2(3) . . ?
C8 C7 H7 121.9 . . ?
C6 C7 H7 121.9 . . ?
O7 C28 C29 110.3(3) . . ?
O7 C28 H28A 109.6 . . ?
C29 C28 H28A 109.6 . . ?
O7 C28 H28B 109.6 . . ?
C29 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
O1 C9 O2 127.9(3) . . ?
O1 C9 N1 121.2(4) . . ?
O2 C9 N1 111.0(3) . . ?
C22 C23 C24 120.8(3) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
O6 C30 C31 107.1(3) . . ?
O6 C30 H30A 110.3 . . ?
C31 C30 H30A 110.3 . . ?
O6 C30 H30B 110.3 . . ?
C31 C30 H30B 110.3 . . ?
H30A C30 H30B 108.5 . . ?
C25 C24 C23 120.0(3) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
C14 C2 C3 130.2(3) . . ?
C14 C2 C1 124.1(3) . . ?
C3 C2 C1 105.7(3) . . ?
C26 C27 C22 120.9(3) . . ?
C26 C27 H27 119.5 . . ?
C22 C27 H27 119.5 . . ?
C5 C6 C7 122.3(3) . . ?
C5 C6 Br1 120.1(3) . . ?
C7 C6 Br1 117.6(3) . . ?
C6 C5 C4 120.3(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C2 C14 C15 121.3(3) . . ?
C2 C14 C00S 122.5(3) . . ?
C15 C14 C00S 116.2(3) . . ?
C14 C00S C21 113.3(3) . . ?
C14 C00S H00A 108.9 . . ?
C21 C00S H00A 108.9 . . ?
C14 C00S H00B 108.9 . . ?
C21 C00S H00B 108.9 . . ?
H00A C00S H00B 107.7 . . ?
C18 C19 C20 120.9(4) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C20 C15 C16 119.2(3) . . ?
C20 C15 C14 121.0(3) . . ?
C16 C15 C14 119.8(3) . . ?
C16 C17 C18 120.2(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C15 C20 C19 119.7(3) . . ?
C15 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C19 C18 C17 119.5(3) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C26 C25 C24 119.4(3) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 120.3(3) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C17 C16 C15 120.5(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
O2 C10 C12 110.6(4) . . ?
O2 C10 C13 102.3(3) . . ?
C12 C10 C13 111.8(4) . . ?
O2 C10 C11 109.1(4) . . ?
C12 C10 C11 112.0(5) . . ?
C13 C10 C11 110.6(5) . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_refine_diff_density_max         0.433
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.111

####################################################################### 
# 
# 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_mj556_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2024642'
loop_
_audit_author_name
_audit_author_address
'Manish Kumar jaiswal'
;IIT Delhi
India
;
_audit_update_record             
;
2020-08-21 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H35 Br N O7 P'
_chemical_formula_sum            'C32 H35 Br N O7 P'
_chemical_formula_weight         656.48

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.5171(3)
_cell_length_b                   9.8455(6)
_cell_length_c                   48.456(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3109.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    302(2)
_cell_measurement_reflns_used    251
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      28.319

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            WHITE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.421
_shelx_estimated_absorpt_T_min   0.970
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_process_details   '(SADABS; Bruker; 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      302(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\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            24109
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_theta_min         2.111
_diffrn_reflns_theta_max         28.271
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7717
_reflns_number_gt                5197
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_max     0.990
_reflns_Friedel_fraction_full    0.989

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1000P)²+1.2032P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1633 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.030(5)
_chemical_absolute_configuration R
_refine_ls_number_reflns         7675
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1200
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_restrained_S_all      0.819
_refine_ls_shift/su_max          0.007
_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 1.20214(9) 0.12785(8) 0.29224(2) 0.0612(2) Uani 1 1 d . . . . .
P002 P -0.07836(17) 0.43036(13) 0.42255(3) 0.0303(3) Uani 1 1 d . . . . .
O4 O 0.3139(5) 0.4194(3) 0.41550(8) 0.0377(8) Uani 1 1 d . . . . .
H4 H 0.4242 0.3810 0.4178 0.057 Uiso 1 1 calc R U . . .
O5 O -0.2679(5) 0.3509(4) 0.42190(8) 0.0423(8) Uani 1 1 d . . . . .
O7 O -0.0488(6) 0.5064(4) 0.45059(7) 0.0451(9) Uani 1 1 d . . . . .
O6 O -0.0658(5) 0.5453(4) 0.40013(7) 0.0377(8) Uani 1 1 d . . . . .
O3 O 0.3633(6) 0.5617(4) 0.30422(8) 0.0507(10) Uani 1 1 d . . . . .
N1 N 0.5302(6) 0.3895(4) 0.32473(8) 0.0340(9) Uani 1 1 d . . . . .
O1 O 0.2325(6) 0.4427(4) 0.34872(9) 0.0575(12) Uani 1 1 d . . . . .
C8 C 0.3715(8) 0.3677(6) 0.34482(10) 0.0361(11) Uani 1 1 d . . . . .
C1 C 0.6731(8) 0.2823(5) 0.32542(9) 0.0312(10) Uani 1 1 d . . . . .
O2 O 0.6615(8) 0.4928(6) 0.28686(12) 0.100(2) Uani 1 1 d . . . . .
C18 C 0.1743(7) 0.2325(5) 0.44321(9) 0.0295(10) Uani 1 1 d . . . . .
C6 C 0.6136(7) 0.1866(5) 0.34502(9) 0.0319(10) Uani 1 1 d . . . . .
C16 C 0.1223(7) 0.2432(6) 0.39047(9) 0.0331(11) Uani 1 1 d . . . . .
H16A H 0.0217 0.1722 0.3936 0.040 Uiso 1 1 calc R U . . .
H16B H 0.0670 0.3042 0.3766 0.040 Uiso 1 1 calc R U . . .
C7 C 0.4265(7) 0.2355(5) 0.35870(9) 0.0319(10) Uani 1 1 d . . . . .
C17 C 0.1529(6) 0.3241(5) 0.41790(9) 0.0286(10) Uani 1 1 d . . . . .
C10 C 0.3772(7) 0.0477(5) 0.39222(10) 0.0335(11) Uani 1 1 d . . . . .
C32 C 0.5263(9) 0.4866(6) 0.30333(11) 0.0429(13) Uani 1 1 d . . . . .
C23 C 0.3269(8) 0.2522(6) 0.46294(11) 0.0409(12) Uani 1 1 d . . . . .
H23 H 0.4218 0.3218 0.4606 0.049 Uiso 1 1 calc R U . . .
C2 C 0.8502(8) 0.2680(6) 0.31006(11) 0.0377(12) Uani 1 1 d . . . . .
H2 H 0.8942 0.3353 0.2980 0.045 Uiso 1 1 calc R U . . .
C5 C 0.7248(9) 0.0665(6) 0.34739(11) 0.0418(12) Uani 1 1 d . . . . .
H5 H 0.6843 -0.0003 0.3598 0.050 Uiso 1 1 calc R U . . .
C3 C 0.9589(7) 0.1486(6) 0.31355(11) 0.0426(13) Uani 1 1 d . . . . .
C9 C 0.3160(7) 0.1796(5) 0.37939(9) 0.0324(10) Uani 1 1 d . . . . .
C19 C 0.0373(8) 0.1269(6) 0.44761(11) 0.0444(13) Uani 1 1 d . . . . .
H19 H -0.0659 0.1110 0.4348 0.053 Uiso 1 1 calc R U . . .
C24 C -0.2012(10) 0.5488(6) 0.37661(12) 0.0504(14) Uani 1 1 d . . . . .
H24A H -0.3430 0.5463 0.3827 0.060 Uiso 1 1 calc R U . . .
H24B H -0.1764 0.4707 0.3649 0.060 Uiso 1 1 calc R U . . .
C20 C 0.0510(10) 0.0449(7) 0.47067(12) 0.0554(16) Uani 1 1 d . . . . .
H20 H -0.0428 -0.0252 0.4732 0.067 Uiso 1 1 calc R U . . .
C4 C 0.8981(9) 0.0476(6) 0.33089(11) 0.0450(13) Uani 1 1 d . . . . .
H4A H 0.9714 -0.0333 0.3317 0.054 Uiso 1 1 calc R U . . .
C21 C 0.2024(11) 0.0663(7) 0.48997(11) 0.0571(16) Uani 1 1 d . . . . .
H21 H 0.2116 0.0111 0.5055 0.068 Uiso 1 1 calc R U . . .
C15 C 0.5305(9) 0.0421(6) 0.41179(12) 0.0453(13) Uani 1 1 d . . . . .
H15 H 0.5985 0.1211 0.4170 0.054 Uiso 1 1 calc R U . . .
C14 C 0.5834(11) -0.0810(6) 0.42370(13) 0.0562(16) Uani 1 1 d . . . . .
H14 H 0.6868 -0.0839 0.4369 0.067 Uiso 1 1 calc R U . . .
C22 C 0.3393(9) 0.1698(6) 0.48600(11) 0.0495(15) Uani 1 1 d . . . . .
H22 H 0.4420 0.1850 0.4990 0.059 Uiso 1 1 calc R U . . .
C28 C 0.3237(11) 0.6644(7) 0.28315(14) 0.0635(19) Uani 1 1 d . . . . .
C13 C 0.4855(11) -0.1983(6) 0.41625(14) 0.0563(16) Uani 1 1 d . . . . .
H13 H 0.5221 -0.2804 0.4244 0.068 Uiso 1 1 calc R U . . .
C11 C 0.2787(11) -0.0719(6) 0.38539(13) 0.0573(16) Uani 1 1 d . . . . .
H11 H 0.1719 -0.0700 0.3727 0.069 Uiso 1 1 calc R U . . .
C12 C 0.3353(11) -0.1943(7) 0.39704(16) 0.0654(19) Uani 1 1 d . . . . .
H12 H 0.2701 -0.2741 0.3917 0.078 Uiso 1 1 calc R U . . .
C26 C 0.0514(17) 0.6348(9) 0.45461(15) 0.088(3) Uani 1 1 d . . . . .
H26A H 0.1457 0.6500 0.4394 0.106 Uiso 1 1 calc R U . . .
H26B H -0.0510 0.7062 0.4540 0.106 Uiso 1 1 calc R U . . .
C25 C -0.1605(12) 0.6760(8) 0.36120(14) 0.068(2) Uani 1 1 d . . . . .
H25A H -0.1799 0.7524 0.3732 0.102 Uiso 1 1 calc R U . . .
H25B H -0.2534 0.6825 0.3459 0.102 Uiso 1 1 calc R U . . .
H25C H -0.0218 0.6754 0.3545 0.102 Uiso 1 1 calc R U . . .
C31 C 0.1193(13) 0.7206(10) 0.2910(2) 0.103(4) Uani 1 1 d . . . . .
H31A H 0.0218 0.6479 0.2925 0.154 Uiso 1 1 calc R U . . .
H31B H 0.0746 0.7837 0.2772 0.154 Uiso 1 1 calc R U . . .
H31C H 0.1301 0.7664 0.3084 0.154 Uiso 1 1 calc R U . . .
C30 C 0.4874(18) 0.7691(10) 0.2830(3) 0.154(6) Uani 1 1 d . . . . .
H30A H 0.5113 0.8000 0.3015 0.231 Uiso 1 1 calc R U . . .
H30B H 0.4454 0.8443 0.2717 0.231 Uiso 1 1 calc R U . . .
H30C H 0.6114 0.7307 0.2757 0.231 Uiso 1 1 calc R U . . .
C29 C 0.309(2) 0.5957(12) 0.25527(18) 0.148(5) Uani 1 1 d . . . . .
H29A H 0.4337 0.5470 0.2516 0.222 Uiso 1 1 calc R U . . .
H29B H 0.2883 0.6631 0.2412 0.222 Uiso 1 1 calc R U . . .
H29C H 0.1956 0.5335 0.2553 0.222 Uiso 1 1 calc R U . . .
C27 C 0.160(2) 0.6448(11) 0.4796(2) 0.126(4) Uani 1 1 d . . . . .
H27A H 0.0721 0.6808 0.4936 0.190 Uiso 1 1 calc R U . . .
H27B H 0.2760 0.7041 0.4771 0.190 Uiso 1 1 calc R U . . .
H27C H 0.2077 0.5564 0.4850 0.190 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C3 1.903(5) . ?
P002 O5 1.463(3) . ?
P002 O7 1.563(4) . ?
P002 O6 1.570(4) . ?
P002 C17 1.848(5) . ?
O4 C17 1.413(5) . ?
O4 H4 0.8200 . ?
O7 C26 1.437(9) . ?
O6 C24 1.442(6) . ?
O3 C32 1.295(7) . ?
O3 C28 1.460(7) . ?
N1 C1 1.408(6) . ?
N1 C32 1.411(7) . ?
N1 C8 1.436(6) . ?
O1 C8 1.183(6) . ?
C8 C7 1.509(7) . ?
C1 C2 1.380(7) . ?
C1 C6 1.393(7) . ?
O2 C32 1.190(7) . ?
C18 C19 1.387(7) . ?
C18 C23 1.393(7) . ?
C18 C17 1.528(6) . ?
C6 C5 1.391(7) . ?
C6 C7 1.469(6) . ?
C16 C9 1.508(7) . ?
C16 C17 1.562(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C7 C9 1.351(7) . ?
C10 C15 1.379(7) . ?
C10 C11 1.382(8) . ?
C10 C9 1.494(7) . ?
C23 C22 1.383(8) . ?
C23 H23 0.9300 . ?
C2 C3 1.383(8) . ?
C2 H2 0.9300 . ?
C5 C4 1.396(7) . ?
C5 H5 0.9300 . ?
C3 C4 1.361(8) . ?
C19 C20 1.381(8) . ?
C19 H19 0.9300 . ?
C24 C25 1.482(9) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C20 C21 1.376(9) . ?
C20 H20 0.9300 . ?
C4 H4A 0.9300 . ?
C21 C22 1.368(9) . ?
C21 H21 0.9300 . ?
C15 C14 1.386(8) . ?
C15 H15 0.9300 . ?
C14 C13 1.368(9) . ?
C14 H14 0.9300 . ?
C22 H22 0.9300 . ?
C28 C30 1.483(13) . ?
C28 C31 1.492(10) . ?
C28 C29 1.514(12) . ?
C13 C12 1.351(9) . ?
C13 H13 0.9300 . ?
C11 C12 1.381(9) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C26 C27 1.407(12) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 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
O5 P002 O7 112.2(2) . . ?
O5 P002 O6 114.5(2) . . ?
O7 P002 O6 104.5(2) . . ?
O5 P002 C17 112.6(2) . . ?
O7 P002 C17 106.0(2) . . ?
O6 P002 C17 106.3(2) . . ?
C17 O4 H4 109.5 . . ?
C26 O7 P002 126.5(4) . . ?
C24 O6 P002 122.1(3) . . ?
C32 O3 C28 121.1(4) . . ?
C1 N1 C32 122.5(4) . . ?
C1 N1 C8 110.4(4) . . ?
C32 N1 C8 125.9(4) . . ?
O1 C8 N1 124.5(5) . . ?
O1 C8 C7 130.4(5) . . ?
N1 C8 C7 105.1(4) . . ?
C2 C1 C6 122.1(5) . . ?
C2 C1 N1 128.1(5) . . ?
C6 C1 N1 109.8(4) . . ?
C19 C18 C23 117.3(5) . . ?
C19 C18 C17 120.4(4) . . ?
C23 C18 C17 122.3(4) . . ?
C5 C6 C1 119.1(4) . . ?
C5 C6 C7 132.3(5) . . ?
C1 C6 C7 108.5(4) . . ?
C9 C16 C17 114.1(4) . . ?
C9 C16 H16A 108.7 . . ?
C17 C16 H16A 108.7 . . ?
C9 C16 H16B 108.7 . . ?
C17 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C9 C7 C6 130.1(5) . . ?
C9 C7 C8 123.7(4) . . ?
C6 C7 C8 106.2(4) . . ?
O4 C17 C18 113.0(3) . . ?
O4 C17 C16 111.3(4) . . ?
C18 C17 C16 113.2(4) . . ?
O4 C17 P002 103.9(3) . . ?
C18 C17 P002 108.1(3) . . ?
C16 C17 P002 106.7(3) . . ?
C15 C10 C11 117.9(5) . . ?
C15 C10 C9 121.0(5) . . ?
C11 C10 C9 121.2(4) . . ?
O2 C32 O3 126.9(5) . . ?
O2 C32 N1 121.0(5) . . ?
O3 C32 N1 112.1(4) . . ?
C22 C23 C18 120.9(5) . . ?
C22 C23 H23 119.5 . . ?
C18 C23 H23 119.5 . . ?
C1 C2 C3 116.7(5) . . ?
C1 C2 H2 121.6 . . ?
C3 C2 H2 121.6 . . ?
C6 C5 C4 119.2(5) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C4 C3 C2 123.2(5) . . ?
C4 C3 Br1 119.9(4) . . ?
C2 C3 Br1 116.9(4) . . ?
C7 C9 C10 121.3(4) . . ?
C7 C9 C16 122.8(4) . . ?
C10 C9 C16 115.9(4) . . ?
C20 C19 C18 121.4(5) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
O6 C24 C25 108.0(5) . . ?
O6 C24 H24A 110.1 . . ?
C25 C24 H24A 110.1 . . ?
O6 C24 H24B 110.1 . . ?
C25 C24 H24B 110.1 . . ?
H24A C24 H24B 108.4 . . ?
C21 C20 C19 120.4(6) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C3 C4 C5 119.5(5) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C22 C21 C20 119.1(5) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C10 C15 C14 120.1(5) . . ?
C10 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C13 C14 C15 120.8(5) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C21 C22 C23 120.8(5) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
O3 C28 C30 110.9(7) . . ?
O3 C28 C31 103.7(5) . . ?
C30 C28 C31 112.6(8) . . ?
O3 C28 C29 109.0(6) . . ?
C30 C28 C29 110.6(9) . . ?
C31 C28 C29 109.7(9) . . ?
C12 C13 C14 119.7(6) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C12 C11 C10 121.5(5) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C12 C11 120.0(6) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C27 C26 O7 114.1(8) . . ?
C27 C26 H26A 108.7 . . ?
O7 C26 H26A 108.7 . . ?
C27 C26 H26B 108.7 . . ?
O7 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
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 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

_refine_diff_density_max         0.451
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.061

